Buehler® SumMet™

The Sum Of Our Experience

A Guide to Materials Preparation & Analysis

Fourth Edition

Acknowledgement:
Special thanks to George F. Vander Voort, Director, Research & Technology for writing the first edition of the Buehler®
SumMet™ (2007). Patrick Voos as editor of the second (2013 &2015) editions of the book. Special contributions from
Ahmed Wase, George Blann, Damien Crozet, Todd Danielczyk, Paula Didier, Cornelius Johnson, Don Fisher, Matthias
Pascher, Daniel Peters, Lee Garrett, Henrietta Ho, Scott Holt, Mike Keeble, Janice Klansky, Benny Leung, Gabe Lucas,
Marcel van Banning and Tim Weber.
Buehler® SumMet™ - A Guide to Materials Preparation and Analysis
Copyright © 2007 Buehler, a division of Illinois Tool Works Inc.

All rights reserved. No part of this publication may be reproduced, stored in a retrieval system or
transmitted in any form or by an means, electronic, mechanical, photocopying, recording or otherwise,
without permission of the copyright holder.

ISBN: 0-9752898-0-2

4th Edition

Buehler, an ITW Company

Worldwide Headquarters
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Lake Bluff, IL 60044 USA

www.buehler.com

FN NUMBER: FN01255

Printed in Germany 2013

First Printing: January 2011

Second Printing: July 2013

Third Printing: September 2015

Fourth Printing: January 2018

This book was produced by Buehler.

Trademarks
All terms mentioned in this book that are known to be trademarks or service marks have been appro-
priately capitalized.

Warning and Disclaimer

Every effort has been made to make this book as complete and as accurate as possible, but no warranty
or fitness is implied. The information provided is on an “as is” basis. The authors and the publisher shall
have neither liability nor responsibility to any person or entity with respect to any loss or damages arising
from the information contained in this book.
TABLE OF CONTENTS

Introduction............................................................... 2 Aluminum................................................ 32

Sampling.................................................................... 3 Magnesium.............................................. 34

Beryllium.................................................. 35
Goals of Specimen Preparation.............................. 4

Low Melting Point Metals:

Method Development.............................................. 4
Sb, Bi, Cd, Pb, Sn and Zn....................... 36
Sectioning.................................................................. 5
Refractory Metals: Ti, Zr, Hf, Cr, Mo,
Abrasive Cutting............................................... 5
Nb, Re, Ta, V and W................................. 38
Precision Sectioning......................................... 8
Titanium................................................... 38
Mounting of Specimens........................................ 10
Zirconium and Hafnium......................... 39
Clamp Mounting............................................. 10
Other Refractory Metals: Cr, Mo, Nb,
Compression Mounting................................. 10
Re, Ta, V and W........................................ 41
Castable Mounting Systems.......................... 11
Ferrous Metals................................................. 43
Edge Preservation........................................... 13
Cast Iron................................................... 45
Grinding .................................................................. 16
Copper, Nickel & Cobalt................................ 47
Grinding Media............................................... 16
Copper..................................................... 47
Grinding Equipment...................................... 18
Nickel....................................................... 48
Polishing.................................................................. 18
Cobalt...................................................... 49
Mechanical Polishing...................................... 19
Precious Metals............................................... 51
Manual “Hand” Polishing............................... 19
Thermal Spray Coatings................................. 53
Automated Polishing...................................... 20
Sintered Carbides........................................... 55
Polishing Cloths.............................................. 21
Ceramics.......................................................... 57
Polishing Abrasives......................................... 21

Minerals........................................................... 59
Vibratory Polishing.......................................... 23

Preparation Methodology............................. 23 Glass................................................................. 60

Electrolytic Polishing & Etching.................... 24 Composites..................................................... 62

Anodizing........................................................ 26 Printed Circuit Boards.................................... 65

Examples of Preparation Procedure.................... 27 Electronic Materials........................................ 67

The Traditional Method.................................. 27
Polymers........................................................... 70
Contemporary Methods................................ 27
Etching............................................................. 72
Procedures for Specific Materials........................ 30 Etching Procedures................................ 72
Periodic Table of Elements............................ 31 Selective Etching.................................... 73
Light Metals: Al, Mg and Be.......................... 32 Electrolytic Etching and Anodizing...... 76

i
TABLE OF CONTENTS
Heat Tinting............................................. 76 Laboratory Safety.................................................110

Interference Layer Method.................... 77 Laboratory Equipment.................................111

Commonly Used Etchants for Personal Protective Equipment (PPE).........111

Metals and Alloys................................... 78 Chemicals, Storage and Handling..............112

Light Optical Microscopy...................................... 84 Etchants.........................................................112

The Light Microscope.................................... 84 Solvents..........................................................113

Microscope Components.............................. 85 Acids...............................................................115

Resolution........................................................ 88 Bases..............................................................118

Depth of Field................................................. 89 Other Chemicals...........................................119

Imaging Modes............................................... 90 Summary........................................................119

Image Capture & Analysis..................................... 93 Summary................................................................121

Image Capture................................................ 93 Glossary ................................................................122

Clarification..................................................... 96 References.............................................................126
Operator Interactive Measurements............ 96
Appendix...............................................................128
Automated Measurements............................ 96
ASTM Metallography Standards........................134
Thresholding................................................... 96
ISO Standards.......................................................135
Binary Operations........................................... 96
Other National Standards...................................136
Common Applications................................... 99
Buehler Trademarks.............................................139
Hardness Testing..................................................101
Educational Courses............................................144
Brinell Testing................................................102

Rockwell Testing...........................................103

Factors Affecting Accuracy, Precision

and Bias for Rockwell Testing......................104

Vickers Testing...............................................105

Knoop Testing...............................................106

Factors Affecting Accuracy, Precision

and Bias for Vickers and Knoop..................108

Automation....................................................108

ii
The Sum Of Our Experience

Buehler is a worldwide leader in materials preparation, testing and analysis. As your partner in
all aspects, we provide not only a complete line of equipment and consumables, but a strong
team dedicated to application knowledge, technical support, and when need be, service. With
more than 80 locations across the globe offering telephone and email support, training courses,
webinars, and one-on-one custom training, Buehler is there offer support to our customers,
industries and applications. Dedicated to your needs, we strive for fast consumable deliveries,
efficient service support and 24/7 access to our online preparation guide.

Strong Partner, Reliable Solutions

INTRODUCTION
Proper specimen preparation is essential if the polishing exhibit a range of resilience depend-
true microstructure is to be observed, identified, ing on whether they are non-woven polymeric
documented and measured. Indeed, when or chemo-textiles, woven napless materials, or
metallographers have difficulty seeing or mea- napped materials. Resilience influences edge
suring microstructures, these problems can retention, relief control and cutting rate (“aggres-
almost always be traced to improper specimen siveness”). Polishing must remove the damage
preparation procedures, or failure to properly remaining after grinding, with the final step
execute the preparation steps. When a spec- reducing the damage to where it is insignificant,
imen is prepared properly, and the structure or can be removed by the etchant. In this way,
is revealed properly, or a phase or constitu- the true microstructure is revealed. For most
ent of interest is revealed selectively and with metals and alloys, and many non-metallic ma-
adequate contrast, then the actual tasks of terials, polishing down to a 1µm, or even a 3µm
examination, interpretation, documentation and diamond finish may yield a surface suitable for
measurement are generally quite simple. Experi- routine examination, although finer abrasives
ence has demonstrated that getting the required are usually needed for more critical work, such
image quality to the microscope is by far the as failure analysis.
greatest challenge. Despite this, the specimen
preparation process is often treated as a trivial Polishing was historically performed with abra-
exercise. However, specimen preparation quality sive slurries, most commonly using alumina,
is the determining factor in the value of the ex- but with limited use of MgO, Cr2O3 or CeO for
amination. This is in agreement with the classic specific materials. Diamond abrasives were
computer adage, “garbage in = garbage out.” introduced in the late 1940s. Cloths such as
canvas, billiard, felt, and cotton are not used
Historically, people tend to divide specimen as much today as they tend to promote relief
preparation (after mounting) into two steps, and edge rounding, or other artifacts. Modern
grinding and polishing, further sub-divided, preparation methods have focused on reducing
somewhat arbitrarily, into coarse and fine stag- the number of SiC grinding steps and replacing
es. Years ago, these divisions were quite clear. SiC paper with other abrasives and surfaces,
Both processes involve the same mechanism, although there are some materials that respond
chip formation by micro-machining. Grinding better to grinding with a series of finer and
removes material from the specimen surface finer SiC papers. But, most materials can be
using randomly oriented, fixed abrasives on a prepared with one grinding step, often called
substrate such as paper or cloth. The abrasive planar grinding when an automated system
size range has generally been in the range of is used, and two or more polishing steps. The
about 240 to 5µm, with silicon cabide (SiC) pa- second step uses relatively hard, non-resilient
per used exclusively until recently. surfaces with a relatively coarse diamond size (15
or 9µm, for example) and the abrasive is added
Traditionally, polishing has been defined in as a suspension or paste. Initially, the particles
terms of industrial polishing rather than me- move between the specimen surface and the
tallographic polishing, simply stating that it is substrate. Technically, this is lapping. But, after
a smoothing of the surface to a high luster. A a short time, the diamond particles become
polished surface was defined as “a surface that embedded in the surface and produce cutting
reflected a large proportion of incident light in action. We tend to call this polishing, although
a specular manner.” These definitions are true, the historic definitions are not as clear here. If the
but they are inadequate for metallography. Pol- substrate is a rigid grinding disc, the action may
ishing also produces micro- machining action, be more correctly called grinding than polishing,
but scratch depths are shallower in polishing, as the surface finish will be dull. The same abra-
as the abrasives are smaller. They are not fixed sive when used on a hard, woven surface such
initially to a substrate, but are applied using as as an UltraPol silk cloth, will yield a much more
a paste or suspension. After a short time, the lustrous appearance, but with less stock removal
abrasive particles become fixed in the cloth and shallower scratches. Napped cloths, if they
producing cutting action. The cloths used in are used, are generally restricted to the final step
with the finest abrasives.

2
SAMPLING
The samples selected for preparation must be example of multiple sample selection is
representative of the material to be examined. the evaluation of the inclusion content of steels.
Random sampling, as advocated by statisticians, One sample is not representative of the whole lot
can rarely be performed by metallographers. A of steel, so multiple sampling becomes more im-
good exception is the testing of fasteners where portant. ASTM standards E45, E1122 and E1245
a production lot can be sampled randomly. But, give advice on sampling procedures for inclusion
a large forging or casting cannot be sampled at studies. To study grain size, it is common to use a
random as the component would be rendered single specimen from a lot. This may or may not
commercially useless. Instead, test locations are be adequate, depending upon the nature of the
chosen systematically based on ease of sam- lot. Good engineering judgment should guide
pling. Many material specifications dictate the sampling, in such cases. In many cases, a product
sampling procedure. In failure analysis studies, specification may define the procedure rigor-
specimens are usually removed to study the ously. Grain structures are not always equiaxed
origin of the failure, to examine highly stressed and it may be misleading to select only a plane
areas, to examine secondary cracks, and so oriented perpendicular to the deformation axis,
forth. This, of course, is not random sampling. a “transverse” plane, for such a study. If the grains
As testing costs are usually closely controlled, it are elongated due to processing, which does
is more likely that inadequate sampling occurs happen, the transverse plane will usually show
than excessive sampling. that the grains are equiaxed in shape and smaller
in diameter than the true grain size. To study
Normally, a sample must be removed from a the effect of deformation on the grain shape of
larger mass and then prepared for examina- wrought metals, a minimum of two sections are
tion. This requires application of one or more needed — one perpendicular to, and the other
sectioning methods. For example, in a manu- parallel to, the direction of deformation.
facturing facility, a piece may be cut from a bar
of incoming metal with a power hacksaw, or an
abrasive cutter used dry, i.e., without a coolant.
The piece is then forwarded to the laboratory
where it is cut smaller to obtain a size more
convenient for preparation. All sectioning
processes produce damage; some methods
(such as flame cutting or dry abrasive cutting)
produce extreme amounts of damage. Tradi- HELPFUL HINTS
tional laboratory sectioning procedures, using
abrasive cutters, introduce a minor amount
FOR SAMPLING
of damage that varies with the material being When developing a sampling plan for an
cut and its thermal and mechanical history. It is unfamiliar part or component, determine
generally unwise to use the original face cut in the orientation of the piece relative to the
the shop as the starting point for metallograph- original wrought or cast starting material
ic preparation as the depth of damage at this and prepare sections on the longitudi-
location may be quite extensive. This damage nal, transverse and planar surfaces, or
must be removed if the true structure is to be re- radial and transverse surfaces, to reveal
the desired information. Remember that
vealed. However, because abrasive grinding and
the microstructure may look much more
polishing steps also produce damage, where
homogeneous than it is on a transverse
the depth of damage decreases with decreasing plane compared to a longitudinal or
abrasive size, the preparation sequence must planar surface. If the starting material was
be carefully planned and performed; otherwise, cold worked, or not fully recrystallized
preparation-induced artifacts will be interpreted after hot working, grain structures will
as structural elements. appear to be equiaxed and smaller on a
transverse plane, but non-equiaxed and
Many metallographic studies require more larger on a longitudinal or planar surface
than one sample and sectioning is nearly al-
ways required to extract the sample. A classic

3
GOALS OF SPECIMEN PREPARATION
The preparation procedure and the prepared Method Development
specimen should have the following character- The methods presented in this book use times
istics to reveal the true microsctructure*: that are conservative so that the vast majority of
compositions of alloys or materials of a specific
• Deformation induced by sectioning, grinding
type can be prepared to yield the true microstruc-
and polishing must be removed or be shallow
ture without artifacts or observable scratches.
enough to be removed by the etchant.
They were developed using an 8in [203mm]
diameter platen system with six 1.25in [32mm]
• Scratches introduced during coarse grinding
diameter mounted specimens. For each catego-
must be removed; very fine polishing scratches
ry, except beryllium, a wide variety of specimens
may be tolerable for routine production work.
with different processing histories were prepared
using the stated methods.
• Pullout, pitting, cracking of hard particles,
smear, and other preparation artifacts, must
For any metal or material category, there are
be avoided.
compositions or processing conditions that
make those specimens easier, or more difficult,
• Relief (i.e., excessive surface height variations
to prepare compared to the “average” specimen.
between structural features of different hard-
In general, even the most difficult specimens of
ness) must be minimized; otherwise portions
a given type can be prepared perfectly using
of the image will be out of focus at high mag-
these methods with no more than one etch and
nifications.
re-polish (repeat last step) cycle. For perfect color
• The surface must be flat, particularly at etching results, it may be necessary to follow the
edges (if they are of interest) or they cannot cycle with a brief vibratory polish, depending
be imaged. upon the material.

• Coated or plated surfaces must be kept flat if When working with easier to prepare specimens,
they are to be examined, measured or photo- or for routine work where a high level of per-
graphed. fection is not required, the user can reduce the
times, or eliminate one or two steps, or the final
• Specimens must be cleaned adequately step, and get satisfactory results. Modifications
between preparation steps, after preparation, to the recommended procedures are left to the
and after etching. user based upon their knowledge of the degree
of difficulty in preparing their specimens and the
• The etchant chosen must be either general or desired quality of preparation.
selective in its action (reveal only the phase
or constituent of interest, or at least produce
strong contrast or color differences between
two or more phases present), depending upon
the purpose of the investigation, and must pro-
duce crisp, clear phase or grain boundaries,
and strong contrast.

If these characteristics are met, then the true

structure will be revealed and can be interpreted,
measured and recorded. The preparation meth-
od should be as simple as possible, should yield
consistent high quality results in a minimum of
time and cost and must be reproducible.

Preparation of metallographic specimens [1-3]

generally requires five major operations: (a)
sectioning, (b) mounting (c) grinding, polishing
and etching (d) image analysis and (e) hardness
testing.
* Not all of these apply to every specimen.

4
SECTIONING
SECTIONING
Bulk samples for subsequent laboratory sectioning
may be removed from larger pieces using methods
such as core drilling, band or hack-sawing, flame
cutting, or similar methods. However, when these
techniques are used, precautions must be taken to
avoid alteration of the microstructure in the area
of interest. Laboratory abrasive cutting is recom-
mended to establish the desired plane of polish.
In the case of relatively brittle materials, sectioning
may be accomplished by fracturing the specimen
Figure 1.2. Cutting damage (top) and a “burr” after sectioning of
at the desired location. an annealed CP titanium specimen (mod. Weck’s reagent, 100X,
polarized light plus sensitive tint).
Abrasive Cutting
may be a resin, rubber, or a mixture of resin and
The most commonly used sectioning device in
rubber. Alumina (aluminum oxide) is the preferred
the metallographic laboratory is the abrasive
abrasive for ferrous alloys and silicon carbide is the
c u tt e r, Fi g u re 1 . 1 . A l l s e c t i o n i n g s h o u l d
preferred abrasive for nonferrous metals and min-
be performed wet. An ample flow of
erals. Wheels have different bond strengths and are
c o o l a n t , w i t h a n a d d i t i v e f o r c o r ro s i o n
recommended based on the suitability of their bond
protection and lubrication, should be directed
strength and abrasive type for the material to be
into the cut. Wet cutting will produce a smoother
sectioned. In general, as the hardness of a material
surface finish than a comparable dry
increases, the abrasives dull more quickly requiring
c u t a n d , m o s t i m p o r t a n t l y, w i l l g u a r d
that the binder must break-down and release the
against excessive surface damage caused
dull abrasives. As this occurs, fresh abrasive particles
by overheating. Abrasive wheels should be
are revealed, allowing the system to maintain cutting
selected according to the manufacturer ’s
speed and efficiency. If the wheel does not wear
recommendations. Table 1.1 summarizes the Bue-
at the proper rate, dull abrasives will rub against
hler recommendations for our machines. Samples
the region being cut generating heat and possibly
must be fixtured securely during cutting, and
altering the existing true microstructure. If this heat
cutting pressure should be applied carefully to
becomes excessive, it can lead to grain or particle
prevent wheel breakage. Some materials, such as
coarsening, softening or phase transformations, and
commercial purity (CP) titanium, Figure 1.2, are
in extreme case, to burning or melting. Different
quite prone to sectioning damage.
materials have different sensitivities to this problem.
But, the need to balance the wheel break-down rate
Wheels consist of abrasive particles, chiefly alumina
with the hardness of the piece being sectioned,
or silicon carbide, and filler in a binder material that
produces the various recommendations listed for
cutting different materials and metals with different
hardnesses, such as steels.

The size of the abrasive cutter also affects wheel

parameters. As the diameter of the wheel is
increased, to permit sectioning of larger specimens,
the wheel thickness is generally increased. Even
so, for a given diameter wheel, there may be a
range of thicknesses available. Thicker wheels are
stronger but remove more material in the cut. This
may, or may not, be a problem. But, thicker wheels
do generate more heat during cutting than a thin-
ner wheel, everything else being held constant.
Consequently, for cases where the kerf loss or heat
generation must be minimized, select the thinnest
available wheel of the proper bond strength and
Figure 1.1. Delta Orbital Large abrasive. The AcuThin Wheels offer the thinnest
possible for delicate abrasive sectioning. Buehler
SECTIONING

Table 1.1. Buehler’s Abrasive Cutting Recommendations

Available Diameters

Recommended Use Bond Abrasive (Inches) (mm)

General Usage Blades
9, 10, 12, 230, 254, 305,
Tools, Steels, 60HRC+ Carburized Steels Rubber Resin Al2O3
14, 16, 18 356, 406, 455
9, 10, 12, 230, 254, 305,
Hard Steel 50HRC Rubber Resin Al2O3
14, 16, 18 356, 406, 455
9, 10, 12, 230, 254, 305,
Medium Hard Steel 35-50HRC Rubber Resin Al2O3
14, 16, 18 356, 406, 455
9, 10, 12, 230, 254, 305,
Soft or Annealed Steel 15-35HRC, 46-90HRB Rubber Al2O3
14, 16, 18 356, 406, 455
Medium Hard Nonferrous Materials, Uranium, 9, 10, 12, 230, 254, 305,
Rubber SiC
Titamium, Zirconium 14, 16, 18 356, 406, 455
Soft Nonferrous Materials, 9, 10, 12, 230, 254, 305,
Rubber SiC
Aluminum, Brass, etc. 14 356
9, 10, 12, 14, 254, 305, 356,
Superalloys Rubber Al2O3
16, 18 230, 406, 455
Thin Blades to Minimize Kerf Loss and Cutting Deformation
127, 230, 254,
Tool, Hard Steel, < 45RC Rubber Al2O3 5, 9, 10, 12, 14
305, 356
5, 7, 9, 10, 12, 127, 178, 230,
Tool, Hard Steel, > 45RC Rubber Al2O3
14 254, 305, 356
Hard or Soft Nonferrous Materials Rubber SiC 7 178
Refer to the Buehler Product Catalogue for ordering information and exact dimensions of arbor sizes, outer diameter and thickness.

also offers diamond and CBN blades with resin applied to the grains is inadequate for cutting, then
bonded or Rimlock1 metal bonded blade forms in heat is generated which may not be dissipated by
sizes from 8in [203mm] to 16in [406mm] diameters. the coolant, which causes deformation damage,
Resin-bonded diamond blades are ideal for cutting phase changes and possibly burning or melting.
very hard cemented carbide specimens; Rimlock or
continuous rim blades are recommended for cutting A chop cutter may be set up to pulse as the
rocks and petrographic specimens. load is applied, that is, the wheel is fed into the
sample, and then feeding is halted momentar-
Historically, the most common cutter design has ily, Figure 1.3b. Pulsing causes the wheel to be
been the so-called “chop” cutter. Basically, the stress shocked which removes both dull and
blade is attached to a motor and the operator pulls sharp abrasive from the wheel as new abrasive
a handle to drive the blade downward into the work is exposed to the cut. While a better cut may
piece. Because of the design, the blade moves be obtained, cutting time and wheel wear are
through an arc as it is pulled downward, Figure 1.3a. increased. For small parts, a Y-feed cut (see Figure
For efficient cutting, the piece must be oriented to 1.3c) can provide a faster cutting time.
minimize the contact area with the wheel. For small
parts, this is generally easy to do, but for larger parts, Optimal cutting, with the least damage to the sam-
it may not be possible to orient the sample properly ple, is obtained by keeping the pressure on each
for optimal cutting. When a round wheel is used to abrasive particle in the wheel constant and as low
cut a round bar in chop mode, the contact area is as possible by keeping the contact area between
initially very small. As the cut progresses, the cut wheel and sample constant and low. This idea is
widens until the maximum diameter is reached. Af- called the minimum area of contact cutting (MACC)
ter this, the contact area decreases until sectioning method. This can be achieved with several different
is completed. Under application of a constant load, cut types.
the pressure on the abrasive particles in the cut de-
creases as the contact area increases. If the pressure Several other options for MACC are the “planar”
Rimlock is a registered trademark of Felker Operations.
1

6
SECTIONING
or “saw” cut type, Figures 1.3d and 1.3e. A strip of be moved an increment downwards in each cycle.
material is removed by moving either the wheel or Consequently, cut times are longer, but may not be
the work piece perpendicular to the cut direction. possible otherwise. The wheel traverse length must
After this, the cutter must move back to the side be greater than the specimen width. This machine
where the cut began. The wheel is dropped down must be programmed for each size part to obtain
a fixed increment and another strip is removed. In cutting. The primary difference in these cut types
this approach, the wheel must move to the end of is that in planar, the cut is performed only in the
the stroke, return to the starting point, and then forward direction while in travese and increment or

Figure 1.3. Illustration of cutter types and the wheel path during sectioning

CUTTING STYLE AND WHEEL PATH

Wheel Path

Sample
1.3a Chop Cutting
The traditional form of machine operation.
Wheel contact arc is governed by sample
size. Generally a struggle with large/
difficult parts.

1.3b Chop Cutting with Pulsing

Wheel contact still governed by sample
size. The pulsing action gives a shock
to the wheel causing abrasives to break
away. Wheel wear is generally high with
this method.

1.3c Y-Feed Cut

The abrasive wheel is stationary and the
cutting table moves forward completing
a one time cut into the sample. Wheel
contact arc is governed by sample size.

1.3d Planar Cut

The abrasive wheel lowers into the sample
at an incremental rate before the cutting
table moves in the forward motion. Wheel
contact arc is determined by cut depth.

1.3e Saw Cut

The wheel contact arc can be precisely
controlled via depth increment. The
traverse stroke must always exceed the
part length to avoid a change in wheel
contact arc area. Machine needs to be set
for each part.

1.3f Orbital
Similar in action to traverse and increment
but on a curved path. Simpler and quicker
in operation. Part size is irrelevant as
the orbital action produces a minimum
contact arc area during cutting.

7
SECTIONING
saw, the cut is performed in both directions with different abrasive sizes and bonds to provide
optimum cutting for a wide variety of applications.
Orbital cutting, Figure 1.3f, combines the best
features of chop, oscillation and traverse-and-in-
crement cutters, while minimizing cutting time.
As the wheel is fed into the sample, the arbor
is also rotated in a small ellipse planar with the
wheel permitting the wheel to cut a small strip
of material from the sample. But no time is lost,
as with the traverse and increment cutter, as the
wheel is ready to cut on the original side. With
the elliptical orbit and a controlled feed, the
conditions for minimum area of contact cutting
are obtained, irrespective of work piece size.
Special programming is not needed. The orbital
cutting concept is available in many of the Delta
cutters from Buehler. These also feature SmartCut, Figure 1.4. IsoMet High Speed Precision Cutter
which will sense motor overloading during a cut, if
it occurs, and reduce the feed rate automatically.
When it is safe to return to the original feed rate,
HELPFUL HINTS
SmartCut will do so.
FOR SECTIONING
Precision Sectioning When cutting a difficult specimen with
Precision cutters, Figure 1.4, are commonly used the recommended consumable abrasive
in metallographic preparation to section mate- wheel, if the cutting action has become
rials that are small, delicate, friable, extremely very slow, pulse the applied force. This will
hard, where the cut must be made as close as help break down the abrasive bonding,
possible to a feature of interest, or where the cut exposing fresh, sharp abrasives to enhance
width and material loss must be minimal. As the the cutting action. However, if you are
name implies, this type of saw is designed to make using a resin-bonded diamond blade to
very precise cuts. They are smaller in size than cut cemented carbides, or other very hard
the usual laboratory abrasive cut-off saw and use materials, do not pulse the applied force,
much smaller blades, typically from 3 - 8in [76 - as this will shorten wheel life.
203mm] in diameter. These blades can be made
of copper-based alloys or copper plated steel with
diamond or cubic boron nitride abrasive bonded
to the periphery of the blade; or, they can be an
abrasive wheel using alumina or silicon carbide
abrasives with a rubber-based bond. Blades for the
precision saws are much thinner than the abrasive
wheels used in an abrasive cutter and the load
applied during cutting is much less. Consequently,
less heat is generated during cutting and damage
depths are reduced. While pieces with a small
section size, that would normally be sectioned with
an abrasive cutter can be cut with a precision saw,
the cutting time will be appreciably greater but the
depth of damage will be much less. Precision saws
are widely used for sectioning sintered carbides, ce-
ramic materials, thermally sprayed coatings, printed
circuit boards, electronic components, bone, teeth,
etc. Table 1.2 lists selection criteria for precision
saw blades. Blades for precision saws are available

8
SECTIONING
Table 1.2. Selection Criteria for Precision Blades

3 x 0.007in 4 x 0.012in 5 x 0.015in 6 x 0.015in 7 x 0.025in 8 x 0.035in

BLADE SERIES [76 x 0.15mm] [102 x 0.3mm] [127 x 0.4mm] [152 x 0.5mm] [178 x 0.6mm] [203 x 0.9mm]
IsoMet Diamond Wafering Blades
Series 30HC, polymers,
rubber, soft gummy X** X** X
materials
Series 20HC, aggressive
X* X X
sectioning of metals
Series 15HC, metal matrix
composites, PCBs, bone, X X X X X X
Ti, TSC
Series 20LC, hard tough
materials, structural X* X X
ceramics
Series 15LC, hard brittle
materials, glass, Al2O3, X X X X X X
Zr2O3, concrete
Series 10LC, medium to
soft ceramics, glass fiber X X X* X
reinforced composites
Series 5LC,soft friable ce-
ramics, composites with
X X
fine reinforcing, CaF2,
MgF2, carbon composites
IsoCut CBN Wafering Blades
Low Concentration, Fe,
Co, Ni based alloys and X X X X X X
superalloys
High Concentration Fe,
Co, Ni based alloys and X X X X X
superalloys
General Usage and AcuThin Abrasive Wheels For sectioning small, delicate specimens or where minimal deformation and kerf loss is
the primary concern

Bond/ 5 x 0.019in 7 x 0.03in

Abrasive [127 x 0.5mm] [178 x 0.8mm]

Tool Steel, hard Steel ≥

R/Al2O3 X
HRC45
Medium hard, soft steel ≤
R/Al2O3 X
HRC45
Soft materials R/Al2O3 X
Tough materials or gen-
R/SiC X
eral use
*Alternate blade thickness of 0.020in [0.5mm] **Alternate blade thickness of 0.030in [0.8mm]
For a complete listing of Buehler consumable supplies for use with the IsoMet Precision Cutters, please refer to the Buehler Product
Catalogue.

9
MOUNTING
The primary purpose of mounting metallographic seepage of fluids from crevices between specimens
samples is for convenience in handling samples of does not occur. The outer clamp edges should be
difficult shapes or sizes during the subsequent steps beveled to minimize damage to polishing cloths. If
of metallographic preparation and examination. clamps are improperly used so that gaps exist be-
A secondary purpose is to protect and preserve tween specimens, fluids and abrasives can become
extreme edges or surface defects during metal- entrapped and will seep out obscuring edges and
lographic preparation. The method of mounting can cause cross contamination. This problem can be
should in no way be injurious to the microstructure minimized by proper tightening of clamps, by use of
of the specimen. Pressure and heat are the most plastic spacers between specimens, or by coating
likely sources of injurious effects. specimen surfaces with epoxy before tightening.

Phenolic plastics were introduced to metallography

in 1928 for encapsulating specimens by hot com-
Compression Mounting
pression mounting. Prior to that time, samples were The most common mounting method uses
prepared unmounted, or mounted in flours of sulfur, pressure and heat to encapsulate the sample with
wax or low-melting point alloys, such as Wood’s met- a thermosetting or thermoplastic mounting mate-
al. These “mounting compounds” were not without rial. Common thermosetting compounds include
their problems. Introduction of polymers was a big phenolic (PhenoCure), diallyl phthalate and epoxy
improvement over these methods. Subsequently, (EpoMet) while methyl methacrylate (TransOptic )
many polymers were evaluated for use as mounting is the most commonly used thermoplastic mount-
compounds, as they were introduced to the market. ing compounds. Table 2.1 lists the characteristics
Development of castable resins in the 1950’s added of the compression mounting compounds. Both
new resins to the metallographer’s tool chest. The thermosetting and thermoplastic materials require
simplicity of mounting without using a press, and heat and pressure during the molding cycle; but,
their low curing temperatures, made castable resins after curing, mounts made of thermoplastic com-
an attractive alternative. pounds must be cooled under pressure to at least
158°F [70°C] while mounts made of thermosetting
materials may be ejected from the mold at the
Clamp Mounting maximum molding temperature. However, cool-
Clamps have been used for many years to ing thermosetting compounds under pressure to
mount cross sections of thin sheet specimens. near ambient temperature before ejection will
Several samples can be clamped conveniently in significantly reduce shrinkage gap formation. Never
sandwich form making this a quick, convenient rapidly cool a thermosetting mount with water after
method for mounting thin sheet specimenss. When hot ejection from the molding temperature. This
done properly, edge retention is excellent, and causes the metal to pull away from the mounting

Table 2.1: Characteristics of Compression Mounting Compounds

Best Edge Retention;

Very Low Shrinkage; Near Zero Electrical
Fine Particle Size; Best Edge Retention; Resistance
Materials General Purpose Fills Smallest Crevices Very Low Shrinkage SEM - EDS/WDS Clear
Ceramics PhenoCure EpoMet F EpoMet G ProbeMet TransOptic
Steels PhenoCure EpoMet F EpoMet G ProbeMet TransOptic
Plated
PhenoCure EpoMet F EpoMet G ProbeMet TransOptic
Layers
Aluminum PhenoCure ProbeMet TransOptic
Copper/
PhenoCure ProbeMet TransOptic
Brass
Black, Red or
Color Black Black Copper Transparent
Green
Temperature 300°F [150°C] 300°F [150°C] 300°F [150°C] 300°F [150°C] 350°F [177°C]
2100 psi [145
Pressure 4200 psi [290 bar] 4200 psi [290 bar] 4200 psi [290 bar] 4200 psi [290 bar]
bar]

Rimlock is a registered trademark of Felker Operations.

1

10
compound producing shrinkage gaps that promote Also, placing a number of mounted specimens
poor edge retention, see Figure 2.1, because of in a holder for semi- or fully-automated grinding
the different rates of thermal contraction. EpoMet, and polishing is easier with standard mounts than

MOUNTING
a thermosetting epoxy, provides the best edge for unmounted specimens. Mounted specimens
retention, Figure 2.2, of these compounds and is
virtually unaffected by hot or boiling etchants while
phenolics are badly damaged.

a
Figure 2.3. SimpliMet 4000 Automatic Mounting Press

are easier on the grinding/polishing surfaces than

unmounted specimens.

Castable Mounting Systems

Most castable mounting systems require
neither pressure nor external heat and are recom-
b mended for mounting specimens that are sensitive
Figure 2.1. Edge retention of this improperly carburized 8620 to heat and/or pressure. Acrylic systems, such
alloy steel was degraded by a shrinkage gap between the
specimen and the phenolic mount: a) 500X; b) 1000X (2% nital). as VariDur and SamplKwick, are the most widely
used castable systems due to their low cost and
Mounting presses vary from simple laboratory jacks short curing time. However, shrinkage can be a
with a heater and mold assembly to full automat- problem with acrylics. Epoxy systems, although
ed devices that include the SmartCool intelligent more expensive than acrylics, are commonly used
cooling system that ends the process as soon as because epoxy will physically adhere to specimens,
the specimen is safe to handle, as shown in Figure have low shrinkage, and can be drawn into cracks
2.3. An advantage of compression mounting is and pores, particularly if a vacuum impregnation
production of a mount of a predicable, convenient chamber, as shown in Figure 2.4, is employed and
size and shape. Further, considerable information a low viscosity epoxy, such as EpoThin 2, is used.
can be engraved on the backside – this is always Epoxies are very suitable for mounting fragile or
more difficult with unmounted specimens. Manual, friable specimens and corrosion or oxidation spec-
or hand, polishing is simplified, as the specimens imens. Dyes or fluorescent agents may be added
are easy to hold.

Figure 2.2. Excellent edge retention of a borided 42CrMo4 alloy

steel specimen mounted in EpoMet resin (1000X, 2% nital). Figure 2.4. Vacuum Impregnation Equipment

11
MOUNTING
to epoxies for the study of porous specimens such ductive Filler particles can be added to the castable
as thermal spray coated specimens. Most epoxies systems, though the viscosity increases.
are cured at room temperature, and curing times
can vary from 1 to 9 hours. Some can be cured When preparing castable resin mounts, particularly
at slightly elevated temperatures in less time, as epoxy mounts by manual “hand” methods, the me-
long as the higher temperature does not adversely tallographer will observe that the surface tension
affect the specimen. Table 2.2 lists the characteris- between the mount and the working surface is
tics of castable systems. much higher than with a compression mount. This
can make holding the mount more challenging. If
Cast epoxy systems provide better edge reten- automated devices are used, the metallographer
tion than cast acrylic systems, mainly due to the may hear “chatter,” or noise, during rough grinding
better adhesion of epoxy to the specimen and due to the greater surface tension. The chatter can
their lower shrinkage. Acrylics usually do not be reduced or stopped by changing to contra mode
bond to the specimen and a gap is sometimes (head and platen rotate in opposite directions).
formed between specimen and mount, with
VariDur 3003 being the exception. When a Acrylics, and some epoxies, do generate consid-
shrinkage gap is present, edge retention is usually erable heat during curing and this can be strongly
poor. To improve edge retention with castable influenced by the molding technique used. Nelson
mounts, the specimen can be plated with electroless [4] measured the exotherm produced by polym-
nickel, or Flat Edge Filler particles can be added to erizing an acrylic system using two procedures:
the system. To obtain electrical conductivity, Con- a glass mold on a glass plate (insulative) and an
aluminum mold on an aluminum plate (conductive).

Table 2.1: Characteristics of Compression Mounting Compounds

Peak Shore D Recommended

Name Type Temperature Cure Hardness* Time Mold Comments
Clear, very low viscosity, low
EpoThin 2 Epoxy <149°F [65°C] 78 9 hours Any shrinkage, best for vacuum
impregnation
Clear, general pupose epoxy
EpoxiCure 2 Epoxy <104°F [40°C] 80 6 hours Any
system, low shrinkage
Clear, fast curing epoxy system,
EpoKwick FC Epoxy <250°F [121°C] 82 2 hours Any
low shrinkage, very low viscosity
Clear epoxy system, long pot
EpoHeat CLR Epoxy <324°F [162°C] 82 1 hour Any life allows product to be mixed
in large batches
15-30 Very low shrinkage with high
VariDur 3003 Acrylic <252°F [122°C] 90 Any
minutes hardness
5-8 Translucent, general purpose
SamplKwick Acrylic <179°F [81°C] 85 Any
minutes system, some shrinkage
Clear, general purpose acrylic
system, requires pressure
vessel for clear mounts, minimal
5-15
VariKleer Acrylic <212°F [100°C] 84 SamplKup shrinkage. To acheive crystal
minutes
clear samples, reusable silicon
or EPDM molds should not be
used.
Semi transparent, low odor
VariDur 10 Acrylic <212°F [100°C] 80 8 minutes Any system, low shrinkage, high
viscosity
5-8 Dark blue, low odor system, low
VariDur 200 Acrylic <212°F [100°C] 85 Any
minutes shrinkage, high viscosity

* Hardness differences appear negligible but abrasion resistance has a significant effect on edge rounding

12
Polymerization produced a maximum exotherm of contrast at an interface between a specimen and
270°F [132°C] using the insulative approach but the electroless nickel may be inadequate for certain
only 108°F [42°C] using the conductive approach. evaluations. Figure 2.5 shows the surface of a speci-

MOUNTING
Note that 270°F [132°C] is not much less than the men of 1215 free-machining steel that was salt bath
302°F [150°C] temperature used in compression nitrided. One specimen was plated with electroless
mounting. Nelson also measured the exotherm nickel; both were mounted in EpoMet G. It is hard
produced when an epoxy system was cured in a to tell where the nitrided layer stops for the plated
phenolic ring form placed on a pasteboard base. specimen, Figure 2.5a, which exhibits poor image
Although this was an insulative approach, the max- contrast between the nickel and the nitrided surface.
imum temperature during polymerization was only This is not a problem for the non-plated specimen,
45°F [7°C], a vast improvement over the acrylics. Figure 2.5b.

Nelson’s work applies to specific acrylic and

epoxy resins molded upon specific conditions.
While the epoxy that he used exhibited a low
exotherm, this does not imply that all epoxy
systems will exhibit such low exotherms in polym-
erization. Epoxy systems that cure in short time
periods develop much higher exotherms, that can
even exceed that of acrylic systems. In addition
to the speed of curing of the epoxy system, other
factors do influence the magnitude of the exotherm a
during polymerization. The larger the mass of
epoxy in the mount, the faster it will set and the
greater the exotherm. Indeed, very large mounts
can generate enough heat to crack extensively.
Heating the system makes it less viscous and
speeds up curing, also generating more heat
during polymerization. The mold material also
can influence curing time and temperature.
For example, EpoxiCure 2 cures fastest in b
SamplKup plastic molds, slower in ring forms, and Figure 2.5. Example of a) poor coating edge visibility due to a
still slower in the reuseable EPDM mounting cups. lack of contrast between the protective nickel plating and the
salt bath nitrided surface (arrow) of 1215 free-machining carbon
Consequently, the exotherm will be greater when steel; and, b) good contrast and visibility between EpoMet
resin and nitrided surface (arrow) plus excellent edge retention
using the SamplKup type mold and lowest when (1000X, 2% nital).
using the EPDM mounting cups. All of these fac-
tors must be considered if the exotherm must be
minimized. Introduction of new technology has greatly
reduced edge preservation problems [5,6]. Gaps
that form between specimen and mount media are
a major contributor to edge rounding, as shown
Edge Preservation in Figure 2.1. Staining at shrinkage gaps may also
be a problem, as demonstrated in Figure 2.6. Use
Edge preservation is a classic preparation prob-
of semi-automatic and automatic grinding/polish-
lem and many “tricks” have been promoted (most
ing equipment, rather than manual preparation,
pertaining to mounting, but some to grinding and
increases surface flatness and edge retention. To
polishing) to enhance edge flatness. These methods
achieve the best results, however, the position of
[2] include the use of backup material in the mount,
the specimen holder, relative to the platen, must
the application of coatings to the surfaces before
be adjusted so that the outer edge of the specimen
mounting or the addition of a filler material to the
holder rotates out over the edge of the surface on
mounting system. Plating [2] of a compatible metal
the platen during grinding and polishing, particu-
on the surface to be protected (electroless nickel
larly for 8in [203mm] diameter platens. The use of
has been widely used) is generally considered to
harder, woven or non-woven, napless surfaces for
be the most effective procedure. However, image

13
MOUNTING
polishing with diamond abrasives (rather than softer
cloths such as canvas, billiard and felt) maintains
flatness. Final polishing with low nap cloths for short
times introduces very little rounding compared to
use of higher nap, softer cloths.

Figure 2.6. Staining (thin arrows) due to etchant bleed out from
a shrinkage gap (wide arrows) between the phenolic mount and
the M2 high speed steel specimen (500X, Vilella’s reagent).

These procedures will produce better edge

retention with all thermosetting and thermoplastic b
Figure 2.7. Poor edge retention (arrows) at the salt bath nitrided
mounting compounds. Nevertheless, there are surface of 1215 free-machining carbon steel mounted in a)
still differences among the polymeric materials phenolic resin and in b) methyl methacrylate and polished in the
same holder as those shown in Figure 2.5 (1000X, 2% nital).
used for mounting. Thermosetting compounds
provide better edge retention than thermoplastic
compounds. Of the thermosetting compounds,
diallyl phthalate provides little improvement over
the much less expensive phenolic compounds. The
best results are obtained with EpoMet G or EpoM-
et F an epoxy based thermosetting compounds
that contains a filler material. For comparison,
Figure 2.7 shows micrographs of a nitrided 1215
specimen mounted in a phenolic (Figure 2.7a),
and in methyl methacrylate (Figure 2.7b), at 1000X.
These specimens were prepared in the same
specimen holder as those shown in Figure 2.5,
but neither displays acceptable edge retention at
1000X. Figure 2.8 shows examples of perfect edge a
retention, as also demonstrated in Figure 2.5.

Very fine aluminum oxide spheres have been

added to castable epoxy systems to improve
edge retention, but this is really not a satisfactory
solution as the particles are extremely hard (~2000
HV) and their grinding-polishing characteristics
are incompatible with softer metals placed inside
the mount. Howver, use of a soft ceramic shot
b
(~775 HV) has grinding/polishing characteristics
Figure 2.8. Excellent edge retention for a) complex coated
compatible with metallic specimens placed in (arrow) sintered carbide insert (1000X, Murakami’s reagent) and
for b) iron nitrided (arrow points to a white iron nitride layer; an
the mount. Figure 2.9 shows an example of edge embedded shot blasting particle is to the left of the arrow) H13
retention with the Flat Edge Filler soft ceramic shot hot work die steel specimen (1000X, 2% nital). EpoMet was
used in both cases.
in an epoxy system.

14
Following are general guidelines for obtaining the the text) with an automated grinder-polisher
best possible edge retention. All of these factors as this method provides better flatness than
contribute to the overall success, although some single, or individual, pressure mode (defined

MOUNTING
are more critical than others. later in the text).

• Orient the position of the smaller diameter spec-

imen holder so that, as it rotates, its periphery
slightly overlaps the periphery of the larger
diameter platen.

• Use PSA-backed SiC grinding paper (if SiC is

used), rather than plain backed paper on the
platen and a peripheral hold-down ring, and
PSA-backed or magnetic polishing cloths rather
Figure 2.9. Flat Edge Filler shot was added to Epoxicure 2 resin than stretched cloths.
to improve the edge retention of this annealed H13 hot work
die steel specimen (500X, 4% picral).
• Apex DGD and UltraPrep diamond grinding
discs produce excellent flat surfaces for a wide
• Properly mounted specimens yield better edge variety of materials.
retention than unmounted specimens, as round-
ing is difficult, if not impossible, to prevent at • Use “hard” napless surfaces for rough polishing
a free edge. Compression mounts yield better (until the final polishing step), such as TexMet C,
edge preservation than castable systems. UltraPol or UltraPad cloths, and fine polishing,
such as a TriDent cloth. Use a napless, or a low-
• E l e c t r o l y t i c o r e l e c t r o l e s s N i p l a t - to medium-nap cloth, depending upon the
ing of the surface of interest material being prepared, for the final step and
provides excellent edge retention. If the keep the polishing time brief.
compression mount is cooled too quickly af-
ter polymerization, the plating may be pulled • Rigid grinding discs, such as the Apex Hercules
away from the specimen leaving a gap. When H and S discs, produce excellent flatness and
this happens, the plating is ineffective for edge edge retention and should be used whenever
retention. possible.

• Thermoplastic compression mounting com-

pounds are less effective than thermosetting HELPFUL HINTS
compounds. The best thermosetting compound FOR MOUNTING
for edge retention is EpoMet G, an epoxy-based
resin containing a hard filler material. Epoxy is the only resin that will physically
adhere to a specimen. If its viscosity is low,
• Never hot eject a thermosetting compound after
epoxy can be drawn into pores and cracks
polymerization and cool it quickly to ambient
by vacuum impregnation. Acrylics are not
(e.g., by cooling it in water) as a gap will form
ideal for vacuum impregnation due to
between specimen and mount due to the
short cure times and generally have high
differences in thermal contraction rates. Fully
viscosity.
automated mounting presses cool the mounted
specimen to near ambient temperature under Castable resins are sensitive to shelf life. It
pressure and this greatly minimizes gap forma- is a good practice to date your containers
tion due to shrinkage. when you get them.

• Automated grinding-polishing equipment

produces flatter specimens than manual prepa-
ration.

• Use the central force mode (defined later in

15
GRINDING & POLISHING
Grinding replace SiC paper. For very hard materials
Grinding should commence with the finest grit size such as ceramics and sintered carbides, one, or
that will establish an initially flat surface and remove more, metal-bonded or resin-bonded diamond
the effects of sectioning within a few minutes. An discs (the traditional type) with grit sizes from about
abrasive grit size of 180-240 [P180-P280] is coarse 240 to 9µm can be used. The traditional metal- or
enough to use on specimen surfaces sectioned by resin-bonded diamond disc has diamond spread
an abrasive wheel. Hack-sawed, bandsawed, or oth- uniformly over its entire surface. Apex DGD and
er rough surfaces usually require abrasive grit sizes Apex DGD Color, ranging in grit size from 320 to
in the range of 120-180 grit [P120-P180}. The abra- 0.5µm, are also available as resin bonded diamond
sive used for each succeeding grinding operation grinding discs covering a variety of material appli-
should be one or two grit sizes smaller than that used cations. An alternate type of disc, the UltraPrep disc,
in the preceding step. A satisfactory fine grinding has diamond particles applied in small spots to the
sequence might involve SiC papers with grit sizes of disk surface, so that surface tension is lessened.
240, 320, 400, and 600 grit [P280, P400, P800 and UltraPrep metal-bonded discs are available in six
P1200]. This sequence is used in the “traditional” diamond sizes from 125 to 6µm while UltraPrep resin
approach. bonded discs are available in three diamond sizes
from 30 to 3µm. Once planar surfaces have been
As with abrasive cutting, all grinding steps should be obtained, there are several single-step procedures
performed wet provided that water has no adverse available for avoiding the finer SiC papers. These
effects on any constituents of the microstructure. include the use of platens, thick woven polyester
Wet grinding minimizes specimen heating, and cloths, silk, or rigid grinding discs. With each of
prevents the abrasive surface from becoming these, an intermediate diamond size, generally 9
loaded with metal removed from the specimen to 3µm, is used.
being prepared.
Grinding Media
Each grinding step, while producing damage
The grinding abrasives common-
itself, must remove the damage from the previ-
ly used in materials preparation are
ous step. The depth of damage decreases with
silicon carbide (SiC), aluminum oxide (Al 2O 3),
the abrasive size but so does the metal remov-
emery (Al2O3 - Fe3O4), composite ceramics and
al rate. For a given abrasive size, the depth of
diamond. Emery paper is rarely used today in
damage introduced is greater for soft materials than
materials preparation due to its low cutting effi-
for hard materials.
ciency. SiC is more readily available as waterproof
paper than aluminum oxide. These abrasives are
For automated preparation using a multiple-speci-
bonded to paper, polymeric or cloth backing mate-
men holder, the intital step is called planar grinding.
rials in the form of discs and belts of various sizes.
This step must remove the damage from sectioning
Limited use is made of standard grinding wheels
while establishing a common plane for all of the
with abrasives embedded in a bonding material.
specimens in the holder, so that each specimen
The abrasives may be used also in powder form by
is affected equally in subsequent steps. Silicon
charging the grinding surfaces with the abrasive
carbide and alumina abrasive papers are com-
in a premixed slurry or suspension. SiC particles,
monly used for the planar grinding step and are
particularly with the finer size papers, embed easi-
very effective. Besides these papers, there are a
lywhen grinding soft metals, such as Pb, Sn, Cd and
number of other options available. One option is
Bi (see Figure 3.1). Embedding of diamond abrasive
to planar grind the specimens with a conventional
is also a problem with these soft metals and with
alumina or Silicon carbide grinding stone. This
aluminum, but mainly with slurries when napless
requires a special purpose machine, as the stone
cloths are used, see Figure 3.2.
must rotate at a high speed, ≥1500 rpm, to cut ef-
fectively. The stone must be dressed regularly with
Silicon Carbide paper manufactured in the
a diamond tool to maintain flatness and refresh the
United States is typically made according to the
abrasive surface for effective grinding.
ANSI/CAMI standard (B74. 18-1996) while paper
manufactured in Europe are made according to
Other materials have also been used both for
the FEPA standard (43-GB-1984, R 1993). Both
the planar grinding stage or, afterwards, to

16
Figure 3.1. SiC grit particle (arrow) embedded in a 6061-T6 Figure 3.2. 6µm diamond particles (arrows) embedded in lead
aluminum weldment (500X, aqueous 0.5% HF). (1000X).

GRINDING & POLISHING

standards use the same methods for sizing the broader size range allows cutting to begin faster
abrasives and the same standards to calibrate these at lower pressures than with a narrower size range,
devices (sieving for the coarsest grits, sedimen- so less heat is generated and less damage results.
tation grading for intermediate grits (240-600 However, the broader size range does produce a
[P280-P1200]), and the electrical resistance wider range of scratch depths; but, these should
method for very fine grit sizes). The grit size be removed by the next step in the preparation
numbering systems differ above 180 grit [P180], sequence. Generation of less damage to the struc-
but equivalent sizes can be determined using ture is considered to be more important than the
Table 3.1. As with many standards, they are not surface finish after a particular grinding step, as it
mandatory and manufacturers can, and do, make is the residual damage in the specimen that may
some of their papers to different mean particle prevent us from seeing the true microstructure at
sizes than defined in these specifications. There is the end of the preparation sequence.
a philosophical difference in the two systems. ANSI/
CAMI papers use a wider particle size distribution
(centered on the mean size) than FEPA papers. A

Table 3.1: European/US Equilivancy Guide

FEPA (Europe) ANSI/CAMI (US)

Grit Number Micron Grit Number Micron Emery Grit
P60 269 60 268
P80 201 80 188
P100 162 100 148
P120 127 120 116
P180 78 180 78 3
P240 58.5 220 66 2
P280 52.2 240 51.8
P320 46.2
P360 40.5 280 42.3 1
P400 35 320 34.3 0
P500 30.2 360 27.3
P600 25.8
P800 21.8 400 22.1 00
P1000 18.3 500 18.2 000
P1200 15.3 600 14.5
P1500 12.6 800 12.2 0000
P2000 10.3 1000 9.2
P2500 8.4 1200 6.5
P4000* 5.0*
The chart shows the midpoints for the size ranges for ANSI/CAMI graded paper according to ANSI standard B74.18-1996 and for FEPA graded paper
according to FEPA standard 43-GB-1984 (R1993). The ANSI/CAMI standard lists SiC particles sizes ranges up to 600 grit paper. For finer grit ANSI/
CAMI papers, the particles sizes come from the CAMI booklet, Coated Abrasive (1996).
*FEPA grades finer than P2500 are not standardized and are graded at the discretion of the manufacturer. In practice, the above standard values are
only guidelines and individual manufactures may work to a different size range and mean value.

17
GRINDING & POLISHING
Grinding Equipment as grinding. Some platens, referred to as laps, are
charged with diamond abrasive in a carrier, such as
A Planar grinding machine, like the PlanarMet 300
paste, oil based suspenstion or water based suspen-
shown in Figure 3.3, utilizes a fixed abrasive stone
sion. Initially the diamond particles roll over the lap
for rapid sample grinding. This type of automated
surface (just as with other grinding surfaces), but
grinder produces planar samples in 1-2 minutes
they soon become embedded and cut the surface
replacing up to 3 traditional grinding steps. Ma-
producing microchips.
chines like this can be bench-top or floor standing
and typically utilize the same sample holders as
grinder-polishers to integrate the transition to the
next step. Stationary grinding papers, often used
by students, but uncommon in industrial use, are
supplied in strips or rolls. The specimen is rubbed
against the paper from top to bottom. Grinding
in one direction is usually better for maintaining
flatness than grinding in both directions. This proce-
dure can be done dry for certain delicate materials,
but water is usually added to keep the specimen
surface cool and to carry away the grinding debris.

Figure 3.4. EcoMet 250 Grinder-Polisher

Polishing
Polishing is the final step, or steps, in producing a
deformation-free surface that is flat, scratch free,
and mirror-like in appearance. Such a surface is
necessary to observe the true microstructure for
subsequent interpretation, testing or analysis,
both qualitative and quantitative. The polishing
technique used should not introduce extraneous
structures such as disturbed metal (Figure 3.5), pit-
ting (Figure 3.6), dragging out of inclusions, “comet
tailing” (Figure 3.7), staining (Figure 3.8) or relief
Figure 3.3. PlanarMet 300 Planar Grinder

Belt grinders are usually present in most lab-

oratories. These types of devices use coarse
abrasive papers from 60 [P60] to 240 [P280] grit,
and are mainly used for removing burrs from
sectioning, for rounding edges that need not
be preserved for examination, for flattening cut
surfaces to be macroetched, or for removing sec-
tioning damage. Figure 3.5. Preparation damage (arrows) in annealed CP
titanium (500X, DIC, Kroll’s reagent).

Lapping is an abrasive technique in which the

abrasive particles roll freely on the surface of a
carrier disc. During the lapping process, the disc
is charged with small amounts of a hard abrasive
such as diamond or silicon carbide. Lapping discs
can be made of many different materials; cast iron
and plastic are used most commonly. Lapping
produces a flatter specimen surface than grinding,
but it does not remove metal in the same manner
Figure 3.6. Pitting (arrow) on the surface of a cold-drawn brass
(Cu-20% Zn) specimen (100X)

18
polishing step may be followed by polishing with
1µm diamond on a napless, low nap, or medium
nap cloth. A compatible lubricant should be used
sparingly to prevent overheating or deformation
of the surface. Intermediate polishing should be
performed thoroughly so that final polishing may
be of minimal duration. Manual, or hand, polishing,
is usually conducted using a rotating wheel where
the operator rotates the specimen in a circular path
counter to the wheel rotation direction.
Figure 3.7. “Comet tails” at large nitrides in an annealed H13

GRINDING & POLISHING

hot work die steel specimen (200X, DIC).

Figure 3.8. Staining (arrow) on the surface of a of Ti-6% Al-2%

Sn-4% Zr-2% Mo prepared specimen (200X).

(height differences between different constituents,

or between holes and constituents (Figures 3.9
and 3.10). Polishing usually is conducted in several
stages. Traditionally, coarse polishing generally
was conducted with 6 or 3µm diamond abrasives
charged onto napless or low-nap cloths. For hard
b
materials, such as through hardened steels, ceram- Figure 3.10. Differences in relief control in a brazed specimen
ics and cemented carbides, an additional coarse containing shrinkage cavities: a) poor control; and, b) good
control (100X, glyceregia).
polishing step may be required. The initial coarse

Mechanical Polishing
The term “mechanical polishing” is frequently
used to describe the various polishing procedures
involving the use of fine abrasives on cloth. The
cloth may be attached to a rotating wheel or a
vibratory polisher bowl. Historically, cloths have
been either stretched over the wheel and held
a in place with an adjustable clamp on the platen
periphery, or held in place with a pressure sensitive
adhesive (PSA), magnetic or high friction surface-
bonded to the back of the cloth. If a stretched cloth
moves under the applied pressure during polishing,
cutting will be less effective. If an automated polish-
ing head is used, stretched cloths are more likely to
rip, especially if unmounted specimens are being
prepared. In mechanical polishing, the specimens
are held by hand, held mechanically in a fixture, or
b
Figure 3.9. Examples of freedom from relief a) and minor relief merely confined within the polishing area, as with
b) at the edges of large primary hypereutectic silicon particles in the VibroMet 2 polisher.
an as-cast Al-19.85% Si specimen (200X, aqueous 0.5% HF).

19
GRINDING & POLISHING
Manual “Hand” Polishing
Aside from the use of improved polishing cloths
and abrasives, hand-polishing techniques still
follow the basic practice established many
years ago:

1. Specimen Movement. The specimen is held with

one or both hands, depending on the operator’s
preference, and is rotated in a direction counter
to the rotation of the polishing wheel. In addi-
tion, the specimen is continually moved back
and forth between the center and the edge of
the wheel, thereby ensuring even distribution
of the abrasive and uniform wear of the pol-
ishing cloth. (Some use a small wrist rotation
Figure 3.11. EcoMet 300 Grinder-Polisher and AutoMet 300
while moving the specimen from the center to Power Head
the edge of one side of the wheel.) After each devices produce the best surface flatness and edge
step, the specimen is rotated 45 to 90° so that retention. There are two approaches for handling
the abrasion is not unidirectional. specimens. Central force utilizes a specimen holder
with each specimen held in place rigidly. The hold-
2. Polishing Pressure. The correct amount of
er is pressed downward against the preparation
applied pressure must be determined by experi-
surface with the force applied to the entire holder.
ence. In general, a firm hand pressure is applied
Central force yields the best edge retention and
to the specimen.
specimen flatness. If the results after etching are
inadequate, the specimens must be placed back
3. Washing and Drying. The specimen is washed
in the holder and the entire preparation sequence
by swabbing with a liquid detergent solution,
must be repeated. Instead of doing this, most tech-
rinsed in warm running water, then with ethanol,
nicians will repeat the final step manually and then
and dried in a stream of warm air. Alcohol usu-
re-etch the specimen.
ally can be used for washing when the abrasive
carrier is not soluble in water or if the specimen
The second method utilizes a specimen holder
cannot tolerate water. Ultrasonic cleaning may
where the specimens are held in place loosely.
be needed if the specimens are porous or
Force is applied to each specimen by a piston,
cracked.
hence the term “individual or single force” for this
approach. This method provides convenience in
4. Cleanness. The precautions for cleanness, as
examining individual specimens during the prepa-
previously mentioned, must be strictly ob-
ration cycle, without the problem of regaining
served to avoid contamination problems. This
planarity for all specimens in the holder on the next
involves the specimen, the user’s hands, and
step. Also, if the etch results are deemed inade-
the equipment.
quate, the specimen can be replaced in the holder
to repeat the last step, as planarity is achieved in-
Automated Polishing dividually rather than collectively. The drawback to
Mechanical polishing can be automated to a high this method is that slight rocking of the specimen
degree using a wide variety of devices ranging may occur, especially if the specimen height is too
from relatively simple systems, Figure 3.11, to rather great, which degrades edge retention and flatness.
sophisticated, programmable or even touch screen
operated devices. Units also vary in capacity from a Polishing Cloths
single specimen to a half dozen or more at a time The requirements of a good polishing cloth
and can be used for all grinding and polishing include the ability to hold the abrasive media,
steps. These devices enable the operator to pre- long life, absence of any foreign material that
pare a large number of specimens per day with a may cause scratches, and absence of any pro-
higher degree of quality than hand polishing and cessing chemical (such as dye or sizing) that
at reduced consumable costs. Automatic polishing may react with the specimen. Many cloths of

20
different fabrics, weaves, or naps are available for Ultra pastes use synthetic polycrystalline diamonds.
specimen polishing. Napless or low nap cloths are Figure 3.13 shows the shape differences between
recommended for coarse polishing with diamond monocrystalline and polycrystalline diamonds.
abrasive compounds. Napless, low, medium, and oc- Studies have shown that cutting rates are higher
casionally high nap cloths are used for final polishing. for many materials using polycrystalline diamond
This step should be brief to minimize relief. Table 3.2 compared to monocrystalline diamond.
lists current polishing cloths, their characteristics and
applications. Colloidal silica was first used for polishing wafers
of single crystal silicon where all of the damage
on the wafer surface must be eliminated before a
Polishing Abrasives

GRINDING & POLISHING

device can be grown on it. The silica is amorphous
Polishing usually involves the use of one or more of and the solution has a basic pH of about ~10. The
the following abrasives: diamond, aluminum oxide silica particles are actually nearly spherical in shape,
(Al2O3), and amorphous silicon dioxide (SiO2) in
collidal suspension. For certain materials, cerium
oxide, chromium oxide, magnesium oxide or iron

Figure 3.14. Amorphous silica particles in colloidal silica (TEM,

300,000X).
a
Figure 3.14, the polishing action is slow, and is due
to both chemical and mechanical action. Dam-
age-free surfaces can be produced more easily
when using colloidal silica than with other abrasives
during final polishing. Etchants can respond differ-
ently to surfaces polished with colloidal silica. For
example, an etchant that produces a grain contrast
etch when polished with alumina may instead reveal
the grain and twin boundaries with a “flat” etch
b
Figure 3.13. Comparison of monocrystalline a) and
when polished with colloidal silica. Color etchants
polycrystalline b) synthetic diamond grain shapes (SEM, 450X). frequently respond better when colloidal silica is
used producing a more pleasing range of colors
oxide may be used, although these the late 1920s, and a crisper image. But, cleaning of the specimen
as Hoyt [7] mentions a visit to the Carboloy plant in is more difficult. For manual work, use a tuft of cot-
West Lynn, Massachusetts, where he saw sapphire ton soaked in a detergent solution. For automated
bearings being polished with diamond dust in an systems, stop adding suspension about 10-15
oil carrier. He used some of this material to pre- seconds before the cycle ends and. For the last 10
pare sintered carbides and published this work in seconds, flush the cloth surface with running water.
1930. Diamond abrasives were first introduced in Then, cleaning is simpler. Amorphous silica will crys-
a carrier paste but later aerosol and slurry forms tallize if allowed to evaporate. Crystalline silica will
were introduced. Virgin natural diamond was used scratch specimens, so this must be avoided. When
initially, and is still available as MetaDi diamond opening a bottle, clean off any crystallized particles
paste. Later, synthetic diamond was introduced, first than may have formed around the opening. The
of the monocrystalline form, similar in morphology safest approach is to filter the suspension before
to natural diamond, and then in polycrystalline use. Additives are used to minimize crystallization,
form. MetaDi II diamond pastes and MetaDi sus- as in MasterMet 2 Colloidal Silica, greatly retarding
pensions use synthetic monocrystalline diamond crystallization.
while MetaDi Supreme suspensions and MetaDi

21
GRINDING & POLISHING
process, and it produces better surface finishes than
alumina abrasives made by the traditional calcina-
For routine examinations, a fine diamond tion process. Calcined alumina abrasives always
abrasive, such as 1µm, may be adequate as the exhibit some degree of agglomeration, regardless
last preparation step. Traditionally, aqueous fine of the efforts to deagglomerate them, while sol-gel
alumina powders and suspensions, such as the alumina is free of this problem. MasterMet colloidal
MicroPolish II deagglomerated alumina powders silica suspensions (~10pH) are newer final polishing
and suspensions, have been used for final polishing abrasives that produce a combination of mechanical
with medium nap cloths. Alpha alumina (0.3µm and chemical action which is particularly beneficial
size) and gamma alumina (0.05µm size) slurries (or for difficult to prepare materials. Vibratory polish-
suspensions) are popular for final polishing, either ers, Figure 3.15, are often used for final polishing,
in sequence or singularly. MasterPrep alumina particularly with more difficult to prepare materials,
suspension utilizes alumina made by the sol-gel for image analysis studies, or for publication of

Table 3.2: Polishing Cloth Selection Guide

Recommended Abrasive
Cloth Micron Size Type Cloth Characteristics Usage Guide Applications
Hard woven, no nap
Used to replace multiple Ferrous materials and thermal
UltraPad 6μm & Up Diamond with high material
SiC grinding steps spray coatings
removal
Excellent surface finished
COARSE

Minerals, coals, ceramics,

Hard woven, used to retain flatness
UltraPol* 6μm & Up Diamond inclusion retention in steels,
nonaggressive silk cloth in medium to hard
and refractory metals
specimens
Ceramics, carbides,
Hardest perforated Used for material removal
petrographic, hard metals,
TexMet P 6μm & Up Diamond woven cloth for hign and flatness of hard
glass, and metal matrix
material removal specimens
composites
Oil resistant, medium Used to retain flatness Ferrous materials, sintered
Nylon* 6μm & Up Diamond
hard woven, no nap and hard phases carbides and cast irons
Ferrous and nonferrous
Diamond Used for harder metals, ceramics, electronic
Non-woven pressed
TexMet C 15-0.02μm AI2O3, specimens and increased packages, PCB’s, thermal spray
cloth used for durability
SiO2 flatness coatings, cast irons, cermets,
minerals, composites, plastics
Used to maximize flatness
Ferrous and nonferrous
INTERMEDIATE

Diamond Soft durable, woven and retain phases while

TriDent* 15-0.02μm metals, microelectronics,
AI2O3 synthetic, no nap provideing excellent
coatings
surface finish
Ferrous and nonferrous
Durable, medium hard Used for rough and final
VerduTex* 9-1μm Diamond metals, microelectronics,
synthetic silk cloth polishing
coatings
Shot-napped, synthetic Steel, nonferrous and soft
VelTex 9-1μm Diamond Ideal for final polishing
velvet cloth metals
Diamond
Soft and durable matted General usage for
WhiteFelt 6-0.02μm AI2O3, Ferrous and nonferrous metals
wool cloth intermediate to fine steps
SiO2
Cast iron, copper and
Medium hard, woven General usage for
PoliCloth 6-1μm Diamond aluminum alloys, coal and
wool cloth intermediate steps
other soft metals
Ferrous and nonferrous
Diamond Soft, versatile, long Most popular, general
metals, ceramics, composites,
MicroCloth 5-0.02μm AI2O3, napped synthetic rayon usage final polishing
PCBs, cast irons, cermets,
SiO2 cloth cloth
plastics, electronics
Diamond
General usage for final Ferrous and nonferrous
MicroFloc 3μm-0.02μm AI2O3, Soft, long napped cloth
polishing materials
SiO2
FINE

AI2O3, Soft synthetic velvet Soft nonferrous and

MasterTex 1-0.05μm Softer final polishing cloth
SiO2 with low nap microelectronic packages
General usage pad that
Titanium, stainless steel,
removes smear metal
AI2O3, Soft, porous, chemically lead/tin, solders, electronic
ChemoMet 1-0.02μm from tough materials
SiO2 resistant, synthetic cloth packages, soft nonferrous
during chemomechanical
metals, plastics
polishing
* Interchangable in many of the following methods

22
quality work. in this book including final polishing. High quality
sample preparation is a basic starting point for this
technique. As already explained above, vibratory
polishing is dedicated to fine diamond or oxide
Vibratory Polishing suspensions typically between 1 and 0.02 microns.

Similarly to electro-polishing, vibratory polishing

provides excellent surface finish without deforma-
tion and with minimal difficulty. The advantage of
vibratory polishing over electro-polishing, however,
is that it requires no hazardous chemicals and is suit-

GRINDING & POLISHING

ed to any material or mix of materials. The VibroMet
2 polisher generates a high frequency, variable
amplitude vibrational motion, which is almost 100%
horizontal without vertical movement. The sample

Figure 3.16. Kikuchi lines obtained by EBSD analysis

Figure 3.15. VibroMet 2 Vibratory Polisher

is polished stress-free. After a few minutes to a few

Figure 3.17. Lead alloy prepared by vibratory polishing.
hours with no further intervention, samples are
polished with excellent surface finish and sharply
defined edges.

Polishing is typically carried out with fine diamond

slurries or suspensions of oxides such as MasterMet,
MasterPrep or MicroPolish. Vibratory polishing is
particularly suitable for the preparation of sensitive
or ductile materials. Samples polished using this
technique are particularly suitable for high precision
analysis techniques such as electron back-scatter Figure 3.18. Vibratory polished ferritic steel, Electron image
detection (EBSD) or nano-indentation hardness overlayed with orientation map normal direction Phase: α - Iron.

testing. Such techniques are highly sensitive to small

amounts of surface deformation, which often cannot Table 3.3: Band Contrast (0 - 255)
be directly observed using standard preparation Material Standard Polishing Vibratory Polishing
techniques. The Table 3.3 shows the improvement Mg 161.2 172.25 (+8.7%)
of diffraction band contrast due to a Vibratory pol- Si-Monocristal 205.75 233.0 (+13.2%)
ishing step. Figure 3.16 shows a vibratory polished Ti 134.0 146.6 (+9.1%)
ferritic steel.
Ni 85.0 102.8 (+20.9%)
Nb 145.6 151.2 (+3.8%)
Preparation Methodology Pb No Pattern 108.0
Before vibratory polishing, the samples must be
properly prepared using the methods described As a recommendation, use the same polishing sus-

23
GRINDING & POLISHING
as this depends on many factors. One of the main
factors is the amplitude strength, which is adjust-
able on the unit. This value changes the strength
or intensity of the vibrations, which has a direct
impact on the polishing time. In the case of new or
unknown materials, the times can be determined
empirically. Typically, if the polishing conditions
are correct, a significant improvement can be seen
in less than 30 minutes of vibratory polishing. The
Figure 3.19. Sample preparation with their own weight. samples can then be examined under a light mi-
croscope or with a scanning electron microscope.
If the polishing quality is not sufficiently improved,
you can repeat the polishing cycle, or amend the
polishing conditions.

Electrolytic Polishing and Etching

Electrolytic polishing or etching is achieved by
the completion of an electrical circuit through an
electrolyte. The specimen is set as the anode in the
Figure 3.20. Preparation with sample holder and adding circuit. The application of current drives an oxidizing
weight.
chemical reaction at the anode to achieve disso-
pension as in the final stage of the standard lution of the metal at the surface of the specimen
where it is in contact with the electrolyte.

The conditions under which such reactions occur

mechanical preparation method. If the process uses
can significantly affect the outcome of the reaction.
a chemical additive such as hydrogen peroxide or
These include:
other etchants, the addition will be optional on the
VibroMet 2. Vibratory polishing is typically carried • Current density (related to the area to be pol-
out without any additional chemical additives. The ished)
suspension should be sufficiently dispersed on the
polishing cloth, and when using oxide suspensions • Voltage
particular care should be taken to ensure that the
polishing cloth remains well moistened throughout • Time
the polishing cycle. If this is not done, then some
polishing suspensions can crystallize. A popular • Electrolyte composition, viscosity and tem-
compound for vibratory polishing is MasterMet 2 – a perature
0.02µm colloidal silica suspension that contains an
additive to prevent crystallization. • Electrolyte movement (“refreshing” the electro-
lyte in the area of the reaction)
The polishing cloth should be a flocked or napped
cloth (such as MicroFloc, MicroCloth, MasterTex or Figure 3.21 is a schematic diagram showing the
VelTex), as the fibres in such cloths ease sample relationship between current density and voltage in
movement on the platen and help ensure a uniform such a polishing cell. At low voltages, rapid disso-
polishing result. lution of the metal will result in etching, as different
areas of the material are removed at different rates.
Sample pressure is applied by the weight of the
sample itself or by the addition of extra weights. If the voltage is increased, passivation processes
The samples must be sufficiently rigid and typically change the nature of the reaction and a polishing
should have a minimum total mass of 4 N [0.4 kg]. effect occurs. In this case, peaks on the surface
If the weight is too low, the samples could corrode dissolve preferentially, microscopically smoothing
or tarnish during the polishing. the surface. As this is purely a chemical effect, there
is no associated mechanical damage from this pro-
There is no fixed rule for vibratory polishing time, cess. As such, electrolytically polished surfaces are

24
particularly useful for surface sensitive tests where
even small amounts of surface deformation are
unacceptable.

Figure 3.22. Electro polished ferritic steel examined with

GRINDING & POLISHING

EBSD [Electron image overlayed with orientation map normal
direction Phase: α - Iron

Figure 3.21. Influence of current density and voltage on the

sample. The optimum area for polishing is shaded. At low Figure 3.23. Aluminum as cast condition with colored dendrites
voltages, the sample is etched. Excessive voltage creates voids in revealed by anodizing with Barker’s reagent 40V for 460
the electrolyte and a pitting effect will occur due to the irregular seconds (polarized light, 25X)
density.

If the voltage is increased further, the passivation be generated during the process.
layer breaks down and oxygen is evolved, resulting
in pitting at the surface of the specimen. One of the common chemicals used in electrolytic
polishing is perchloric acid, which can become
Electrolytic polishing and etching processes can be unstable at higher temperatures (>100°F [38°C])
quick and effective, and highly reproducible when or higher concentrations or if higher concentrations
correctly performed. Historically, most applications occur due to excessive evaporation. Avoid the use
for electrolytic polishing in metallography have
been in process inspection of materials that are
difficult to polish and etch with chemical etchants,
such as superalloys and stainless steel – although
soft materials are also ideal candidates, as mechani-
cal polishing to a high standard can be difficult. The
process has seen particular growth in metallography
during recent years due to the increasing require-
ments for crystallographic analyses such as EBSD
and surface characterization tests such as nano-in-
dentation hardness testing, both of which require
a deformation free surface to attain the best results.

Optimizing the reproducibility of electrolytic pol- Figure 3.24. The electrolyte is conveyed by a circulation pump
between the cathode (-) and the sample (+). By the uniform flow
ishing and etching processes requires good control of the electrolyte the material debris will flushed away and the
sample is uniform wetted. An integrated cooling ensures that
of the conditions. This is most readily achieved by
the electrolyte does not get too warm.
using dedicated equipment, consisting of a good
quality power supply unit and a polishing or etch- of perchloric acid in contact with organic materials,
ing cell that effectively controls the movement of such as mounting media, as unstable perchlorates
the electrolyte as well as the area of the specimen. can form and accumulate in the electrolyte.
Figure 3.24 shows a such cell. It is recommended
to use equipment that has integrated temperature
control and cooling of the electrolyte, as heat can

25
GRINDING & POLISHING
zirconium alloys.
HELPFUL HINTS
FOR GRINDING/POLISHING
Typical sequence for electropolishing of ferritic Specimens that contain cracks or pores
material: that are not filled with epoxy may require
ultrasonic cleaning to remove abrasive and
• Step1: Grinding with 400 grit [P800] and 600
debris from the pores or cracks to avoid
grit [P1200] SiC-Paper on grinding machine
contaminating the next step.
(each 60s.)
Excessive ultrasonic cleaning vibrations can
• Step 2: Electrolytic polishing on electro polish- damage the structure of certain soft metals
ing system ElectroMet 4 (Figure 3.25), at 30Vdc and alloys, particularly precious metals.
for 60 seconds
To remove a tightly adhering cloth, soak
Sometimes, electro polished surfaces are wavy and under hot water for a few minutes. Or apply
this will cause a problem at higher magnifications. release agent to the platen before applying
Electropolishing will tend to round edges or pores a new cloth.
and wash out non-metallic inclusions. Two or more
phase alloys are more difficult to polish, because the
phases will preferentially attacked. Consequently,

Figure 3.25. ElectroMet 4 Electrolytic Etcher/Polisher

electrolytic polishing is not recommended for

failure analysis, but can be used for a few seconds
as a final polishing step to remove the last existing
deformation.

Anodizing
The process of anodizing is related to electrolytic
polishing and etching, in that the specimen is set
as the anode within the electrical circuit. However,
in this case the purpose is to grow an oxide layer
on the surface. The oxide layer, when viewed under
polarized light, will cause interference effects that
can introduce contrast and colour between phases
or crystallographic orientations. This is a particularly
common process for aluminium alloys, but has also
been used on other materials such as titanium and

26
EXAMPLES OF PREPARATION PROCEDURES

The “Traditional” Method Times and pressures could be

varied, as well, to suit the needs of the work, or
Over the past forty years, a general procedure has
the material being prepared. This is the “art”
been developed that is quite successful for prepar-
of materials preparation.
ing most metals and alloys. This method is based
on grinding with silicon carbide waterproof papers
through a series of decreasing abrasive sizes, then Contemporary Methods
rough polishing with one or more diamond abrasive New concepts and preparation materials have been
sizes, followed by fine polishing with one or more introduced that enable technicians to shorten the
alumina suspensions of different particle size. This process while producing better, more consistent
procedure will be called the “traditional” method, results. Much of this effort has centered upon
and is described in Table 4.1. reducing or eliminating the use of silicon carbide
paper in the grinding steps. In all cases, an initial
This procedure is used for manual or automat-
grinding step must be used, but there are a wide
ed preparation, although manual control of the
range of materials that can be chosen instead of
force applied to a specimen would not be as
SiC paper. There is nothing wrong with the use of
consistent. Complementary motion means that
SiC for the first step, except that it has a short life. If
the specimen holder is rotated in the same direc-
an automated device is used that holds a number
tion as the platen, and does not apply to manual
of specimens rigidly (central force), then the first
preparation. Some machines can be set so that
step must remove the sectioning damage on each
the specimen holder rotates in the direction op-
specimen and bring all of the specimens in the

FULL LAB & SOLUTIONS

posite to that of the platen, called “contra.” This
holder to a common plane. The first step is often
provides a more aggressive action but was not
called “planar grinding”. SiC paper is most often
part of the “traditional” approach when automat-
used for this step although more than one sheet
ed. The traditional method is not fixed, as it can
may be needed according to the surface area to
be modified by substitution or the ommission of
be planed down and how much material needs to
one or more of the polishing steps.
be ground back. If it is such that more than a few

Table 4.1: The Traditional Procedure for Preparing Most Metals and Alloys
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

120 [P120] grit SiC

CarbiMet 6 [27] 240-300 Until Plane
water cooled

220 [P240] or 240

CarbiMet [P280] grit SiC water 6 [27] 240-300 1:00
cooled

320 [P400] grit SiC

CarbiMet 6 [27] 240-300 1:00
water cooled

400 [P600] grit SiC

CarbiMet 6 [27] 240-300 1:00
water cooled

600 [P1200] grit SiC

CarbiMet 6 [27] 240-300 1:00
water cooled

6μm MetaDi Diamond

Canvas Cloth Paste with MetaDi Fluid 6 [27] 120-150 2:00
Extender
1μm MetaDi Diamond
Billiard or Felt
Paste with MetaDi Fluid 6 [27] 120-150 2:00
cloths
Extender
Aqueous 0.3μm
MicroCloth α – alumina MicroPolish 6 [27] 120-150 2:00
slurry
Aqueous 0.05μm
MicroCloth γ – alumina MicroPolish 6 [27] 120-150 2:00
slurry

= Platen = Specimen Holder

27
EXAMPLES OF PREPARATION PROCEDURES
sheets of SiC paper are needed, then the use of a Contra rotation, where the polishing head moves
more aggressive and more durable surface such as in the direction opposite to the platen, is preferred
ZirMet paper or diamond grinding discs (Apex or as the abrasive suspension stays on the cloth bet-
UltraPrep Diamond Discs) may be used. With this ter, although this will not work if the head rotates
huge array of products to choose from, how can the at a high rpm. Examples of generic contemporary
lab technician decide what to use? Each of these preparation practices follow in Tables 4.2 – 4.4.
products has advantages and disadvantages, and Specific procedures for a wide range of materials
this is only the first step. are given in the next section.

One or more steps using diamond abrasives on The starting SiC abrasive size is chosen based upon
napless surfaces usually follow planar grinding. the degree of surface roughness and depth of
PSA-backed silk, nylon or polyester cloths are wide- cutting damage and the hardness of the material.
ly used. These give good cutting rates, maintain Never start with a coarser abrasive than necessary
flatness and minimize relief. Silk cloths, such as the to remove the cutting damage and achieve planar
UltraPol cloth, provide the best flatness and excel- conditions in a reasonable time.
lent surface finishes relative to the diamond size
used. UltraPad cloth, a thicker, hard, woven cloth, A similar scheme can be developed using
is more aggressive, gives nearly as good a surface rigid grinding discs, such as the Apex Hercules H
finish, similar excellent flatness, and longer life than Disc. These discs are generally restricted to ma-
an UltraPol cloth. Synthetic chemotextile surfaces, terials above a certain hardness, such as 175 HV,
such as TexMet C, give excellent flatness and are although some softer materials can be prepared
more aggressive than silk. They are excellent for using them. This disc can also be used for the pla-
retaining second phase particles and inclusions. nar grinding step. An example of such a practice,
Diamond suspensions are most popular with auto- applicable to nearly all steels (results are marginal
mated polishers as they can be added easily during for solution annealed austenitic stainless steels) is
polishing; although it is still best to charge the cloth given in Table 4.3.
initially with diamond paste of the same size to get
polishing started quickly. Final polishing could be Th e p l a n a r g r i n d i n g s t e p c o u l d a l s o b e
performed with a very fine diamond size, such as performed using a 45µm metal bonded, or a
0.1µm diamond, depending upon the material, your 30µm resin bonded, UltraPrep disc or with the
needs and personal preferences. Otherwise, final Apex Hercules H rigid grinding disc and 15 or
polishing is performed with MasterMet colloidal 30µm diamond, depending upon the material. Rigid
silica or with MicroPolish or MasterPrep alumina grinding discs contain no abrasive; they must be
suspensions using napless, or low to medium nap charged during use and suspensions are the easiest
cloths. For some materials, such as titanium and zir- way to do this. Polycrystalline diamond suspensions
conium alloys, an attack polishing solution is added are favored over monocrystalline synthetic diamond
to the slurry to enhance deformation and scratch suspensions for most metals and alloys due to their
removal and improve polarized light response. higher cutting rate.

Table 4.2: Generic Contemporary Preparation Procedure for Many Metals and Alloys
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]
120 [P120] to 240
CarbiMet [P280] grit SiC water 6 [27] 300 Until Plane
cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 4:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 6 [27] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *MetaDi Fluid Extender as desired

28
EXAMPLES OF PREPARATION PROCEDURES

The Apex Hercules S rigid grinding disc, designed

for soft metals and alloys, is used in a similar man-
ner. This disc is quite versatile and can be used to
prepare harder materials as well, although its wear
rate will be greater than the H disc when used to
prepare very hard materials. A generic four step
practice is given below for soft metals and alloys.

The planar grinding step can be performed with

the 30µm resin bonded diamond disc, or with
a second Apex Hercules S disc and 15 or
30µm diamond, depending upon the metal or
alloy. For some very difficult metals and alloys,
a 1µm diamond step on a TriDent cloth (similar to
step 3, but for 3 minutes) could be added, and/or
a brief vibratory polish (use the same cloths and
abrasives as for step 4) may be needed to produce
perfect publication quality images. Four steps may
suffice for routine work.

FULL LAB & SOLUTIONS

Table 4.3: 4-Step Contemporary Procedure for Steels Using a Rigid Grinding Disc
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]
120 [P120] to 320
CarbiMet [P400] grit SiC water 6 [27] 300 Until Plane
cooled

9μm MetaDi Supreme

Apex Hercules H 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 4:00
Diamond*

0.05μm MasterPrep
ChemoMet 6 [27] 150 2:00
Alumina

= Platen = Specimen Holder *MetaDi Fluid Extender as desired

Table 4.4: 4-Step Contemporary Procedure for Nonferrous Metals Using a Rigid Grinding Disc
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]
220 [P280] to 320
CarbiMet [P400] grit SiC water 5 [22] 300 Until Plane
cooled

6μm MetaDi Supreme

Apex Hercules S 5 [22] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 5 [22] 150 4:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 5 [22] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *MetaDi Fluid Extender as desired

29
PROCEDURES FOR SPECIFIC MATERIALS
Following are our recommendations for preparing mounts in a central-force holder to obtain a prop-
a wide range of materials arranged, in the case of er weight balance, but, two specimens could be
metals, according to common characteristics, ba- dummy mounts (mounts without specimens). In
sically in accordance with their classification in the general, as the area of the specimen in the mount
periodic table of the elements. This break down increases, as the diameter and the number of
is further modified, especially in the case of iron specimens increases, the time and pressure must
based alloys, as required due to the wide range of increase to obtain the same degree of preparation
properties that can be experienced. perfection.

The elements shown in Figure 5.1 categorizes If the area of the mounts is used, rather than the
metallic, nonmetallic and metalloid elements area of the embedded specimens, and we as-
according to similarities in atomic structure and is sume that we are preparing six 1in [25mm], six
a good starting point, aided by similarities in phys- 1.25in [32mm] or three 1.5in [38mm] diameter
ical properties and behavior, for grouping ele- specimens, then we can adjust the pressures rel-
ments and their alloys that have reasonably similar ative to the standard values in the tables (for six
preparation procedures. 1.25in [32mm] diameter specimens) using an 8in
[203mm] diameter platen format machine. A com-
Of course, technicians prepare materials oth- parison of the cross-sectional areas would suggest
er than metals. These have been grouped and that for the six 1in [25mm] specimens, the pres-
sub-divided according to the nature of these ma- sures could be reduced to 65% of the standard
terials, as follows: values while for three 1.5in [38mm] diameter spec-
imens, the pressures and times could be reduced
• Sintered Carbides to about 70% of the standard values.
• Ceramics
• Composites: Metal Matrix, Polymer Matrix and Changing the platen diameter increases the dis-
Ceramic Matrix tance that the specimens travel in a given time. For
• Printed Wiring Boards example, for the same rpm values, specimens trav-
• Electronic Materials el 1.25 and 1.5 times as far using a 10 or 12in [254
• Plastics and Polymers or 305mm] diameter platen, respectively, com-
pared to an 8in [203mm] platen. This suggests that
The procedures discussed in this book were devel- the times could be reduced to 80 or 67% of that
oped and tested extensively using machines with used for the 8in [203mm] diameter platen when
an 8in [203mm] diameter platen with six 1.25in using 10 or 12in [254 or 305mm] diameter plat-
[32mm] diameter specimens in a 5in [127mm] di- ens. While preparation times may be shorter using
ameter holder. These procedures produced the a larger format machine, consumable cost is great-
same results when the specimens were prepared er and larger machines are needed only when the
using a 10in [254mm] or a 12in [305mm] diam- specimen throughput needs are very high or with
eter platen. When using the 8in [203mm] platen large specimens.
and a 5in [127mm] diameter specimen holder, the
machine’s head position was adjusted so that the
specimens rotate out over the outer periphery of
the surface of the platen. This procedure makes
maximum use of the working surface and im-
proves edge retention. This alignment practice is
less critical with the larger diameter platens when
using the same diameter holder. However, if the
7in [178mm] diameter specimen holder is used
with the 12in [305mm] diameter platen, the head
position should be adjusted so that the specimens
rotate out over the platen’s edge.

In general, it is difficult to make accurate predic-

tions about variations in time and load when using
different format platens and mount sizes. Different
mount sizes per se should not be used as the basis
for calculations as the area of the specimens within
the mount is more important than the mount area
itself. For example, the same specimen cross sec-
tional area could be present in 1, 1.25 or 1.5in [25,
32 or 38mm] diameter polymer mounts. Further,
the number of specimens in the holder can vary
substantially. It is necessary to put at least three

30
PROCEDURES FOR SPECIFIC MATERIALS

Light Metals
13 12 4

Al
Aluminium
Mg
Magnesium
Be
Beryllium

Low Melting Point Alloys

30 48 50 51 82 83

Zn Zinc
Cd
Cadmium
Sn Tin
Sb
Antimony
PbLead
Bi
Bismuth

Refractory Metals
22 40 72 23 24 41 42 73

Ti
Titanium
Zr
Zirconium
Hf
Hafnium
V
Vanadium
Cr
Chromium
Nb
Niobium
Mo
Molybdenum
Ta
Tantalum

74 75

FULL LAB & SOLUTIONS

W
Tungsten
Re
Rhenium

Ferrous Metals Copper, Nickel, and Cobalt

26 29 28 27

FeIron
Cu
Copper
Ni
Nickel
Co
Cobalt

Precious Metals
44 45 46 47 76 77 78 79

Ru
Ruthenium
Rh
Rhodium
Pd
Palladium
AgSilver
Os
Osmium
Ir
Iridium
Pt
Platinum
AuGold

Other Material Groups

Thermal Sintered Ceramics Minerals Composites Electronic Printed Polymers

TSCSpray SC
Carbides
C M CM EM
Materials
PWB
Wiring
P
Coatings Boards

Figure 5.1. Providing a recommendation for preparing a specific material is fairly straight-forward for the grinding-polishing procedure.
However, there are many more variables to be considered when making recommendations for the other 4 segments of preparation. In the
following chapters, you will find additional information on each material for sectioning, mounting, imaging & analysis and hardness testing.
The recommendations are based on best practices for the most typical situation.

31
Light

LM
Metals LIGHT METALS
LIGHT METALS: Al, Mg and Be may be needed to completely remove any trace of
damage or scratches. The five-step practice is rec-
ommended for super pure (SP) and commercially
13
13

Al
Aluminium
Aluminiu m
pure (CP) aluminum and for wrought alloys that are
difficult to prepare.

Aluminum Either 240 [P280] or 320 [P400] grit SiC waterproof

paper may also be used for the planar grinding
Aluminum is a soft, ductile metal. Deformation in-
step. An UltraPol cloth produces better surface
duced damage is a common preparation problem
finishes than an UltraPad cloth, but the UltraPad
in the purer compositions. After preparation, the
cloth has a longer useful life. A ChemoMet cloth
surface will form a tight protective oxide layer that
is recommended when edge retention is critical.
makes etching difficult. Commercial grades contain
Pure aluminum and some alloys are susceptible
many discrete intermetallic particles with a variety
to embedment of fine diamond abrasive particles,
of compositions. These intermetallic particles are
especially when suspensions are used. If this occurs,
usually attacked by etchants before the matrix.
switch to diamond in paste form, which is much less
Although the response to specific etchants has
likely to cause embedding. SP and CP aluminum
been used for many years to identify these phases,
can be given a brief vibratory polish (same products
this procedure requires careful control. Today, en-
as last step) to improve scratch control, although
ergy-dispersive analysis is commonly performed
for phase identification due to its greater reliability.

Five and four-step practices for aluminum alloys are

presented in Table 6.1 and 6.2 with expected results
as in Figure 6.1. While MgO was the preferred final
polishing abrasive for aluminum and its alloys, it is
a difficult abrasive to use and is not available in very
fine sizes. Colloidal silica has replaced magnesia as
the preferred abrasive for the final step and is finer
in size. For color etching work, and for the most Figure 6.1. Dendritic segregation in as cast 206 aluminum
revealed by color etching with Weck’s reagent (polarized light,
difficult grades of aluminum, a brief vibratory polish 200X).

Table 6.1: 5-Step Method for Soft Aluminum Alloys

Sectioning Abrasive Cutter with a wheel recommended for use on non-ferrous materials
Mounting Compression or Castable, typically with PhenoCure, EpoxiCure, EpoThin or SamplKwick
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 5 [22] 300 Until Plane
water cooled

9μm MetaDi Supreme

TexMet C 5 [22] 150 5:00
Diamond*

TexMet C 3μm MetaDi Paste* 5 [22] 150 4:00

TexMet C 1μm MetaDi Paste* 5 [22] 150 2:00

0.06μm MasterMet
ChemoMet 5 [22] 150 1:30
Colloidal Silica

= Platen = Specimen Holder *MetaDi Fluid Extender as desired

Imaging & Analysis Dendritic spacing, Porosity Assessment, Grain Size (depending on the type of aluminum and its processing)

Hardness Testing Vickers, Knoop

32
this is generally not required. MasterPrep alumina
suspension has been found to be highly effective
as a final polishing abrasive for aluminum alloys,
however, the standard alumina abrasives made by
the calcination process are unsuitable for aluminum.

For many aluminum alloys, excellent results can

be obtained using a four step procedure, such as
shown below in Table 6.2 with expected results as
shown in Figure 6.2. This procedure retains all of
Figure 6.2. Deformed, elongated grain structure of extruded
the intermetallic precipitates observed in aluminum 6061-F aluminum after shearing revealed by anodizing with
and its alloys and minimizes relief. Synthetic napless Barker’s reagent (polarized light, 100X).

cloths may be used for the final step with colloidal

silica and they will introduce less relief than a low
or medium nap cloth, but may not remove fine
polishing scratches as well. For very pure aluminum HELPFUL HINTS
alloys, this procedure could be followed by vibratory FOR ALUMINUM
polishing to improve the surface finish, as these are
quite difficult to prepare totally free of fine polishing Many low-alloy aluminum specimens
scratches. are difficult to polish to a perfect finish
using standard methods. A vibratory pol-
isher can be used quite effectively with

LIGHT METALS
MasterMet colloidal silica to produce
deformation-free, scratch-free surfaces for
anodizing or color etching and examination
with polarized light or Nomarski DIC.

Table 6.2: 4-Step Method for Aluminum Alloys

Sectioning Abrasive Cutter with a wheel recommended for use on non-ferrous materials
Mounting Compression or Castable, typically with PhenoCure, EpoxiCure, EpoThin or SamplKwick
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 5 [22] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 5 [22] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 5 [22] 150 4:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 5 [22] 150 1:30
Met Colloidal Silica

= Platen = Specimen Holder *MetaDi Fluid Extender as desired

Imaging & Analysis Dendritic spacing, Porosity Assessment, Grain Size (depending on the type of aluminum and its processing)

Hardness Testing Vickers, Knoop

33
Light

LM
Metals LIGHT METALS
12
12 coolant, as fine Mg dust is a fire hazard. Because of
Mg the presence of hard intermetallic phases, relief may
Magnesiu
Magnesiumm be difficult to control, especially if napped cloths
are used. Following is a five-step procedure for
Magnesium magnesium and its alloys, see Table 6.3.
Preparation of magnesium and its alloys is rather
difficult due to the low matrix hardness and the MasterPolish is nearly water-free and yields excellent
higher hardness of precipitate phases that lead to results as the final abrasive (Figures 6.3 - 6.4). After
relief problems, and from the reactivity of the met- the last step, wash the specimens with ethanol.
al. Mechanical twinning may result during cutting, Cleaning after the last step, without using water, is
grinding, or handling if pressures are excessive. difficult. Holding the specimen under running water
Final polishing and cleaning operations should for about a second eased the cleaning problem
avoid or minimize the use of water and a variety of and did not appear to harm the microstructure.
solutions have been proposed. Pure magnesium is Cosmetic cotton puffs can scratch the surface when
attacked slowly by water while Mg alloys may exhibit swab etching. For best results, etch-polish-etch
much higher attack rates. Some authors state that cycle may be needed. Magnesium has a hexagonal
water should not be used in any step and they use close-packed crystal structure and will respond
a 1 to 3 mixture of glycerol to ethanol as the cool- to polarized light. To enhance the response, use
ant even in the grinding steps. Always grind with a a brief vibratory polish with the materials used in
the last step.

HELPFUL HINTS
FOR LIGHT METALS

For polishing, apply diamond paste and

use lapping oil, or use oil-based MetaDi
diamond suspension, available down to
a 0.05µm size, with a medium nap cloth.
Figure 6.3. Mechanical twinning in deformed high-purity
magnesium (99.8% Mg) (acetic-picral etch, crossed polarized
light plus sensitive tint, 50X).

Table 6.3: 5-Step Method for Magnesium Alloys

Precision saw, with no water and a 15HC blade recommended for use onMetal Matrix Composites, PCBs,
Sectioning
Bone, TI, TSC
Mounting Castable, typically with PhenoCure, EpoxiCure, EpoThin or SamplKwick
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC*

CarbiMet 3 [13] 300 Until Plane
water cooled

9μm MetaDi Oil-based

TexMet C 3 [13] 150 6:00
Diamond

3μm MetaDi Oil-based

TexMet C 3 [13] 150 5:00
Diamond

1μm MetaDi Oil-based

TexMet C 3 [13] 150 4:00
Diamond

ChemoMet 0.05μm MasterPolish 4 [18] 150 1:30

= Platen = Specimen Holder *SiC surfaces were coated with wax to minimize embedment

Imaging & Analysis Dendritic spacing, Porosity Assessment, Grain Size

Hardness Testing Brinell

34
For the final step, mix hydrogen peroxide (30%
concentration – avoid physical contact!) with the
MasterMet colloidal silica in a ratio of one part hy-
drogen peroxide to five parts colloidal silica. Oxalic
acid solutions (5% concentration) have also been
used with alumina for attack polishing. For optimal
polarized light response, follow this with vibratory
polishing using a one-to-ten ratio of hydrogen
Figure 6.4. As-cast microstructure of a magnesium alloy with peroxide to colloidal silica.
2.5% of rare earth elements, 2.11% Zn and 0.64% Zr showing
a film of the rare earth elements in the grain boundaries, alloy
segregation within grains (“coring” revealed by color variations
within grains) and a few mechanical twins in the grains (acetic-
picral etch, crossed polarized light plus sensitive tint, 100X).

Be
Berylliu
Berylliumm

Beryllium
Beryllium is also a difficult metal to prepare and
presents a health risk to the metallographer. Only
those familiar with the toxicology of Be, and are
Figure 6.5. Grain structure of wrought, P/M beryllium (unetched,
properly equipped to deal with these issues, should

LIGHT METALS
cross-polarized light, 100X).
work with the metal. The grinding dust is extremely
toxic. Wet cutting prevents air contamination but the
HELPFUL HINTS
grit must be disposed of properly. As with Mg, Be
is easily damaged in cutting and grinding forming
FOR LIGHT METALS
mechanical twins. Light pressures are required.
Although some authors claim that water cannot Small diamond abrasive sizes are prone to
be used, even when grinding Be, others report no embedment when applied as a suspension
difficulties using water. Attack-polishing agents or by spraying. Charge the cloth using
are frequently used when preparing Be and many diamond paste to eliminate embedding.
are recommended [2]. Table 6.4 shows a four-step Another technique is to use both a fine
practice for beryllium with expected results as diamond paste and MasterPrep alumina
shown in Figure 6.5. suspension – simultaneously – to prevent
embedding.
Table 6.4: 4-Step Method for Beryllium

Precision saw, with no water and a 15HC blade recommended for use onMetal Matrix Composites, PCBs,
Sectioning
Bone, TI, TSC
Mounting Castable, typically with PhenoCure, EpoxiCure, EpoThin or SamplKwick
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 4 [18] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 4 [18] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 4 [18] 150 4:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 3 [13] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *MetaDi Fluid Extender as desired

Imaging & Analysis Dendritic spacing, Porosity Assessment, Grain Size

Hardness Testing Brinell

35
Low
LMP
Melting
Melting
Point
LOW MELTING POINT METALS
LOW-MELTING POINT METALS:
Sb, Bi, Cd, Pb, Sn and Zn
30 48
48 50

Zn Zinc
Cd
Cadmiu m
Cadmium
SnTin

51 82 83
83

Sb
Antimony
PbLead
Bi
Bismut
Bismuthh a

As pure metals, antimony, bismuth, cadmium, lead,

tin, and zinc are all very soft and difficult to prepare.
Pure antimony is quite brittle, but alloys containing
Sb are more common, see Figure 7.1. Bismuth is
a soft metal, but brittle, and not difficult to pre-
pare. However, retaining bismuth particles in free
machining steels is difficult. Cadmium and zinc,
both with hexagonal close-packed crystal struc-
tures, are quite prone to mechanical twin forma-
tion if sectioning or grinding is performed too b
aggressively (Figure 7.2). Zinc is harder than tin Figure 7.2. a) Cadmium dendrites and a Cd-Bi eutectic in an
or lead and tends to be brittle. Zinc is widely used as-cast Cd – 20% Bi alloy (unetched, crossed polarized light
plus sensitive tint, 50X). b) As-cast microstructure of Zn – 0.1%
to coat sheet steel (galvanized steel) for corrosion Ti – 0.2% Cu alloy exhibiting mechanical twins and a three-
protection, and is a common metallographic sub- phase eutectic (alpha-Zn, Cu-Zn and Zn15Ti) in a cellular pattern
ject. Pure zinc is very difficult to prepare. Lead is (Palmerton reagent, crossed polarized light plus sensitive tint,
very soft and ductile and pure specimens are ex- 200X).

tremely difficult to prepare; however, lead alloys

are considerably easier. Tin, which is allotropic Many authors have recommended coating the SiC
with a body-centered tetragonal crystal structure paper surface with bees wax, but this does not
at room temperature, is soft and malleable and solve the problem. Paraffin (candle wax) is much
less sensitive to twinning. Pure tin, like pure lead, better for reducing embedding. Embedding is
is very difficult to prepare. Due to their low melt- most common with the finer grit size papers. Di-
ing points, and low recrystallization temperatures, amond is not a very effective abrasive with these
metals. Alumina works quite well. Following is a
procedure for these alloys, see Table 7.1.

For best results, follow this with a vibratory polish

using MasterMet colloidal silica on MicroCloth
pad for times up to 1-2 hours. This will improve po-
larized light response for the hcp Cd and Zn and
the rhombohedral Bi. The 1µm alumina step will
remove any embedded silicon carbide particles
much more effectively than a diamond abrasive
step.
Figure 7.1. Proeutectic dendrites of Cu2Sb surrounded by a
eutectic mixture of antimony and Cu2Sb, in an as-cast Sb – 30%
Cu specimen (unetched, polarized light, 200X).

cold setting resins are usually recommended as re-

crystallization may occur during hot compression
mounting. Some of these metals in the pure, or
nearly pure form, will deform under the pressures
used in compression mounting. Alloys of these
metals are easier to prepare, as they are usual-
ly higher in hardness. Heating of surfaces during
grinding must be minimized. Grinding of these
metals is always difficult, as SiC particles tend to
embed heavily.

36
Table 7.1: 6-Step Method for Low-Melting Temperature Alloys

Sectioning Precision saw, with a 30HC blade recommended for use on soft gummy materials
Mounting Castable, typically with EpoThin
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]
320 [P400] grit SiC
CarbiMet water cooled 4 [18] 150 Until Plane
(wax coated)*
400 [P800] grit SiC
CarbiMet water cooled 4 [18] 150 1:00
(wax coated)*
600 [P1200] grit SiC
CarbiMet water cooled 4 [18] 150 1:00
(wax coated)*
1200 [P2500] grit SiC
CarbiMet water cooled 4 [18] 150 1:00
(wax coated)*

1μm MicroPolish II
MicroFloc 5 [22] 150 5:00
Alumina

0.05μm MasterPrep
MicroFloc 4 [18] 150 4:00
Alumina**

LOW MELTING OINT METALS

= Platen = Specimen Holder

*Rub candle was lightly across rotating disc prior to grinding **See vibratory polish recommendation in text

Imaging & Analysis Grain Size, Measurement & Analysis applications

Hardness Testing N/A

HELPFUL HINTS FOR

LOW-MELTING POINT METALS

Embedment of fine abrasive particles is a

common problem when preparing soft,
low-melting point specimens. To reduce
embedment of SiC abrasive particles, coat
the paper with wax before grinding. John-
son [47] showed that candle wax is far more
effective than paraffin. However, if the layer
is applied too thickly, the metal-removal
rate in grinding will be reduced drastically.

37
Refractory

RMMetals REFRACTORY METALS

REFRACTORY METALS: Ti, Zr, Hf, must be mounted in a castable resin with a very
low exotherm (long curing times favor lower heat
Cr, Mo, Nb, Re, Ta, V and W
generation, and vice versa). Titanium is very difficult
22
to section and has low grinding and polishing rates.
Ti
Titanium
The following practice for titanium and its alloys
demonstrates the use of an attack-polishing agent
Titanium added to the final polishing abrasive to obtain
Pure titanium is soft and ductile, but is very easily the best results, especially for commercially pure
damaged by twinning in sectioning and grinding. titanium, a rather difficult metal to prepare free of
Preparation of commercially pure titanium, which is deformation for color etching, heat tinting and/or
a popular grade, is very difficult, while preparation polarized light examination of the grain structure.
of the alloys is somewhat easier. Some authors have Attack polishing solutions added to the abrasive
stated that titanium alloys should not be mounted slurry or suspension must be treated with great care
in phenolic resins as the alloys can absorb hydro- to avoid burns. Use good, safe laboratory practices
gen from the resin. Further, it is possible that the and it is advisable to wear protective gloves. This
heat from mounting could cause hydrides to go three step practice could be modified to four steps
into solution. This is also possible with castable by adding a 3 or 1µm diamond step, but this is usu-
resins if the exothermic reaction of polymerization ally unnecessary, see Table 7.1 and Figures 8.1 – 8.1
generates excessive heat. If the hydride phase for expected results.
content is a subject of interest, then the specimens
A number of attack polishing agents have been

Figure 8.1. Alpha at the surface of heat treated (1038 ºC, water Figure 8.2. Basket-weave alpha-beta structure of as-cast Ti – 6%
quench) Ti – 3% Cr alloy after tint etching with Beraha’s reagent Al – 4% V revealed by heat tinting (polarized light, 100X).
(polarized light, 500X).

Table 7.1: 3-Step Method for Ti Alloys

Sectioning Abrasive Cutter with a wheel recommended for use on ductile materials
Mounting Compression, typically with EpoMet
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 10:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 5 [22] 150 10:00
Met Colloidal Silica**

= Platen = Specimen Holder

* Plus MetaDi Fluid Extender as desired

** Attack polish may be used, 1 part Ammonium Persulfate solutions (10g Ammonium Persulfate per 100mℓ distilled water) or 30% Hydrogen Peroxide
to 5 parts Silica.

Imaging & Analysis Grain Size, Measurement & Analysis Applications

Hardness Testing Vickers

38
used. The simplest is a mixture of 10mℓ hydrogen
peroxide (30% concentration – avoid skin contact)
and 50mℓ colloidal silica. Some metallographers
add either a small amount of Kroll’s reagent to this
mixture, or a few mℓ of nitric and hydrofluoric acids
(avoid contact). These latter additions may cause the
suspension to gel. In general, these acid additions
do little to improve the action of the hydrogen per-
oxide (the safer 3% concentration is not effective). a
Polarized light response of CP titanium can be
improved by following this procedure with a brief
vibratory polish using colloidal silica.

40 72
72

Zr
Zirconium
Hf
Hafniu
Hafniumm

Zirconium and Hafnium b

Pure zirconium and pure hafnium are soft, ductile
hexagonal close-packed metals that can deform

REFRACTORY METALS
by mechanical twinning if handled aggressively in
sectioning and grinding. As with most refractory
metals, grinding and polishing removal rates are
low and eliminating all polishing scratches and de-
formation can be difficult. It may even be possible
to form mechanical twins in compression mounting.
Both can contain very hard phases that make relief
c
control more difficult. To improve polarized light Figure 8.3. a) Equiaxed grain structure of wrought zirconium
response, it is common practice to chemically polish (unetched, crossed polarized light, 100X). b) Equiaxed grain
structure of wrought hafnium (unetched, crossed polarized
specimens after mechanical polishing, see Figures light plus sensitive tint, 100X). c) Fine grain recrystallized
8.3 – 8.4. Alternatively, attack polishing additions microstructure of wrought Zr - 1.14% Cr strip in the as-polished
condition at 200X using polarized light plus sensitive tint.
can be made to the final polishing abrasive slurry, or

Table 8.2: 4-Step Method for Zirconium and Hafnium

Sectioning Precision Saw with a 15LC blade recommended for use on hard brittle materials
Mounting Compression, typically with EpoMet
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 5 [22] 300 Until Plane
water cooled*

9μm MetaDi Supreme

UltraPad 5 [22] 150 5:00
Diamond**

3μm MetaDi Supreme

TriDent 5 [22] 150 3:00
Diamond**

0.02 - 0.06μm Master-

ChemoMet 5 [22] 150 7:00
Met Colloidal Silica

= Platen = Specimen Holder

*Rub candle wax lightly across rotating disc prior to grinding **Plus MetaDi Fluid Extender as desired

Imaging & Analysis Grain Size, Measurement & Analysis Applications

Hardness Testing Vickers

39
Refractory

RMMetals REFRACTORY METALS

vibratory polishing may be employed. Table 8.2 is a
four-step procedure that can be followed by either
chemical polishing or vibratory polishing.

Several attack polishing agents have been used

for Zr and Hf. One is a mixture of 1-2 parts hy-
drogen peroxide (30% concentration – avoid
all skin contact) to 8 or 9 parts colloidal silica.
Another is 5mL of a chromium trioxide solution
a
(20g CrO 3 to 100mℓ water) added to 95mℓ
colloidal silica or MasterPrep alumina slurry.
Additions of oxalic, hydrofluoric or nitric acids have
also been used. All of these attack polishing addi-
tions must be handled with care as they are strong
oxidizers. Skin contact must be avoided. Chemical
polishing solutions are reviewed in [2]. Cain’s has
been popular. Use under a hood and avoid skin
contact. Ann Kelly developed an excellent chemical
polish for refractory metals, such as Zr, Hf, and Ta. b
Figure 8.4. a) Cold worked microstructure of wrought zirconium
It consists of 25mℓ lactic acid, 15mℓ nitric acid and alloy XL (Zr - 3% Sn - 0.8% Nb - 0.8% Mo) in the as-polished
5mℓ hydrofluoric acid. Swab vigorously for up to 2 condition at 200X with polarized light plus sensitive tint. b)
Microstructure (α-Zr + AlZr3) of wrought Zr - 8.6% Al in the as-
minutes. To prepare ultra-pure Zr and Hf, the above polished condition at 200X with polarized light.
method is unsatisfactory and a procedure, such as in
Table 7.1 (add a 5 or 3µm alumina step) is needed,
as diamond is ineffective. Use the chromium trioxide
attack polish with the alumina and conclude with
Kelly’s chemical polish. HELPFUL HINTS FOR
REFRACTORY METALS

Due to their very low rate of grinding and

polishing, the more aggressive contra ro-
tation gives suitable surfaces in less time.

Refractory metal preparation is aided by

using attack-polishing additives. Polar-
ized light response may be improved by
following preparation by swabbing with a
chemical polishing solution.

40
OTHER REFRACTORY METALS: Cr, depending upon composition. It is susceptible to
deformation damage in sectioning and grinding.
Mo, Nb, Re, Ta, V and W
Pure niobium (columbium) is soft and ductile and
23 24
24 41 42 difficult to prepare while its alloys are harder and
V
Vanadium
Cr
Chromiu
Chromiumm
Nb Niobium
Niobiu m
Mo
Molybdenum
simpler to prepare. Grinding and polishing rates
have been reported to vary with crystallographic
orientation. Rhenium is very sensitive to cold work
73 74
74 75
and will form mechanical twins. Tantalum is softer
Ta
Tantalum
W
Tungste
Tungstenn
Re
Rhenium
than niobium and more difficult to prepare as it
easily forms damaged layers in sectioning and
T hese refractory metals have body-centered grinding. Tantalum may contain hard phases that
cubic crystal structures (except for rhenium promote relief control problems. Vanadium is a soft,
which is hexagonal close packed) and are soft ductile metal but may be embrittled by hydrogen;
and ductile when pure, but some are brittle in otherwise it can be prepared much like a stainless
commercial form. They can be cold worked easily, steel (Figure 8.7b). Tungsten is not too difficult to
although they do not work harden appreciably, so it prepare, although grinding and polishing rates are
may be difficult to get completely deformation-free low. Hard carbides and oxides may be present in
microstructures. these metals that introduce relief control problems,
see Figures 8.5 and 8.8.

OTHER REFRACTORY METALS

Mechanical polishing often incorporates an
attack-polishing agent in the final step or
is followed by vibratory polishing or chem-
ical polishing. Manual preparation of these
metals and their alloys tends to be very tedious
due to their low grinding and polishing rates.
Automated approaches are highly recommended,
especially if attack polishing is performed. Follow-
ing is a generic four step practice suitable for these
Figure 8.5. Microstructure of powder-made W – 5.6% Ni – 2.4%
Fe revealing tungsten grains surrounded by a nickel-iron matrix metals and their alloys, see Table 8.3.
(unetched, Nomarski DIC, 200X).

Many attack-polishing additives [2] have been

suggested for these metals and their alloys.
Pure chromium is soft and brittle; but, when encoun-
A good general purpose attack polish consists
tered commercially, for example, as a plated layer,
of a mixture of 5mℓ chromium trioxide solution (20g
it is hard and brittle. Chromium alloys are relatively
CrO3 in 100mℓ water) to 95mℓ MasterMet colloidal
easy to prepare, although difficult to etch. Molybde-
silica. Avoid skin contact as this is a strong oxidizing
num (Figures 8.6 and 8.7a) may be tough or brittle
solution. A number of chemical polishing solutions

Table 8.3: 4-Step Method for Refractory Metals

Load - lbs [N] /

Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 10:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 8:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet Met Colloidal Silica plus 6 [27] 150 5:00
attack polish agent**

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired **See text for agent

41
Refractory

RMMetals
OTHER REFRACTORY METALS
have been suggested [2]. For Nb, V and Ta, use a
solution consisting of 30mℓ water, 30mℓ nitric acid,
30mℓ hydrochloric acid and 15mℓ hydrofluoric
acid. Swab or immerse at room temperature. An
alternative chemical polish for Nb, V and Ta consists
of 120mℓ water, 6g ferric chloride, 30mℓ hydro-
chloric acid and 16mℓ hydrofluoric acid. Eary and
Johnson recommend immersing the specimen in
this solution 1 minute for V, 2 minutes for Nb and a
3 minutes for Ta. Vibratory polishing is also very
helpful for these metals and their alloys.

b
Figure 8.7. a) Non-recrystallized grain structure of wrought pure
molybdenum, longitudinal plane (500X, polarized light, etch
a of water, hydrogen peroxide (30% conc) and sulfuric acid in
7:2:1 ratio). b) Equiaxed alpha grain structure in wrought pure
vanadium (200X, etch: glycerol-nitric acid-hydrofluoric acid,
1:1:1 ratio).

c
Figure 8.6. a) Alpha grains in Mo – 47.5% Re. The small spots
are sigma phase (Murakami’s reagent, 200X). Deformed alpha
grains in W – 25% Re containing sigma phase (black spots)
revealed using b) bright field and c) Nomarski DIC which reveals b
the cold work much better (Murakami’s reagent, 500X).
Figure 8.8. a) Wrought tungsten - 10 atomic % Ti containing
a small amount of alpha-Ti, beta-Ti-W eutectic and grains of
beta-Ti,W of varying composition and crystal orientation (500X,
Kroll’s reagent/Murakami’s reagent at room temperature). b)
Fine grain boundary precipitates (not identified) in wrought,
cold worked Fan Steel 85-03 alloy (Nb - 28% Ta - 10.5% W -
0.9% Zr), longitudinal plane (500X, etchant: lactic acid-nitric
acid-hydrofluoric acid, 30:10:5 ratio).

42
Ferrous

FERROUS METALS FM Metals

Ferrous Metals metals and alloys. Table 4.3 presented a variation of

the method given in Table 9.1. This practice is also
26 useful for cast iron specimens including graphitic
FeIron
cast irons, however, due to their high silicon content
and the potential for staining problems, it is best to
Iron-based alloys account for a large portion of all use the MasterPrep alumina suspension for the final
metals production. The range of compositions and polishing step.
microstructures of iron-based alloys is far wider
than any other system. Pure iron is soft and ductile. For softer steels, use the 320 [P400] grit SiC pa-
Development of scratch-free and deformation-free per, for step 1. The Apex Hercules S disc can be
grain structures is difficult, excellent results are used but this is not usually necessary. However, if
shown in Figure 9.1. Sheet steels present the same substituted, use 6µm MetaDi Supreme for the
problem, which can be complicated by protective second step instead of 9µm, as shown in Table 9.2.
coatings of zinc, aluminum or Zn-Al mixtures. In
general, harder alloys are much easier to prepare. This practice is well suited for solution annealed
Cast irons may contain graphite, which must be austenitic stainless steels and for soft sheet steels.
retained in preparation. Inclusions are frequently UltraPol or UltraPad cloths could be substitute for
evaluated and quantified. Volume fractions can the rigid grinding discs, if desired. For perfect pub-
vary from nearly 2% in a free machining grade lication quality images, or for color etching, follow
to levels barely detectable in a premium, double this practice with a brief vibratory polish using the
vacuum melt alloy. A wide range of inclusion, cloths and abrasives in the last step.

FERROUS METALS
carbide and nitride phases has been identified in
steels. Addition of 12 or more percent chromium
dramatically reduces the corrosion rate of steels,
producing a wide range of stainless steel alloys. Tool
steels cover a wide range of compositions and can
attain very high hardnesses. Preparation of ferrous
metals and alloys is quite straightforward using
the contemporary methods. Edge retention (see
guidelines on pages 13-15) and inclusion retention
are excellent, especially if automated equipment is Figure 9.1. Normalized carbon steel shows coarse ferritic-
used. The following procedures are recommended pearlitic (grains with lamellar cementite) structure. Etched with
3% Nital (200X).
and are adequate for the vast majority of ferrous

Table 9.1: 4-Step Method for Hard Steel

Sectioning Abrasive Cutter with a wheel recommended for use on ferrous materials HRC35-60
Mounting Compression or Castable, typically with EpoMet or VariDur 3000
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

75μm Diamond
Apex DGD Red 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

Apex Hercules H 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 3:00
Diamond*

0.05μm MasterPrep
MicroCloth 6 [27] 150 2:00
Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Grain Size, Phase Area Percent, Object Measurement, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop, Rockwell

43
Ferrous

FM
Metals
FERROUS METALS

Table 9.2: 4-Step Method for Soft Steel

Sectioning Abrasive Cutter with a wheel recommended for use on ferrous materials HRC15-35
Mounting Compression or Castable, typically with EpoMet or VariDur 200
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320grit [P400] SiC

CarbiMet 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

VerduTex 6 [27] 150 3:00
Diamond*

0.05μm MasterPrep
MicroCloth 6 [27] 150 2:00
Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Grain Size, Object Measurement, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop

Many steels, particularly the harder steels, can be and for annealed maraging grades, use the Apex
prepared in three steps with excellent results. A Hercules S disc or the UltraPol cloth and a 30um
recommended practice is given in Table 9.3. Instead MetaDi Supreme polycrystalline diamond supsen-
of the diamond grinding disc, SiC can be used if sion for best results. Start with 120 grit [P120] SiC
preferred. For soft alloys, use 240 or 320 [P280 or paper only if it is a very hard martensitic stainless
P400] grit SiC paper; harder alloys use 120 [P120], steel, such as type 440C. The solution annealed aus-
180 [P180], or 240 [P280] grit SiC paper, depending tenitic stainless steels and the fully ferritic stainless
upon the starting surface finish and the hardness of steels (Figure 9.2) are the most difficult to prepare.
the alloy. The UltraPad cloth can also be used for It may be helpful to add a 1µm diamond step on a
the second step for steels of any hardness. TriDent cloth before the last step, or to follow the last
step with a brief vibratory polish using colloidal silica
The following practice is recommended for stainless on MicroCloth or a ChemoMet cloth, see Table 9.4.
steels and maraging steels. For solution annealed
austenitic grades and for ferritic stainless grades

Table 9.3: 3-Step Method for Heat-Treated Steel

Sectioning Abrasive Cutter with a wheel recommended for use on ferrous materials HRC35-60
Mounting Compression or Castable, typically with EpoMet or VariDur 3000
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

75μm Diamond
Apex DGD Red 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

Apex Hercules S 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

MicroFloc 6 [27] 150 3:00
Diamond*

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Case Depth, Decarburization Depth Assessment, Grain Size, Phase Area Percent, Object Measurement, Measurement &
Imaging & Analysis
Analysis Applications

Hardness Testing Vickers, Knoop, Rockwell

44
Ferrous

FERROUS METALS FM Metals

form of the graphite it contains. The graphite is in the

form of spherical nodules rather than flakes, which
Cast Iron helps prevent the creation of cracks and provides
Cast iron is a ferrous material with high carbon improved ductility as shown in Figure 9.4. This form
content (> 2%), Silicon (> 1.5%) and other com- is achieved by desulphurization of the melt and the
ponents such as manganese, chromium or nickel. addition of small amounts of magnesium, cerium or
In general there is a distinction between gray cast calcium prior to casting. Preparation artifacts can
iron (carbon is in the form of graphite) and white occur due to insufficient time or too low material
cast iron (carbon is in the form of cementite). The removal rates. The effects are visible as pull outs of
simplest type of cast iron is grey cast iron (ASTM A
48), also called “GJL” according to the European
Norm. Grey cast iron, or grey iron, has graphite
flakes which act as notches when tensile forces are
applied, so the tensile strength is relatively low, as
in Figuer 9.3. Compared to this the compressive
strength is much better. Cast iron “GJS” (DIN EN
1563 cast iron, ductile iron, spherolitic graphite) has
better mechanical properties, due to the spheroidal

Figure 9.3. Pearlitic gray cast iron, etched with Beraha’s CdS tint
(1300X).

FERROUS METALS
Figure 9.2. Microstructure of a duplex (ferrite tan, austenite Figure 9.4. Nodular graphite, lower bainite and retained
white) stainless steel held at 816º C for 48 hours which forms austenite in austempered ductile iron, etched with modified
sigma phase (orange particles) revealed by electrolytic etching Beraha-martensite reagent (~1300X).
with aqueous 20% NaOH at 3 V DC, 9 seconds (500X).

Table 9.4: 4-Step Method for Stainless and Maraging Steel

Sectioning Abrasive Cutter with a wheel recommended for use on ferrous materials HRC35-50
Mounting Compression, typically with EpoMet
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]
120 [P120] to 320grit
CarbiMet [P400] SiC 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 3:00
Diamond*

0.05μm MasterPrep
ChemoMet 6 [27] 150 2:00
Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Grain Size, Phase Area Percent, Object Measurement, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop, Rockwell

45
Ferrous

FM
Metals
FERROUS METALS
the graphite flakes or nodules. Table 9.5 shows a
Table 9.5: 5-Step Method for Cast Iron
good practice to prepare cast iron.
Sectioning Abrasive cutter with a wheel recommended for use on ferrous materials HRC35-50
Mounting Compression or Castable
Load - lbs [N] / Time
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation [min:sec]

320grit [P400] SiC

CarbiMet 5 [22] 300 Until Plane
water cooled

9μm MetaDi Diamond

TexMet C 5 [22] 150 5:00
Supreme*

3μm MetaDi Diamond

TriDent 5 [22] 150 4:00
Supreme*

0.05μm MasterPrep
MicroCloth 5 [22] 150 2:00
Alumina

= Platen = Specimen Holder

Imaging & Analysis Graphite in Cast Iron

Hardness Testing Brinell

46
Copper
Copper

COPPER, NICKEL, COBALT CNC

Nickel
Nickel
Cobal t
Cobalt

29

Cu
Copper

Copper
Pure copper is extremely ductile and malleable.
Copper and its alloys come in a wide range
of compositions, including several variants of
nearly pure copper for electrical applications
to highly alloyed brasses and bronzes and to Figure 10.1. Alpha grains containing annealing twins in
phosphorous-deoxidized arsenical bronze that was annealed
precipitation hardened high strength alloys. and lightly cold drawn (Klemm’s I reagent, polarized light, 50X).
Copper and its alloys can be easily damaged
by rough sectioning and grinding practices and
the depth of damage can be substantial. Scratch
removal, particularly for pure copper and
brass alloys, can be very difficult. Following the
preparation cycle with a brief vibratory polish
using colloidal silica is very helpful for scratch
removal. Attack-polish additions have been

COPPER, NICKEL, COBALT

used in the past to improve scratch removal but
usually are not necessary using the contemporary
method followed by vibratory polishing, see Table
10.1 and Figure 10.1 for results.

Planar grinding can be performed using the

PlanarMet 300 or resin bonded Apex DGD col-
or with 35µm for any copper alloy. Avoid the use
of metal bonded discs as they introduce too much
mechanical stress.

Table 10.1: 5-Step Method for Cu and Cu Alloys

Sectioning Abrasive Cutter with a wheel recommended for use on non-ferrous materials
Mounting Compression or Castable, typically with PhenoCure or VariDur
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]
220 [P240] to 320
CarbiMet [P400] grit SiC 5 [22] 300 Until Plane
water cooled

9μm MetaDi Supreme

TexMet C 5 [22] 150 5:00
Diamond*

3μm MetaDi Supreme

VerduTex 5 [22] 150 3:00
Diamond*

1μm MetaDi Supreme

VerduTex 5 [22] 150 2:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 5 [22] 150 1:30
Met Colloidal Silica**

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired **Plus attack polishing reagent (see text for details)

Imaging & Analysis Grain Size, Coating Thickness Layer, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop

47
Copper
Copper

CNC
Nickel
Nickel
Cobal t
Cobalt
COPPER, NICKEL, COBALT
28
before the final step.

Ni
Nickel For pure nickel, nickel-copper and nickel-iron
alloys, a five step practice is preferred, as given
Nickel below. The planar grinding step can be performed
Nickel and its alloys have face-centered cubic using either the 30µm resin-bonded UltraPrep dia-
crystal structures and are prepared in basically mond disc or with 240 [P280] or 320 [P400] grit SiC
the same way as austenitic stainless steels. Pure papers with equal success, see Table 10.3.
nickel is more difficult to prepare than the
alloys. The Ni-Fe magnetic alloys are rather dif- Attack-polishing agents are not often used with
ficult to prepare scratch free unless vibratory these alloys to eliminate fine polishing scratches or
polishing is used. The Monel (Ni-Cu) and the high- residual damage. If this is a problem, and some of
ly corrosion resistant (Ni-Cr-Fe) alloys are more these grades are very difficult to get perfectly free of
difficult to prepare than the nickel-based superal- scratches and deformation damage, a brief vibrato-
loys. Solution annealed superalloys are always more ry polish, using the same materials as in the last step,
difficult to prepare than age hardened superalloys will provide the needed improvement. MasterPrep
(Figure 10.2). Age hardened superalloys can be alumina may give better results than colloidal silica
prepared using the Apex Hercules H disc; for all for the more pure nickel compositions.
other nickel alloys, use the Apex Hercules S disc for
best results. The following practice works well for
nickel based superalloys (and Fe-Ni based super
alloys) and the highly corrosion resistant Ni-Cr-Fe
alloys, see Table 10.2.

If color etching is to be performed, follow the last

step with a brief vibratory polish using the same
materials as in the last step. This step is also helpful
for the most difficult to prepare solution annealed Figure 10.2. Alpha grains containing annealing twins of solution
alloys. Alternatively, for the most difficult specimens, annealed and double aged Waspaloy nickel-based superalloy
(Beraha’s reagent, 100X).
or when color etching is being performed, a 1µm
diamond step on a Trident cloth can be added

Table 10.2: 4-Step Method for Ni-Based Superalloys

Sectioning Abrasive Cutter with a wheel recommended for use on SuperAlloys

Mounting Compression, typically with EpoMet
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

240 [P280] grit SiC

CarbiMet 6 [27] 300 Until Plane
water cooled

Apex Hercules 9μm MetaDi Supreme

6 [27] 150 5:00
H or S Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 5:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 6 [27] 150 2:00
Met Colloidal Silica**

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired **Plus attack polishing reagent (see text for details)

Imaging & Analysis Grain Size, Porosity Assesment, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop

48
Copper
Copper

COPPER, NICKEL, COBALT CNC

Nickel
Nickel
Cobal t
Cobalt

Table 10.3: 5-Step Method for Ni, Ni-Cu and Ni-Fe Alloys

Sectioning Abrasive Cutter with a wheel recommended for use on SuperAlloys

Mounting Compression, typically with EpoMet

Load - lbs [N] /

Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

240 [P280] grit SiC

CarbiMet 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 3:00
Diamond*

1μm MetaDi Supreme

TriDent 6 [27] 150 2:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 6 [27] 150 2:00
Met Colloidal Silica**

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired **Plus attack polishing reagent (see text for details)

Imaging & Analysis Grain Size, Porosity Assesment, Measurement & Analysis Applications

COPPER, NICKEL, COBALT

Hardness Testing Vickers, Knoop

27
recommended two chemical polishing solutions:

Co
Cobal t
equal parts of acetic and nitric acids (immerse) or
40mℓ lactic acid, 30mℓ hydrochloric acid and 5mℓ
nitric acid (immerse). A wide variety of Co-based
Cobalt alloys have been prepared with the method Table
Cobalt and its alloys are more difficult to 10.4 without need for chemical polishing. The 1µm
prepare than nickel and its alloys. Cobalt is a diamond step could be eliminated for routine work.
tough metal with a hexagonal close-packed
crystal structure and is sensitive to deformation
damage by mechanical twinning. Grinding and
polishing rates are lower for Co than for Ni,
Cu or Fe. Preparation of cobalt and its alloys is
somewhat similar to that of refractory met-
als. Despite its HCP crystal structure, crossed
polarized light is not very useful for examining
cobalt alloys compared to other HCP metals and
alloys. Following is a practice for preparing Co and
its alloys, see Table 10.4 and Figure 10.3 for results.

Two steps of SiC paper may be needed to get the

Figure 10.3. Equiaxed grain structure of Elgiloy (Co – 20% Cr –
specimens co-planar. If the cut surface is of good 15% Fe – 15% Ni – 7% Mo – 2% Mn – 0.15% C – 0.05% Be) after
quality, start with 320 [P400] grit paper. Cobalt and hot rolling and annealing revealing annealing twins (Beraha’s
reagent, crossed polarized light plus sensitive tint, 100X).
its alloys are more difficult to cut than most steels,
regardless of their hardness. Attack polishing has
not been reported but chemical polishing has been
used after mechanical polishing. Morral (2) has

49
Copper
Copper

CNC
Nickel
Nickel
Cobal t
Cobalt
COPPER, NICKEL, COBALT
Table 10.4: 5-Step Method for Co

Sectioning Abrasive Cutter with a wheel recommended for use on SuperAlloys

Mounting Compression, typically with EpoMet
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

TexMet C 6 [27] 150 5:00
Diamond*

1μm MetaDi Supreme

TexMet C 6 [27] 150 3:00
Diamond*

0.02 - 0.06μm
ChemoMet 6 [27] 150 2:00
MasterPrep Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Grain Size, Porosity Assesment, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop

50
Precious

PRECIOUS METALS PM Metals

PRECIOUS METALS: Au, Ag, Ir, Os, the precious metals. Platinum is soft and malleable.
Its alloys are more commonly encountered. Abrasive
Pd, Pt, Rh and Ru
embedment is a problem with Pt and its alloys. Rho-
44 45 46 47
dium is a hard metal and is relatively easy to prepare.

Ru
Ruthenium
Rh
Rhodium
Pd
Palladium
AgSilver
Rh is sensitive to surface damage in sectioning and
grinding. Ruthenium is a hard, brittle metal that is
not too difficult to prepare.
76 77 78 79

Os
Osmium
Ir
Iridiu m
Pt
Platinum
Au Gold
Stewart (Tech-Notes, Vol. 2, Issue 5) has described
a method for preparing jewelry alloys. Invariably,
these are small pieces, due to their cost, and must
Relatively few metallographers work with precious
be mounted. Stewart uses EpoMet G resin for most
metals, other than those used in electronic devices.
specimens. If transparency is need, he uses Tran-
Preparing precious metals within an integrated cir-
sOptic resin. Fragile beads and balls are mounted
cuit is discussed later (see Electronic Materials). The
in castable resins. Grinding and polishing was
precious metals are very soft and ductile, deform
conducted at 400 rpm. His practice with equivalent
and smear easily, and are quite challenging to pre-
current materials is shown in Table 11.1.
pare. Pure gold is very soft and the most malleable
metal known. Alloys, which are more commonly
encountered, are harder and somewhat easier to
prepare. Gold is difficult to etch. Silver is very soft
and ductile and prone to surface damage from de-

PRECIOUS METALS
formation, see Figure 11.1. Embedding of abrasives
is a common problem with both gold and silver
and their alloys. Iridium is much harder and more
easily prepared. Osmium is rarely encountered in
its pure form, even its alloys are infrequent subjects
for metallographers. Damaged surface layers are Figure 11.1. Eutectic microstructure of Ag – 28% Cu where
easily produced and grinding and polishing rates Klemm’s reagent has colored the copper particles and the silver
phase is uncolored (500X).
are low. It is quite difficult to prepare. Palladium is
malleable and not as difficult to prepare as most of

Table 11.1: Stewart’s Manual Procedure for Precious Metals

Sectioning Precision Cutter with 30HC blade recommended for use on soft gummy materials
Mounting Castable, typically with EpoThin
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Time [min:sec]
240 [P280] grit SiC
CarbiMet water cooled Moderate 400 Until Plane
(wax coated)*
320 [P400] grit SiC
CarbiMet water cooled Moderate 400 1:00
(wax coated)*
400 [P600] grit SiC
CarbiMet water cooled Moderate 400 1:00
(wax coated)*
600 [P1200] grit SiC
CarbiMet water cooled Moderate 400 1:00
(wax coated)*
6μm MetaDi Supreme
TriDent Moderate 400 2:00
Diamond**
1μm MetaDi Supreme
MasterTex Moderate 400 2:00
Diamond**

*Rub candle was lightly across rotating disc prior to grinding **Plus MetaDi Fluid Extender as desired

Imaging & Analysis Porosity Assessment, OmniMet Object Measurements, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop

51
Precious

PM
Metals
PRECIOUS METALS
This can be followed by a brief vibratory polish using For 18 karat gold (Figure 11.2) and higher (≥75%
colloidal silica on MasterTex, ChemoMet or Micro- Au), it is necessary to use an attack polish agent in
Cloth surfaces to further enhance the quality of the the final step. An aqueous solution of 5g CrO3 in
preparation; but, a 1µm diamond finish is adequate 100mℓ water works well. Mix 10mℓ of the attack
for most work. Attack-polishing has been used to polish agent with 50mℓ of MasterPrep suspension.
prepare gold and its alloys and chemical polishing This will thicken, so add about 20-30mℓ water to
has been performed after mechanical polishing of make it thinner. A 3 to 6 minute attack polish step
silver, but neither practice is commonly performed. will remove the fine polishing scratches. Wear pro-
Alternate etch-polish cycles may be needed to tective gloves as the chromium trioxide solution is
remove fine polishing scratches, especially for a strong oxidizer.
annealed specimens.

A procedure for an automated system was

developed after experimentation with a num-
ber of precious metal specimens. Most of these
metals and alloys are quite soft, unless they have
been cold worked, and they are susceptible to
embedding of abrasives. In this method, only one
silicon carbide step is used. The TexMet C cloth is
used for the diamond steps, as it will hold the abra-
sive in its surface well, which minimizes embedding.
Only diamond paste is used, as slurries will be more
prone to embedding, as we observed in high gold
alloys. Use only a small amount of distilled water
as the lubricant. Do not get the cloth excessively
wet. Final polishing is with a ChemoMet cloth and
MasterPrep alumina. Due to their excellent corro-
Figure 11.2. Equiaxed grain structure of cold rolled and
sion resistance, colloidal silica is not effective as an annealed 18-karat gold (Neyoro 28A: 75% Au – 22% Ag – 3%
abrasive for precious metals. The ChemoMet cloth Ni) revealing annealing twins (equal parts 10% NaCN and 30%
H2O2, 50X).
has many fine pores to hold the abrasive. The cycle
is given in Table 11.2.

Table 11.2: 5-Step Method for Precious Metals

Sectioning Precision Saw with a blade recommended for use on soft gummer materials
Mounting Castable, typically with EpoThin
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 3 [13] 150 Until Plane
water cooled

9μm MetaDi Supreme

TexMet C 3 [13] 150 5:00
Diamond*

3μm MetaDi Supreme

TexMet C 3 [13] 150 3:00
Diamond*

1μm MetaDi Supreme

TexMet C 3 [13] 150 2:00
Diamond*

0.05μm MasterPrep
ChemoMet 2 [9] 150 2:00
Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Porosity Assesment, OmniMet Object Measurements, Measurement & Analysis Applications

Hardness Testing Vickers, Knoop

52
Thermall
Therma

THERMAL SPRAY COATINGS TSC Spra y

Spray
Coatings
Coatings

Thermal spray coatings (TSC) and thermal barri- would be seen with bright field illumination. Filling
er coatings (TBC) are widely used on many metal the pores with epoxy also makes it easier to keep
substrates. Invariably, these coatings are not 100% the pore walls flat to the edge during preparation.
dense but contain several types of voids, such as Aside from this mounting requirement, TSC and
porosity and linear detachments. Hot compression TBC specimens are prepared using all of the fac-
mounting is not recommended as the molding tors needed for good edge retention (see pages
pressure can collapse the voids. Use a low-viscos- 14-17). A variety of procedures can be used. The
ity castable epoxy with vacuum infiltration to fill Apex Hercules H rigid grinding disc produces ex-
the connected voids with epoxy. Fluorescent dyes ceptional edge flatness for these specimens. Two
may be added to the epoxy. When viewed with four-step procedures for TSC and TBC specimens
fluorescent illumination, the epoxy-filled voids ap- for specimens with metallic coatings and one pro-
pear bright yellow-green. This makes it easy to dis- cedure for specimens with ceramic coatings are
criminate between dark holes and dark oxides, as given, see Tables 12.1–12.3.

Table 12.1: 4-Step Method for TSC and TBC Specimens with Metallic Coatings

Sectioning Precision Saw with 15HC blade recommend for thermal spray coatings
Mounting Castable, typically with epoxy drawn under vacuum
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

THERMAL SPRAY COATINGS

35μm Diamond
Apex DGD Yellow 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 5:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 4 [18] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Porosity Assessment, Coating Layer Thickness, Particle Sizing, Phase Area Percent

Hardness Testing Vickers, Knoop

Table 12.2: Alternate 4-Step Method for TSC and TBC Specimens with Metallic Coatings

Sectioning Precision Saw with 15HC blade recommend for thermal spray coatings
Mounting Castable, typically with epoxy drawn under vacuum
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

Apex Hercules H 30μm MetaDi Diamond* 6 [27] 300 Until Plane

9μm MetaDi Supreme

UltraPad 6 [27] 150 4:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 3:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 4 [18] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Porosity Assessment, Coating Layer Thickness, Particle Sizing, Phase Area Percent

Hardness Testing Vickers, Knoop

53
Thermall
Therma

TSC
Spra y
Spray THERMAL SPRAY COATINGS
Coatings
Coatings

The 30µm resin bonded, or the 45µm metal bond- UltraPol or UltraPad cloths can be used in the sec-
ed UltraPrep diamond discs, can be substituted for ond step (Tables 12.1 and 12.3) with results shown
the planar grinding step. (Tables 12.1 and 12.2). in Figures 12.1 and 12.2.

Figure 12.1. NiCrAlY thermally-spray coated steel specimen Figure 12.2. Microstructure of a steel substrate covered by two
revealing a small amount of porosity (black spots), linear thermally-sprayed layers, a NiAl bond coat and yittria-zirconia
detachments (elongated black lines), and inclusions (gray top coat (unetched, 100X). The bond coat contains pores, linear
particles) (unetched, 100X). detachments and inclusions while the top coat is quite porous.

Table 12.3: 4-Step Method for Ceramic Thermal Spray Coatings

Sectioning Precision Saw with 15HC blade recommend for thermal spray coatings
Mounting Castable, typically with epoxy drawn under vacuum
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

35μm Diamond
Apex DGD Yellow 5 [22] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 5 [22] 150 5:00
Diamond*

3μm MetaDi Supreme

TriDent 6 [27] 150 5:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 6 [27] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Porosity Assessment, Coating Layer Thickness, Particle Sizing, Phase Area Percent

Hardness Testing Vickers, Knoop

54
Sintered

SINTERED CARBIDES SC Carbides

Sintered carbides are very hard materials made

by the powder metallurgy process and may
by reinforced with several types of MC-type
carbides besides the usual tung-
sten carbide (WC) as shown in Figure 13.1
– 13.3. The binder phase is normally cobalt
although minor use is made of nickel. Mod-
ern cutting tools are frequently coated with a
variety of very hard phases, such as alumina,
titanium carbide, titanium nitride and titanium
carbonitride. Sectioning is normally performed
Figure 13.1. Surface of a WC – 11.5% Co cutting tool enriched
with a precision saw, so surfaces are very good with 1.9% Ta and 0.4% Nb (form complex carbides, the dark
regions in the matrix) and coated with alumina (arrows) for
and rough abrasives are not usually required. enhanced tool life (Murakami’s reagent, 1000X).
Listed below are two alternate procedures
for preparing sintered carbides using Apex DGD
metal-bonded UltraPrep discs or the Apex Hercules
H rigid grinding discs. A further option would be the
use of the traditional metal-bonded diamond discs. HELPFUL HINTS
FOR SINTERED CARBIDES
If a greater amount of material must be removed in
the planar grinding step, use either the 30µm resin The ability to see the boundaries between

SINTERED CARBIDES
bonded or the 45µm metal-bonded UltraPrep disc the WC particles and cobalt binder in the
for step one, in Table 13.1. as-polished condition depends on the sur-
face of the polishing cloth used in the last
The final step in these two procedures, Tables step. To see no boundaries, which makes
13.1 and 13.2, employs either MasterMet colloidal it easier to see graphite or eta phase, use
silica or MasterPrep alumina suspensions as they a napless surface, such as TriDent, TexMet
will produce the best definition of the structure, or UltraPol cloths. To see the phase bound-
particularly if the surfaces have a complex series aries between WC particles and the cobalt
of coatings for improved wear resistance, as used binder, use a medium nap surface, such as
in some coated carbide inserts. However, if such a MicroCloth, MasterTex cloths.
coating is not present, the matrix grain structure can
be observed quite clearly after the 3µm diamond

Table 13.1: 4-Step Method for Sintered Carbides

Sectioning Precision Saw with 20LC blade recommended for hard tough materials
Mounting Castable, typically epoxy with added flat-edge filler
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

UltraPrep 45μm Diamond

6 [27] 300 5:00†
Metal-Bonded water cooled

9μm MetaDi Supreme

TexMet P 6 [27] 150 4:00
Diamond*

3μm MetaDi Supreme

VerduTex 6 [27] 150 3:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 6 [27] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Porosity Assessment, Particle Sizing, Coating Layer Thickness

Hardness Testing N/A

†
Grind longer than “until plane”

55
Sintered

SC
Carbides
SINTERED CARBIDES
Table 13.2: 4-Step Method for Sintered Carbides

Sectioning Precision Saw with 20LC blade recommended for hard tough materials
Mounting Castable, typically epoxy with added flat-edge filler
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

30μm MetaDi Supreme

Apex Hercules H 6 [27] 150-200 5:00†
Diamond*

9μm MetaDi Supreme

Apex Hercules S 6 [27] 150 4:00
Diamond*

3μm MetaDi Supreme

VerduTex 6 [27] 150 3:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 6 [27] 150 2:00
Met Colloidal Silica

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Porosity Assessment, Particle Sizing, Coating Layer Thickness

Hardness Testing Vickers

†
Grind longer than “until plane”

Figure 13.2. Microstructure at the surface of a multilayered,

b
CVD-coated WC - 8% Co cutting tool. The arrows point to the
CVD layers of TiCN, TiN, TiC and alumina. The region below Figure 13.3. Microstructure of cold isostatically pressed and age
the coatings is made higher in Co to improve crack resistance hardened Ferro-Titanit Nikro 128 (Fe - 13.5% Cr - 9% Co - 4%
and complex carbide forming elements (Ta, Ti and Nb) are Ni - 30% TiC) cutting tool; a) etched with Murakami’s reagent at
added to the matrix (dark spots at bottom) for wear resistance room temperature to darken the TiC; and b) electrolytic etched
(Murakami’s reagent, 1000X). with aqueous 1% chromium trioxide at 2 V DC, 30 seconds to
reveal the martensitic matrix (1000X).

step. For routine examination there is little need to

go beyond the third step. It is also possible to use
a 1µm diamond step, similar to step three, but for
2 minutes, as an alternative fourth step.

56
Ceramics

CERAMICS C

Ceramic materials are extremely hard and brittle

and may contain pores. Sectioning must be per-
formed using diamond blades. If the specimen is to
be thermally etched, then it must be mounted in a
resin that permits easy demounting, and vacuum in-
filtration of epoxy into the voids should not be done.
Deformation and smearing are not problems with
ceramics due to their inherent characteristics. But, it
is possible to break out grains or produce cracking
during preparation. Figure 14.2. Microstructure of hot-pressed silicon nitride (binder
unknown) (unetched, 500X).
Pullouts are a major problem to control as they can be
misinterpreted as porosity. Mechanical preparation
has been done successfully with laps, metal-bonded
diamond discs, rigid grinding discs, or hard cloths.
SiC paper is rather ineffective with most ceramics, as
they are nearly as hard or as hard as the SiC abrasive.
Consequently, diamond is commonly used for nearly
all preparation steps. Automated preparation is high- HELPFUL HINTS
ly recommended when preparing ceramic materials FOR CERAMICS
as very high forces arise between the specimen
and the working surface, often too high for manual Cut specimens as close as possible to

CERAMICS
preparation. Listed are two generic procedures for the desired examination plane using a
preparing ceramics using different approaches, see saw and blade that produces the least
Tables 14.1 and 14.2 also Figures 14.1 and 14.2 for possible amount of damage, producing
results. the best possible surface for subsequent
preparation. Rough grinding is slow and
MasterPolish 2 suspension is specifically formulated
tedious and does considerable damage
for final polishing ceramic materials and this step
to the structure and should be avoided as
can me added for a more thorough examination as
much as possible.
it will yield a better surface finish than 1µm diamond.
Coarse abrasives for grinding may be
needed at times. However, severe grain
pull-outs can result from use of coarse
abrasives and it is recommended to use the
finest possible coarse abrasive for grinding.

b
Figure 14.1. a) Microstructure of an alumina (matrix), zirconia
(gray), silica (white) refractory material (unetched, 200X). b)
Silicon - SiC ceramic etched electrolytically with 10% oxalic acid
(500X).

57
Ceramics

C CERAMICS
Table 14.1: 4-Step Method for Ceramic

Sectioning Precision Saw with 10LC or 20LC blade recommended for medium to soft ceramics or structural ceramics
Mounting Castable, typically epoxy with flat edge filler if for very hard ceramic applications
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

UltraPrep 45μm Diamond

8 [36] 150 Until Plane
Metal-Bonded water cooled

9μm MetaDi Supreme

Apex Hercules H 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

VerduTex 6 [27] 150 5:00
Diamond*

1μm MetaDi Supreme

TexMet C 10 [44] 150 5:00
Diamond*

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Grain Size, Porosity Assessment

Hardness Testing Vickers

Table 14.2: 4-Step Method for Ceramic

Sectioning Precision Saw with 10LC or 20LC blade recommended for medium to soft ceramics or structural ceramics
Mounting Castable, typically epoxy with flat edge filler if for very hard ceramic applications
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

75μm Diamond
Apex DGD Red 8 [36] 150 Until Plane
water cooled

15μm MetaDi Supreme

TexMet P 6 [27] 150 6:00
Diamond*

6μm MetaDi Supreme

VerduTex 6 [27] 150 4:00
Diamond*

3μm MetaDi Supreme

Diamond*,
TexMet C MasterMet Colloidal 6 [27] 150 4:00
Silica
(50:50 Simultaneously)

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Grain Size, Porosity Assessment

Hardness Testing Vickers

58
Minerals

MINERALS M
A mineral is comprised of solid substance with a
Table 15.2: Mohs Hardness Scale
defined chemical composition that formed naturally
Mohs
with the aid of varying geological conditions. A rock Mineral Chemical Formula
Hardness
is a solid aggregate of minerals. Some of these
1 Talc Mg3Si4O10(OH)2
mineral groups can be seen in Table 15.1.
2 Gypsum CaSO4•2H2O

There are two commonly used techniques for 3 Calcite CaCO3

preparing geological specimens; thin section and 4 Flurite CaF2

bulk mount. Thin sections are typically prepared 5 Apatite Ca5(PO4)3(OH,Cl,F)
at 30µm for transmitted polarized light analysis for 6 Orthoclase KAlSi3O8
mineralogy and optical petrology. Bulk mounts are 7 Quartz SiO2
typically prepared for reflected light microscopy 8 Topaz Al2SiO4(OH,F)2
and is primarily used to examine opaque specimens
9 Corundum Al2O3
that such as ore microscopy, coal and opaque min-
10 Diamond C
erals, see example in Figure 15.1.

Most geological specimens can be grouped into

categories based on the variation in hardness and
the water sensitivity. The most common scale of
measurement is the Mohs hardness scale (Table
15.2). Which is defined by ten indicators (a mineral
with a higher index scratches those below it). The

MINERALS
scale ranges from talc to diamond.

Care should be taken when working with water

sensitive minerals as they can eroded (soils), swell
(clays), react (salts), accelerate reactions (cements) Figure 15.1. Microstructure of a cement clinker (Portland cement
among other issues. Table 15.3 describes a generic used for construction), showing various phases such as alite
and belite.The specimen has been etched with 2% nital, ~260x.
preparation method for most non-water sensitive Reflected light.
minerals of varying hardness. In case of water sensi-
tive materials preparation would be similar with the
replacement of water with either AutoMet Lapping
Oil or glycol for the grinding steps. Diamonds paste
(with Lapping Oil as extender) or Oil based suspen-
sions can be used for the 9µm and 3µm polishing
step. A final polish with MicroCloth and MicroPolish
II 0.05µm alumina polishing powder combined with
a 50:50 mixture of propylene glycol and alcohol is
recommended.

Table 15.1: Minerals Groups

Minerals Group Example

Sulfides Cobaltite, Pyrite, Realgar
Oxides and Hydroxides Microlite, Spinel
Halides Cryolite, Fluorite, Halite, Prosopite
Nitrates, Carbonates, Borates Magnesite, Malachite, Mother of Pearl, Rhodozite
Sulfates Crocoite, Chromates Gypsum
Phosphates, Arsenates, Vanadates Lazulite, Purpurite, Pyromorphite, Variscite, Zenotime
Silicates Analcime, Smaragdite, Smoky Quartz Zektzerite, Zircon
Non-minerals Amber, Coal, Opal, Pearl, Vulcanite

59
Minerals

M MINERALS
Table 15.3: Four Step Procedure for Preparing Bulk Mounts

Sectioning Precision Saw with 15LC blade recommended for hard brittle materials
Mounting Castable, typically EpoThin or EpoHeat
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

45μm Diamond water

Apex DGD 5 [22] 300 3:00
cooled

9μm MetaDi Supreme

TriDent 3 [13] 150 4:00
Diamond Suspension

3μm MetaDi Supreme

TriDent 3 [13] 150 4:00
Diamond Suspension

0.05μm MasterPrep
TexMet 4 [18] 150 2:00
Alumina Suspension

= Platen = Specimen Holder

Imaging & Analysis Phase Area Percent

Hardness Testing N/A

Glass
Glass preparation was historically prepared using
silicon carbide followed by multiple steps of cerium
oxide. The traditional preparation sequence (Table
15.4) can be used for a wide range of glass but the
method can lead to the risk of edge chipping as
the abrasive rolls along the leading edge of the
unmounted sample. More recent advancements
in fixed abrasive has led to the use of diamond
grinding discs for glass preparation, such as in Table
Figure 15.2. Quartz tube after 6μm polish.
15.5, as it has become critical for flat scratch free
surfaces for testing including FTIR and interferom-
eters, results shown in in Figure 15.2.

Table 15.4: Traditional Procedure for Glass

Sectioning Precision Saw with 15LC blade recommended for hard brittle materials
Mounting Castable, typically EpoThin or EpoHeat
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 5[22] 300 Until Plane
water cooled

400 [P800] grit SiC

CarbiMet 5[22] 300 1:00
water cooled

TexMet P MiroMet (CeO) 1μm 5[22] 150 5:00

MicroCloth MiroMet (CeO) 1μm 5[22] 150 2:00

= Platen = Specimen Holder

Imaging & Analysis Measurement & Analysis Applications

Hardness Testing N/A

60
Minerals

MINERALS M
Table 15.5: Five Step Procedure for Glass

Sectioning Precision Saw with 15LC blade recommended for glass

Mounting Castable
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

45μm Diamond water

Apex DGD 5[22] 300 5:00
cooled

15μm Diamond water

Apex DGD 5[22] 300 5:00
cooled

3μm Diamond water

Apex DGD 5[22] 300 5:00
cooled

3μm MetaDi Supreme

TexMet C 5[22] 150 4:00
Diamond Suspension

MasterTex MasterPolish 2 5[22] 150 4:00

= Platen = Specimen Holder

Imaging & Analysis Measurement & Analysis Applications

Hardness Testing N/A

MINERALS

61
Composites

CM COMPOSITES
The diverse and highly adjustable characteristics of
composite materials have caused a rapid increase in
their use worldwide. From light weight golf clubs to
high-performance airplane parts, reinforced com-
posite materials are becoming more popular due to
their unique physical properties and the capability
to be manufactured readily into complex geome-
tries. The term composites covers an extremely wide
range of materials, generally grouped under the a
subcategories polymer-matrix composites (PMC),
metal-matrix composites (MMC), and ceramic-ma-
trix composites (CMC). Consequently, preparation
schemes can be quite difficult to generalize.

The differences in hardness and grinding/polishing

characteristics from this range of materials mean
that relief control is one of the major concerns
during preparation. Pull out and fracture problems
are also very common. Sectioning frequently pro- b
Figure 16.1. a) Microstructure of a polymer-matrix composite,
duces considerable damage that must be removed graphite fabric-reinforced polysulfone (unetched, polarized
in subsequent preparation steps. Mounting with light, 100X). b) Microstructure of alumina fibers in an aluminum -
lithium alloy matrix (500X, as-polished, Nomarski DIC).
castable epoxy resin along with vacuum impreg-
nation is frequently performed.
Table 16.1 shows a useful general approach for the
preparation of many polymer matrix composites.
Polymer Matrix Composites However, some reinforcing materials – especially
The most common analysis requirement for polymer those that are smaller than ~10µm in size – can
matrix composites, as in Figure 16.1, is the deter- be prone to brittle fracture when diamond based
mination of void content and fibre characteristics preparation is used. In such cases, an alternative
such as percentage area and size distribution. For approach is to replace the 3µm diamond stage
all of these analyses, relief control is paramount with 0.3µm alumina on a TexMet C cloth. For many
for retaining accuracy. The investigation of failure analyses (such as void counting, fiber analysis and
mechanisms and microstructural analysis of fea- delamination examinations) this provides a suitable
tures such as matrix modifiers and fillers can also finish and limits possible relief effects. A shortened
be required. polishing stage can then be used to remove any
remaining artifacts in the softer matrix material.
There are many types of thermosetting and ther-
moplastic materials that are used as matrices in
fibre-reinforced composites. The matrix can also
contain dispersed phases known as modifiers that
can range in size from tens of microns to nano scale.
Materials used for the reinforcing phase include
carbon, glass, plastic, natural fibres and boron.

Interface characteristics are important to the overall

properties of these materials and examination of
features such as inter-ply delamination are import-
ant to the understanding of failure mechanisms in
many polymer matrix composites. Honeycomb and
foam materials are also being incorporated into
composite structures, to improve physical charac-
teristics against weight – particularly important in
Figure 16.2. Microstructure of a metal-matrix composite, SiC in a
the aerospace industry CP titanium matrix (unetched, Nomarski DIC, 100X).

62
Table 16.1: 4-Step Method for Polymer-Matrix Composites

Sectioning Precision Saw with 15HC blade recommended for metal matrix composites
Mounting Castable, typically epoxy
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC

CarbiMet 6 [27] 300 Until Plane
water cooled

9μm MetaDi Supreme

TexMet P 6 [27] 150 5:00
Diamond*

3μm MetaDi Supreme

VerduTex 6 [27] 150 5:00
Diamond*

0.05μm MasterPrep
MicroCloth 6 [27] 150 1:30
Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Phase Area Percent, Porosity Assessment, OmniMet Object Measurements

Hardness Testing N/A

Metal Matrix Composites

MMCs have been commercially available for many

COMPOSITES
years. They consist of a metal matrix component,
together with a reinforcing component that can be
in various forms (e.g. particle or fibre). The metal
matrix is generally formed from conventional light
metal alloys (aluminium and titanium based) but can
also be special alloys produced primarily for this
type of application.
a
The analysis of metal matrix alloys includes both
details of metallurgical microstructure and also
interface properties. Examination of any chemical
interactions and reactions between the matrix and
the reinforcement component are instrumental
in defining the characteristics of the material. As
such, the dominant concerns during preparation of
these materials will be the prevention of relief and
the recovery of damage at interfaces during initial
sectioning and grinding stages. Table 16.2 provides b
Figure 16.3. a) Synthetic foam made with hollow ceramic
a good standard approach to the preparation of this spheres added to 7075 aluminum (100X original magnification).
material group. If the sectioning technique used is Etched with aqueous 0.5% HF. b) Carbon-reinforced polymer
composite (original at 100X). Specimen is as-polished and
more damaging, or more material needs to be re- viewed with Nomarski DIC illumination.
moved, then a more aggressive grinding stage may
be preferred (for instance, replacing the ApexDGD
preparation characteristics of the different phases do
Color disc with an UltraPrep disc).
not necessarily lead to relief problems. The brittle
nature of many of the component materials can lead
Ceramic Matrix Composites to relatively deep damage if inappropriate section-
Ceramic Matrix Composites see Figure 16.3, typically ing or grinding techniques are used. Combined with
consist of a ceramic matrix, such as alumina or silicon the high wear resistance of these materials, recov-
carbide, combined with a dispersed phase such as ery of such damage can be very slow. The primary
silicon carbide, zirconium oxide, aluminium nitride concern is normally, therefore, to section as closely
or titanium boride. In these systems, the as possible to the area of interest, with the lowest

63
Composites

CM COMPOSITES
Table 16.2: 4-Step Method for Metal-Matrix Composites
Sectioning Precision Saw with 15HC blade recommended for metal matrix composites
Mounting Castable, typically epoxy
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

35μm Diamond
Apex DGD Yellow 5 [22] 300 Until Plane
water cooled

9μm MetaDi Supreme

UltraPad 5 [22] 150 4:00
Diamond*

3μm MetaDi Supreme

VerduTex 6 [27] 150 3:00
Diamond*

0.02 - 0.06μm Master-

ChemoMet 6 [27] 150 1:30
Met Colloidal Silica

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Fiber density, Phase Area Percent, OmniMet Object Measurements

Hardness Testing N/A

Table 16.3: 4-Step Method for Ceramic-Matrix Composites

Sectioning Precision Saw with 15HC blade recommended for metal matrix composites
Mounting Castable, typically epoxy
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

45μm Diamond
UltraPrep 6 [27] 300 Until Plane
water cooled

15μm MetaDi Supreme

UltraPad 6 [27] 150 4:00
Diamond*

6μm MetaDi Supreme

VerduTex 6 [27] 150 3:00
Diamond*

1μm MetaDi Supreme

VerduTex 6 [27] 150 2:00
Diamond*

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Phase Area Percent, Pororsity Assesment, OmniMet Object Measurements

Hardness Testing N/A

damage method available (Table 16.3), usually using HELPFUL HINTS FOR
a diamond blade on a precision saw. An alternative to COMPOSITES
the UltraPrep metal bonded disc would be the use of Sectioning damage can propagate down the
the Apex DGD fixed diamond disc with metadi fluid fibers and can be difficult to remove. Prevent
as a lubricant. As with pure ceramics, the addition of damage by using precision saw sectioning
MasterMet colloidal silica in even proportion with and diamond wafering blades with a very fine
the diamond slurry in the final stage can enhance abrasive, specifically like 5LC and 10LC Series.
the finish. Thinner blades produce less damage. Section as
close as possible to the plane of interest.

Composites can be damaged by compression

mounting. Castable mounting resins with low
peak temperature are preferred.

Avoid aggressive grinding steps by using longer

times and finer abrasives.

64
Printed
Printe d

PRINTED WIRING BOARDS PWB

Wiring
Wiring
Boards
Boards

The vast majority of printed wiring boards (PWB’s)

are of a rigid variety, the bulk of which are com-
posed of layers of woven glass fiber cloth in a
polymeric matrix. Flex circuits, which are becoming
quite common, do not typically contain glass fiber,
but instead, their bulk is often composed of layers
of polyimide. The circuitry in both types of boards
is composed of plated and/or foil metal. The metal
used is generally copper, while in a few cases, gold
and/or nickel plating may be present, as shown in
figure 17.1. Furthermore, depending upon whether
the boards have undergone assembly or shock
testing, solders of various compositions might also
Figure 17.1. Nickel plating on the Plated through Hole of the
be present. Back Panel PWB, 500x

Luckily for the metallographer, the variety of mate-

rials present in PWB’s generally do not complicate
the preparation methods due to the fact that ex-
tremely hard and brittle materials are not commonly
found in the boards. This changes, however, when

PRINTED WIRING BOARDS

‘packed’ boards with ceramic or semiconductor
components must be sectioned. Please refer to

Table Table 17.1: 5-Step Method for Printed Wiring Boards (target preparation)

Sectioning Precision Saw with 15HC blade recommended for PWBs

Mounting Castable, typically a fast cure system like SamplKwick
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

320 [P400] grit SiC Hit edge of the

CarbiMet 3 [13] 150
water cooled target

600 [P1200] grit SiC Hit the level of

CarbiMet 3 [13] 150
water cooled interest

9μm MetaDi Supreme

TriDent 5 [22] 150 3:00
Diamond*

3μm MetaDi Supreme

TriDent 5 [22] 150 3:00
Diamond*

0.05μm MasterPrep
Alumina + 0.06μm
ChemoMet MasterMet Colloidal 4 [18] 150 1:15
Silica
(50:50)

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Manual Interactive Thickness, Porosity Assessment

Hardness Testing Knoop

65
Printe d

PWB
Wiring
Boards
PRINTED WIRING BOARDS
methods of preparation for ceramics or microelec-
tronic materials for information on these cases. A HELPFUL HINTS FOR
generalized method for non-packed PWB’s of both PWBS
the rigid and flex varieties is presented in Table To improve penetration of acrylic mounting
17.1. A 1µm step may be added if needed. This material into the through-holes of a PWB
method is best used to perform targeted grind- specimen, dip the “pinned” PWB coupons
ing on multiple specimens using semi-automic in liquid hardener immediately prior to
equipment. mounting in acrylic. This will “wick” the
acrylic into the through-holes and minimize
Quality control of manufactured PWB’s often the presence of problematic bubbles in
demands statistical analysis based on plating these critical locations.
thickness measurements taken from the centers
of plated through-holes. However, to generate
enough data for a representative sampling, nu-
merous specimens must be prepared. This is
easiest when coupons are taken from PWB’s and are
ganged together in precise alignment. In this man-
ner, the through holes in all of the coupons can be
sectioned at one time, with one set of consumables.
The PC-Met Precision High Volume Printed Wiring
Board and the PWB Met Small Hole Accessories
allow this type of atuomation.

66
Electronicc
Electroni

ELECTRONIC MATERIALS EM
Materialss
Material

The term, ‘electronic materials’ encompasses we must focus on a few individual materials, and de-
an extremely wide range of materials. This is velop a philosophy of preparation in which we give
due to the fact that most microelectronic devic- our attention specifically to the materials of interest.
es are composites, containing any number of
individual components. For example, present day First and foremost in the class of electronic materials
microprocessor failure analysis might require the is silicon. Silicon is a relatively hard, brittle material,
metallographer to precisely cross section through which does not respond well to grinding with large
a silicon chip plated with multiple thin-film layers of silicon carbide abrasives. Silicon carbide papers
oxides, polymers, ductile metals such as copper or contain strongly bonded abrasive particles which,
aluminum, and refractory metals such as tungsten when they collide with the leading edge of a piece
and/or titanium-tungsten. In addition, the pack- of silicon, create significant impact damage. In
aging of such a device might contain materials of addition, they create tensile stresses on the trailing
such varying mechanical properties as toughened edge of silicon, which results in deep and destruc-
aluminum oxide and solder. The solder materials tive cracking. Cutting close to the target area is
may have compositions ranging up to 97% lead. preferable to grinding, but to accurately approach
With such a vast number of materials incorporated the target area within a silicon device, fine grinding
into a single device, and with these materials having is still necessary. This is the point at which silicon
such highly disparate mechanical properties, it is preparation divides into two distinct classes. The first
virtually impossible to develop a general method for is preparation through traditional metallographic
achieving perfect metallographic results. Instead, techniques. The second is preparation of unencap-
sulated silicon chips (or die), using special fixturing

ELECTRONIC MATERIALS
and abrasives. This second category is a specialized
field of metallography, which is discussed in other
texts [8] and is beyond the scope of this book.
Therefore, we will focus on standard metallographic
techniques throughout this discussion.

Standard preparation of epoxy encapsulated

silicon is similar to general metallographic
preparation, with the exception that only very
Figure 18.1. Aluminum circuitry on silicon substrate Heatsink
Small Outline Package (HSOP), 500x fine grades of silicon carbide paper are used.

Table 18.1: 5-Step Procedure for Preparing Silicon in Microelectronic Devices

Sectioning Precision Saw with blade recommeded for microelectronic devices

Mounting Castable, typically EpoThin
Load - lbs [N] /
Surface Abrasive / Size Specimen Base Speed [rpm] Relative Rotation Time [min:sec]

600 [P1200] grit SiC

CarbiMet 3 [13] 100 Until Plane
water cooled

6μm MetaDi Supreme

VerduTex 5 [22] 100 3:00
Diamond*

3μm MetaDi Supreme

VerduTex 5 [22] 100 3:00
Diamond*

1μm MetaDi Supreme

VerduTex 5 [22] 100 3:00
Diamond*

0.06μm MasterMet
ChemoMet 2 [9] 100 2:00
Colloidal Silica

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Measurement & Analysis Applications, Manual Interactive Thickness

Hardness Testing N/A

67
Electronicc
Electroni

EM
Materialss
Material
ELECTRONIC MATERIALS
Table 18.1 illustrates a typical process of prepara- use of MasterPrep alumina would be: when a silicon
tion with results shown in Figure 18.1. die is attached to a lead frame material such as nick-
el-plated copper, and the lead frame and die attach
Using silicon carbide grinding paper with abrasive materials are the materials of interest. In this case,
sizes coarser than 600 [P1200] grit may cause seri- we are not so concerned with the surface finish of
ous damage to the silicon. Therefore, this method the silicon, but instead, we want to be sure that the
often requires precision cutting or cleaving near to nickel doesn’t smear, and that we are able to discern
the target area of the specimen prior to the initial the true microstructure of the lead frame materials
grinding step. Care must be taken to assure that (refer to the preparation methods for copper and
only precision saw blades designed especially for nickel on pages 47-48).
microelectronic materials are used when cutting.
When preparing a silicon device for the purpose
Silicon responds very well to the chemomechanical of inspecting the metalized, thin film circuitry,
polishing effects of colloidal silica, but not as well to the techniques would be the same as those listed
aluminum oxide. However, there are instances when above. Again, the choice of final polishing agent
an aluminum oxide product, such as the MasterPrep would be determined entirely by the features of
suspension, should be used for final polishing. interest. For instance, aluminum circuitry responds
This relates back to the philosophy of preparation extremely well to the chemomechanical effects of
mentioned earlier. An example of the appropriate colloidal silica, but tungsten and titanium-tungsten
are not as effectively polished with colloidal silica
as are the materials by which they are surrounded.
Therefore, colloidal silica often causes such refrac-
tory metals to stand in relief against a well polished
background. This results in edge rounding of the
refractory metals and can make interface analysis
quite difficult. An alternative is to use an extremely
fine diamond suspension for final polishing in order
to reduce these effects.

When lead alloy solders are the materials of interest

Figure 18.2. Microsection of the Pb Solder Connection, 200x in a microelectronic package (Figure 18.2), we can

Table 18.2: 5-Step Procedure for General Electronic Components

Sectioning Precision Saw with blade recommeded for microelectronic devices

Mounting Castable, typically EpoThin
Load - lbs [N] /
Surface Abrasive / Size Base Speed [rpm] Relative Rotation Time [min:sec]
Specimen

320 [P400] grit SiC Hit the edge of

CarbiMet 3 [13] 150
water cooled the target

9μm MetaDi Supreme

TexMet P 5 [22] 150 5:00
Diamond*

3μm MetaDi Supreme

VerduTex 5 [22] 150 3:00
Diamond*

1μm MetaDi Supreme

VerduTex 5 [22] 150 3:00
Diamond*

0.05μm MasterPrep
ChemoMet 3 [13] 150 1:30
Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Measurement & Analysis Applications, Coating Layer Thickness

Hardness Testing N/A

68
Electronicc
Electroni

ELECTRONIC MATERIALS EM
Materialss
Material

often separate them into two general categories. High removal rates and good surface finishes have
The first is the eutectic, or near-eutectic solders. been obtained on ceramic packages when using
These tend to be ductile, but they respond well to diamond paste on the Apex Hercules S discs.
the same general preparation listed in Table 18.2.
During the 3µm polishing step, the best results are Polishing of high-temperature solders attached to
obtained by using diamond paste. ceramics often produces undesired edge rounding.
However, this cannot be completely avoided. The
Pastes contain a waxy base that reduces diamond cushioning effects of polishing pads will tend to
cause the abrasive to preferentially remove material
from ductile materials faster than from hard, brittle
materials. By using stiff, flat polishing surfaces, one
can reduce this effect, but at the expense of having
additional material embedded in the high-tempera-
ture solder. One effective preparation technique
is to perform a grind-polish-grind-polish type of
procedure. In this technique, a polishing step,
which utilizes a napped polishing cloth, is used in
conjunction with a step-down in abrasive size from
Figure 18.3. Pb-Free Solder in Plated Through Hole, 200x. the previous grinding step. This process is used to
polish out the embedded material. The next step
embedding in ductile metals. Limit the use of is a grinding process, utilizing another step-down

ELECTRONIC MATERIALS
extenders in such cases. A few drops of water in abrasive size, to flatten the specimen again. This
lubrication does not break down the waxy base, continues to a sufficiently fine polishing stage at
and therefore it retains the desired properties of which final polishing will produce the desired result.
diamond paste. Table 18.2 illustrates an example of such a process.

The second category of lead solders is the high

temperature solders (in the range of 90% to 97%
lead). These are difficult to prepare, and require
HELPFUL HINTS FOR
special consideration. This is especially true when ELECTRONIC MATERIALS
they are incorporated into a device that contains Consider what area of the specimen is most
a ceramic package. The mechanical properties critical when choosing a final polishing
of these toughened ceramics require aggressive suspension. For example, the chemome-
grinding techniques, which cause ceramic debris chanical nature of colloidal silicas (such as
(and often, the abrasive used for the grinding op- MasterMet and MasterMet 2) make them
eration) to became embedded in the solder. Silicon ideal for polishing silicon, glass, oxides,
carbide abrasives are a poor choice for grinding in aluminum, and to some degree copper.
such cases, as silicon carbide is only slightly harder However, polishing nickel platings and
(and significantly more brittle) than the typical gold ball bonds with these agents often
packaging material they are intended to grind. As results in smearing. For such non-reactive
the silicon carbide abrasive fractures, it produc- materials, use MasterPrep aluminum oxide
es elongated shards, which embed deeply into final polishing suspension to produce a flat,
high-temperature solders. In addition, they do not scratch-free surface.
grind the ceramic package effectively, and therefore
produce extreme edge rounding at the interface
with the solder. Diamond grinding produces a more
desired result since diamond abrasives are blockier
in shape, and are therefore easier to remove after
they have embedded themselves. In addition, they
are capable of creating a flat surface when ceramic
packages are present.

69
Polymers

P POLYMERS
Plastics and polymers are normally quite soft. Many Mounted specimens are much easier to prepare
different sectioning methods have been used. than nonmounted specimens. Castable resins are
A sharp razor blade or scalpel, or even a pair of preferred as the heat from a mounting press may
scissors, can be used. Microtomes have been used, damage or alter the structure of the specimen.
and a surface cut after refrigeration in liquid nitro- However, there may be a visibility problem if a
gen requires very little subsequent preparation. A transparent, clear polymeric specimen is mounted
jeweler’s saw may be used, although the surface in a clear, transparent epoxy. In this case, EpoColor
is somewhat rough. The precision saw produces resin, with its deep red color, will produce excellent
excellent surfaces, while an abrasive cut-off saw color contrast between specimen and mount in
yields a bit more damage and a rougher surface. darkfield or polarized light. Due to their light weight,
Blades and wheels for sectioning polymers are a specimen may float in the epoxy filled mold. To
available from Buehler. Damage from sectioning is prevent this, put double sided adhesive tape on the
quite easy to remove. bottom of the mold cup and set the specimen on
top of the tape. Always use practices that minimize
Surface quality can be degraded by abrasion from the exotherm during polymerization.
the debris produced during grinding and polishing.

Figure 19.1. Micrograph showing multi-layered polymer meat Figure 19.2. Micrograph of high-density polyethylene
casing mounted in epoxy (dark field, 100X). containing a filler (white particles) (unetched, Nomarski DIC,
100X).

Table 19.1: 6-Step Method for Polymers

Sectioning Precision Saw with 30HC blade recommnded for polymers

Mounting Castable, typically EpoThin
Load - lbs [N] /
Surface Abrasive / Size Base Speed [rpm] Relative Rotation Time [min:sec]
Specimen

320 [P400] grit SiC

CarbiMet 4 [18] 300 Until Plane
water cooled

400 [P600] grit SiC

CarbiMet 4 [18] 300 1:00
water cooled

600 [P1200] grit SiC

CarbiMet 4 [18] 300 1:00
water cooled

1200 [P2500] grit SiC

CarbiMet 4 [18] 300 1:00
water cooled

3μm MetaDi II Diamond

TexMet C 5 [22] 150 4:00
Paste*

0.05μm MasterPrep
MasterTex 3 [13] 150 3:00
Alumina

= Platen = Specimen Holder *Plus MetaDi Fluid Extender as desired

Imaging & Analysis Manual Interactive Thickness

Hardness Testing N/A

70
Preparation of plastics and polymers for microstruc-
tural examination follows the same basic principles HELPFUL HINTS FOR
as for other materials. Automated polishing devices POLYMERS
are preferred to manual preparation. Rough grind- Plastics often have little contrast from the
ing abrasives are unnecessary, even for the planar mounting media when viewed under a
grinding step. Pressures should be lighter than used microscope. This makes thickness mea-
for most metals. surement and discerning edges difficult.
Mounting in EpoColor dye enhanced ep-
Water is generally used as the coolant, although oxy will resolve this situation by producing
some plastics and polymers may react with excellent color contrast between the spec-
water. In such cases, use a fluid that will not imens and mount.
react with the particular plastic or polymer. Em-
bedding can be a problem with plastics and Polymers and plastics may react with fluids
polymers. ASTM E 2015 (Standard Guide for during sectioning and preparation. Always
Preparation of Plastics and Polymeric Speci- check your particular polymer and choose
mens for Microstructural Examination) describes the proper fluid, usually a water, or oil
procedures for preparing several types of plastics based solution to avoid a reaction.
and polymers. Table 19.1 contains a generic pro-
cedure for preparing many plastic and polymeric
materials, see the results in Figures 19.1 and 19.2.
Depending upon the material and the surface
roughness after sectioning, it may be possible
to start grinding with 400 [P800] grit or even 600

POLYMERS
[P1200] grit SiC paper.

If flatness is critical, the final step can be altered. Use

a TexMet cloth with MasterPrep alumina abrasive
slurry running in contra rotation mode at 120-
150rpm for 3 minutes.

71
ETCHING
Metallographic etching encompasses all processes distribution of the phases and inclusions that are
used to reveal particular structural characteristics of present. Examination of the microstructure will
a metal that are not evident in the as-polished con- reveal prior mechanical and thermal treatments
dition. Examination of a properly polished specimen give the metal. Many of these microstructural
before etching may reveal structural aspects such as features are measured either according to
porosity, cracks, and nonmetallic inclusions. Indeed, established image analysis procedures, e.g.,
certain constituents are best measured by image ASTM standards, or internally developed
analysis without etching, because etching will reveal methods.
additional, unwanted detail and make detection Etching is done by immersion or by swabbing (or
difficult or impossible. The classic examples are the electrolytically) with a suitable chemical solution
measurement of inclusions in steels and graphite that essentially produces selective corrosion.
in cast iron. Of course, inclusions are present in all Swabbing is preferred for those metals and
metals, not just steels. Many intermetallic precip- alloys that form a tenacious oxide surface layer
itates and nitrides can be measured effectively in with atmospheric exposure such as stainless steels,
the as-polished condition. aluminum, nickel, niobium, and titanium and their
alloys. It is best to use surgical grade cotton that will
In certain nonferrous alloys that have non-cubic not scratch the polished surface. Etch time varies
crystallographic structures (such as beryllium, with etch strength and can only be determined
hafnium, magnesium, titanium, uranium and zir- by experience. In general, for high magnification
conium), grain size can be revealed adequately examination the etch depth should be shallow;
in the as polished condition using polarized light. while for low magnification examination a deeper
Figure 20.1 shows the microstructure of cold-drawn etch yields better image contrast. Some etchants
zirconium viewed in cross-polarized light. This pro- produce selective results in that only one phase will
duces grain coloration, rather than a “flat etched” be attacked or colored. A vast number of etchants
appearance where only the grain boundaries are have been developed; the reader is directed to
dark. references 1-3, 9 and ASTM E 407. Pages 82-87 list
some of the most commonly used etchants for the
Etching Procedures materials described in this book.

Etchants that reveal grain boundaries are very im-

portant for successful determination of the grain
size. Grain boundary etchants are given in [1-3, 9].
Problems associated with grain boundary etching,
particularly prior austenite grain boundary etching,
are given in [2, 10 and 11]. Measurement of grain
size in austenitic or face-centered cubic metals that
exhibit annealing twins is a commonly encountered
problem. Etchants that will reveal grain boundaries,
Figure 20.1. Mechanical twins at the surface of hot worked but not twin boundaries, are reviewed in [2].
and cold drawn high-purity zirconium viewed with polarized
light (200X).

Microscopic examination is usually limited Selective Etching

to a maximum magnification of 1000X — the Image analysis work is facilitated if the etchant
approximate useful limit of the light microscope, chosen improves the contrast between the fea-
unless oil immersion objectives are used. Many ture of interest and everything else. Thousands
image analysis systems use relay lenses that yield of etchants have been developed over the years,
higher screen magnifications that may make but only a small number of these are selective in
detection of fine structures easier. However, nature. Although the selection of the best etchant,
resolution is not improved beyond the limit of and its proper use, is a very critical phase of the
0.2-0.3µm for the light microscope. Microscopic image analysis process, only a few publications
examination of a properly prepared specimen have addressed this problem [12-14]. Selective
will clearly reveal structural characteristics such as etchants, that is, etchants that preferentially
grain size, segregation, and the shape, size, and attack or color a specific phase, are listed in

72
ETCHING
[1-3, 9, 13 and 14] and illustrated in 13 and 14. exists as simple grain boundary films) but no ferrite
Stansbury [15] has described how potentiostatic grain boundaries. If one is interested in the amount
etching works and has listed many preferential and nature of the cementite (which can influence
potentiostatic etching methods. The potentiostat formability), then the picral etch is far superior to
offers the ultimate in control over the etching pro- the nital etch as picral revealed only the cementite.
cess and is an outstanding tool for this purpose. Tint etching with Beraha’s solution (Klemm’s I could
Many tint etchants act selectively in that they col- also be used) colored the grains according to their
or either the anodic or cathodic constituent in a crystallographic orientation. With the development
microstructure. Tint etchants are listed and illustrat- of color image analyzers, this image can now be
ed in several publications [1-3, 16-21]. used quite effectively to provide accurate grain size
measurements since all of the grains are colored.
A classic example of the different behavior of
etchants is given in Figure 20.2 where low-carbon Figure 20.3 shows a somewhat more complex
sheet steel has been etched with the standard nital example of selective etching. The micrograph
and picral etchants, and also a color tint etch. Etch- shows the ferrite-cementite-iron phosphide ter-
ing with 2% nital reveals the ferrite grain boundaries nary eutectic in gray iron. Etching sequentially
and cementite. Note that many of the ferrite grain with picral and nital revealed the eutectic, Figure
boundaries are missing or quite faint; a problem that 20.3a, surrounded by pearlite. Etching with boiling
degrades the accuracy of grain size ratings. Etching alkaline sodium picrate, Figure 20.3b, colored the
with 4% picral reveals the cementite aggregates cementite phase only, including in the surrounding
(one could not call this pearlite as it is too nonla- pearlite (a higher magnification is required to see
mellar in appearance and some of the cementite the very finely spaced cementite that is more lightly

ETCHING
a
a

b b

c c
Figure 20.2. Microstructure of low-carbon sheet steel etched Figure 20.3. The ternary eutectic (α-Fe3C-Fe3P) in gray cast iron
with (a, top) 2% nital, (b, middle) 4% picral; and (c, bottom) revealed by etching a) in picral and nital to “outline” the phases
Beraha’s reagent (100mℓ water, 10g Na2S2O3 and 3g K2S2O5) at b) boiling alkaline sodium picrate to color the cementite. c)
100X. boiling Murakami’s reagent to color the phosphide (200X).

73
ETCHING
colored). Etching with boiling Murakami’s reagent, lective characteristics. Of the four shown in Figures
Figure 20.3c, colors the iron phosphide darkly and 20.4c to f, only aqueous 60% nitric acid produced
will lightly color the cementite after prolonged any gray level discrimination between the phases,
etching. The ferrite could be colored preferentially and that was weak. All revealed the phase boundar-
if Klemm’s I was used. ies nicely, however. Two electrolytic reagents, shown
in Figures 20.4g and h, are commonly used to color
Selective etching has been commonly applied to ferrite in dual phase grades and delta ferrite in
stainless steels for detection, identification and martensitic grades. Of these, aqueous 20% sodium
measurement of delta ferrite, ferrite in dual phase hydroxide, Figure 20.4g, usually gives more uniform
grades, and sigma phase. Figure 20.4 shows exam- coloring of the ferrite. Murakami’s and Groesbeck’s
ples of the use of a number of popular etchants to reagents have also been used for this purpose.
reveal the microstructure of a dual phase stainless Tint etchants have been developed by Beraha that
steel in the hot rolled and annealed condition. Fig- color the ferrite phase nicely, as demonstrated in
ure 20.4a shows a well delineated structure when Figure 20.4i.
the specimen was immersed in ethanolic 15% HCl
for 30 minutes. All of the phase boundaries are Selective etching techniques are not limited to iron-
clearly revealed, but there is no discrimination be- based alloys, although these have more thoroughly
tween ferrite and austenite. Twin boundaries in the developed than for any other alloy system. Selective
austenite are not revealed. Glyceregia, a etchant etching of beta phase in alpha-beta copper alloys
for stainless steels, was not suitable for this grade, has been a popular subject. Figure 20.5 illustrates
Figure 20.4b, as it appears to be rather orientation coloring of beta phase in Naval Brass (UNS 46400)
sensitive. Many electrolytic etchants have been used using Klemm’s I reagent. Selective etching has a
for etching stainless steels, but only a few have se- long historical record for identification of interme-

a b

c d

e f
Figure 20.4. Microstructure of a duplex stainless steel revealed using a) alcoholic 15% HCl by immersion (30 min.); and, with b) glyceregia
by swabbing (2 min.) c) aqueous 60% HNO3 (1 V DC, 20 seconds); with d) aqueous 10% oxalic acid (6 V DC, 75 seconds); with e) aqueous
10% CrO3 (6 V DC, 30 seconds); and, with (f) aqueous 2% H2SO4 (5 V DC, 30 seconds) at 200X.

74
ETCHING

g
Figure 20.5. Beta phase colored in Naval Brass (Cu-39.7% Zn-
0.8% Sn) by immersion color etching with Klemm’s I reagent
(200X).

Electrolytic Etching and Anodizing

The procedure for electrolytic etching is basical-
ly the same as for electropolishing except that
voltage and current densities are considerably
lower. The specimen is made the anode, and
some relatively insoluble but conductive material
such as stainless steel, graphite, or platinum is
used for the cathode. Direct current electrolysis
is used for most electrolytic etching. Electrolytic
etching is commonly used with stainless steels,
either to reveal grain boundaries without twin

ETCHING
boundaries, or for coloring ferrite (as illustrated)
in Figure 20.4i, delta ferrite, sigma or chi phases.
Anodizing is a term applied to electrolytic etchants
that develop grain coloration when viewed with
i crossed-polarized light, as in the case of aluminum,
Figure 20.4. Selective coloring of ferrite in a duplex stainless
steel by electrolytic etching with g) aqueous 20% NaOH (4 tantalum, titanium, tungsten, uranium, vanadium
V DC, 10 seconds) and with h) aqueous 10 N KOH, (3 V DC, and zirconium [2]. Figure 20.8 shows the grain
4 seconds); and by immersion color etching i) with Beraha’s
reagent (100mℓ water, 10mℓ HCl and 1g K2S2O5) at 200X. structure of 5754 aluminum revealed by anodizing
with Barker’s reagent, viewed with crossed-polar-
tallic phases in aluminum alloys. This method was ized light. Again, color image analysis makes this
used for many years before the development of en- image useful now for grain size measurements.
ergy-dispersive spectroscopy. Today, it is still useful
for image analysis work. Figure 20.6 shows selective
coloration of theta phase, CuAl2, in the Al-33%
Cu eutectic alloy. As a final example, Figure 20.7
illustrates the structure of a simple WC-Co sintered
carbide, cutting tool. In the as-polished condition,
Figure 20.7a, the cobalt binder can be seen faintly
against the more grayish tungsten carbide grains. A
few particles of graphite are visible. In Figure 20.7b,
light relief polishing has brought out the outlines
of the cobalt binder phase, but this image is not
Figure 20.6. Theta phase, CuAl2, colored in the α-Al/CuAl2
particularly useful for image analysis. Etching in a eutectic in an as-cast Al-33% Cu specimen by immersion color
etching with the Lienard and Pacque etch (200mℓ water, 1g
solution of hydrochloric acid saturated with ferric ammonium molybdate, 6g ammonium chloride) at 1000X.
chloride, Figure 20.7c, attacks the cobalt and pro-
vides good uniform contrast for measurement of the
cobalt binder phase. Following this with Murakami’s Heat Tinting
reagent at room temperature reveals the edges of Although not commonly utilized, heat tinting
the tungsten carbide grains, useful for evaluation [2] is an excellent method for obtaining color
of the WC grain size, Figure 20.7d. contrast between constituents or grains. An

75
ETCHING

a
Figure 20.8. Grain structure of annealed 5754 aluminum sheet
revealed by anodizing with Barker’s reagent (30 V DC, 2 min.)
and viewing with polarized light plus sensitive tint (100X).

Interference Layer Method

The interference layer method [2], introduced
by Pepperhoff in 1960, is another procedure for
obtaining a film over the microstructure that
generates color by interference effects. In this
b method, a suitable material is deposited on the
polished specimen face by vapor deposition to
produce a low-absorption, dielectric film with a high
refractive index at a thickness within the range for
interference. Very small differences in the natural
reflectivity between constituents and the matrix can
be dramatically enhanced by this method. Suitable
materials for the production of evaporation layers
have been summarized in [22,23]. The technique is
universally applicable, but does require a vacuum
c
evaporator. Its main weakness is difficulty in obtain-
ing a uniformly coated large surface area for image
analysis measurements.

d
Figure 20.7. Microstructure of WC-Co cutting tool: a) as-polished
revealing graphite particles; b) relief polished revealing the
cobalt binder phase; c) after immersion in Chaporova’s etch (HCl
saturated with FeCl3) to attack and “darken” the cobalt; and,
d) after (c) plus Murakami’s reagent to outline the WC grains
(1000X). Figure 20.9. Grain structure of annealed CP titanium revealed by
unmounted polished specimen is placed face up heat tinting on a hot plate (100X, polarized light plus sensitive
tint).
in an air-fired furnace at a set temperature and
held there as an oxide film grows on the surface.
Interference effects, as in tint etching, create col- See Tables 20.1 – 20.13 for a list of the most com-
oration for film thicknesses within a certain range, mon etchants used for metals and alloys.
about 30-500nm. The observed color is a function
of the function of the film thickness. Naturally, the
thermal exposure cannot alter the microstructure.
The correct temperature must be determined by the
trial-and-error approach, but the procedure is repro-
ducible and reliable. Figure 20.9 shows the grain
structure of CP titanium revealed by heat tinting.

76
COMMON ETCHANTS FOR METALS & ALLOYS3
Table 20.1: Light Metals - Aluminum Alloys
Composition Comments
1. 95mℓ water Keller’s reagent, very popular general purpose reagent for Al and Al alloys, except high-Si
2.5mℓ HNO3 alloys. Immerse sample 10-20 seconds, wash in warm water. Can follow with a dip in conc.
1.5mℓ HCl HNO3. Outlines all common constituents, reveals grain structure in certain alloys when used by
1.0mℓ HF immersion.
2. 90-100mℓ water General purpose reagent. Attacks FeAl3, other constituents outlined. The 0.5% concentrations of
0.1-10mℓ HF HF is very popular.
3. 84mℓ water
15.5mℓ HNO3 Graff and Sargent’s etchant, for grain sizes of 2XXX, 3XXX, 6XXX, and 7XXX wrought alloys.
0.5mℓ HF Immerse specimen 20-60 seconds with mild agitation.
3g CrO3
Barker’s anodizing method for grain structure. Use 0.5-1.5 A/in2, 30-45 V DC. For most alloys
4. 1.8% fluoboric acid in
and tempers, 20 seconds at 1 A/in2 and 30 V DC at 68° [20°C] is sufficient. Stirring not needed.
water
Rinse in warm water and dry. Use polarized light; sensitive tint helpful.
5. 4g KMnO4 Weck's tint etchant for Al and Al alloys, a very popular etchant for general purpose, especially
1g NaOH good for reveal the grain of wrought alloys. Immerse sample for 15-20 seconds and gently wave
100mℓ water the sample until the surface is colored.

Table 20.2: Magnesium and Alloys

Composition Comments
6. 25mℓ water
Glycol etch, general purpose etch for pure MG and alloys. Swab specimen seconds for F and T6
75mℓ 3-5 ethylene glycol
temper alloys, 1-2 minutes for T4 and 0 temper alloys.
1mℓ HNO3

ETCHING
7. 19mℓ water
Acetic glycol etchant for pure Mg and alloys. Swab specimen 1-3 seconds for F and T6 temper
60mℓ ethylene glycol
alloys, 10 seconds for T4 and 0 temper alloys. Reveals grain boundaries in solution treated
20mℓ acetic acid
castings and most wrought alloys.
1mℓ HNO3
8. 100mℓ ethanol
10mℓ water For MG and alloys. Use fresh. Immerse specimen for 15-30 seconds. Produces grain contrast.
5g picric acid

HELPFUL HINTS FOR ETCHING

Many etchants can be used by swabbing
or by immersion. Swabbing is preferred for
those specimens that form a tight protective
oxide on the surface in air, such as Al, Ni, Cr,
stainless steels, Nb (Cb), Ti and Zr. However,
if the etchant forms a film, as in tint etchants,
then immersion must be used as swabbing
will keep the film from forming. Keller’s
reagent reveals the grain size of certain
aluminum alloys by forming a film. This will
not occur if the etch is used by swabbing.

Many etchants, and their ingredients, do

present potential health hazards to the
user. ASTM E 2014, Standard Guide on
Metallography Laboratory Safety, describes
many of the common problems and how to
avoid them.

3
When water is specified, always use distilled water. It is best to use reagent grade chemicals. Etchants can be quite dangerous and it is advisable to
consult with a chemist when dealing with new etchants that may be potentially dangerous. ASTM E 2014, Standard Guide on Metallographic Laboratory
Safety, is a valuable reference.

77
COMMON ETCHANTS FOR METALS & ALLOYS3
Table 20.3: Low Melting Point Metals - Sb, Bi, Cd, Pb, Sn and Zn
Composition Comments
9. 100mℓ water
30mℓ HCl For Sb, Bi and alloys. Immerse specimen up to a few minutes.
2g FeCl3
10. 100mℓ water
25mℓ HCl to a For Sb-Pb, Bi-Sn, Cd-Sn, Cd-Zn and Bi-Cd alloys. Immerse specimen up to a few minutes.
8g FeCl3
For Cd, Cd alloys, Sn, Zn alloys, Pb and alloys, Bi-Sn eutectic alloy and Bi-Cd alloys. Can add a
11. 95-99mℓ ethanol
few drops of zephiran chloride. Immerse sample. For Pb and alloys, if stain forms, wash in 10%
1-5mℓ HNO3
alcoholic HCl.
12. 100mℓ water
10g ammonium Pollack’s reagent for Pb and alloys. Immerse specimen 15-30 seconds. Other compositions used
molybdate are: 100mℓ: 9g: 15g and 100mℓ: 10g: 25g.
10g citric acid
13. 100mℓ water
2mℓ HCl For Sn-based babbitt metal. Immerse specimen up to 5 minutes.
10g FeCl3
14. 200mℓ water
Palmerton reagent for pure Zn and alloys. Immerse specimen up to 3 minutes. Rinse in 20%
40g CrO3
aqueous CrO3.
3g Na2SO4
15. 200mℓ water
Modified Palmerton reagent for Zn die-casting alloys. Immerse specimen for several seconds,
10g CrO3
rinse in 20% aqueous CrO3.
1g Na2SO4
16. 50mℓ Stock Solution*
Klemm's I Reagent. For Zn and lean alloys. Immerse the sample and gently shake it until the
1g K2S2O5
surface is colored, usually 30s.

* Stock solution: aqueous cold-saturated Na2S2O3 solution

3
When water is specified, always use distilled water. It is best to use reagent grade chemicals. Etchants can be quite dangerous and it is advisable to
consul with a chemist when dealing with new etchants that may be potentially dangerous. ASTM E 2014, Standard Guide on Metallographic Laboratory
Safety, is a valuable reference.

78
COMMON ETCHANTS FOR METALS & ALLOYS3
Table 20.4: Refractory Metals - Ti, Zr, Hf, Cr, Mo, Re, Nb, Ta, W and V
Composition Comments
17. 100mℓ water
1-3mℓ HF Kroll’s reagent for Ti alloys. Swab specimen 3-10 seconds or immerse specimen 10-30 seconds.
2-6mℓ HNO3
18. 200mℓ water For Ti, Zr and alloys. Swab or immerse specimen. Higher concentrations can be used but are
1mℓ HF prone to staining problems.
19. 30mℓ lactic acid
For Ti alloys. Swab specimen up to 30 seconds. Decomposes, do not store. Good for alpha-beta
15mℓ HNO3
alloys.
30mℓ HF
20. 30mℓ HCl
15mℓ HNO3 For Zr, Hf and alloys. Swab specimen 3-10 seconds or immerse specimen up to 2 minutes.
30mℓ HF
21. 45mℓ H20 (H2O2 or
Cain’s chemical polish and etch for Hf, Zr and alloys. Can dilute aqueous solution with 3-5 parts
glycerol)
water to stain the structure (swab specimen) after chemical polishing. Chemically polish and
45mℓ HNO3
etch specimen by swabbing 5-20 seconds. Use polarized light.
8-10mℓ HF
22. 60mℓ HCl Aqua regia. For Cr and alloys. Immerse or swab specimen up to 1 minute. Use under a hood
20mℓ HNO3 with care, do not store.
23. 30mℓ HCl
45mℓ glycerol Modified “Glyceregia.” For Cr and alloys. Immerse specimen up to a few minutes.
15mℓ HNO3
24. 100mℓ water
Murakami’s reagent. For Cr, Mo, Re, Ta-Mo, W, V and alloys. Use fresh, can immerse sample for
10g KOH or NaOH
up to 1 minute.
10g K3Fe(CN)6
25. 70mℓ water
For Mo alloys. Immerse specimen 2 minutes. Wash with water and dry; immersion produces
20mℓ H2O2 (30%)
colors, swabbing produces grain-boundary etch.

ETCHING
10mℓ H2SO4
26. 10-20mℓ glycerol
10mℓ HNO3 For Mo and Mo-Ti alloys. Immerse specimen for up to 5 minutes.
10mℓ HF
27. 100mℓ water
5g K3Fe(CN)6 For Mo-Re alloys. Use at 68°F [20°C] by immersion.
2g KOH
28. 50mℓ acetic acid
20mℓ HNO3 For Nb, Ta and alloys. Swab specimen 10-30 seconds.
5mℓ HF
29. 50mℓ water
14mℓ H2SO4 DuPont Nb reagent. For Nb-Hf and Nb alloys.
5mℓ HNO3
30. 50mℓ water
50mℓ HNO3 Fo Nb-Zr and Nb-Zr-Re alloys. Swab specimen.
1mℓ HF
31. 30mℓ lactic acid
10mℓ HNO3 For Re and W-Re alloys. Swab specimen.
5mℓ HF
32. 10mℓ HF
For V and alloys; grain-boundary etch for Ta alloys. Swab specimen. Equal parts used for Ta and
10mℓ HNO3
high Ta alloys.
10-30mℓ glycerol
Modified Weck's tint etchant. Good etchant for Ti and Ti alloys to reveal the grain structure. Use
33. 100mℓ water
by immersion of sample until the sample surface is colored, usually around 15-25 seconds. The
50mℓ Ethanol
color thin film formation is more uniform if gently shake the sample during the etching process.
2g NH4HF2
The etch artifacts produced can be eliminated using only 25mℓ ethanol.

3
When water is specified, always use distilled water. It is best to use reagent grade chemicals. Etchants can be quite dangerous and it is advisable to
consul with a chemist when dealing with new etchants that may be potentially dangerous. ASTM E 2014, Standard Guide on Metallographic Laboratory
Safety, is a valuable reference.

79
COMMON ETCHANTS FOR METALS & ALLOYS3
Table 20.5: Iron and Steel
Composition Comments
Nital. Most common etchant for Fe, carbon and alloy steels, cast iron. Reveals alpha grain
34. 90-99mℓ methanol or
boundaries and constituents. Excellent for martensitic structures. The 2% solution is most
ethanol
common, 5-10% used for high alloy steels (do not store). Use by immersion or swabbing of
1-10mℓ HNO3
sample for up to about 1 minute.
35. 100mℓ ethanol Picral. Recommented for structures consisting of ferrite and carbide. Does not reveal ferrite
4g picric acid grain boundaries. Addition of 0.5-1% zephiran chloride improves etch rate and uniformity.
Vilella’s reagent. Good for ferrite-carbide structures. Produces grain contrast for estimating
36. 100mℓ ethanol
prior austenite grain size. Results best on matentsite tempered at 572-932°F [300-500°C].
5mℓ HCl
Occasionally reveals prior-austenite grain boundaries in high alloys steels. Outlines constituents
1g picric acid
in stainless steels. Good for tool steels and martensitic stainless steels.
Bechet and Beaujard’s etch, most successful etchant for prior-austenite boundaries. Good
for martensitic bainitic steels. Many wetting agents have been used, sodium tridecylbenzene
37. Saturated aqueous
sulfonate is one of the most successful (the dodecyl version is easier to obtain and works as
picric acid solution grain
well). Use at 68-212°F [20-100°C]. Swab or immerse sample for 2-60 minutes. Etch in ultrasonic
plus small amount of a
cleaner (see ref. 2, pg 219-223). Additions of 0.5 CuCl2 per 100mℓ solution or about 1% HCl
wetting agent
have been used for higher alloy steels to produce etching. Room temperature etching most
common. Lightly back polish to remove surface smut.
38. 150mℓ water
50mℓ HCl
Modified Fry’s reagent. Used for 18% Ni maraging steels, martensitic and PH stainless steels.
25mℓ HNO3
1g CuCl2
Alkaline sodium picrate. Best etch for McQuaid-Ehn carburized samples. Darkens cementite.
39. 100mℓ water
Use boiling for 1-15 minutes or electrolytic at 6 V DC, 0.5 A/in2, 30-120 seconds. May reveal
25g NaOH
prior-austenite grain boundaries in high carbon steels when no apparent grain boundary film is
2g picric acid
present.
40. 3 parts HCl
“Glyceregia.” For austenitic stainless steels. Reveals grain structure, outlines sigma and carbides.
2 parts glycerol
Mix fresh, do not store. Use by swabbing.
1 part HNO3
41. 100mℓ ethanol Kalling’s no. 2 (“waterless” Kalling’s) etch for austenitic and duplex stainless steels. Ferrite
100mℓ HCl attacked readily, carbides unattacked, austenite slightly attacked. Use at 68°F [20°C] by
5g CuCl2 immersion or swabbing. Can be stored.
42. 15mℓ HCl
10mℓ acetic acid
Acetic glyceregia. Mix fresh, do not store. Use for high alloy stainless steels.
5mℓ HNO3
2 drops glycerol
Murakami’s reagent. Usually works better on ferritic stainless grades than austenitic grades. Use
43. 100mℓ water at 68°F [20°C] for 7-60 seconds: reveals carbides sigma faintly attacked with etching up to 3
10g K2Fe(CN)6 minutes. Use at 176°F [80°C] to boiling for 2-60 minutes: carbides dark, sigma blue (not always
10g KOH or NaOH attacked), ferrite yellow to yellow-brown, austenite unattacked. Do not always get uniform
etching.
Use for stainless steels at 6 V DC. Carbides reveal by etching for 15-30 seconds, grain
44. 100mℓ water
boundaries after 45-60 seconds, sigma outlined after 6 seconds. 1-3 V also used. Dissolves
10g oxalic acid
carbides, sigma strongly attacked, austenite moderately attacked, ferrite unattacked.
45. 100mℓ water Used to color ferrite in martensitic, PH or dual-phase stainless steels. Use at 3-5 V DC, 68°F
20g NaOH [20°C], 5 seconds, stainless steel cathode. Ferrite outlines and colored tan.
Electrolytic etch to reveal austenite boundaries but not twin boundaries in austenitic stainless
46. 40mℓ water
steels (304, 316, etc.). Voltage is critical. Pt cathode preferred to stainless steel. Use at 1.4V DC,
60mℓ HNO3
2 minutes (see ref.2, pgs 235, 238 and 239).
Klemm's I Reagent. Immerse at room temperature until surface is colored. It is good to color
47. 50mℓ Stock Solution*
ferrite in steel, reveals P segregation and overheating, etching time is 40-100 seconds. For
1g K2S2O5
coloring ferrite and martensite in cast iron low-alloy steels, usually up to 3 minutes.
Klemm's II Reagent. For steel sample, immerse for 30-90 seconds at 20°C, reveals P segregation.
48. 50mℓ Stock Solution*
For austenitic Mn Steels, gamma yellow to brown or light to dark blue, alpha-martensite dark
5g K2S2O5
brown. Good for austenitic manganese steels.
Beraha's Selenic Acid Etch 1. For cast iron, steels, and tool steels. For better result, Nital pre-etch
49. 100mℓ Ehtanol
is recommended. Use by immersion of sample until the sample surface is colored, usually up
2mℓ HCl
to 6 minutes. Cementite colored red-violet, ferrite colored yellow or brown, phosphide colored
0.5mℓ H2SeO4
blue-green.
Beraha’s Selenic Acid Etch 2. In general, immerse sample at 20°C for 1-10 minutes. A yellow or
50. 100mℓ Ethanol
light-brown surface color is formed to detect carbides and nitrides or an orange to red surface
5-10mℓ HCl
is formed to detect delta ferrite. Can use 20-30mℓ HCl for higher alloy grades, immersion time
1-3mℓ H2SeO4
decrease with higher HCl.
* Stock solution: aqueous cold-saturated Na2S2O3 solution

3
When water is specified, always use distilled water. It is best to use reagent grade chemicals. Etchants can be quite dangerous and it is advisable to
consul with a chemist when dealing with new etchants that may be potentially dangerous. ASTM E 2014, Standard Guide on Metallographic Laboratory
Safety, is a valuable reference.
80
COMMON ETCHANTS FOR METALS & ALLOYS3
Table 20.6: Copper, Nickel and Cobalt: Copper and Alloys
Composition Comments
51. 25mℓ NH4OH
General purpose grain contrast etch for Cu and alloys (produces a flat etch for some alloys). Use
25mℓ water (optional)
fresh, add peroxide last. Use under a hood. Swab specimen 5-45 seconds.
25-50mℓ H2O2 (3%)
52. 100mℓ water
General purpose etch for Cu and alloys. Immerse or swab for 3-60 seconds. Reveals grain
10g ammonium
boundaries but is sensitive to crystallographic orientation.
persulfate
53. 100mℓ water
3g ammonium persulfate General purpose etch for Cu and alloys, particulatly Cu-Be alloys.
1mℓ NH4OH
54. 70mℓ water
Excellent general purpose etch, reveals grain boundaries well. Immerse specimen 10-30
5g Fe(NO3)3
seconds.
25mℓ HCl
Beraha's Selenic Acid Etchant for brass and Cu-Be alloys. Pre-etch the sample is useful for clear
55. 300mℓ Ethanol
grain-boundary. Immerse sample until surface is violet-blue to blue. Use plastic tongs and
2mℓ HCl
storage in dark bottle. If the reaction is too fast and the color changes too quick, use 0.5mL
0.5 -1mℓ Selenic Acid
selenic acid.
56. 50mℓ Stock Solution* Klemm’s I reagent. It is a good etchant for beta brass, alpha-beta brass, and bronzes. Immerse
1g K2S2O5 for 2 minutes or more and gently wave the sample until the surface is colored. For alpha brass,
the reaction is very slow, usually up to 60 minutes.

Klemm's III reagent. Excellent etchant for copper alloys and best for the cartridge brass.
57. 50mℓ Stock Solution*
Although the color range was limited, results were very good in bright field. Polarized light and
1g K2S2O5
sensitive tint improves color response. Immerse sample 3-5 minutes for bronze alloys.

58. 5mℓ Stock Solution* Klemm's III reagent. Excellent etchant for copper alloys and best for the cartridge brass.
45mℓ Water Although the color range was limited, results were very good in bright field. Polarized light and
20g K2S2O5 sensitive tint improves color response. Immerse sample 3-5 minutes for bronze alloys.

ETCHING
* Stock solution: aqueous cold-saturated Na2S2O3 solution

Table 20.7: Nickel and Alloys

Composition Comments
59. 5g FeCl3
2mℓ HCl Carapella’s etch for Ni and Ni-Cu (Monel) alloys. Use by immersion or swabbing.
99mℓ ethanol
60. 40-80mℓ ethanol
Kalling’s no. 2 etch (“waterless” Kalling’s) for Ni-Cu alloys and superalloys. Immerse or swab
40mℓ HCl
specimen up to a few minutes.
2g CuCl2
61. 50mℓ water
Marble’s reagent for Ni, Ni-Cu and Ni-Fe alloys and superalloys. Immerse or swab sample 5-60
50mℓ HCl
seconds. Reveals grain structure of superalloys.
10g CuSO4
62. 15mℓ HCl
“Glyceregia,” for superalloys and Ni-Cr alloys. Swab specimen for 5-60 seconds. Mix fresh. Do
10mℓ glycerol
not store. Use under hood.
5mℓ HNO3
63. 60mℓ glycerol
Modified Glyceregia for superalloys. Reveals preciptates. Use under hood; do not store. Add
50mℓ HCl
HNO3 last. Discard when dark yellow. Immerse or swab specime 10-60 seconds.
10mℓ HNO3

3
When water is specified, always use distilled water. It is best to use reagent grade chemicals. Etchants can be quite dangerous and it is advisable to
consul with a chemist when dealing with new etchants that may be potentially dangerous. ASTM E 2014, Standard Guide on Metallographic Laboratory
Safety, is a valuable reference.

81
COMMON ETCHANTS FOR METALS & ALLOYS3
Table 20.8: Cobalt and Alloys
Composition Comments
64. 60mℓ HCl
15mℓ water For Co and alloys. Mix fresh and age 1 hour before use. Immerse specimen for up to 30 seconds.
15mℓ acetic acid Do not store.
15mℓ HNO3
65. 200mℓ ethanol
7.5mℓ HF General etch for Co and alloys. Immerse specimen 2-4 minutes.
2.5mℓ HNO3
66. 50mℓ water
50mℓ HCl Marble’s reagent for Co high temperature alloys. Immerse specimen for up to 1 minute.
10g CuSO4
67. 80mℓ lactic acid
10mℓ H2O2 (30%) For Co alloys. Use by swabbing.
10mℓ HNO3

Table 20.9: Precious Metals: Au, Ag, Ir, Os, Pd, Pt, Rh and Ru
Composition Comments
68. 60mℓ HCl For gold, silver, palladium and high noble metal alloys. Use under hood. Immerse specimen up
40mℓ HNO3 to 60 seconds. Equal parts of each acid also used.
69. 60mℓ HCl
Aqua regia for pure gold, Pt and alloys, some Rh alloys. Use boiling for up to 30 minutes.
20mℓ HNO3
70. 1-5g CrO3
For Au, Ag, Pd, and alloys. Swab or immerse specimen up to 60 seconds.
100mℓ HCl
71. 30mℓ water
25mℓ HCl For pure Pt. Use hot, immerse specimen up to 5 minutes.
5mℓ HNO3
72. Conc. HCl For Rh and alloys. Use at 5 V AC, 1-2 minutes, graphite cathose, Pt lead wires.
73. Solution A:
100mℓ water
For Ru. Mix 4 parts Solution A to 1 part Solution B, use 5-20 V AC, 1-2 minutes, graphite cathode,
40g NaCl
Pt-lead wires.
Solution B:
Conc. HCl
74. 50mℓ NH4OH For pure Ag, Ag solders and Ag-Pd alloys. Mix fresh. Swab specimen up to 60 seconds. Discard
20mℓ H2O2 (3%) after etching. Use a 50:50 mix for sterling silver; for fine silver, use 30% conc. hydrogen peroxide.
75. Solution A:
10g NaCN For gold alloys up to 18 karat. Mix equal amounts of A and B directly on the specimen using eye
100mℓ water droppers. Swab and replenish the etchants until desired etch level is obtained. If brown stain
Solution B: forms, swab with A to remove it.
H2O2 (30%)

Table 20.10: Sintered Carbides

Composition Comments
76. 100mℓ water
Murakami’s reagent, for WC-Co and complex sintered carbides. Immerse specimen seconds
10g KOH or NaOH
to minutes. Use 2-10 seconds to identify eta phase (colored). Longer times attack eta. Reveals
10g K3Fe(CN)6
phase and grain boundaries.
Normally used at 20°C
77. 97mℓ water For WC, MO2C, TiC or Ni in sintered carbides. Use boiling for up to 60 seconds. For coarse
3mℓ H2O2 (30%) carbides or high Co content, use short etch time.
78. 15mℓ water
30mℓ HCl
For WC, WiC, TaC and Co in sintered carbides. Use at 68°F [20°C] for 5-30 seconds.
15mℓ HNO3
15mℓ acetic acid
79. 100mℓ water
To darken Co (or Ni) binder phase. Mix fresh. Swab 10 seconds.
3g FeCl3

3
When water is specified, always use distilled water. It is best to use reagent grade chemicals. Etchants can be quite dangerous and it is advisable to
consul with a chemist when dealing with new etchants that may be potentially dangerous. ASTM E 2014, Standard Guide on Metallographic Laboratory
Safety, is a valuable reference.

82
COMMON ETCHANTS FOR METALS & ALLOYS3
Table 20.11: Ceramics and Nitrides
Composition Comments
For alumina, Al2O3, and silicon nitride, Si3N4. Use by immersion at 482°F [250°C] for up to a few
80. Phosphoric acid
minutes for Al2O3 or up to 15 minutes for Si3N4.
81. 100mℓ water
For magnesia, MgO. Use by immersion at 77-140°F [25-60°C] for several minutes.
15mℓ HNO3
82. 100mℓ water
5g NH4FHF For titania, TiO2. Immerse up to a few minutes.
4mℓ HCl
83. 50mℓ water
For zirconia, ZrO2. Use by immersion in boiling solution for up to 5 minutes.
50mℓ H2SO4
84. HCl For calcia, CaO, or MgO. Immerse for up to 6 minutes.
85. HF For Si3N4, BeO, BaO, MgO, ZrO2 and Zr2O3. Immerse for up to 6 minutes.

Table 20.12: Plastics and Polymers

Composition Comments
86. 100mℓ water
For polypropylene (PP). Immerse for up to several hours at 158°F [70°C].
60g CrO3
87. HNO3 For polyethylene (PE). Immerse for up to a few minutes.
88. Xylol Reveals spherolites in polyethylene (PE). Immerse for up to a few days at 158°F [70°C].
89. 70mℓ water
For polyoxymethylene (POM). Immerse up to 20 seconds.
30mℓ HCl
For polyamid (PA) and polyethylene (PE). Use at 158°F [70°C] for 60 seconds. For Nylon 6, use at
90. Xylene

ETCHING
149-158°F [65-70°C] for 2-3 minutes. For Nylon 6, use at 167°F [75°C] for 3-4 minutes.

Table 20.13: Electrolytic Etching

Composition Comments
91. 700mℓ ethyl alcohol
120mℓ water Electrolyte for polishing and etching of Al and Al alloys. Polishing time is 30-60 seconds. at 30V
80mℓ perchloric acid DC, etching time is 20 seconds at 5-10V DC.
100mℓ butylglycol
92. 625mℓ Ethanol
Electrolyte for polishing of Mg and Mg alloys. Polishing time is up to several mins. at 30-40V DC.
375mℓ Phosphoric Acid
93. 700mℓ ethyl alcohol
120mℓ water Electrolyte for polishing and etching of carbon and HS steels in different conditions. Polishing
80mℓ perchloric acid time is 60-90 seconds at 30-40V DC, etching time is 20 seconds at 5-10V DC.
100mℓ butylglycol
94. 500mℓ water Electrolyte for polishing and etching of Copper and alloys. Polishing time is 60 seconds at 20-
250mℓ Ethanol 30V DC and etching time is 20 seconds at 5-10V DC. Adding the phosphoric slowly at the end
250mℓ Phosphoric Acid and wait till it’s cooled down.

3
When water is specified, always use distilled water. It is best to use reagent grade chemicals. Etchants can be quite dangerous and it is advisable to
consul with a chemist when dealing with new etchants that may be potentially dangerous. ASTM E 2014, Standard Guide on Metallographic Laboratory
Safety, is a valuable reference.

83
LIGHT OPTICAL MICROSCOPY
Metallurgical microscopes differ from biological makes examination of these features most efficient.
microscopes primarily in the manner by which the Some materials do not require etching and, in a few
specimen is illuminated due to the opacity of met- cases, examination is less satisfactory after etching.
als. Unlike biological microscopes, metallurgical
microscopes must use reflected light, rather than For most metals, etching must be used to ful-
transmitted light. Figure 21.1 is a simplified light ly reveal the microstructure. A wide range of
ray diagram of a metallurgical microscope. The processes are used, the most common being
prepared specimen is placed on the stage with etching with either acidic or basic solutions. For
the surface perpendicular to the optical axis of the most metals and alloys, there are a number of
microscope and is illuminated through the objective general-purpose etchants that should be used
lens by light from a lamp or arc source. This light first to reveal the microstructure. Subsequent
is focused by the condenser lens into a beam that examination may indicate that other more
is made approximately parallel to the optical axis specialized techniques for revealing the mi-
of the microscope by the half silvered mirror. The crostructure may be useful. For example, the
light then passes through the objective onto the examination may reveal certain constituents
specimen. It is then reflected from the surface of that the metallographer may wish to measure.
the specimen, back through the objective, the half Measurements, particularly those performed with
silvered mirror, and then to the eyepiece to the automatic image analyzers, will be simpler to per-
observer’s eye, or to a camera port or a film plane. form and more reliable if the desired constituent
can be revealed selectively, and numerous pro-
After the specimen has been properly sectioned cedures are available to produce selective phase
and polished, it is ready for examination. How- contrasting.
ever, in many cases, it is important to begin
the examination with an as-polished specimen,
The Light Microscope
particularly for quality control or failure analysis
work. Certain microstructural constituents, such as When Henry Clifton Sorby made his first examina-
nonmetallic inclusions, graphite, nitrides, cracks tion of the microstructure of iron on 28 July 1863,
or porosity, are best evaluated in the as‑polished he was using a transmitted light petrographic
condition as etching reveals other microstructur- microscope made by Smith, Beck and Beck of
al features that may obscure such details. In the London that he had purchased in 1861. Although
as-polished condition, there is a minimum of extra capable of magnifications up to 400X, most of his
information for the observer to deal with which examinations were conducted at 30, 60 or 100X and

Figure 21.1. Schematic diagram showing the light path through an upright reflected light microscope operating with bright field
illumination.

84
his first micrographs were produced at only 9X. The easy switching from one illumination mode to
objective lenses of this microscope were equipped another using the same set of objective lenses.
with Lieberkühns silvered concave reflectors for Furthermore, the manufacturers have introduced
focusing light on opaque specimens. new glass compositions and lens formulations,
generally by computer-aided design, for
Sorby quickly realized that reflected light improved image contrast and brightness. Tung-
produced with the Lieberkühns reflectors was sten- halogen filament lamps have largely replaced
inadequate and he developed two alternate xenon arc lamps as the preferred light source.
methods for this purpose. Subsequently, others
developed vertical illuminators using prisms or
plane glass reflectors and Sorby’s systems were
Microscope Components
not further developed. In 1886, Sorby reported on Light Sources. The amount of light lost during
the use of “very high power” (650X) for the study of passage from the source through a reflecting type
pearlite. This was accomplished using a 45º cover microscope is appreciable because of the intricate
glass vertical illuminator made for him by Beck. path the light follows. For this reason, it is generally
preferable that the intensity of the source be high,
For many years, photomicroscopy was conducted especially for photomicroscopy. Several types of
using specially built reflected microscopes known light sources are used including tungsten-filament
as metallographs. These devices represented the lamps, tungsten-halogen lamps, quartz-halogen
“top‑of‑the‑line” in metallurgical microscopes and lamps, and xenon arc bulbs. Tungsten-filament
were essential for quality work. In the late 1960’s lamps generally operate at low voltage and high
and early 1970’s, manufacturers developed metal- current. They are widely used for visual examination
lographs that were easier to use from the eyepiece because of their low cost and ease of operation.
viewing position. The temperamental carbon arc
light sources were replaced by xenon arc lamps. Tungsten-halogen lamps are the most popular
The unwieldy bellows systems for altering magni- light source today due to their high light intensi-
fication were replaced by zoom systems. Vertical ty. They produce good color micrographs when
illuminators, previously using single position ob- tungsten-corrected films are employed. Light
jectives, were equipped with four to six position intensity can be varied easily to suit the viewing
rotatable nosepiece turrets to minimize objective conditions by adjusting a rheostat, a distinct
handling. The light path was deflected so that the advantage over arc lamps.
film plane was conveniently near at hand. Universal
type vertical illuminators and objective lenses were Xenon arc lamps produce extremely high intensity

IMAGING & ANALYSIS

introduced so that the illumination mode could light, and their uniform spectra and daylight color
be readily switched from bright field to darkfield, temperature makes them suitable for color photomi-
polarized light or differential interference contrast. crography. The first xenon lamps produced ozone,
Such systems were very attractive in that separate but modern units have overcome this problem. Light
vertical illuminators and objectives were no longer output is constant and can only be reduced using
needed for each illumination mode and handling neutral density filters.
was eliminated. Exposure meters were also added
Condenser. An adjustable lens free of spherical
at this time, chiefly as a result of the rising popularity
aberration and coma is placed in front of the light
of instant films where such devices are needed to
source to focus the light at the desired point in the
minimize film wastage. But, by the late 1970s, these
optical path. A field diaphragm is placed in front
large metallographs had become very expensive,
of this lens to minimize internal glare and reflec-
too expensive for most laboratories.
tions within the microscope. The field diaphragm
In 1979, microscope manufacturers began to is stopped down to the edge of the field of view.
introduce very high quality, reasonably priced,
A second adjustable iris diaphragm, the aperture
compact metallographs. These microscopes
diaphragm, is placed in the light path before
can be obtained with a wide variety of objective
the vertical illuminator. Opening or closing this
lens types and auxiliary accessories to meet
diaphragm alters the amount of light and the angle
the metallographer’s needs. They are available
of the cone of light entering the objective lens.
with universal vertical illuminators that permit
The optimum setting for the aperture varies with

85
LIGHT OPTICAL MICROSCOPY
each objective lens and is a compromise among of the system.
image contrast, sharpness, and depth of field. As
magnification increases, the aperture diaphragm The most commonly used objective is the
is stopped down. Opening this aperture increases achromat, which is corrected spherically for one
image sharpness, but reduces contrast; closing color (usually yellow green) and for longitudinal
the aperture increases contrast, but impairs image chromatic aberration for two colors (usually red
sharpness. The aperture diaphragm should not and green). Therefore, achromats are not suit-
be used for reducing light intensity. It should be able for color photomicroscopy, particularly at
adjusted only for contrast and sharpness. higher magnifications. Use of a yellow-green
filter yields optimum results. However, achromats
Filters. Light filters are used to modify the light do provide a relatively long working distance, that
for ease of observation, for improved photo- is, the distance from the front lens of the objective
microscopy, or to alter contrast. Neutral density fil- to the specimen surface when in focus. The working
ters are used to reduce the light intensity uniformly distance decreases as the objective magnification
across the visible spectrum. Various neutral density increases. Most manufacturers make long-working
filters, with a range of approximately 85 to 0.01% distance objectives for special applications, for
transmittance, are available. They are a necessity example, in hot stage microscopy. Achromats are
when using an arc-lamp but virtually unnecessary usually strain free, which is important for polarized
when using a filament lamp. light examination. Because they contain fewer lens-
es than other more highly corrected lenses, internal
Selective filters are used to balance the color reflection losses are minimized.
temperature of the light source to that of the film.
They may be needed for faithful reproduction of Semi-apochromatic or fluorite objectives provide
color images, depending on the light source used a higher degree of correction of spherical and
and the film type. A green or yellow-green filter chromatic aberration. Therefore, they produce
is widely used in black and white photography to higher quality color images than achromats. The
reduce the effect of lens defects on image quality. apochromatic objectives have the highest degree
Most objectives, particularly the lower cost achro- of correction, produce the best results, and are more
mats, require such filtering for best results. expensive. Plano objectives have extensive correc-
tion for flatness of field, which reduces eyestrain,
Polarizing filters are used to produce plane and are usually found on modern microscopes.
polarized light (one filter) or crossed-polarized light
(two filters rotated 90° to each other to produce With parfocal lens systems, each objective on the
extinction) for examinations of anisotropic noncubic nosepiece turret will be nearly in focus when the
(crystallographic) materials. turret is rotated, preventing the objective front
lens from striking the specimen when lenses are
Objectives. The objective lens forms the prima- switched. Many objectives also are spring load-
ry image of the microstructure and is the most ed, which helps prevent damage to the lens. This
important component of the optical microscope. is more of a problem with high magnification
The objective lens collects as much light as objectives, because the working distance can be
possible from the specimen and combines this light very small.
to produce the image. The numerical aperture (NA)
of the objective, a measure of the light-collecting Certain objectives are designed for use with oil
ability of the lens, is defined as: between the specimen and the front lens of the
objective. However, oil-immersion lenses are rarely
NA = n sin α used in metallography, because the specimen and
lens must be cleaned after use. But, they do provide
where n is the minimum refraction index of the higher resolution than can be achieved when air is
material (air or oil) between the specimen and between the lens and specimen. In the latter case,
the lens, and α is the half-angle of the most the maximum possible NA is 0.95; oil-immersion
oblique light rays that enter the front lens of the lenses produce a 1.3 to 1.45 NA, depending on
objective. Light-collecting ability increases with the lens and the oil-immersion used. Objective
α. The setting of the aperture diaphragm will magnifications from about 25 to 200X are available,
alter the NA of the condenser and therefore the NA

86
depending upon the manufacturer. Use of oil also tomated to produce a direct digital readout of the
improves image contrast, which is valuable when measurement, which is accurate to approximately
examining low reflectivity specimens, such as coal 1µm.
or ceramics.
A 10X magnification eyepiece is usually used;
Eyepieces. The eyepiece, or ocular, magnifies the to obtain standard magnifications, some sys-
primary image produced by the objective; the eye tems require other magnifications, such as 6.3X.
can then use the full resolution capability of the Higher power eyepieces, such as 12, 15, 20, or
objective. The microscope produces a virtual image 25X, are also useful in certain situations. The
of the specimen at the point of most distinct vision, overall magnification is found by multiplying
generally 10in [250mm] from the eye. The eyepiece the objective magnification, Mo, by the eyepiece
magnifies this image, permitting achievement of magnification, Me. If a zoom system or bellows
useful magnifications. The standard eyepiece has a is also used, the magnification should be altered
24mm diameter field of view; wide field eyepieces accordingly.
for plano-type objectives have a 30mm diameter
field of view, which increases the usable area of the Stage. A mechanical stage is provided for focus-
primary image. Today, the wide field plano-objective ing and moving the specimen, which is placed
is standard on nearly all metallurgical microscopes. on the stage and secured using clips. The stage
of an inverted microscope has replaceable
The simplest eyepiece is the Huygenian, which is center stage plates with different size holes.
satisfactory for use with low and medium power The polished surface is placed over the hole for
achromat objectives. Compensating eyepieces viewing. However, the entire surface cannot be
are used with high NA achromats and the more viewed, unless the specimen is smaller than the
highly corrected objectives. Because some lens hole and it is mounted. At high magnifications
corrections are performed using these eyepiec- it may not be possible to focus the objective
es, the eyepiece must be matched with the type near the edge of the hole due to the restricted
of objective used. The newer, infinity-corrected working distance.
microscopes do not perform corrections in
the eyepieces, but in the tube lens. Eyepieces, Using the upright microscope, the specimen is
therefore, are simpler in infinity-corrected placed on a slide on the stage. Because the pol-
microscopes. ished surface must be perpendicular to the light
beam, clay is placed between the specimen bottom
Eye clearance is the distance between the eye lens and the slide. A piece of lens tissue is placed over

IMAGING & ANALYSIS

of the ocular and the eye. For most eyepieces, the the polished surface, and the specimen is pressed
eye clearance is 10mm or less – inadequate if the into the clay using a leveling press. However, pieces
microscopist wears glasses. Simple vision problems, of tissue may adhere to the specimen surface. An
such as near sightedness, can be accommodated alternative, particularly useful with mounted speci-
using the fine focus adjustment. The microscope mens, is to use a ring instead of tissue to flatten the
cannot correct vision problems such as astigmatism, specimen. Aluminum or stainless steel ring forms
and glasses must be worn. High eyepoint eyepieces of the same size as the mounts (flattened slightly
are available to provide an eye clearance of approx- in a vise) will seat on the mount rather than the
imately 20mm, necessary for eyeglasses. specimen.

Eyepieces are commonly equipped with various The upright microscope allows viewing of
reticles or graticules for locating, measuring, the entire surface with any objective, and the
counting or comparing microstructures. The operator can see which section of the specimen is
eyepiece enlarges the reticle or graticule image being viewed – a useful feature when examining
and the primary image. Both images must be in specific areas on coated specimens, welds, and
focus simultaneously. Special eyepieces are also other specimens where specific areas are to be
produced to permit more accurate measure- examined. For mounted specimens, an autolevel-
ments than can be made with a graticule scale. ing stage holder can eliminate leveling specimens
Examples are the filar-micrometer ocular or with clay.
screw-micrometer ocular. Such devices can be au-
The stage must be rigid to eliminate vibrations.

87
LIGHT OPTICAL MICROSCOPY
Stage movement, controlled by x and y microme- If resolution is acceptable but contrast is lacking,
ters, must be smooth and precise; rack and pinion detail cannot be observed. In general, the ability to
gearing is normally used. Many stages have scales resolve two points or lines separated by dis-
for measuring distances in the x and y directions. tance d is a function of the wavelength, λ, of the
The focusing controls often contain rulings for incident light and the numerical aperture, NA, of
estimating vertical movement. Some units have that objective.
motorized stages and focus controls.
kλ
A circular, rotatable stage plate may facilitate po- d=
NA
larized light examination. Such stages, common for
mineralogical or petrographic studies, are gradu-
ated to permit measuring the angle of rotation. A where k is 0.5 or 0.61. Figure 21.2 illustrates this
rectilinear stage is generally placed on top of the relationship for k = 0.61 and four light wave-
circular stage. lengths. Other formulas have also been reported.
This equation does not include other factors that
Stand. Bench microscopes require a rigid stand, influence resolution, such as the degree of
particularly if photomicroscopy is performed on correction of the objectives and the visual acuity
the unit. The various pieces of the microscope of the microscopist. It was based on the work
are attached to the stand when assembled. of Abbe under conditions not present in metal-
In some cases, the bench microscope is placed on lography, such as self-luminous points, perfect
a separate stand that also holds the photographic black-white contrast, transmitted light examina-
system. tion, an ideal point-light source, and absence of
lens defects.

Resolution Using the above equation, the limit of resolution

To see microstructural detail, the optical sys- for an objective with an NA of 1.3 is approximately
tem must produce adequate resolution, or 0.2µm. To see lines or points spaced 0.2µm apart,
resolving power, and adequate image contrast. the required magnification is determined by divid-

RESOLUTION CHART
1.4

1.3

1.2

1.1

1.0 Sodium (589nm)

0.9
Resolution µm

0.8

0.7 Green (546nm)

0.6

0.5

0.4 Ultraviolet
(365nm)
0.3

0.2

0.1 Blue (436nm)

0.0
0.15 0.25 0.35 0.45 0.55 0.65 0.75 0.85 0.95 1.05 1.15 1.25 1.45 1.55
Numerical Aperture (NA)
Figure 21.2. Influence of objective numerical aperture and light wavelength on the resolution of the light microscope.

88
ing by the resolving power of the human eye, which Depth of Field
is difficult to determine under observation condi-
Depth of field is the distance along the optical
tions. Abbe used a value of 0.3mm at a distance of
axis over which image details are observed with
10in [250mm] – the distance from the eye for opti-
acceptable clarity. Those factors that influence
mum vision. This gives 1500x. For light with a mean
resolution also affect depth of field, but in the
wavelength of 0.55µm, the required magnification
opposite direction. Therefore, a compromise must
is 1100 times the NA of the objective. This is the
be reached between these two parameters, which
origin of the 1000·NA rule for the maximum useful
is more difficult as magnification increases. This is
magnification. Any magnification above 1000·NA is
one reason light etching is preferred for high-mag-
termed “empty”, or useless.
nification examination. The depth of field, df, can be
estimated from:
Strict adherence to the 1000·NA rule should be
questioned, considering the conditions under
which it was developed, certainly far different from λ (n 2 −NA2)½
df =
those encountered in metallography. According NA2
to the Abbe analysis, for a microscopist with
optimum 20/20 vision and for optimum contrast where n is the refractive index of the medium
conditions and a mean light wavelength of 550nm, between the specimen and the objective (n ~
the lowest magnification that takes full advantage 1.0 for air), λ is the wavelength of light, and NA is
of the NA of the objective is 500 times the NA. the numerical aperture. This equation shows that
This establishes a useful minimum magnification to depth of field increases as the NA decreases and
use with a given objective. It has been suggested when longer wavelength light is used, as shown in
that the upper limit of useful magnification for the Figure 21.3.
average microscopist is 2200·NA, not 1000·NA.

DEPTH OF FIELD CHART

100

IMAGING & ANALYSIS

Sodium (589nm)
10
Green (546nm)
Depth od Field µm

Blue (436nm)

0.1

Index of Refraction = 1.0

0.01

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Numerical Aperture (NA)

Figure 21.3. Influence of the objective numerical aperture and light wavelength on the depth of field of the light microscope.

89
LIGHT OPTICAL MICROSCOPY
Imaging Modes the eyepieces to the eyes where it will appear
Most microscopical studies of metals are made
to be bright or white. Light that strikes grain
using bright field illumination. In addition to this
boundaries, phase boundaries, and other
type of illumination, several special techniques
features not perpendicular to the optical axis will
(oblique illumination, dark field illumination,
be scattered at an angle and will not be collected
differential interference contrast microscopy
by the objective. These regions will appear to
and polarized light microscopy) have particular
be dark or black in the image. Bright field is
applications for metallographic studies.
the most common mode of illumination used
by metallographers.
Nearly all microscopes using reflected or trans-
mitted light employ Köhler illumination because
Oblique Illumination. The surface relief of a
metallographic specimen can be revealed using
it provides the most intense, most even illumi-
oblique illumination. This involves offsetting the
nation possible with standard light sources. The
condenser lens system or, as is more usually done,
reflected light microscope has two adjustable
moving the condenser aperture to a position
diaphragms: the aperture diaphragm and the field
slightly off the optical axis. Although it should
diaphragm, located between the lamp housing
be possible to continually increase the contrast
and the objective. Both are adjusted to improve
achieved by oblique illumination by moving the
illumination and the image. To obtain Köhler illu-
condenser farther and farther from the optical
mination, the image of the field diaphragm must
axis, the numerical aperture of a lens is reduced
be brought into focus on the specimen plane.
when microstructural image is brought into fo-
This normally occurs automatically when the
cus. The filament image must also be focused on
microstructural image is brought into focus.
the aperture diaphragm plane. This produces
The filament image must also be focused on
uniform illumination of the specimen imaged at
the aperture diaphragm plane. This produces
the intermediate image plane and magnified by
uniform illumination of the specimen imaged at
the eyepiece.
the intermediate image plane and magnified by
the eyepiece.
Dark Field. Another method that can be used
to distinguish features not in the plane of the
Bright Field. In bright field illumination, the sur-
polished and etched surface of a metallographic
face of the specimen is normal to the optical axis
specimen is dark field (also called dark ground)
of the microscope, and white light is used. A ray
illumination. This type of illumination (see
diagram for bright-field illumination is illustrated
Figure 21.5 for a ray diagram) gives contrast
in Figure 21.4. Light that passes through the
completely reversed from that obtained with
objective and strikes a region of the specimen
bright-field illumination — the features that are light
surface that is perpendicular to the beam
in bright field will be dark in dark field, and those
will be reflected back up the objective through

Figure 21.4. Schematic diagram showing the light path in bright Figure 21.5. Schematic diagram showing the light path in dark
field illumination. field illumination.

90
that are dark in bright field will be light, appearing Differential Interference Contrast (DIC). When
to be self luminous in dark field. This highlighting crossed polarized light is used along with a double
of angled surfaces (pits, cracks, or etched grain quartz prism (Wollaston prism) placed between
boundaries) allows more positive identification of the objective and the vertical illuminator, Figure
their nature than can be derived from a black image 21.7, two light beams are produced which exhibit
with bright field illumination. Due to the high image coherent interference in the image plane. This leads
contrast obtained and the brightness associated to two slightly displaced (laterally) images differing
with features at an angle to the optical axis, it is often in phase (λ/2) that produces height contrast. The im-
possible to see details not observed with bright age produced reveals topographic detail somewhat
field illumination. similar to that produced by oblique illumination but
without the loss of resolution. Images can be viewed
Polarized Light. Because many metals and metallic with natural colors similar to those observed in
and nonmetallic phases are optically anisotropic, po- bright field, or artificial coloring can be introduced
larized light is particularly useful in metallography. by adding a sensitive tint plate.
Polarized light is obtained by placing a polarizer
(usually a Polaroid filter) in front of the condenser As an example of the use of these different imaging
lens of the microscope and placing an analyzer modes, Figure 21.8 shows the micro this happens
(another Polaroid filter) before the eyepiece, as because only a structure of an aluminum bronze
illustrated in Figure 21.6. The polarizer produces specimen that was water quenched from the beta
plane polarized light that strikes the surface and is field forming martensite. The specimen was pre-
reflected through the analyzer to the eyepieces. If pared but not etched. A minor amount of relief was
an anisotropic metal is examined with the analyzer introduced in final polishing. Figure 21.8a shows the
set 90° to the polarizer, the grain structure will be surface in bright field illumination. Due to the relief
visible. However, viewing of an isotropic metal (cu- present, a faint image of the structure is visible. Dark
bic metals) under such conditions will produce a field, Figure 21.8c, and differential interference con-
dark, “extinguished” condition (complete darkness trast, Figure 21.8d, make use of this relief to reveal
is not possible using Polaroid filters). Polarized light much more detail than in bright field. However, as
is particularly useful in metallography for revealing the martensite is noncubic in crystal structure, it
grain structure and twinning in anisotropic metals responds well to crossed polarized light, Figure
and alloys (see the appendix for crystal structure 21.8b. Of course, not every material can be exam-
information) and for identifying anisotropic phases ined using all four illumination modes, but there
and inclusions. are many cases where two or more modes can be

IMAGING & ANALYSIS

effectively utilized to reveal more information than
given by bright field alone.

Figure 21.6. Schematic diagram showing the light path in Figure 21.7. Schematic diagram showing the light path for
polarized light with an optional lambda plate (sensitive tint differential interference contrast (DIC) illumination.
plate).

91
LIGHT OPTICAL MICROSCOPY

HELPFUL HINTS FOR

OPTICAL MICROSCOPY
It can be difficult to determine which
objective you are using with an inverted
microscope due to the limited view from
above, as the magnification value may not
be easily observed. However, each objective
a has a color-coded ring on it that is usually
visible. The colors and corresponding mag-
nifications are: red – 5X, yellow – 10X, green
– 20X, blue – 50X, and white – 100X.

d
Figure 21.8.Carbon fiber reinforced composite images
illustrating microscopy imaging modes. a) Brightfield is standard
imaging mode for cursory analysis, b) Darkfield highlights cracks
that might not be readily visible in bright field.
c) Polarised imaging helps with fiber orientation analysis,
whereas d) differential interference contrast provides a
topographic view of the imaged surface without loss of
resolution.

92
IMAGE CAPTURE & ANALYSIS
The progress in computer and video technology allowing the exporting of data to Microsoft Excel®.
has created a movement toward electronic image The OmniMet Express and OmniMet Enterprise
acquisition. These images can be used in software products include automated measurement capa-
applications such as word processing or desktop bilities in addition to the manual measurements
publishing programs allowing for fast report gen- found in the Capture products. OmniMet Express
eration and electronic distribution. In addition, can incorporate a variety of application specific me-
associated data can be stored with the images in a tallographic analysis modules. OmniMet Enterprise
database allowing for easy retrieval of information is a full featured system including a routine builder
through searches. which enables the user to generate custom analysis
solutions to meet their specific needs.
When adding imaging capabilities to the laboratory,
it is important to consider your goals. Oftentimes,
images are just another step in the documentation
process. For example, in a failure investigation it is
useful to capture the image of a complete compo-
nent before the sectioning process. Or, an image
of the microstructure might be attached to a report
as an indication of a pass/fail condition. Additional
functionality of an imaging system might include a
scale marker overlay and point-to-point or other op-
erator interactive measurements. Fully automated
image analysis includes detection of the features of
interest based on grey level or color differences as
well as morphological characteristics such as size
and shape. Automated imaging applications are Figure 22.1. OmniMet Digital Imaging System
based on a fundamental series of steps shown in
Table 22.1. Depending on your goals, some or all Image Capture
of these steps may be utilized.
Image capture is a term used to describe image ac-
quisition by means of a camera and frame grabber
Aligned with these imaging goals, Buehler offers a
or a digital camera. Because of the many choices of
series of upgradeable OmniMet imaging products
camera types, a video microscopy system must be
(Figure 22.1). The OmniMet Capture Basic System
flexible. Analog CCD cameras, black and white or
provides digital or analog image capture, manual in-

IMAGING & ANALYSIS

color, or digital CCD or CMOS are most frequently
teractive measurements (length, parallel width, area,
used. Component video (Y/C or S-Video) and com-
curve (string lenth), text annotation and scale bars),
posite video signals and a number of color video
basic report generation in Microsoft® Word®, and
standards such as NTSC, PAL and SECAM are gen-
databasing of saved images and measurements.
erally supported. Images acquired in the materials
The OmniMet Capture Advanced system expands
laboratory are optimized in real time by adjusting
upon the Capture Basic capabilities by including
brightness, contrast, and color saturation. The ana-
additional interactive measurements (radius, an-
log output camera signal is then digitized utilizing
gle, and counting), adding a results window, and

Table 22.1: Primary Imaging Steps

Imaging Steps Description
Capture Capture, load or import an image
Clarification Develop the necessary contrast and clarity for detecting the features of interest
Thresholding Detect the features of interest
Binary Operations Clean-up any detection discrepancies, categorize features and overlay grids
Measurements Conduct fiels or feature measurements
Data Analysis Evaluate statictics and relevance of the measurements
Archive Stor images, annotations and associated measurements in a database
Distribution Printing or electronic distribution of images and results

93
IMAGE CAPTURE & ANALYSIS
an analog input frame grabber board. white), then one bit is enough to store information
for one pixel. If an image is colored or uses various
Alternatively, digital cameras may be integrated shades of grey, then additional bits are required to
with an IEE 1394 firewire or USB connection. Since store color and shading information. Table 22.2 lists
the late 1990’s digital video cameras have become some of the more common bit depths referred to in
the preferred choice for scientific imaging applica- imaging software and camera literature.
tions. This is largely accounted for by two factors:
Table 22.2: Bit Depth
1) higher pixel densities in the acquired images
Bits
potentially provide higher spatial resolution and
1 21 or 2 tones, black and white
2) the cost range of digital cameras has merged
with the combined cost of an analog camera and 8 28 or 256 grey scale shades

specialized capture board. Capturing an image with 24 224 or 16.7 million colors
a digital camera is often a two-stage process, first a 32 232 or 4.29 billion colors
preview image is viewed for focusing and selecting
the field of interest and then a snapshot of the image When working in grayscale, 256 values are used to
is taken. The preview image window displays the represent each shade of grey, starting with black
image at a lower pixel density and the refresh rate at 0 and transitioning to white at 255. For example,
of the camera will determine the amount of lag time the information stored for the image in Figure 53
between the operator adjusting the microscope would be a combination of the x and y positions and
and the new image being displayed. In order to be a number from 0 to 255. For color images there are
comparable to an analog camera, the refresh rate two common models used to numerically represent
should approach 25 frames per second. color, RGB and HLS. Each requires storing three val-
ues, in addition to the x and y position of the pixel,
The resulting image files are based on two primary in order to recreate the image. In general, you will
formats, bit-map and vector. The majority of scien- notice the file sizes for color images are larger than
tific imaging programs are based on bit-mapped grey scale images of the same pixel density.
images. Bit-mapped graphics are essentially grids,
consisting of rows and columns of pixels. When The RGB model is based on three primary colors
the image is zoomed to observe details, the indi- – red, green and blue – that can be combined in
vidual pixels will become visible. Pixels, or picture various proportions to produce different colors.
elements, are the smallest part of an image that a This scheme is considered additive because, when
computer, printer or monitor display can control. combined in equal portions, the result is white.
An image on a monitor consists of hundreds of Likewise, an absence of all three is black. The three
thousands of pixels, arranged in such a manner that primary colors are each measured as a value from
they appear to be connected. Figure 22.2 displays a 0-255. The colors produced by combining the
cast iron image with a small segment zoomed such three primaries are a result of the relative values
that the pixels are observed. of each primary. For example, pure red has a red
value of 255, a green value of 0, and a blue value
Each pixel in a bitmap is stored in one or more of 0. Yellow has a red value of 255, a green value of
data bits. If an image is monochromatic (black and 255, and a blue value of 0. This system is modeled
as a cube with three independent directions: red,
green, and blue, spanning the available space. The
body diagonal of the cube contains luminance, in
other words, colorless information about how light
or dark the signal is.

The HLS model uses the concept of Hue, Luminance,

and Saturation. Hue is the color tone. For example,
an etchant might highlight the different phases
as unique shades of brown or blue. Saturation is
complementary to the hue. It describes how brilliant
or pure – as opposed to washed out or grayish a
particular color is. Luminance is correlated with
Figure 22.2. A small segment of an image zoomed to display the
individual pixels..

94
the light intensity and viewed as comparable to is accomplished with a stage micrometer. Each of
the greyscale values where zero is black and 255 the objectives will have its own unique calibration
is white. The HLS color space can be viewed as a factor. If the aspect ratio of the camera pixels is un-
double cone, in which the z-axis of the cone is the known, it can be determined by calibrating in both
grayscale progression from black to white, distance the x and y direction. If the aspect ratio is known,
from the central axis is the saturation, and the direc- then calibration only needs to be completed in the
tion or angle is the hue. x direction. This calibration technique is repeated
for each objective or working magnification. It is also
The illustration in Figure 22.3 represents pixels of possible to calibrate images that have been import-
nine different color values. These values are shown ed from another source. The only requirement is to
in Table 22.3 for the greyscale, RGB, and HLS mod- have a feature within the image that is of a known
els. When the pixels are not true grayscale tones, dimension. A scale marker is usually the best choice.
the greyscale number is not given.

Resolution is primarily the imaging system’s ability

to reproduce object detail by resolving closely
spaced features. In digital microscopy, the resolu-
tion is examined in terms of both the microscope
limitations and the pixel array of the camera. The
clarity and definition of a digital image depends
largely on the total number of pixels used to create
it. Typical pixel array densities range from 640 x 480
to 5120 x 4096. Multiplying the two numbers gives
you the total number of pixels used to create the
image. Because a large number of pixels leads to
sharper images, you might conclude that it is always
desirable to capture images with the largest pixel
array possible. That is not necessarily always true.
The problem with large array images is that they
consume a lot of storage space. As a result, these
images are not recommended for posting on web
sites or email use. It is important to take into account
what you intend to do with your images when se-

IMAGING & ANALYSIS

Figure 22.3. A representation of nine pixels with different color
lecting the appropriate camera. values.

In order to perform measurements, the image or

the image source must first be calibrated. Calibra-
tion is achieved by assigning a known distance to
a pixel count. When using a light microscope this

Table 22.3: Values based on color models

HLS Method RGB Method
Pixels Greyscale Hue Luminance Saturation Red Green Blue
1 192 0 192 0 192 192 192
2 150 0 150 0 150 150 150
3 128 0 128 0 128 128 128
4 0 127 255 255 0 0
5 85 127 255 0 255 0
6 170 127 255 0 0 255
7 60 98 100 255 255 0
8 310 36 79 148 31 129
9 25 100 176 169 113 31

95
IMAGE CAPTURE & ANALYSIS
Clarification Automated Measurements
Image clarification is also referred to as image When more detailed measurements are required
enhancement and is largely achieved through or a large quantity of measurements is important,
the use of greyscale filters. Filters perform one it is useful to automate the process. For example,
of several standard functions: edge detection, consider the coating that was measured in Figure
photographic enhancement, or grey level modifica- 22.5. It is possible to duplicate that measurement as
tion. Image clarifications, which modify the values of well as to evaluate any variation across the coating
the pixels across an entire image, are conducted in and determine the percentage porosity within the
one of two ways: adjusting limits such as contrast, coating. A typical process for determining coating
brightness and gamma or comparing the values thickness is outlined in Figure 22.6 and is described
of neighboring pixels. The latter is referred to as a below.
convolution or kernel operation. The neighborhood
sizes are typically squares of pixels from 3x3, 5x5,
7x7, etc. A typical need is to increase the local
contrast at the phase boundaries. Often times, the
use of a neighborhood transformation filter results
in a more narrow gray scale distribution of a given
phase, making the subsequent thresholding or
detection process easier.

Operator Interactive Measurements

Interactive measurements require the operator to

use a mouse to select the start and end points for
each measurement. The most common of these Figure 22.5. An example of an operator estimating coating
thickness with the use of a parallel tool.
are linear measurements (point-to-point), parallel,
radius or diameter, curvilinear, and angle (Figure Thresholding
22.4). An operator will typically make several mea-
Thresholding is the method for representing ranges
surements over the area of interest. These are either
of pixel grey or color values with different color
electronically transferred to a file or transcribed
bitplane overlays. The bitplanes are a binary layer
by hand. This method is appropriate for a limited
placed over the image plane superimposing the
number of measurements or where an average is of
phase(s) of interest. Most of the measurements are
interest rather than variation. Figure 22.5 represents
accomplished on this layer not on the actual image.
the most direct way to take an average measure-
ment of thickness using a parallel line tool. One line
The first step of the thresholding process is the de-
is aligned with the interface and then the opposite
velopment of a threshold histogram. Each pixel is
line is aligned with the median of the rough surface.
assigned a value and then the frequency is graphed.
When working in grayscale with an 8-color image,
the same 256 values correspond to luminance.
Figure 22.8 demonstrates a yellow bitplane being
assigned to the coating (Figure 22.7) based on the
HLS values of the pixels as discussed previously.
Figure 22.4. Operator interactive tools founds in imaging
software.

In addition to measurements, other annotations are Binary Operations

often placed on electronic images. Annotations After the thresholding process has been accom-
can be as simple as a label that is referenced in the plished, the different phases and features in an
image caption or a complete text description of a image are represented by different bitplane color
feature within the image. A recommended anno- overlays. It is possible that more than one phase or
tation is a scale marker in the lower corner of the feature of interest is detected by the same bitplane
image. This is particularly important for distributing color because of a similar gray level range. A binary
the image electronically because the final size of the operation is the process that separates and classifies
printout is at the discretion of the recipient. features within the same bitplane, based on mor-

96
Acquire image

Yes Need to improve

Clarification
Filter contrast or clarity?

No

Threshold coating

Yes
Binary Over
Remove artifacts detection?
No

Yes
Binary Under
Fill gaps detection?
No

Binary
Place grid over layer

IMAGING & ANALYSIS

Binary
Boolean command AND detect overlap

Binary Yes
Are there gaps in
Close the grid lines the grid lines?
No

Feature Measurement
Measure the individual grid lines

Figure 22.6. A flowchart of the logic used when creating an automated measurement routine for coating thickness.

97
IMAGE CAPTURE & ANALYSIS
phology or size. Additionally, not all images are would include the relative area fraction of porosity
detected as desired. There may be over-detected as well as the average thickness. Before either of
or under-detected regions that need to modified. these measurements can be made it is necessary
In general, binary operations allow the operator to to define the total area of the coating. A combi-
isolate the features that are of interest. nation of the binary commands Fill and Close are
used to eliminate the holes (undetected areas)
Two common measurements on this type of coating that are totally enclosed by the detected bitplane.
The thickness is determined by averaging a series
of chord measurements across the coating, rather
than a single measurement of the yellow bitplane.
An additional binary layer is superimposed in the
form of a grid using a Grid command. Figure 22.9
demonstrates the effects of these commands on
the coating.

To define the individual chords, where the grid

overlaps the coating, a Boolean command is
Figure 22.7. A TSC color image captured at 1200 x 1600 employed. Boolean operations perform logical
pixels. functions between bitplanes. The two most com-
mon are OR and AND. AND takes those portions
of two bitplanes that overlap and integrates them
into a single destination bitplane. In the coating,
for example, AND considers only those segments of
the red grid bitplane that overlap the yellow coating
bitplane. Figure 22.10 shows the red chords which
result from the AND command. The OR combines
two source bitplanes together to form a single

Figure 22.9. The effect of the Binary commands, Close, Fill,

and Grid on the detected coating.

destination bitplane. For example, if two different

inclusion types, oxides and sulfides, are detected
initially, they can be combined to measure the total
inclusion content.

One of the most powerful binary functions is the

ability to categorize individual features based
b on shape or size. It can be a single specification
Figure 22.8. Thresholding the coating with a yellow (>5µm) or multiple specifications (>2 and <5) sepa-
bitplane overlay using the HLS color model.
rated by an AND or an OR. If a maximum allowable

98
pore size is specified, all pores that exceed that limit
can be flagged. The limit itself can be based on aver-
age diameter, maximum diameter, area, aspect ratio,
etc. Additionally, the shape of the pore may have
some significance. For example, in cast materials,
a gas bubble tends to be circular while a shrinkage
cavity will have a more complex shape. Common
shape factors examine the relationship between
the perimeter and area of the feature.

Figure 22.11. The histogram of results representing the

chords shown in Figure 22.8.

a specimen. A fairly common field measurement is

area percentage. An area percentage measurement
results from dividing the number of pixels in the
bitplane of interest by the total number of pixels in
the image. In the case of the coating, there is a need
to measure the area percent porosity relative to the
Figure 22.10. The chords that result from the overlapping coating area and not the entire image area. This is
coating and grid lines. calculated by dividing the number of pixels in the
bitplane of interest, i.e. the pores in the coating, by
the total number of pixels representing the coating.
For this coating, the pores were separated from the
elongated oxides to insure that the porosity level
was not overestimated. Common Applications
Throughout our involvement in image analysis, a
Returning to Figure 22.10, where grid lines are number of applications stand out and may be of
placed across the coating, the length of all the in- interest to most image analysis users. Below is a
dividual grid lines can be measured. The data can listing of these applications:
be shown as a histogram offering the minimum,

IMAGING & ANALYSIS

maximum, mean and standard deviation of the Grain Size. Image analysis provides a rapid and
measurements across the coating, see Figure 22.11. accurate means for determining grain size ac-
cording to ASTM E112. Even if etching is unable
Most measurements fall into one of two categories: to produce complete grain boundaries, or if there
field or feature-specific measurements. The grid are twins that could skew the data, binary modifi-
lines across the coating are typical of feature mea- cations can be employed to make corrections. If a
surements. Each individual feature is measured and specification cites maximum grain size limitations,
then plotted based on frequency in the histogram the excessively large grains may be transferred
and contributes to the overall statistics. In the case to a different bitplane color to provide visual and
of grain or particle size measurements, features on numerical feedback.
the edge of the image are eliminated because the
complete size of the feature is unknown. Porosity. Porosity is detrimental to the physical
properties of most engineering materials. Image
Field measurements are performed on the entire analysis is able to characterize the pores according
field of view or a framed portion of the image, to the total number of pores, number per unit area,
providing the sum of the individual measurements maximum size, average size and the size distribution
in the selected area. Statistical information for field in the form of a histogram.
measurements is only generated if multiple fields
are analyzed. This can be employed to observe Linear Measurements. Simple point-to-point mea-
microstructural variations within different fields of surements are widely used for making occasional

99
IMAGE CAPTURE & ANALYSIS
measurements; however, in cases where a high
quantity of measurements and more statistics are HELPFUL HINTS FOR
required, automated image analysis is time saving. IMAGE CAPTURE & ANALYSIS
A coating or layer is detected based on the pixel Determine the required pixel density of
values and then, after binary isolation of the coating, a camera system based on the size of the
grid lines are superimposed. Using Boolean logic to features of interest and acceptable file size
evaluate the common pixels between the layer and
grid lines, the result is many chords representing the When distributing an image, always add a
thickness at given points in the coating. scale bar

Feature Shape and Size. The shape of the graphite When saving images for analysis at a later
constituent in ductile irons is critical. Ductile iron time, verify that the image is stored as cap-
was developed such that the graphite would occur tured, i.e., without any filters applied.
in the form of spherical nodules with the result
of dramatically improved mechanical properties.
However, variations in chemistry and other factors
can cause the nodules to be irregular, leading to
some degradation of the properties. The ability to
monitor the graphite shape or determine “nodular-
ity” is another ability of image analysis. These same
techniques are applicable to any constituent that
can be detected.

Phase Percentage. The area percent of various

phases in a microstructure influences the proper-
ties. The tensile strength of grey iron, for example,
is directly related to the percentage of pearlite in
its microstructure. In addition, in a single image,
multiple phases can be detected, measured and
presented in one graph. For example, when eval-
uating the inclusion content of steels, it would be
useful to examine the overall inclusion content as
well as isolating particular inclusion types, such as
oxides and sulfides.

100
HARDNESS TESTING
A BRIEF HISTORY OF HARDNESS sions of the scratch test were introduced including
integrated microscope, stage and diamond appa-
TESTING
ratus that applied increasing loads up to 3 grams.
Hardness, as applied to most materials, and in par- The material to be tested was scratched under load
ticular metals, is a valuable, revealing and commonly variants and then compared to a standard set of
employed mechanical test that has been in use in scratches of known value.
various forms for more than 250 years. Although
Later, indentation type hardness was introduced.
hardness is not considered a fundamental physi-
One early form developed around 1859, was based
cal property, its value and importance cannot be
on the load required to produce a 3.5 millimetre
understated. The information from a hardness test
indent in the material. The first widely accepted
can complement, and often be used in conjunction
and standardized indentation-hardness test was
with, other material verification techniques such as
proposed by J. A. Brinell in 1900 [35]. The Brinell
tensile or compression testing to provide critical
hardness test, still widely used today, involves
performance information.
indenting the metal surface with a 1 to 10mm di-
Over the years, various methods for determining ameter steel ball (now Tungsten Carbide) at loads
the hardness of materials have been developed and of up to 3,000 kilograms. The resultant impression,
employed. From early forms of scratch testing to the diameter of the indentation, is measured and a
sophisticated automated imaging, hardness testing mathematically calculated hardness value derived.
has evolved into an efficient, accurate and valued
The hardened steel ball of the Brinell test limited
material test method.
the test to materials with a hardness of less than
While testing techniques and hardware have sig- ~450 HBS (~48HRC). The harder tungsten carbide
nificantly improved in step with rapidly advancing ball extends this range to ~650HBW, but this was
electronics, computer, hardware and programming not available in 1925.
capabilities, earlier basic forms of hardness testing,
such as the simple scratch test, sufficed for the
needs of the relevant era.

Some of the earliest forms of bar scratch testing

date back to about 1722. These tests were based
on a bar that increased in hardness from end to end.
The point at which the material being tested could
form a scratch on the bar was the determining fac-
Figure 23.1. A legacy Wilson "J" Series Rockwell tester, circa
tor in the specimen’s hardness. In 1822, hardness
1960s.
testing techniques were introduced that included
scratching material surfaces with a diamond and Although conceived as an idea in 1908 by a Vi-
measuring the width of the resultant line. This ennese professor, Paul Ludwik [36], the Rockwell
approach eventually developed into the Mohs indentation test did not become of commercial
scale, a hardness reference that is still widely used importance until around 1914 when brothers
in geological circles. Stanley and Hugh Rockwell used a conical dia-
mond indention test based on displacement and
The Mohs scale [34] consists of 10 minerals, ordered applied for a patent for a Rockwell tester design.
The principal criterion for this tester was to provide
from hardest at 10 (diamond) to softest at 1 (talc).
HARDNESS TESTING

a quick method for determining the effects of heat

Each mineral can scratch those that fall below it in treatment on steel bearing races.
the scale hierarchy. The Mohs scale is not linear;
the difference in hardness between 9 and 10 is Patent applications were made and approved be-
significantly more than that between 1 and 2. To tween 1919 and 1924 refining the test method, and
put the Mohs scale into perspective, a tangible Stanley Rockwell simultaneously started commercial
example is that of hardened tool steel which falls production of Rockwell testers in collaboration
at approximately 7 or 8 on the scale. with instrument manufacturer Charles H. Wilson
in Hartford, CT, a later Rockwell model is shown
During the next 75 years, other more refined ver- in figure 23.1. The company grew into the Wilson

101
HARDNESS TESTING
Mechanical Instrument Co. and became known as Hardness testing technology remained fairly con-
the premium producer of Rockwell testers. After sistent throughout the mid to late 1900s, with most
some ownership changes through the latter 1900s, systems typically utilizing the dead weight method
Wilson became an integral part of Illinois Tool Works of applying the test forces. While the deadweight
after it was acquired by Instron in 1993 and subse- technique is fairly simple, reliable and was widely
quently Buehler in 2011. Acquisitions of Wolpert accepted, the method is not without some ambi-
Hardness and Reicherter Hardness have resulted guities. Labour-intensive production, coupled with
in the engineering and production of cutting edge the complexities involved in a highly mechanical
hardness testing systems. systems depending on levers, pivots and guides led
to the need for further development and it became
The Rockwell test remains one of the most efficient evident that other newly developed forms of force
and widely used hardness test types in use. Howev- regulation used in measurement instrumentation
er, a major disadvantage of Rockwell type tests are could be applied to hardness testing as well.
the different scales (15 standard and 15 superficial)
that are required in order to evaluate the full mate- With increasing demands for productivity, accu-
rial hardness range. racy, user features and repeatability, closed-loop,
load cell technology became a factor in hardness
Originally conceived as an alternative to the Bri- testing. During the 1950s, Instron pioneered the
nell method, the Vickers hardness [37] test was use of closed loop systems on tensile testing instru-
developed around 1922 by Smith and Sandland, ments. Closed loop systems differ from open loop
at Vickers Ltd., a British engineering conglomerate. (deadweight) systems in that they have a means
In designing the new indenter, they chose a geom- to electronically measure the force being applied
etry that would produce hardness numbers nearly during every test and feed (or loop) the information
identical to Brinell numbers in the range where both back to the control system. With the teaming up of
tests could be used. This was a very wise decision Instron and Wilson, the ability to adapt the closed
as it made the Vickers test very easy to adopt. The loop control effectively to hardness testers led to
ideal d/D ratio (d = impression diameter, D = ball the development of systems with repeatability never
diameter) for a spherical indenter is 0.375. If tan- before realized. During the 1990s this technology
gents are drawn to the ball at the impression edges was introduced first to Rockwell testers, and later
for d/D = 0.375, they meet below the center of the to Knoop/Vickers, as well as Brinell systems. Today
impression at an angle of 136°, the angle chosen the technology is a popular and widely used for-
for the Vickers indenter. This resulted in a more mat. Together with advances in computer control,
consistent and versatile hardness test that could fully automated systems are now available that can
evaluate any material (except diamond) and had the achieve higher levels of speed and accuracy than
very important advantage of placing the hardness ever before.
of all materials on one continuous scale.

The original Vickers testers were developed for test A SUMMARY OF HARDNESS TEST
loads of 1 to 120kgf – which produces rather large METHODS
indents. Recognizing the need for lower test loads,
the National Physical Laboratory (UK) reported Brinell Testing
on use of lower test loads in 1932. Lips and Sack Brinell test methods are defined in the following
developed the first low-load Vickers tester in 1936. standards: ASTM E10 and ISO 6506. It is recom-
mended that operators have a current copy of the
In 1939, an alternative to the Vickers test was intro- relevant standards, which are updated regularly.
duced by Fredrick Knoop at the U.S. National Bureau
of Standards. The Knoop hardness [38] test utilized a The Brinell test consists of applying a constant
shallower, elongated form of the diamond pyramid load or force, usually between 187.5 and
and was designed for use under lower test forces 3000Kgf, for a specified time (from 10 - 30 sec-
than the Vickers hardness test, allowing for more onds) typically using a 2.5 or 10mm diameter
accurate testing of brittle or thin materials. Both tungsten carbide ball, see schematic in Figure
the Vickers and Knoop tests continue as popular 23.3. The time under load (dwell) period is re-
hardness analysis methods today. quired to ensure that plastic flow of the metal

102
are usually not tested by the Brinell method.
L As such, Brinell testers are often manufactured
to accommodate large parts such as engine
castings and large diameter piping. A minimum
material thickness of at least 8x the testing depth

D is recommended (ISO 6506).

Due to the wide number of ball sizes and loads

available, it is possible to test a very wide range of
hardness values using the Brinell method. This is
constrained by the indenter ball itself, which can
d become deformed by testing harder materials.

It should be noted that there is a relationship

Figure 23.3. Schematic of the Brinell ball indenter making an
impression in a test surface. between load and ball diameter (L/D2), whereby
has ceased. Lower forces and smaller diameter tests with load/indenter combinations having the
balls are also used in specific applications. Similar same ratio give the equivalent HB values. Tests
to Knoop and Vickers testing, the Brinell test ap- with different ratios are not comparable. Errors
plies only a single test force. After removal of the in Brinell measurement are usually attributable
load, the resultant recovered round impression to poor surface condition or operator errors in
is measured across the indent at right angles optical measurement, but due to the large size
using a low-power microscope or an automatic of indent these errors tend to be limited.
measuring device and the average value used
to calculate hardness. Rockwell Testing
The actual Brinell hardness (HB) is calculated
by factoring the indent size and the test force,
such that:

HB = 2L
πD
2 (D - √D - d )
2 2

Where L = load, D = diameter of the ball indent-

er and d=diameter of the impression. It is not
necessary to make the actual calculation for each
test - calculation tables have been published for
Figure 23.4. Schematic of the Rockwell indentation process,
various combinations of diameters of impres-
using a diamond brale indenter.
sions, load and ball size. In addition various forms
of automatic Brinell reading devices are available Rockwell test methods are defined in the following
to perform these tasks. standards: ASTM E18 Metals, ISO 6508 Metals, and
ASTM D785 Plastics. It is recommended that oper-
Brinell testing is typically used in testing alu- ators have a current copy of the relevant standards,
minium and copper alloys (at lower forces) and which are updated regularly.
HARDNESS TESTING

steels and cast irons at the higher force ranges.

As the Brinell test uses relatively high loads, and The Rockwell test is based on the measurement of
therefore relatively large indent, it is frequently the depth to which an indenter is forced by a heavy
used to determine the hardness in circumstances (major) load beyond the depth resulting from a
where the overall material properties are being previously applied preliminary (minor) load. The
ascertained and local variations in hardness or test follows the sequence, see Figure 23.4:
surface conditions make other methods un-
suitable, such as forgings or castings of large
parts. Highly hardened steel or other materials
• Application of minor load. A ‘zero’ position is

103
HARDNESS TESTING
Table 23.1: Some common scales in Rockwell and Superficial Rockwell testing
Scale Minor Load (kg) Major Load (kg) Penetrator
HRA 10 60 Diamond
HRB 10 100 1/16in ball
HRC 10 150 Diamond
HR15N 3 15 Diamond
HR30N 3 30 Diamond
HR45N 3 45 Diamond

recorded. cone ground at 120 degrees for testing hardened

steels and carbides. Softer materials are typically
• Gradual application of load until the major load tested using tungsten carbide balls ranging in di-
is reached. The maximum penetration position ameters from 1/16 in up to 1/2in. The combination
is recorded. of indenter and test force make up the Rockwell
scale. These combinations make up 30 different
• Removal of load until the minor load is reached scales and are expressed as the actual hardness
number followed by the letters HR and then the
The resulting Rockwell number represents the dif- respective scale. A recorded hardness number of
ference in depth from the zero datum position as 63HRC signifies a hardness of 63 on the Rockwell C
a result of the application of the major load. The scale. Higher values indicate harder materials such
entire procedure requires as little as a few seconds as hardened steel or tungsten carbide. These can
(up to 15 for plastics), so the major advantage of the have HRC values in excess of 70HRC. Rockwell test
Rockwell test is that results are quickly and directly forces can be applied by either closed-loop load
obtained without the need for a secondary, dimen- cell or traditional deadweight systems.
sional measurement requirement.

There are two types of Rockwell test (Table 23.1): Factors Affecting Accuracy,
Precision and Bias for Rockwell
1. Rockwell: the minor load is 10 kgf, the major Testing
load is 60, 100, or 150 kgf. One of the primary factors affecting the precision
and reliability in the Rockwell test is the test machine
2. Superficial Rockwell: the minor load is 3 kgf and itself. Variability in test results is the sum of the
major loads are 15, 30, or 45 kgf. variability from the equipment and variability from
the operator and environmental conditions. Tests
In both tests, the indenter may be either a diamond
of Gauge Repeatability and Reproducibility (GR&R)
cone or tungston carbide ball, depending upon the
can show the degree to which machine variability
characteristics of the material being tested. Rockwell
takes up the available process tolerance. High
hardness values are expressed as a combination of
variability (or a narrow process tolerance) results
a hardness number and a scale symbol representing
in high GR&R. A GR&R test on different equipment
the indenter and the minor and major loads. The
used for the same process allows the user to directly
hardness number is expressed by the symbol HR
compare the in-built variability of the machine
and the scale designation.
values (the lower the GR&R value, the better the
performance of the equipment), see Figure 23.5.
The most common indenter type is a diamond
Research has shown [39] that closed-loop loading
Closed Loop 2.8
systems, as well as other design factors and build
Closed Loop 1.93
quality, can greatly improve the performance of
Dead Weight, Digital 10.18

Dead Weight, Digital 12.1

the equipment.
Dead Weight, Analog 15.73
Motorized
Dead Weight, Analog
Motorized 17.71 Rockwell testing is usually perceived to be one of
Dead Weight, Analog
Dashpot
22.2 the simpler testing methods, and indeed in prin-
0 5 10 15 20 25
ciple it can be very quick and accurate. However,
GR&R Value it is important to ensure that the condition of the
Figure 23.5. GR&R results of various Rockwell testers.
machine, specimen and set-up are correct to ensure

104
consistent and accurate results. There are, in fact, Vickers Testing
many factors that can adversely affect the Rockwell
Vickers and Knoop test methods are defined in the
result. For the most part, they can be avoided by
following standards: ASTM E384 and ISO 6507. It is
ensuring that correct practices are carried out, and
by proper calibration and maintenance.
Vickers
One of the more common sources of error is simply
indenter damage. Diamond indenters are very
hard, but also relatively brittle, and so it is possible
for them to be damaged by a heavy impact. Such
damage (or excessive wear of the tip) will change
the resistance to penetration, and typically result in
a high hardness reading. A deformed Ball indenter
can similarly induce high readings.

Another common cause of error is deflection in the

loading train. This can come from many sources,
all of which will typically cause low readings for
Rockwell hardness. If the anvil is damaged, or per-
haps has had an indent put into it, then any raised
Figure 23.6. Schematic of the Vickers indenter and the shape of
material at the surface will absorb some deflection an impression.
under loading. Similarly, if there is dirt or grease in
the contact area between the anvil and the elevat-
recommended that operators have a current copy of
ing screw or the elevating screw mechanism itself
the relevant standards, which are updated regularly.
this will cause excess deflection and change the
hardness reading.
In the Vickers test, a load is applied smoothly, with-
out impact, forcing a diamond indenter into the
The specimen itself is clearly of importance in
test piece, as illustrated in Figure 23.6. The Vickers
getting good results. While Rockwell testing is
diamond produces a square based pyramidal shape
insensitive to surface preparation relative to optical
with a depth of indentation of about 1/7th of the
test methods, the better the surface condition the
diagonal length. The indenter is held in place for
more accurate and reproducible will be the results.
10 to 15 seconds and then fully unloaded. The
The under-side of the specimen must also contact
physical quality of the indenter and the accuracy of
the anvil securely and without interference from
the applied load (which are defined in E 384) must
debris or other loose material. Specimens should
be controlled in order to get the correct results.
always be cleaned before testing. The specimen
must also be held in a stable manner during the test,
The two impression diagonals are measured, usually
as any movement of the specimen can significantly
to the nearest 0.1μm, and averaged. The Vickers
affect the result. A movement of 2µm is equivalent
hardness (HV) is calculated using:
to 1 Rockwell point. Excess vibration from the local
environment or unsuitable table can cause similar
problems. 1854.4L
HV =
d2
It should be apparent from the above that if the
HARDNESS TESTING

operator is adequately trained on proper fixturing Where the load L is in gf and the average diagonal
and testing techniques, the environment is suitable d is in μm (this produces hardness number units of
for testing, and that proper cleanliness and main- gf/μm2 although the equivalent units kgf/mm2 are
tenance regimes are carried out then most of the preferred; in practice the numbers are reported
problems described above can be avoided. without indication of the units). Tables or automatic
electronic or imaging measurements are a more
common and convenient way to generate Vickers
hardness numbers.

105
HARDNESS TESTING
Since the 1960s, the standard symbol for Vickers “Microindentation Vickers” (10 - 1000g) and “Mac-
hardness per ASTM E 2 and E384, has been HV. This roindentation Vickers” (1 - 100kg), to cover all
should be used in preference to the older, obsolete testing requirements. The indenter is the same for
symbols DPN or VPN. Rigorous application of the SI both ranges; therefore Vickers hardness values are
system results in hardness units expressed not in continuous over the total range of hardness for met-
the standard, understandable kgf/mm2 values but als (typically HV100 - HV1000). Because the shape of
in GPa units that are meaningless to most engineers the Vickers indentation is geometrically similar at all
and technicians. ASTM recommends a ‘soft” metric test loads, the HV value is constant, within statistical
approach in this. precision, over a very wide test load range as long
as the test specimen is reasonably homogeneous.
In the Vickers test, it is assumed that elastic recovery
does not occur once the load is removed. How-
ever, elastic recovery does occur, and sometimes
Microindentation Hardness Testing
its influence is quite pronounced. Generally, the Microindentation hardness testing, more commonly
impression (Figure 23.7) appears to be square, and (but incorrectly) called microhardness testing, is
widely used to study fine scale changes in hardness.
Although the term “microhardness” is generally
understood by its users, the word implies that the
hardness is extremely low, which is not the case. The
applied load and the resulting indent size are small
relative to bulk tests, but the same hardness number
is obtained. Consequently, ASTM Committee E-4
on Metallography recommends use of the term
“microindentation hardness testing” which could
be given the acronym MHT.
Figure 23.7: Example of a well-formed Vickers indentation
(400X).
The only difference between standard Vickers
testing and micro-indentation testing is the lower

Knoop

Figure 23.8: Example of a distorted Vickers indentation (400X).

the two diagonals have similar lengths. As with the

Brinell test, the Vickers hardness number is calcu-
lated based on the surface area of the indent rather
than the projected area. If the impression shape is
distorted due to elastic recovery (very common in
anisotropic materials), Figure 23.8, should the hard- Figure 23.9. Schematic of the Knoop indenter and the shape of
an impression
ness be based on the average of the two diagonals?
It is possible to calculate the Vickers hardness based
on the projected area of the impression, which can loads (<1kg) used. The indents made in the mate-
be measured by image analysis. While rigorous rial are therefore smaller, and this means that more
studies of this problem are scant in the literature, the localised areas of the material can be assessed.
diagonal measurement is the preferred approach For example, heat treaters have utilized the tech-
even for distorted indents, at this time. nique for many years to evaluate the success of
surface hardening treatments or to detect and
The Vickers test has two distinct force ranges, assess decarburization, by measuring hardness at
finely spaced intervals from the specimen surface.

106
Metallographers and failure analysts use the meth- are a more common and convenient way to gener-
od for a host of purposes including evaluation of ate Knoop hardness numbers.
homogeneity, characterization of weldments, as an
aid to phase identification, or simply to determine Aside from minor savings of time, one chief merit of
the hardness of specimens too small for traditional the Knoop test is the ability to test thin layers more
bulk indentation tests. easily. Around any indent in a material there will be
an area of plastic deformation. If this deformed area
coincides with an interface (such as the edge of the
Knoop Testing material) or a similar deformed area from another
The Knoop test uses a rhombohedral-shaped indent, then the resultant hardness reading will
diamond indenter, Figure 23.9. The long diago- be incorrect. This deformed area is linked to the
nal is seven times (7.114 actually) as long as the indent size, and to ensure correct tests it is usually
short diagonal. With this indenter shape, elastic recommended that the indents should be at least
recovery can be held to a minimum. The Knoop 2.5x the diagonal of the indent apart. The elongat-
test is conducted in the same manner, and with the ed form of the Knoop indent means that they can
same tester, as the Vickers test. However, only the be placed much closer together than a Vickers test
long diagonal is measured. This, of course, saves using the same load. Furthermore, if the hardness
a little time. varies strongly with the depth, the Vickers indent
can be distorted by this change; that is, the diagonal
The Knoop hardness is calculated from: parallel to the hardness change will be affected by
the hardness gradient. Care should also be taken
14229L that the thickness of the material is sufficient for
HV =
d2 testing. For Vickers tests, the thickness should also
be at least 2.5x the diagonal measurement. How-
ever, because the Knoop indent is shallower than
where the load L is in gf and the long diagonal d
the Vickers at the same load, significantly thinner
is in µm. The Knoop hardness is expressed in the
specimens can be tested.
same manner as the Vickers hardness; i.e., 375
HK0.3 means that a 300 gf load produced a Knoop
The down side of the Knoop indent is that the three
hardness of 375. (The kgf/mm2 unit information
dimensional indent will change with test load and,
is no longer reported). Again, the symbol HK was
consequently, HK varies with load. At higher loads
adopted in the early 1960’s while other terms; e.g.,
this variation is not substantial. Conversion of HK
HKN or KHN, are obsolete and should not be used.
values to other test scales can only be done reliably
for HK values performed at the standard load, gen-
Knoop tests, like Microindentation Vickers, are typi-
erally 500gf, used to develop the correlations. All
cally performed at test forces from 10 - 1000g. The
hardness scale conversions are based on empirical
measured area is used in a formula that includes
data. Conversions are not precise but are estimates.
applied force to determine a hardness value. Tables
or automatic electronic or imaging measurements

Table 23.3: Factors Affecting Precision and Bias in Microindentation Hardness Testing
Instrument Factors Measurement Factors Material Factors
Accuracy of the applied load Calibration of the measurement system Heterogenity of the specimen
HARDNESS TESTING

Strength of crystallographic texture, if

Inertia effects, speed of loading Numberical aperture of the objective
present
Lateral movement of the indenter or
Magnification Quality of specimen preparation
specimen
Indention time Inadequate image quality Low reflectivity or transparency
Indenter shape deviations Uniformity of illumination Creep during indentation
Damage to the indenter Distortion in optics Fracture during indentation
Inadequate spacing between indents
Operator’s visual acuity Oil, grease or dirt on indenter or specimen
or form edges
Angle of indentation Focusing of the image

107
HARDNESS TESTING
Factors Affecting Accuracy, dicular (±1°) to the stage plate. Next, the specimen
surface must be perpendicular to the indenter. Most
Precision and Bias for Vickers and
testers provide holders that align the polished face
Knoop
perpendicular to the indenter (parallel to the stage).
Numerous studies of microindentation hardness
If a specimen is simply placed on the stage surface,
test results conducted over a wide range of test
its back surface must be parallel to its polished
loads have shown that results are not constant at
surface. Tilting the surface of the specimen by more
very low loads. This problem, called the “indentation
than 1° from perpendicular results in non-symmetri-
size effect”, or ISE, has been attributed to funda-
cal impressions and can produce lateral movement
mental characteristics of the material. However, the
between specimen and indenter.
same effect is observed at the low load test range
(1-10kgf) of bulk Vickers testers [41] and an ASTM
In most cases, the major source of error is not the
interlaboratory “round robin” of indents made by
mechanical indentation process - although this can
one laboratory but measured by twelve different
occur [45], and it is important to check the perfor-
people, reported all three possible ISE responses
mance of your tester regularly using a certified test
[42, 43] , for the same indents!
block. It is best to use a test block manufactured for
microindentation testing and certified for both the
Many factors (see Table 23.3) can influence the
test type (Vickers or Knoop) and the load that you
quality of microindentation test results [42]. In the
intend to use. However, because of the light loads
early days of low-load (< 100gf) hardness testing,
used, vibration can contribute to loading inaccuracy.
it was quickly recognized that improper specimen
Micro-indentation hardness testers should always
preparation may influence hardness test results.
be placed on a level, sturdy (preferably dedicated
There are cases where improper preparation can
anti-vibration) surface. The surface should not be in
lead to higher test results and other cases that can
contact with an adjoining table or wall, as vibration
lead to lower results. For many years, it was consid-
can be transferred by such prosaic events as a slam-
ered necessary to electrolytically polish specimens
ming door, or by someone working on an adjoining
so that the preparation-induced damage could
surface. Similarly, the floor on which the test table
be removed, thus permitting bias-free low-load
is placed should be solid.
testing. However, the science behind mechanical
specimen preparation, chiefly due to the work of
Len Samuels [44] , has led to the development of
excellent mechanical specimen preparation proce-
dures, and electropolishing is no longer required.
Specimen preparation quality becomes more
important as the load decreases, and it must be at
an acceptable level.

There are several operational factors that must be

controlled in order to obtain optimum test results.
First, it is a good practice to inspect the indenter
periodically for damage, for example, cracking or
chipping of the diamond. If you have metrology
equipment, you can check the face angles and
Figure 23.10. Wilson® VH3100 Automatic Vickers/Knoops
the sharpness of the tip. Specifications for Vickers Hardness Tester.
and Knoop indenter geometries are given in E384
or ISO 6507. Place the indent in the center of the
The greatest source of error is in the process of actu-
measuring field, if it is not already there, as lens
ally measuring the indent, as has been documented
image quality is best in the center. The light source
in an ASTM inter-laboratory tests [41, 42]. Because
should provide adequate, even illumination to en-
of the method of defining HV and HK, where we
sure maximum contrast and resolution.
divide by d2, measurement errors become more
critical as d gets smaller.
One source of error in the tests is the alignment of
the specimen surface relative to the indenter. The
For the Knoop indent, the main problem in resolving
indenter itself must be properly aligned perpen-

108
the diagonal accurately is the image contrast at the always selectable.
indent tips, which can be very narrow. This tends
to result in undersized indents that, along with the Microindentation hardness testing is a very valuable
variable indent shape, both result in increasing tool for the materials engineer but it must be used
HK with decreasing test load. For the Vickers test, with care and a full understanding of the potential
although both under-sizing and over-sizing can problems that can occur.
occur, experience suggests that oversizing is much
more commonly encountered for low loads and • Always try to use the highest possible load de-
small indents. pending upon the indent spacing or closeness
to edges.

Automation • Try to keep indents greater than 20μm in diam-

Manual microindentation hardness testing can be eter, as recommended in ASTM standard E384
tedious for an operator, so anything that can be and ISO 6507.
done to simplify testing is valuable, especially for
laboratories that do substantial testing. Many ad- If you have not read the standards mentioned
juncts to indent measurement have been tried and a above, or it has been some time since you read it
variety of such systems are available. There has been (standards must be reviewed and revised, if neces-
considerable interest in applying image analyzers sary, regularly), get the latest copy and go over it.
to the indent measurement task. Further, with stage Sections such as ‘Precision and Bias’ and appendix
automation, it is possible to automate the indenting X1 of E384 contain a wealth of practical advice.
process itself, and with the same equipment. Figure
23.10 shows a Wilson automated hardness testing
system. Such systems can be used in fully automatic, HELPFUL HINTS FOR
semiautomatic or manual modes, depending upon MICROINDENTION HARDNESS
the nature of the testing. An automated system can TESTING
be programmed to make multiple indents in either
If you suspect that the test results obtained on
a defined pattern or statistical groups.
a specimen are questionable, verify the tester
using a certified test block. When testing thin
The system then makes the indents at the requested
coatings, use the Knoop indenter with the
loads and locations, measures each indent, cal-
long axis parallel to the surface. If you have a
culates the hardness (and desired conversions to
specimen where the hardness changes rapid-
other scales), and prints/plots the results. Statistical
ly, Vickers indents may be distorted badly in
analysis can also be done.
the direction of the hardness gradient. Switch
to a Knoop indenter and place the long axis
In general, Vickers indents are easier to measure by
perpendicular to the hardness gradient.
image analysis than Knoop due to the lower contrast
at the tip of the Knoop indents (leads to undersizing
and higher HK values). Metal flow (plastic defor-
mation) or surface debris around the indent edges
can also interfere with measurement precision.
Vickers indents, like the ones shown in Figure 23.6,
exhibit excellent contrast and shape and are easily
measured. If the magnification is too high (and this
HARDNESS TESTING

may be influenced by the numerical aperture of the

objective) for a given indent size, image contrast
suffers and correct detection of the indent will be
very difficult. On the other hand, if the indent is very
small on the screen, it will be hard for the system to
detect it automatically. As such, properly selected
magnifications are very important to achieving
accurate results over a range of conditions. Some
systems are available with “zoom” objectives, that
effectively ensure the optimum magnification is

109
LABORATORY SAFETY
The metallographic laboratory is a relatively safe
working environment; however, there are dangers
inherent to the job. Included in these dangers
is exposure to heat, acids, bases, oxidizers and
solvents. Specimen preparation devices, such as
drill presses, shears and cutoff saws, also present
hazards. In general, these dangers can be minimized
if the metallographer consults documents such as
ASTM E 2014 (Standard Guide on Metallographic
Laboratory Safety) and relevant Safety Data Sheets Figure 24.1. Carelessness in the laboratory can result in
(SDS) before working with unfamiliar chemicals. dangerous chemical spills and a clean-up nightmare.

Common sense, caution, training in basic laboratory

skills, a laboratory safety program, access to safety Many of these chemicals used in metallography
reference books – these are some of the ingredients can cause serious damage on contact. It is best to
of a recipe for laboratory safety. Table 24.1 lists assume that all chemicals are toxic and all vapors or
the main requirements for a comprehensive safety fumes will be toxic if inhaled or will be damaging to
program. the eyes. A hood will prevent the working area from
being contaminated with these fumes. However, you
Safe working habits begin with good housekeeping. will not be protected when your head is inside the
A neat, orderly laboratory promotes safe working hood. In most cases, a protective plastic or shatter-
habits, while a sloppy, messy work area invites proof glass shield can be drawn across the front of
disaster. Good working habits include such obvi- the hood for further protection from splattering or
ous, commonsense items as washing the hands any unexpected reactions.
after handling chemicals or before eating. Simple
carelessness can cause accidents (see Figure 24.1). All laboratories should be equipped with a shower
For example, failure to clean glassware after use and eyewash for emergency use. This equipment
can cause an accident for the next user. Another should be near the work area so that the injured can
common problem is burns due to failure to properly reach it quickly and easily. Fire alarms and fire extin-
clean acid spills or splatter. guishers (CO2 type) should be available and tested
periodically. A good first aid kit and a chemical spill
Most reagents, chemical or electrolytic polishing treatment kit should be readily available.
electrolytes, and solvents should be used under a
ventilation hood designed for use with chemicals.

Table 24.1. Elements of a Comprehensive Metallography Laboratory Safety Plan

1. Emergency Response 6. Equipment Use (JSAs)
a. First Responders a. Sectioning
b. Emergency Phone Numbers b. Mounting
c. First Aid c. Grinding and Polishing
d. Spills d. Electropolishing
2. Chemical Procurement, Distribution, and Storage e. Etching
a. SDS Management 7. Facility
b. Labeling/Storage a. Facility and Equipment Maintenance
3. Laboratory SOPs b. Housecleaning
a. Handling Chemicals c. Fume Hood Air Flow
b. Mixing Chemicals d. Fire Extinguishers and Fire Protection
c. Rules e. Spill Response
d. Hygiene f. Showers and Eye Washes
g. Air Lines and Filters
4. Employee Health and Exposure
h. Plumbing
a. Personal Protective Equipment
i. Electricals
b. Monitoring of exposure levels
c. Medical Evaluations 8. Employee Training
d. Additional protections for employees working with a. Safety
particularly hazardous substances (carcinogens, toxins) b. Indications and Symptoms of Exposure
c. Job Functions
5. Disposal of Hazardous Materials
a. Etchants and Chemicals 9. Scheduled and Documented Safety Inspections and
b. Recirculating Tanks Meetings
c. Lubricants and Abrasives

110
FULL LAB & SOLUTIONS
Laboratory Equipment drill and spun around, inflicting serious lacerations.
Hair, ties, and shirt cuffs can become tangled in a
Specimen preparation devices used in metallo-
drill, inflicting serious injuries. Safety glasses should
graphic laboratories are generally quite safe to use.
always be worn when using drill presses or when
Information supplied by the manufacturer usually
cutting or grinding. Mounting presses or laboratory
describes safe operating procedures. It is good
heat-treatment furnaces present potential burn
laboratory practice to prepare a job safety analysis
hazards. It is a good practice to place a “hot” sign in
(JSA) detailing potential hazards and describing
front of a laboratory furnace when it is in use. Gloves
the safe operating procedure for each piece of
should be worn when working with these devices.
equipment. This information should be provided
Modern mounting presses that cool the cured resin
to all users and it must be revised and reviewed
back to near room temperature dramatically reduce
periodically.
the potential for burns.
Band saws or abrasive cutters are commonly used
It is occasionally necessary to heat solutions during
by metallographers. The cutting area of band saws
their preparation or use. Although Bunsen burners
is exposed and potentially dangerous. Your hands
are commonly employed for this purpose, it is much
should never be used to guide the work piece
safer to use a hot plate or water bath and thus avoid
during cutting. A guiding device or block of wood
the use of an open flame. If a Bunsen burner is used,
should always be used between the work piece
the flame should never be applied directly to a flask,
and your hands. After cutting is completed, the saw
beaker, or dish. Plain- or asbestos-centered wire
should be turned off before pieces near the blade
gauze should always be placed between the flame
are removed. Samples should be handled careful-
and the container.
ly, because considerable heat can be generated.
In addition, sharp burrs are often present, which
should be carefully removed by filing or grinding. Personal Protective Equipment (PPE)
Abrasive cutoff saws are safer to use because the Metallographers must take certain precautions to in-
cutting area is closed off during use. The chief sure their personal safety. A laboratory coat is useful
danger is from flying pieces from a broken wheel. for protecting the operator’s clothing, and should
Fortunately, the closed cover contains these pieces be changed regularly and cleaned professionally.
within the cutting chamber. Wheel breakage usually When handling caustics, a rubberized or plastic
occurs when the part is not firmly clamped in place coated apron provides better protection. Gloves
or if excessive pressure is applied, a bad practice should be worn when handling bulk samples, work-
from the standpoint of specimen damage as well. ing with hot material, or using hazardous solutions.
Lightweight surgeons’ gloves are very popular,
Dust produced during grinding of metals is always
because the operator retains the ability to “feel.”
dangerous. For certain metals, like beryllium, mag-
Many metallographers wear these to protect their
nesium, lead, manganese, and silver, the dusts are
skin when mounting with epoxies and polishing
extremely toxic. Wet grinding is preferred both for
with oxide suspensions. When using these gloves
dust control and for preventing thermal damage to
with chemicals, always inspect for holes, as they
the specimen. Bench grinders must be firmly mount-
are easily punctured. Thick rubber gloves are often
ed to prevent sudden movement. Care must be
used for handling specimens during macroetching,
exercised to avoid grinding one’s fingers or striking
chemical polishing, pickling, etc. The gloves should
the edge of a grinding belt, which will cause painful
always be checked first for small holes or cracks,
lacerations. With nearly all materials, wet grinding
because gloves can impart a false sense of security.
is preferred and produces best results. For routine
The operator’s hands generally perspire when using
handling of dangerous metals, grinding should be
rubber gloves and it is sometimes difficult to tell
done wet under a ventilation hood. Waste must be
if the moisture is due solely to perspiration or to
handled carefully and disposed of properly. Radio-
leakage. Safety glasses should be worn during pro-
active materials require special remote- handling
cesses that generate particulate matter. Goggles are
facilities and elaborate safety precautions.
appropriate for use with chemicals, and a chemical
face shield is recommended when handling large
A drill press is frequently used in the laboratory.
quantities of hazardous liquids. The appropriate
Drilling holes in thin sections requires secure clamp-
PPE will be specified on the SDS for most laboratory
ing; otherwise the sample can be grabbed by the
chemicals and products.

111
LABORATORY SAFETY
Chemicals, Storage and Handling laboratory balance provides adequate weighing
accuracy, while graduated cylinders provide accept-
Many of the chemicals used in metallography
able accuracy for volumetric measurements. These
are toxic, corrosive, flammable, or potentially
devices should be cleaned after use to prevent ac-
explosive. Whenever possible, purchase small quan-
cidents to the next user. For weight measurements,
tities that are likely to be used within a reasonably
a clean piece of filter paper, or a cup, should be
short time. Flammable solvents should be stored in
placed on the balance pan to hold the chemical,
fireproof steel cabinets. Acids and bases should be
to protect the pan surface, and to facilitate transfer
stored separately, again in fireproof steel cabinets.
to the mixing beaker. A large graduated beaker is
Strong oxidants must not be stored along with acids,
usually employed for mixing solutions.
bases or flammable solvents.

Reagent-grade chemicals or solvents of highest pu-

rity are recommended. Although more expensive,
the amounts used are small and the gain in safety
and reliability compensates for the cost difference.
Chemicals may deteriorate during storage. Expo-
sure to light can accelerate deterioration of some
chemicals. Hence, they should be stored in a closed
metal cabinet.

Etchants
Most laboratories mix commonly used reagents in
quantities of 250 to 1000mℓ and then store them
as stock reagents. Many reagents can be safely Figure 24.2. When mixing etchants, use a magnetic stirring
handled in this manner. It is best to store only those plate with a magnetic bar for stirring. Slowly add the liquid
ingredients to the solvent by dripping them down a glass
reagents that are used regularly. Glass-stoppered stirring rod. If the solution is more dangerous than this one, wear
bottles are commonly used as stock reagent bottles. protective gloves and use a face shield. If mixing generates
substantial heat, it is a good practice to place a cooling jacket
If these bottles are opened regularly, the stopper around the beaker.
will not become “frozen”. However, if they are used
infrequently, a frozen stopper often results. Holding With many etchants, the mixing order is import-
the neck of the bottle under a stream of hot water ant, especially when dangerous chemicals are
will usually loosen them. If thermal expansion does used. When water is specified, distilled water
not free the stopper, the stopper can be gently should always be used, because most tap wa-
tapped with a piece of wood. Glass bottles with ter contains minerals or may be chlorinated or
plastic screw-on tops can be used so long as the fluorinated. Tap water can produce poor results or
solution does not attack the plastic. These bottles unexpected problems. Cold water should always be
are useful for holding solutions, such as nital, that used, never warm or hot water, which can cause a
can build up gas pressure within a tightly stoppered reaction to become violent. In mixing, one should
bottle. A small hole can be drilled through the cap start with the solvents, such as water and alcohol;
top to serve as a pressure relief vent. Tightly stop- then dissolve the specified salts. A magnetic stirring
pered bottles of nital and some other solutions device is of great value, as shown in Figure 24.2.
have exploded as the result of pressure buildup. Then, the dangerous chemicals, such as acids,
Be certain that the reagent is safe to store and store should be added carefully and slowly while the solu-
only small quantities. All bottles should be clearly la- tion is being stirred. Whenever sulfuric acid (H2SO4)
beled. Polyethylene bottles are required for etchants is specified, it should be added last. It should be
containing hydrofluoric acid, which attacks glass. added slowly, while stirring, and it should be cooled,
if necessary, to minimize heating. Never just pour
Most recipes for etchants or electrolytes list the in- one liquid into another, as shown in Figure 24.3. If
gredients by weight if they are solids and by volume sulfuric acid is added to water without stirring, it
if they are liquids. In a few cases, all amounts are can collect at the bottom of the beaker and enough
given in weight percentages. In most cases, reagent local heating can occur to throw the contents out
compositions are not extremely critical. An ordinary of the beaker.

112
FULL LAB & SOLUTIONS
can travel along the ground and can be ignited at
a distance. Acetone can form explosive peroxides
on contact with strong oxidizers such as acetic acid,
nitric acid and hydrogen peroxide. It is an irritant
to the eyes and respiratory tract, and will cause the
skin to dry and crack.

Butyl cellosolve (HOCH2CH2OC4H9), or ethylene

glycol monobutyl ether, is a colorless liquid with
a rancid odor that is used in electropolishing solu-
tions. It is combustible and may form explosive
peroxides. It is toxic in contact with the skin, can
be absorbed through the skin, can cause serious
Figure 24.3. Illustration of a bad mixing practice. The acid damage to the eyes, irritation to the skin and re-
ingredient was poured into an empty acid bottle and the spiratory tract.
solvents were added without stirring or cooling. The solution
may erupt in the metallo-grapher’s face at any moment. It is
recommended to keep the hands clear of the area and remove Carbitol (C2H5OCH2CH2OCH2CH2OH), or diethylene
rings.
glycol monoethyl ether, is a colorless, viscous sol-
The literature contains references to a great many vent that is compatible with water and is used in
formulas for etchants, chemical polishes, and electropolishing solutions. It irritates the skin, eyes,
electrolytes that are potentially dangerous or ex- mucous membranes, and upper respiratory tract,
tremely dangerous. Few of these references contain and is harmful if inhaled or swallowed.
comments regarding safe handling procedures or
potential hazards. Fortunately, metallographic ap- Ethylene glycol (HOCH 2CH 2OH) is a colorless,
plications involve small quantities of these solutions, hygroscopic liquid with a sweet taste (but do not
and accidents do not usually produce catastrophic swallow as it is poisonous) that reacts with strong
results. However, even with small solution volumes oxidants and strong bases. It is flammable. The
considerable damage can be, and has been, done. substance irritates the eyes, skin, and the respira-
Table 24.2 lists examples from the literature [27-29] tory tract.
of chemical polishing solutions, electrolytic polish-
ing solutions and etchants that have been involved Glycerol (glycerin) (CH2OHCHOHCH2OH) is a col-
in accidents. Table 24.3 lists a number of commonly orless or pale yellow, odorless, hygroscopic, syrupy
used chemicals and incompatible chemicals. liquid with a sweet, warm taste. It is relatively nontox-
ic and nonvolatile but can cause iritis (inflammation
Solvents of the iris). It is combustible and is a moderate fire
Numerous organic solvents are used for cleaning hazard. Glycerol should never be used in anhy-
or are ingredients in chemical or electrolytic pol- drous solutions containing nitric and sulfuric acids,
ishing solutions or etchants, where they are used because nitroglycerin can form. Glycerol should
to control ionization or the speed and mode of not be used with strong oxidizing agents, such as
attack. Commonly employed solvents include wa- chromium trioxide and potassium permanganate,
ter, acetone, ethyl ether, ethylene glycol, glycerol as an explosion may occur. Glycerol is often added
(glycerin), kerosene, petroleum ether, trichloro- to aqua regia (glyceregia). This mixture decomposes
ethylene, butyl cellosolve, and alcohols, such as readily and should be discarded immediately after
amyl alcohol, ethanol, methanol, and isopropyl use. This etchant should not be allowed to stand for
alcohol. Most are flammable and their vapors can more than about 15 minutes after mixing.
form explosive mixtures with air. They should be
kept closed when not in use and should be stored Kerosene is occasionally employed in grinding
in a cool place away from heat and open flames. samples and with diamond paste as a lubricant.
Only the deodorized form should be used. It is
Acetone (CH3COCH3) is a colorless liquid with flammable, but the vapors do not readily explode.
a fragrant mint-like odor. It is volatile and highly Contact defattens the skin and can cause dermatitis,
flammable. It is an irritant to the eyes and the mu- irritation or infections.
cous membranes. Its vapor is denser than air and
Trichloroethylene (CHCl:CCl 2 ) is a stable,

113
LABORATORY SAFETY
Table 24.2: Chemical and Electrolytic Polishing Solutions and Etchants Known to be Dangerous
Solution Use Problems
5 parts Lactic Acid Chemical polishing solution for Zr Lactic and nitric acids react automatically.
5 parts HNO3 Explosion can occur if stored
2 parts water
1 part HF
50 parts Lactic Acid Chemical polishing solution for Lactic and nitric acids react automatically.
30 parts HNO3 Ta, Nb, and alloys Explosion can occur if stored
2 parts HF
3 parts Perchloric Acid Electropolishing solution for Al Mixture is unstable and can, and has, exploded with
1 part Acetic Anhydride heating or in the presence of organic compounds
adding to the potential hazard.
60-90 parts Perchloric Acid Electropolishing solution Solution will explode at room temperature.
10-40 parts Butyl Cellosolve Solutions with ≤30% HClO4 will be safe if T is <20°C
100g CrO3 Electropolishing solution CrO3 was dissolved in water, cooled to about 20°C;
200mℓ water the acetic anhydride was added very slowly with
700mℓ Acetic Anhydride stirring. The solution became warm to the touch.
About 20 seconds later it erupted from the beaker.
1 part HNO3 Electropolishing solution for Mixture is unstable and cannot be stored.
2 parts Methanol Muntz (Cu-40% Zn) metal
20mℓ HF Etchant fo Nb, Ta, Ti, V, Zr This etchant is unstable. At 20°C, it reacted after
10mℓ HNO3 18 hours. at 30-35°C, it reacted after 8 hours with
30mℓ Glycerol violence. At 100°C, it will react after 1 minute.
20-30mℓ HCl Etchant for Ni and stainless steels Two incidents occurred when a violent reaction
10mℓ HNO3 resulted producing NO2 and a spray of acid after the
30mℓ Glycerol etch was left standing for 2-3 hours.
40mℓ Acetic Acid Etchant for Ni A closed bottle exploded about 4 hours after it was
40mℓ Acetone mixed. Authors state that solutions without the acetic
40mℓ HNO3 acid also cannot be stored.
10mℓ HNO3 Etchant The solution reacted spontaneously about 2 minutes
10mℓ Acetic Acid after mixing with evolution of heat and fumes
20mℓ Acetone (nitrous and nitric oxides). The mixed acids were
poured into the acetone. The beaker was externally
cooled.
50mℓ Nitric Acid Etchant Mixtures have exploded violently after mixing or
90mℓ Isopropyl Alcohol about 20 minutes after mixing.

Table 24.3: Some Incompatible Chemicals

Chemical Use in Metallography Do Not Mix with the Following:
Acetid Acid Chemical polishing, Electrolytic Chromic acid, glycol, hydroxol compounds, nitric
polishing acid, peroxides, permanganates
Acetone Degreasing, cleaning, etchants Concentrated solutions of nitric and sulfuric acid
Chromic Acid Electropolishing Acteic acid, flammable liquid, glycerol
Hydrogen Peroxide Chemical polishing, etchants Flammable liquid, organic materials
Nitric Acid (conc) Chemical polishing, etchants Acetic acid, chromic acid, flammable liquids,
isopropyl alcohol
Perchloric Acid Electropolishing Acetic anhydride, alcohol, some organics, oil, grease
Sulfuric Acid Etchants Methyl alcohol, potassium chlorate, potassium
perchorate and potassium permanganate

114
FULL LAB & SOLUTIONS
colorless liquid with a chloroform-like odor. liquid and is a dangerous fire hazard. Metallogra-
Effective laboratory ventilation is necessary. At phers have used it as a substitute for ethanol but
ambient temperatures it is nonflammable and isopropyl alcohol has quite different characteristics
nonexplosive, but becomes hazardous at higher temp- and should not be used. Fatal injuries and explo-
eratures. In the presence of strong alkalies, with sions have been reported due to its use.
which it can react, it can form explosive mixtures.
In the presence of moisture, the substance can be
Acids
decomposed by light to corrosive hydrochloric acid.
It is carcinogenic to humans, and toxic when inhaled Inorganic and organic acids are common constitu-
or ingested, which may cause acute poisoning. ents in chemical and electrolytic polishing solutions
and in etchants. The inorganic, or mineral acids,
Amyl alcohol (CH3(CH2)4OH), or 1-Pentanol, is a col- including the very familiar acids such as hydro-
orless liquid with noxious odor. It is flammable and chloric, nitric, perchloric, phosphoric, and sulfuric,
the vapors may form explosive mixtures at elevated are highly corrosive and poisonous.They should
temperatures. The substance reacts violently with be stored in a cool, well-ventilated location away
strong oxidants and attacks alkaline metals. The from potential fire hazards and, of course, away
fumes are irritating to the eyes, upper respiratory from open flames. They should not be stored in a
tract, and skin. The substance is toxic through in- location that receives direct sunlight. When the pure
gestion, inhalation, or absorption through the skin. acids contact metals, most liberate hydrogen gas –
a fire and explosion hazard. The organic acids are
Ethyl alcohol (CH3CH2OH), or ethanol, is a colorless, naturally occurring substances in sour milk, fruits,
inoffensive solvent commonly used in metallog- and plants and include the following acids: acetic,
raphy. Ethanol is miscible with water and rapidly lactic, citric, oxalic, and tartaric.
absorbs up to 5% water from the air. The denatured
version is less expensive and contains 5% absolute Hydrochloric acid (HCl), commonly used in metal-
methanol and is suitable for any recipe requiring lography, is a colorless gas or fuming liquid with a
ethyl alcohol. It is a dangerous fire hazard, and its sharp, choking odor. It is very dangerous to the eyes
vapors are irritating to the eyes and upper respi- and irritating to the nose and throat. It attacks the
ratory tract. High concentrations of its vapor can skin strongly causing severe burns.
produce intoxication. Because ethanol is completely
burned in the body, it is not a cumulative poison Nitric acid (HNO3), also commonly used in metal-
like methanol. lography, is a colorless or yellowish fuming liquid,
highly toxic and dangerous to the eyes. If it contacts
Methyl alcohol (CH3OH) is an excellent, non-hy- organic material or other easily oxidizable materials,
groscopic solvent, but it is a cumulative poison. it can cause fires and possibly explosions. When it
Ingestion, inhalation or absorption through the reacts with other materials, toxic oxides of nitro-
skin in toxic levels can damage the central nervous gen are produced. The oxides, which vary with the
system, kidneys, liver, heart, and other organs. conditions, include nitrous acid, nitrogen dioxide,
Blindness has resulted from severe poisoning. It is nitric oxide, nitrous oxide, and hydroxylamine. A
particularly dangerous because repeated low-level commonly encountered problem involves pouring
exposures can also cause acute poisoning as a nitric acid into a graduated cylinder that contains
result of accumulation. Ethanol should be used some methanol or ethanol from prior use. The
whenever possible. When using methanol, always brown fumes given off are quite harmful. Mixtures of
work under a ventilation hood. Mixtures of methanol nitric acid and alcohols higher than ethanol should
and sulfuric acid can form dimethyl sulfate, which not be stored. Mixtures of concentrated nitric and
is extremely toxic. Solutions of methanol and nitric sulfuric acids are extremely dangerous, while strong
acid are more stable than mixtures of nitric acid and mixtures of nitric acid and glycerin or glycols can
higher alcohols. be explosive. Aqua regia, a mixture of one part
nitric acid and two to four parts hydrochloric acid,
Isopropyl alcohol [CH3CH(OH)CH3], also known as forms several products including nitrosyl chloride,
2-propanol, is a clear, colorless liquid that, like eth- an exceptionally toxic gas. Aqua regia is a popular
anol, does not accumulate in the body, although it etchant but must be used with care under a hood.
does have a strong narcotic effect. It is a flammable
Ethanol with additions of up to 3% nitric acid (nital)

115
LABORATORY SAFETY
can be safely mixed and stored in small quantities. poured into a graduated cylinder containing only
Higher concentrations result in pressure buildup in remnants of ethanol or methanol.
tightly stoppered bottles. Explosions of 5% nitric
acid in ethanol have occurred as a result of failure Sulfuric acid (H2SO4) is a colorless, oily liquid that
to relieve the pressure. If higher concentrations is highly corrosive, a strong oxidizing agent, and
are desired, they can be mixed daily, placed in an dangerously reactive. It reacts violently with bases
open dish, and used safely. Discard the etchant at and is corrosive to most metals forming flammable/
the end of the day. Mixtures of methanol with up explosive hydrogen gas. It reacts violently with water
to 5% nitric acid are safe to use and store in small and organic materials with evolution of heat. Upon
quantities. Mixtures of methanol with more than 5% heating, toxic sulfur oxides are formed. slowly to
nitric acid if heated are subject to violent decompo- water with constant stirring. If added without stirring,
sition. Mixtures of 33% nitric acid in methanol have it will produce a pocket of steam in the bottom of
decomposed suddenly and violently. the vessel, throwing the contents out of the vessel.
Concentrated sulfuric acid can cause severe, deep
Never add nitric acid to isopropyl alcohol. Anderson burns on contact with the skin, and permanent vision
[27] reported that a liter bottle of 5% nitric acid loss on contact with the eyes. Tissue is destroyed
in isopropyl alcohol was mixed and placed in a by the acid’s dehydrating action. Lungs may be af-
cabinet. Although this had been done many times fected by long-term or chronic exposure to aerosol.
in the past without problems, twenty minutes later Skin lesions, tooth erosion, and conjunctivitis are
the bottle exploded destroying the cabinet, other other long-term effects.
stored bottles, and throwing debris up to 20 feet
away. Anderson [27] also reported that a metallog- Hydrofluoric acid (HF) is a clear, colorless, fuming
rapher was pouring a freshly mixed liter of 5% nitric liquid or gas with a sharp, penetrating odor. It is very
acid in isopropyl alcohol into another bottle when dangerous to the eyes, skin, and upper respiratory
it exploded. The person died within three hours tract. The substance can be absorbed into the body
without being able to tell anyone what happened. by inhalation, through the skin and by ingestion.
As with the other explosion, this same procedure A harmful concentration of the gas in air can be
had been performed many times previously without reached quickly, making it very dangerous to han-
mishap. Anderson recommends avoiding use of dle. Exposure by ingestion, inhalation or contact,
isopropyl alcohol completely. can be fatal. Undissociated HF poses a unique threat
in that it can destroy soft tissues and result in de-
Most metallographers consider nital to be very safe calcification of the bone. Moreover, the effects may
to use, and indeed it is. However, even with such an be delayed. Laboratories where HF is used should
apparently safe solution, one can have accidents. stock an antidote kit to be used in case of exposure.
One such accident occurred when an employee, Although it is a relatively weak mineral acid, HF
not a skilled metallographer, was replenishing a will attack glass or silicon compounds, and should
stock of 5% nitric acid in ethanol using a procedure be measured, mixed, and stored in polyethylene
that he had claimed to have performed many times vessels. HF reacts with many compounds, including
previously (he was not taught the safe way to mix metals, and will liberate explosive hydrogen gas.
nital as it was a union chemist’s job to mix nital
i.e., not his job). The worker began by adding the Orthophosphoric acid (H3PO4), a colorless thick
desired volume of concentrated nitric acid into the liquid or hygroscopic crystal, is a medium strong
container that contained a small residual amount of acid. It is corrosive to the skin, eyes and respiratory
stale 5% nital. To his surprise, the contents began tract. Phosphoric acid decomposes on contact with
“boiling” and spewing out of the container along alcohols, aldehydes, cyanides, sulfides, ketones, and
with dense, brown fumes. The acid splashed the can react with halogenated organic compounds
worker, resulting in burns on his forehead, face and forming organophosphorus nerve-gas type com-
eyes. The small amount of aged nitric acid solution pounds that are extremely toxic. It reacts violently
(the concentration may have been increased due to with bases, and will generate hydrogen gas when
evaporation of the alcohol), present in the container it reacts with metals.
when the fresh acid was added, created a danger-
ous chemical reaction. An experiment also showed Perchloric acid (HClO 4) is a colorless, fuming,
that a similar reaction can occur when nitric acid is hygroscopic liquid. It is extremely unstable in

116
FULL LAB & SOLUTIONS
Figure 24.4. Diagram developed by Médard, Jacquet and Sartorius showing safe (A and 1 to 9) nonexplosive electropolishing solutions
and explosive (C, E and Los Angeles) compositions of perchloric acid, acetic anhydride and water (brought in by the perchloric acid, but not
corrected for the effect of acetic anhydride).

concentrated form and may explode by shock or on February 20, 1947, in an electroplating factory
concussion when dry or drying, so commercially in Los Angeles. In this accident 17 people were
available perchloric acids come in concentrations of killed and 150 were injured [29]. Medard, Jacquet,
65 to 72%. In this form, contact with perchloric acid and Sartorius have prepared a ternary diagram
will cause irritation and burns, while its fumes are showing safe compositions of perchloric acid, acetic
highly irritating to the mucous membranes. Contact anhydride, and water, Figure 24.4. Anderson, how-
with organic, or other easily oxidized material, can ever, states that accidents have still occurred with
form highly unstable perchlorates, which can ignite solutions in the “safe” region of this diagram [27].
and cause explosions. Regular use of perchloric Electropolishing solutions composed of perchloric
acid requires that the ventilation system must be acid and acetic anhydride are not recommended.
specifically designed and maintained for perchloric Many companies forbid the use of such mixtures,
acid. Special fume hoods with a waterfall-type fume and some cities have banned their use. Electrop-
washer will remove the perchlorate fumes before olishing solutions of perchloric acid and alcohol,
they can enter the exhaust system. with or without organic additions, and mixtures of
perchloric acid and glacial acetic acid are safe to
Perchloric acid is very useful in electropolishing use. Nevertheless, in using these “safe” mixtures,
solutions. Never electropolish samples mounted one should follow the formula instructions carefully,
in phenolic (Bakelite) or other plastics in perchloric mix only small quantities, keep the temperature un-
acid solutions as explosions can result. The mixture der control, and avoid evaporation. These solutions
of perchloric acid and acetic anhydride, which was should not be stored.
developed by Jacquet, is difficult to prepare and
highly explosive. Jacquet has reviewed the acci- Mixtures of acetic acid and 5-10% perchloric
dents involving perchloric acid and has described acid have been commonly used to electropolish
safety procedures [30]. The worst accident occurred iron-based alloys and are reasonably safe. Do

117
LABORATORY SAFETY
not use these solutions to electropolish bismuth, is an irritant to the skin, eyes and respiratory tract;
arsenic or tin, as explosions have occurred. no unusual problems are encountered except for
Anderson suggests that arsenic, antimony, and occasional allergic reactions.
tin may also be incompatible with perchloric
electrolytes [27]. Do not store these electrolytes Lactic acid (CH3CHOHCOOH) is a yellow or color-
. Discard them when they become colored by less thick liquid. It is damaging to the eyes.
dissolved metallic ions (from electropolishing).
Always keep these solutions cool; increasing the Oxalic acid (COOHCOOH·2H 2 O) comes as
temperature increases the oxidizing power of transparent, colorless crystals. It is poisonous if in-
perchloric acid. gested and irritating to the upper respiratory tract
and digestive system if inhaled. Skin contact pro-
Comas et al. have studied the hazards associated duces caustic action and will discolor and embrittle
with mixtures consisting of butyl cellosolve and from the fingernails. It is not compatible with nitric acid,
10 to 95% of 70% perchloric acid [31]. Mixtures with as it reacts violently with strong oxidants. It can also
60 to 90% acid were explosive at room temperature. form explosive compounds due to reacts with silver.
Acid concentrations of 30% or less were inflamma-
ble but were judged to be safe to use as long as Picric acid ((NO2)3C6H2OH), or 2,4,6-trinitrophenol,
the operating temperature does not exceed 20°C. comes as yellow crystals that are wet with 10 to
35% water. When picric acid is dry, it is a dangerous
Acetic acid (CH3COOH) is a clear, colorless liquid explosive. It is toxic and stains the skin and is in-
with a pungent odor. It is a weak acid that reacts with compatible with all oxidizable substances. Picrates,
strong oxidizers, bases and metals. It is flammable which are metal salts of picric acid, are explosive.
and is not easily ignited, although when heated, it When picrates are dry, they can detonate readily,
releases vapors that can be ignited and can travel possibly spontaneously. Purchase in small quanti-
some distance to an ignition source. Contact with ties, keep it moist, and store it in a safe, cool place.
the skin results in serious burns. Inhalation of the If it starts to dry out, add a small amount of water
fumes irritates the mucous membranes. Anderson to keep it moist. The maximum solubilities of picric
states that acetic acid is a good solvent for nitric acid in water and in ethanol are about 1.3 and 8g
acid and that a 50% solution can be prepared, per 100mℓ, respectively. Picral can be stored safely.
but not stored, without danger [27]. Sax, however, During use, the solution should not be allowed to
states that mixtures of nitric and acetic acids are dry out. The etching residue should be discarded
dangerous [32]. at the end of the day to avoid potential explosions.

Acetic anhydride ((CH3CO)2O), or acetic oxide, is

Bases
a colorless liquid with a very strong acetic odor.
It can cause irritation and severe burns to the skin Bases, such as ammonium hydroxide (NH4OH),
and eyes. Acetic anhydride decomposes on heating potassium hydroxide (KOH), and sodium
producing toxic fumes. It reacts violently with boiling hydroxide (NaOH), are commonly used in metallo-
water, steam, strong oxidants (specifically sulfuric graphy, chiefly in etchants.
acid), alcohols, amines, strong bases, and others.
Ammonium hydroxide is a colorless liquid with a
It attacks metals, and is very corrosive, especially
strong, obnoxious odor. Solutions are extremely
in presence of water or moisture. It is extremely
corrosive and irritating to the skin, eyes, and mucous
flammable and should be avoided. The electrolytic
membranes. It reacts exothermically with sulfuric
polishing mixtures of acetic anhydride and per-
acid and other strong mineral acids, producing
chloric acid (4-to-1 to 2-to-1 mixtures) developed
boiling solutions.
by Jacquet, as mentioned above, are exceptionally
dangerous and should never be used. Dawkins [33]
Sodium and potassium hydroxides are strong bas-
reported an accident involving a mixture of chro-
es, available as white deliquescent pellets that are
mium trioxide and acetic anhydride that had been
soluble in water. They can rapidly absorb carbon
used for electropolishing (Table 24.2).
dioxide and water from the air. Solutions stored in
flasks with ground glass stoppers may leak air and
Citric acid (C3H4(OH)(COOH)3·H2O) comes as col-
freeze the stoppers, making re-opening difficult.
orless, odorless crystals that are water-soluble. It
Dissolving NaOH or KOH in water will generate

118
FULL LAB & SOLUTIONS
considerable heat. Do not dissolve either in hot explosion can result.
water. Never pour water onto these hydroxides;
always add the pellets slowly to the water. Alkali Potassium dichromate (K2Cr2O7), a bright orange
metal hydroxides react violently with acid, and are crystalline powder, is another powerful oxidant that
corrosive in moist air to metals like zinc, aluminum, is used in etchants. Contact can cause ulceration of
tin and lead forming flammable/explosive hydro- the hands, severe damage to nasal tissue, or asthma
gen gas. They are very corrosive to skin, eyes and and allergies with long-term exposure.
respiratory tract. Long-term exposure may lead to
dermatitis. Potassium hydroxide is somewhat more Cyanide compounds are occasionally used in
corrosive than sodium hydroxide. metallographic applications. Potassium cyanide
(KCN) and sodium cyanide (NaCN) are extremely
dangerous and highly toxic. Exposure by eye or
Other Chemicals skin contact, or by ingestion, is fatal. NaCN and
Hydrogen peroxide (H2O2) is available as a liquid in KCN vapors are intensely poisonous. They are par-
concentrations of either 3 or 30%. The 3% solution ticularly hazardous when brought in contact with
is reasonably safe to use, while the 30% solution is acids or acid fumes because of liberation of hydro-
a very powerful oxidant whose effect on the skin is gen cyanide, which is extremely toxic and highly
about as harmful as that produced by contact with flammable. Potassium ferricyanide (K3Fe(CN)6), a
sulfuric acid. Hydrogen peroxide by itself is not ruby-red crystalline powder and an ingredient in
combustible, but if brought in contact with combus- Murakami-type reagents, is poisonous but stable
tible materials, it can produce violent combustion. and reasonably safe to use.
Hydrogen peroxide is very damaging to the eyes.
Because release of oxygen can cause high pressures A number of nitrates, such as ferric nitrate
to develop within the container, the container caps [Fe(NO 3) 3·6H 2O], lead nitrate [Pb(NO 3) 6], and
are vented. silver nitrate (AgNO3), are employed by metallo-
graphers. Since they are powerful oxidizers, they
Bromine (Br2), a fuming reddish brown liquid with pose a dangerous fire hazard, especially when in
a pungent, suffocating odor, is commonly used in contact with organic materials. They may evolve
deep-etching solutions. It is very corrosive, reacting toxic fumes, such as oxides of nitrogen and lead,
violently with easily oxidized substances, including and are poisonous and corrosive to the eyes, skin
some metals. Bromine is a dangerous liquid that and respiratory tract.
should only be handled by well-qualified personnel.
Its vapors are extremely irritating to the eyes, skin,
and mucous membranes. Skin contact produces Summary
deep, penetrating burns that are slow to heal. Con- In general, the metallographic laboratory is a rea-
tact with organic matter can cause fires. sonably safe environment. However, depending on
the materials being prepared, dangerous situations
Chromic acid (H2CrO4) is formed when chromium can arise. Some hazards, such as the preparation of
trioxide (CrO3) is dissolved in water. CrO3 is used in radioactive or reactive metals, are quite obvious,
electropolishing solutions (see previous comment while others are not. In the preceding discussion,
and Table 49 about explosive nature of mixtures some of the potential hazards that can be encoun-
with acetic anhydride). Dilute aqueous solutions tered are summarized; others undoubtedly exist
are widely used for attack polishing. It is a powerful that are not covered.
oxidant; always wear gloves when using it for at-
tack polishing or use automatic devices and avoid Most accidents can be prevented by simple com-
contact potential. Chronic or long-term inhalation mon sense rules. It is best to assume that all metal
exposure may produce asthma-like reactions. dust and all chemicals are hazardous. Inhalation of
dust and fumes, ingestion, or bodily contact should
Potassium permanganate (KMnO4), a black crystal- be avoided. Personal protective equipment is very
line powder, is a powerful oxidant used in etchants. useful, but it should not be used as a substitute
It is a dangerous fire and explosion hazard, especial- for good laboratory procedures. The use of such
ly when in contact with organic materials. Ingestion equipment does not guarantee freedom from injury.
produces serious damage. KMnO4 and sulfuric acid
should never be mixed together because a violent

119
LABORATORY SAFETY
The metallographic literature contains many ref-
erences to the use of dangerous materials, often HELPFUL HINTS FOR
without any mention of the dangers involved or safe LABORATORY SAFETY
handling procedures. This is unfortunate because Purchase relatively small quantities of chem-
the unwary may be injured. Many of us are tempted icals that are used routinely, especially those
to experiment when a recommended procedure that have a short shelf life, or are dangerous.
does not work as claimed. The development of
electrolytes, chemical polishing agents, or etchants After pouring acids, carefully replace the cap,
should be left to those who are fully versed in the wash the exterior of the bottle under running
potential dangers. Metallographic laboratories water, and dry off the surface with a paper
should have some of the referenced safety publi- towel before replacing the acid bottle in its
cations (see bibliography) readily available in the fireproof cabinet.
laboratory and these safety publications should be
Schedule regular time periods for labora-
consulted when working with new or infrequently
tory clean-ups. These should be weekly for
used materials.
high volume laboratories. A clean lab is an
essential ingredient in all laboratory safety
programs.

120
FULL LAB & SOLUTIONS
SUMMARY
Preparation of metallographic specimens is based
upon scientific principles that are easily understood.
Sectioning creates damage that must be removed
by the grinding and polishing steps if the true
structure is to be examined. Each sectioning process
exhibits a certain amount of damage, thermal and/
or mechanical. Consequently, choose a procedure
that produces the least possible damage and use
the correct wheel or blade. Grinding also causes
damage, with the depth of damage decreasing
as the abrasive size decreases. Materials respond
differently to the same size abrasive, so one cannot
generalize on removal depths. Removal rates also
decrease as the abrasive size decreases. Through an
understanding of these factors, good, reproducible
preparation procedures, such as presented in this
guide, can be established for the materials being
prepared. Automation in specimen preparation
offers much more than reduced labor. Specimens
properly prepared using automated devices consis-
tently exhibit much better flatness, edge retention,
relief control and freedom from artifacts such as
scratches, pull out, smearing and comet tailing, than
specimens prepared manually.

121
GLOSSARY OF TERMS
Abrasive Cutting – the process of removing a Central Force – an approach for applying down-
sample from a part or component using an abra- ward pressure to an entire specimen holder with
sive wheel and cutter, typically performed wet; the specimens evenly against the preparation sur-
also referred to as abrasive sectioning face

Acrylic – a compression mounting compound Chop Cut – cut style where wheel is pulled down-
that produces a clear mount; a two part castable ward through the work piece; can be pulsed to as-
mounting system with fast cure times sist in revealing fresh abrasive

Agglomeration – a mass or cluster of particles, Clamp Mounting – the clamping of several

particularly in a powder or suspension; when used specimens in sandwich form typically used with
in polishing, an agglomerated material will act thin sheets
more aggressive then a deagglomerated material
of the same micron size Clarification – image enhancement largely
achieved through the use of grey scale filters
Analysis – the process of examining, interpreting,
documenting and measuring a material for struc- Cloth – a fabric surface to which a polishing sus-
tural or processing details pension or paste is added when used in materials
preparation, typically with a backings of pressure
Anvil – a test fixture that helps ensure accurate sensitive adhesive, magnetic or high friction mate-
results by supporting the test piece during the ap- rials for easily application
plication of the major load during a hardness test
Comet Tail – dull, broad depressed lines ema-
Artifact – a substance or structure not naturally nating from a hard particle or from a hole in a spec-
present imen in a pattern that resembles the tail of a comet

Aspect Ratio – ratio of the width to height in a Compression Mounting – the process of
camera mounting samples using heat and pressure to en-
capsulate the specimen
Automated Imaging – detection of the features
of interest based on grey level or color differences Condenser – an adjustable lens free of spherical
or morphological characteristics aberration and coma placed in front of the light
source to focus light at the desired point in the op-
Automated Preparation - the use of a grind- tical path
er-polisher with both a base and a power head
to prepare a specimen or group of specimens for Deagglomerated – process in which loose-
analysis ly adhered clumps of particles are broken apart,
particularly in a powder or suspension containing
Blade – a metal or resin bonded cutting tool con- abrasive; when used in polishing, a deagglomer-
taining abrasive, particularly related to a precision ated material will act less aggressive than an ag-
saw or precision sectioning glomerated material of the same micron size

Bright Field – the surface of the specimen is Dark Field – provides contrast completely re-
normal to the optical axis of the microscope and versed from that obtained with bright-field illu-
a white light is used; grain boundaries, phase mination, highlighting angled surfaces allowing
boundaries and other features not perpendicular more positive identification of details such as pits,
will appear dark in the image cracks or etched grain boundaries

Calibration – as related to microscopy or imag- Deformation – microstructure that has been al-
ing, the assignment of a known distance to a pixel tered due to cutting or grinding-polishing
count; calibration should be applied to each ob-
jective in the x & y direction Depth of Field – the distance along the optical
axis over which image details are observed with
Castable Mounting – the process of mounting acceptable clarity
samples that are sensitive to high pressures and/
or temperatures, contain high levels or porosity, or Diallyl Phthalate – a thermoset resin compres-
have high levels of corrosion; typically a two part sion mounting compound that provides good
liquid or liquid and powder system edge retention

122
FULL LAB & SOLUTIONS
Differential Interference Contrast (DIC) –
crossed polarized light used along with a double Hardness testing – the fifth primary segment of
quartz prism placed between the objective and materials preparation and analysis used to deter-
the vertical illuminator mine a material's resistance to permanent inden-
tation; an empirical test, not a material property,
Disc – in reference to sample preparation, a grind- determined by the particular test method and pa-
ing surface like silicon carbide paper or diamond rameters used
grinding discs used on a platen
Image Analysis – the fourth primary segment of
Dwell Time – the amount of time a load is ap- materials preparation and analysis used to detect
plied to a work piece during a hardness test the features of interested based on gray level or
color differences as well as morphological charac-
Edge Rounding – when the edge or edges of teristics such as size and shape
a specimen are abraded at a faster rate than the
interior, leading to a change in flatness at the edge Image Capture – the acquisition of an image by
such that the edge cannot be brought into focus means of a camera and frame grabber or digital
along with the interior camera

Electrolytic Anodizing – the electrolytic pro- Immersion – as it applies to materials prepara-

cess of growing an oxide layer on the surface of tion and analysis, placing a specimen completely
the specimen; differs from electrolytic polishing into an etch
and etching in that the specimen is set as the an-
ode within the electrical circuit Indentation – the deformation mark left by a
hardness test
Electrolytic Etching – achieved through the
completion of an electrical circuit through an elec- Indenter – the tool that contacts the specimen
trolyte; also applies to electrolytic polishing during a hardness test; indenter sizes and shapes
vary depending on the scale and test type used
Embedding – hard abrasive particles that be-
come fixed in the surface of a softer specimen Individual Force – an approach for applying
downward pressure to an individual specimen
Epoxy – two part liquid systems that physically against the preparation surface; also known as sin-
adhere to specimens; typically low viscosity, low gle force
shrinkage and can
Interactive Measurements – measurements in
Etching – a process used to reveal particular image analysis that require the operator to select
structural characteristics of metal that are not ev- the start and end points for the measurement
ident in the as polished condition
Knoop Test – a hardness test that uses a rhombo-
Eyepiece – magnifies the primary image pro- hedral-shaped diamond indenter with the 7.114
duced by the objective, otherwise known as ocular ratio of long diagonal to short diagonal, keeping
elastic recovery to a minimum; only the long diam-
Filter – used to modify the light for ease of obser- eter is measured in this test
vation, for improved photo-microscopy, or to alter
contrast
Lapping – an abrasive action in which the parti-
cles roll freely on the grinding or polishing surface;
Grinding – the process of removing deformation in standard materials preparation, this action exists
induced by sectioning from a specimen; part of
briefly until the abrasive embeds in the disc
the third step in material preparation

Grinding & Polishing – the third primary seg- Linear Measurement – simple point to point
ment of materials preparation and analysis during measuremnts used for making the occasional
which the true microstructure or characteristics of measurment
a material are revealed
MACC – minimal area of contact cutting, a tech-
Grinding Media – the abrasive systems used in nique that keeps the contact area between an
grinding; typically these are silicon carbide paper abrasive wheel and a sample constant and low,
or discs, diamond grinding discs, or other medi- allowing for lower wheel wear, less induced de-
as like alumina or zirconia bonded to discs, strips, formation and the sectioning of larger parts; also
belts or cloths; can also include rigid grinding reffered to as MAC (minimal area of contact)
discs with added abrasives

123
GLOSSARY OF TERMS
Macroindentation – a test performed using Objective – the objective lens forms the primary
1-100kg force image of the microstructure

Manual Preparation – in materials preparation Orbital Cutting – combines the best

the process of preparing a specimen without an features of chop, oscillation and traverse-and-in-
automated power head; also referred to as hand crement cutters, while minimizing cutting time
polishing or hand preparation
Paste – a type of polishing compound made
Materials Analysis – the examination, inter- from finely ground or powdered diamond parti-
preation, documentation and measurment of a cles, usually water based
specimen to gather detailed information on the
material's characteristics such as case depth, coat-
ing thickness, grain size, hardness, phase percent-
Phenolic – a thermoset resin compression
mounting compound that provides good edge
age porosity
retention and moderate shrinkage
Materials Preparation – a multi step process in-
cluding sectioning, mounting, grinding-polishing,
Planar Grinding – the intial grinding step that
established a common plane for all specimens
image anaysis and hardness testing to reveal the
in the holder; applies primarily to central force
true mictrostructure or characteristics of a materi-
holders
al; also referred to as met prep, metallographic
preparation or metallography
Platen – the work surface to which grinding discs
and polishing cloths are applied; occassionally
Metallographer – a person involved in the study
referred to as a wheel
of metals or materials

Metallographic Preparation – see materials Precision Sectioning – the process of remov-

ing a sample from a part or component using
preparation
an blade and saw, typically performed wet; also
referred to as precision cutting
Metallography – the study of metals and alloys;
can also be referred to as material science which
broadens the study to include metals and alloys,
Preparation Procedure – the multi step pro-
cess followed during grinding-polishing
ceramics, polymers, composites, biomaterials,
electronics, etc.
Polarized Light – light obtained by placing a
polarizing filter in front of the condenser lens of
Method – typically the parameters of grind-
the microscope and placing an anaylzer before
ing-polishing, including grinding surface, abrasive
the eyepice; when used with an anisotropic metal
suspensions or pastes, polishing cloths, platen
with the analyzer set to 90degrees to the polaizer,
speed, power head direction, force, time, etc
the grain structure will be visible
Microindentation – a test performed using 10-
1000g force
Polishing – the process of removing the final
layers of deformation induced by grinding from
a specimen; part of the third step in material
Microstructure – the structure of a material as preparation
viewed in a microscope
Polishing Abrasives – the fine abrasives, typi-
Mounting – the second primary segment in cally diamond, alumina or colloidal silica, used in
materials preparation and analysis during which suspensions for the polishing portion of materials
the sample is encapsulated in a compression or preparation
castable mounting compound or system
Porosity – the ratio of the volume of the pores
Napless – a polishing cloth, woven or chemotex- or voids of a material, to the total volume of the
tile, with no nap mass

Napped – a polishing cloth, typically flocked,

with nap of various length PSA – Pressure Sensitive Adhesive used as a
Nonwoven – a polishing cloth consisting of backing on abrasive discs and polishing cloths
chemotextile material
Pull Out – removal of second phase particles
Numerical Aperature (NA) – a meaure of the during preparation; pull out may be enhanced if
light-collecting ability of the lens the interface between the particle and matrix is
weak or if the particle is particularly brittle

124
FULL LAB & SOLUTIONS
Pulse Cutting – a chop cut style where wheel is Specimen Preparation – a multi step process
pulsed as it is pulled downward through the work including sectioning, mounting, grinding-pol-
piece assisting in revealing fresh abrasive ishing, image analysis and hardness testing to
reveal the true microstructure or characteristics of
Relief – an excessive height difference between a material; also referred to as met prep, metallo-
second-phase particles and the matrix due to graphic preparation or metallography
differences in grinding-polishing rates
Stain – a residue left on the surface of a speci-
Resolution – the imaging system's ability to re- men, that may form around second-phase parti-
produce object detail by resolving closely space cles due to interactions between the specimen
features; applies to both the microscope and the and the abrasives and/or lubricants,or may form
pixel array of the camera on the matrix due to inadequate cleaning or
drying or may from due to interactions between
Sample – a material or section of a material the specimens and solvents after preparation or
used for testing; typically referred to as a sample etching
before and during testing, but as a specimen from
the mounting step on Swabbing – as it applies to materials prepara-
tion and analysis, applying an etch to a specimen
Saw Cut – cutting action where the sample is fed using a cotton ball soaked in etch solution
into the wheel, the wheel contact arc is precisely
controlled via depth increment and cutting takes Thresholding – the method for representing
part along both the forward stroke ranges of pixel grey or color values with different
color bitplane overlays
Scratches – a linear cut along the surface of a
specimen due to contact with a correctly oriented Traverse and Increment – cutting action
abrasive particle; a groove caused by the abra- where the sample is fed into the wheel, the wheel
sion process contact arc is precisely controlled via depth
increment and cutting takes part along both the
Sectioning – the process of removing a sample forwards and backwards stroke
from a part or component using an abrasive
wheel and cutter, typically performed wet; also Vibratory Polishing – a polishing process in
referred to as abrasive cutting/sectioning or preci- which the polisher generates a high frequency,
sion sectioning variable amplitude vibrational motion producing
a stress-free polish
Single Force – an approach for applying down-
ward pressure to an individual specimen against Wheel – an abrasive wheel used for cutting; can
the preparation surface; also known as individual also be used in reference to a platen
force
Woven – a fabric formed by interlaced threads
SmartCool – a built in feedback loop in an or fibers
automatic compression mounting system that
intelligently ends the cooling step and completes
the mounting process when a safe handling tem-
perature has been reached

SmartCut – a built in feedback loop in an auto-

matic cutters and saws that prevents overheating
specimens, equipment damage and improves
cut quality by monitoring load at the motor and
adjusting feedrate to safe zones

Smear – matrix flow over voids, cracks or second

phase particles that makes detection of these
features and measurement of their extent difficult
or impossible

Specimen – a mounted sample; typically re-

ferred to as a specimen from the mounting step
on

125
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March 2000, pp. 85-90. 22. H. E. Bühler and H. P. Hougardy, Atlas of
Interference Layer Metallography, Deutsche
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OH, 1979, pp. 99-100. Germany, 1980.
8. J. Benedict, R. Anderson and S. J. Klepeis, 23. H. E. Bühler and I. Aydin, “Applications of the
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Specimen Preparation for Transmission Elec- 1986, pp. 41-51.
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Research Society, Pittsburgh, PA, 1992, Vol. 24. G. F. Vander Voort, “Results of an ASTM E-4
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Measurements of Microindentation Hardness
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OH, 1999. Philadelphia, 1989, pp. 3-39.
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No. 2, September 1995, pp. 135-137. Materials & Processes, Vol. 154, No. 3, Sep-
12. A. Skidmore and L. Dillinger, “Etching tember 1998, pp. 21-25.
Techniques for Quantimet Evaluation,” Micro- 27. R. L. Anderson, “Safety in Metallographic Lab-
structures, Vol. 2, Aug./Sept. 1971, pp. 23-24. oratory,” Westinghouse Research Laboratory
13. G. F. Vander Voort, “Etching Techniques for Science Paper, No. 65 – 1P30 – METLL – P2,
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135-154. and Practice, ASM International, Materials
14. G. F. Vander Voort, “Phase Identification by Park, OH., 1999, pp. 148-159.
Selective Etching,” Applied Metallography, 29. R. C. Nester and G. F. Vander Voort, “Safety in
Van Nostrand Reinhold Co., NY, 1986, pp. the Metallographic Laboratory,” Standardiza-
1-19. tion News, Vol. 20, May 1992, pp. 34-39.
15. E. E. Stansbury, “Potentiostatic Etching,” Ap- 30. P. A. Jacquet, “The Safe Use of Perchlo-
plied Metallography, Van Nostrand Reinhold ric-Acetic Electropolishing Baths,” Met. Finish,
Co., NY, 1986, pp. 21-39. Vol. 47, 1949, pp. 62-69.
16. E. Beraha and B. Shpigler, Color 31. S. M. Comas, R. Gonzalez Palacin and D.
Metallography, American Society for Metals, Vassallo, “Hazards Associated with Perchloric
Metals Park, OH, 1977. Acid-Butylcellosolve Polishing Solutions,”
17. G. F. Vander Voort, “Tint Etching,” Metal Metallography, Vol. 7, 1974, pp. 47-57.
Progress, Vol. 127, March 1985, pp. 31-33, 32. N. I. Sax, Dangerous Properties of Industrial
36-38, 41. Materials, 5th ed., Van Nostrand Reinhold Co.,
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126
FULL LAB & SOLUTIONS
33. A.E. Dawkins, “Chromic Acid-Acetic Anhy- 46. Vander Voort, G.F. and Lucas, G.M. [1998]
dride ‘Explosion,’” J. Iron and Steel Institute, “Microindentation Hardness Testing,” Ad-
Vol. 182, 1956, p. 388. vanced Materials & Processes, Vol. 154, No. 3,
pp. 21-25
34. F. Mohs, "Mohs Hardness" [1822] Grundriß
der Mineralogie (two volumes, 1822 and 47. R.W. Johnson, Wear, Vol 16, 1970 p.351-358
1824): Dresden, Arnoldschen Buchhandlung
Selected Bibliography of Books on Laboratory
(translated to English by Wilhelm Ritter von
Haidinger as Treatise on Mineralogy in 1825 Safety
and published by Constable & Co. Ltd. of
ASTM E-2014, “Standard Guide on Metallograph-
Edinburgh).
ic Laboratory Safety”.
35. Wahlberg, A., “Brinells Method of Determin- N. Van Houten, Laboratory Safety Standards for
ing Hardness and Other Properties of Iron Industry, Research, Academe, Sci. Tech. Pubs.,
and Steel” [1901] J. Iron Steel Inst., Vol 59 No. Lake Isabella, CA. 1990.
I pp243-298 and Vol 60 No. II pp234-271.
E. Gershey, A. Wilkerson and E. Party,
36. Kehl, G.L. [1949], “The Principles of Me- Laboratory Safety in Practice, Van Nostrand
tallographic Laboratory Practice”, 3rd Ed., Reinhold, N.Y., 1991.
McGraw-Hill Book Co., 1949, p 229 A. A. Fuscaldo et al. (eds), Laboratory Safety:
Theory & Practice, Academic Press, San Diego,
37. Grundriß der Mineralogie (two volumes, CA. 1980.
1822 and 1824): Dresden, Arnoldschen Bu-
chhandlung (translated to English by Wilhelm S. B. Pal (ed.), Handbook of Laboratory Health &
Ritter von Haidinger as Treatise on Mineralo- Safety Measures, Kluwer Academic, Norwell, MA.,
gy in 1825 and published by Constable & Co. 1985.
Ltd. of Edinburgh). Norman V. Steere (ed.), Handbook of Laboratory
Safety, 2nd ed., CRC Press, Boca Raton, FL., 1971.
38. Wahlberg, A., “Brinells Method of Determin-
ing Hardness and Other Properties of Iron A. Keith Furr (ed.), Handbook of Laboratory Safety,
and Steel” [1901] J. Iron Steel Inst., Vol 59 No. 3rd ed., CRC Press, Boca Raton, FL., 1989.
I pp243-298 and Vol 60 No. II pp234-271 L. J. Diberardinis et al., Guidelines for Laboratory
Design: Health & Safety Considerations, J. Wiley
39. Kehl, G.L. [1949], “The Principles of Me- & Sons, N.Y., 1987.
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McGraw-Hill Book Co., 1949, p 229 S. R. Rayburn, The Foundations of Laboratory
Safety, Brock-Springer Series in Contemporary
40. O’Neil, B [2010] “Gage Repeatability and Re- Bioscience, Springer-Verlag, N.Y., 1989.
producibility in Rockwell Hardness Testing”, C. A. Kelsey and A. F. Gardner (eds.), Radiation
Advanced Materials and Processes, Nov-Dec Safety for Laboratory Technicians, Warren H.
pp33-35 Green, Inc.,
St. Louis, MO., 1983.
41. International System of Units (Le Système
International d'Unités) N. I. Sax, Dangerous Properties of Industrial
Materials, 5th ed., Van Nostrand Reinhold Co., N.Y.,
42. Vander Voort, G. F. [1999] “Metallography: 1979.
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Prudent Practices for Handling Hazardous Chem-
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43. Vander Voort, G.F. [1989] “Results of an ASTM Washington, D.C., 1981.
E-4 Round-Robin on the Precision and Bias of Prudent Practices for Disposal of Chemicals from
Measurements of Microindentation Hardness Laboratories, National Academy Press, Washing-
Impressions,” Factors that Affect the Precision ton, D.C., 1983.
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the Measurement of Microindentation Hard- F. A. Patty (ed.), Industrial Hygiene and Toxicology,
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Tests, and Laboratories, ASTM STP 1057, N.Y., 1980.
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American Society for Metals, Metals Park, OH ical Dictionary, 12th ed., Van Nostrand Reinhold,
New York, 1993.

127
APPENDIX
Table A1: Abrasive Cutting Troubleshooting Guide
Issue Possible Cause Suggested Remedy
Burning Increase coolant flow rate
(bluish discoloration) Reduce cutting pressure
Overheated specimen
Select a wheel with softer bonding (faster
breakdown)
Rapid wheel wear Select a wheel with harder bonding
Wheel bonding breaks down too rapidly
Reduce cutting pressure
Adjust coolant flow to be even on both sides of the
Uneven coolant distribution
wheel

Frequent wheel breakage Loose specimen fixturing Clamp the specimen more securely
Abrupt contact with specimen Start cut contact carefully

Wheel was previously cracked at start up Handle carefully

• Select a wheel with softer boding

• Use a “pulse” cutting mode
Resistance to cutting Slow wheel bond breakdown
• Use cutter with oscillating motion or with Minimal
Area of Contact Cutting* (MACC) ability
• Use cutter with greater horsepower
Inadequate cutter capacity • Reduce pressure or feed rate
• Use with cutter oscillating motion or with MACC
Stalled wheels ability
Pinched blade due to movement of Tighten the vise on one side less than on the other
specimen side

Figure A1. Abrasive Cutting Troubleshooting Guide

Pointed: Chisel: Glazed Surface:

Wheel bond too hard Nonuniform coolant flow Wrong wheel

Normal: Normal: Normal:

For solid materials For structural or For light tubing or
medium wall tubing other thin wall section

128
FULL LAB & SOLUTIONS
Table A1: Abrasive Cutting Troubleshooting Guide
Thermosetting Resins (Epoxies, Diallyl Phthalates and Phenolics)
Defect Probable Cause Suggested Remedy
Radial splits or cracks Specimen cross sectional area too Use a larger mold size; decrease the
large; specimen with sharp corners specimen size; bevel sharp corners, if
possible

Shrinkage gaps Specimen surfaces dirty; specimen Clean and dry specimens carefully; after
cooled quickly after polymerization; polymerization, cool under pressure to near
wrong resin used ambient; use EpoMet G or EpoMet F

Circumferential cracks Resin contained moisture Keeps resins dry during storage; keep
containers closed when not using; dry resin
by baking at 100-120°F [38-49°C]

Bulging or soft mount Inadequate curing (polymerization) Increase polymerization time and pressure
time

Mount appears grainy and Time at temperature too short; Increase polymerization time, temperature
unfused temperature for polymerization too low; and pressure
molding pressure too low

Thermosetting Resins (Acrylics)

Cottonball Incomplete polymerization of resin; not Use less resin; use longer heating and
enough time at temperature cooling periods; use controlled linear
cooling

Crazing Relief of internal streses upon ejection Cool mount to a lower temperature before
of mount ejection; use controlled linear cooling

Figure A2. Comparison of Six Edge Retention Compression Mounting Compounds

PhenoCure phenolic resin EpoMet thermosetting epoxy resin ProbeMet Cu-filled conductive resin

KonductoMet C-filled conductive resin EpoxiCure cast epoxy resin with SamplKwick cast acrylic resin with
Conductive Filler particles Conductive Filler particles

Micrographs showing the as-forged surface of a hardened modified 5130 alloy steel part mounted using a variety of resins showing
different degrees of edge retention. The specimens were polished simultaneously in the same holder and were etched with 2% nital. The
magnification bars are 20 µm long. Best results were obtained with EpoMet, ProbeMet and EpoxiCure resin with the Conductive Filler
particles.

129
APPENDIX
Table A3: Castable Mounting Selection Guide
Acyrlic Description
• Translucent, general purpose acrylic system
• 5-8 minute cure time at room temperature
SamplKwick
• ~179°F [79°C] Peak Temperature
• ~85 Shore D Hardness
• Clear, general purpose acrylic system
- Requires pressure vessel for clear mounts
VariKleer • 5-15 minute cure time at room temperature
• ~212°F [100°C] Peak Temperature
• ~84 Shore D Hardness
• Semi transparent, low odor system
• Low shrinkage, high viscosity
VariDur 10 • 8 minute cure time
• ~212ºF Peak Temperature
• ~80 Shore D Hardness
• Dark blue, low odor system
• Low shrinkage, high viscosity
VariDur 200 • 8 minute cure time
• ~212ºF Peak Temperature
• ~85 Shore D Hardness
• Blue, mineral filled acrylic system
VariDur 3003 • Hardest castable mounting system
• 15-30 minute cure time at room temperature
• ~252°F [122°C] Peak Temperature
• ~90 Shore D Hardness
Epoxy Description
EpoxiCure 2 • Clear, general purpose epoxy system
• 6hr cure time at room temperature
• <104°F [40°C]Peak Temperature
• ~80 Shore D Hardness
EpoHeat CLR • Transparent clear epoxy system
• Long pot-life allows product to be mixed in large batches
• 1hr cure time in oven at 149ºF [65ºC]
• <324°F [65°C] Peak Temperature
• ~82 Shore D Hardness
EpoThin 2 • Clear, low viscosity epoxy system
• 9hr cure time at room temperature
• <149°F [65°C] Peak Temperature
• ~78 Shore D Hardness
EpoKwick FC • Clear, fast curing epoxy system with low shrinkage
• 2hr cure time at room temperature
• <250°F [121°C] Peak Temperature
• ~82 Shore D Hardness

Curing time is not a precise quantity as it can be influenced by the nature of the mold (how well, or how poorly, the exothermic heat of polymerization is
extracted), by the volume of the cast resin used, by the volume and nature of the specimen being encapsulated, by the temperature of the mix, by room
temperature and air circulation and by the age of the resin and hardener (i.e., curing time is longer for products beyond their normal shelf life). The
values listed are typical for metallic specimens cast in 1.25-inch (30-mm) diameter Sampl-Kup molds at 21 °C (70 °F) using fresh resin and hardener.

130
FULL LAB & SOLUTIONS
Table A4: Final Polishing Abrasives Selection Guide
Name Characteristics Applications
MicroPolish Alumina Powder 1, 0.3 and 0.05µm alumina powder and Inexpensive general purpose abrasive for
and Suspensions suspensions polishing most minerals and metals
MicroPolish II 1 and 0.3 deagglomerated alumina Higher quality alumina suitable for polishing
Deagglomerated Alumina powders suspensions most minerals and metals; produces a better
Powder and Suspensions surface finish than alumina abrasives of the same
size
MasterPrep Deagglomerated 0.05µm sol-gel alumina suspension Unique seeded gel alumina produces better
Seeded Gel Alumina finishes than calcined alumina abrasives;
Suspension excellent with minerals, metals, carbides, PCBs.
Good for precious metals
MasterMet Colloidal Silica 0.06µm amorphous silicia colloidal Chemo-mechanical action produces excellent
Suspension suspension with a pH of ~10 producing a surfaces for metals, minerals, polymers, PCBs,
chemo-mechanical polishing electronic devices, etc., especially soft metals but
not for precious metals
MasterMet 2 Non- 0.02µm non-crystallizing amorphous Non-crystallizing version of colloidal silica
Crystallizing Colloidal Silica colloidal silica suspension with a pH of yields similar results as MasterMet but without
Suspension ~10.5 producing chemo-mechanical the danger of crystallized silica particle
polishing action contamination
MasterPolish Blended Proprietary viscuous blend of high purity Proprietary blend has little water and can be used
Alumina and Colloidal Silica 0.05µm alumina and colloidal silica with with minerals that are sensitive to warer, such as
Suspension a slightly basic pH (can be diluted with Mg and most of its alloys; good for most Fe, Ni,
water) or Co based alloys and Metal Matrix Composites
(MMC)
MasterPolish 2 Proprietary Proprietary 0.06µm abrasive suspension Proprietary blend designed for final polishing
Chemo-Mechanical with a pH of ~10 for chemo-mechanical of ceramic materials, nitrides, carbides and
Suspension polishing action composites

Table A5: Electrolytic Polishing & Etching Troubleshooting Chart

Problem Probable Cause Correction
Increase voltage
Center of the specimen is
No polishing film at the center of specimen Decrease agitation
deeply etched
Use more viscous electrolyte
Increase voltage
Pitting or etching at the
Too vicsous or thick film Decrease agitation
edges of specimen
Use more viscous electrolyte
Try a new electrolyte
Studge on the surface Insoluble anode product Increase temperature
Increase voltage
Increase voltage
Rough or matte surface Insufficient or no polishing film
Use more viscous electrolyte
Insufficient time Increase or decrease agitation
Waviness or streaks on the Incorrect agitation Better pre-preparation
polished surface Inadequate pre-preparation Increase voltage
Too much time Decrease time
Stains on the polished Attach after polising
Try less corrosive electrolyte
surface Current is off
Increase agitation
Unpolished spots
Gas bubbles Decrease voltage
(Bulls-eyes)
Tilt the specimen
Increase voltage
Phases in the relief Insufficient polishing time Better pre-preparation
Decrease time
Better pre-preparation
Too long polishing Decrease voltage
Pitting
Too high voltage Decrease time
Try a different electrolyte

131
APPENDIX
Figure A3. A Guide to Equivalent Loads for Different Mount Sizes

14

12

10
Force (psi)

1in
4 1.25in
1.5in
2in
25mm
2 30mm
40mm
50mm
0

0 5 10 15 20 25

Load (lb)

100

90

80

70
Force (Mpa)

60

50

40
1in
30 1.25in
1.5in
2in
20
25mm
30mm
10 40mm
50mm
0

0 10 20 30 40 50 60 70 80 90 100 110 120

Load (N)

The two graphs plot the load applied per specimen, and the resulting pressure, as a function of mold diameter for both Imperial and metric
units. An example of the use of the graphs is shown. Assume that we have a practice developed using 1.25in diameter mounts that calls
for 5 lbs. load per specimen. We want to use this method with mounts that are 1in in diameter. How much load should we use? Draw a
line vertically at 5 lbs. (shown in green) until it intersects the line for a 1.25in diameter mount. Then draw a horizontal line (shown in blue)
from the intersection point to the line for 1in diameter mounts. Then, draw a vertical line (shown in blue) down to the load axis. This point is
about 3 lbs. So, we would use 3 lbs per specimen for 1in mounts. In similar manner, if we want to use 1.5in diameter specimens, the graph
would suggest that we use about 7 lbs. per specimen (red lines).

132
FULL LAB & SOLUTIONS
Table A5: Preparation Troubleshooting Guide
Defect Probable Cause Suggested Remedy
Comet Tails Poorly bonded very hard phase in softer Use hard, napless cloths; reduce applied pressure;
matrix, or pores in matrix results in reduce step times; impregnate pores with epoxy
unidirectional grooves emanating from or wax; use complementary rotation. In manual
particles of hole. preparation, avoid unidirectional grinding.
Edge Rounding Shrinkage gaps between specimen and Avoid gaps by cooling thermosetting mount under
mount are main problem and, when pressure after polymerization. Use EpoMet resin
present, avoid napped cloths and long (least prone to shrinkage gaps); of castable resins,
polishing times. epoxy is best (adding Flat Edge Filler particles to
epoxy improves edge retention); use central force
rather than individual force; use Apex Hercules
rigid grinding discs; use napless cloths.
Embedding Hard abrasive tends to embed in soft Coat SiC abrasive paper with parafin wax
metals; finer particles are more likely to (candlewax is best, soaps are also effective);
embed then larger particles. beeswax is less effective; reduce applied pressure
rpm and times; avoid finer SiC abrasive papers;
avoid using diamond slurries with fine diamond
sizes (for ≤3µm diamond, paste embeds less than
slurries). SiC embedded in soft metals (e.g. Pb) can
be removed by polishing with alumina slurries
Pull Outs Excessive grinding time on worn SiC Grind no more than 60 seconds on a sheet of
paper; excessive polishing time on napped SiC paper; use napless cloths; reduce applied
cloths; excessive pressure; and inadequate pressure; use proper degree of lubrication.
lubrication lead to pull out of second-phase
particles.
Relief Use of napped cloths, long polishing times Use napless cloths, higher pressures and shorter
and low pressure create height differences times. If relief is observed using contra rotation in
between matrix and second-phase particles. last step, repeat the las step using complementary
rotation.
Scratches Contamination of grinding or polishing Maintain clean operating conditions, washing
surfaces by coarser abrasives; pull out of hands and equipment between steps; for cracked
hard particles from matrix or broken pieces or porous specimens, use ultrasonic cleaning after
of brittle materials; or inadequate grinding each step (especially polishing); execute each
or polishing times. step thoroughly (avoid short cutting methods);
when using the Apex magnetic disc system, store
the discs in a clean drawer or cabinet and scrub
surfaces if contamination is believed to have
occurred; and high pressures can leave a heavy
scratch pattern.
Smear Flow of softer metals may be caused by Use proper degree of lubrication, lower pressures
inadequate lubrication, excessive pressures and rpms; use a medium napped cloth on final
or rpms. step; lightly etch the specimen after final polishing
and repeat the last step; use the vibratory polisher
to remove smeared surface metal.
Stain Stains around second-phase particles Some staining issues are unique to the specimen
can be induced by interactions between but most result from using impure tap water
abrasive and particle, perhaps affected (switch to distilled water; sometimes de-ionized
by water quality; or they can occur due to water is needed) or inadequate drying. When
inadequate cleaning or improper solvents using colloidal silica, which can be hard to remove,
used after the abrasive step. direct the water jet onto the cloth and wash the
specimens (and cloth) for the last 6-10 seconds
of the polishing cycle. This makes subsequent
cleaning easy. Otherwise, scrub the surface with
water containing a detergent solution using
cotton. Then, rinse with alcohol and blow dry
with hot air. Compressed air systems can contain
impurities, such as oils, that can stain the surface.

133
ASTM METALLOGRAPHY STANDARDS
ASTM Metallography Standards Electron Microscope

A247: Visual Classification of Graphite in the E768: Preparing and Evaluating Specimens for
Microstructure of Cast Iron Automatic Inclusion Assessment of Steel

A892: Defining and Rating the Microstructure of E807: Metallographic Laboratory Evaluation
High Carbon Bearing Steels E883: Reflected-Light Photomicrography
B390: Evaluating Apparent Grain Size and E930: Estimating the Largest Grain Observed in a
Distribution of Cemented Tungsten Carbides Metallographic Section (ALA Grain Size)
B588: Measurement of the Thickness of Trans- E975: X-Ray Determination of Retained Austenite
parent or Opaque Coatings by Double-Beam in Steel with Near Random Crystallographic
Interference Microscope Technique Orientation
B657: Metallographic Determination of E986: Scanning Electron Microscope Beam Size
Microstructure in Cemented Tungsten Carbide Characterization
B681: Measurement of Thickness of Anodic E1077: Estimating the Depth of Decarburization
Coatings on Aluminum and of Other Transparent of Steel Specimens
Coatings on Opaque Surfaces Using the
E1122: Obtaining JK Inclusion Ratings Using
Light-Section Microscope
Automatic Image Analysis
B748: Measurement of the Thickness of
E1180: Preparing Sulfur Prints for Macrostructural
Metallic Coatings by Measurement of Cross
Examination
Section with a Scanning Electron Microscope
E1181: Characterizing Duplex Grain Sizes
B795: Determining the Percentage of Alloyed or
Unalloyed Iron Contamination Present in Powder E1245: Determining the Inclusion or Sec-
Forged Steel Parts ond-Phase Constituent Content of Metals by
Automatic Image Analysis
B796: Nonmetallic Inclusion Level of Powder
Forged Steel Parts E1268: Assessing the Degree of Banding or
Orientation of Microstructures
B847: Measurement of Metal and Oxide Coating
Thickness by Microscopical Examination of a E1351: Production and Evaluation of Field
Cross section Metallographic Replicas
C664: Thickness of Diffusion Coating E1382: Determining Average Grain Size Using
Semiautomatic and Automatic Image Analysis
E3: Preparation of Metallographic Specimens
E1508: Quantitative Analysis by Energy-Disper-
E7: Standard Terminology Relating to
sive Spectroscopy
Metallography
E1558: Electrolytic Polishing of Metallographic
E45 Determining the Inclusion Content
Specimens
of Steel
E1920: Metallographic Preparation of Thermal
E82: Determining the Orientation of a
Spray Coatings
Metal Crystal
E1951: Calibrating Reticles and Light Microscope
E112: Determining Average Grain Size
Magnifications
E340: Macroetching Metals and Alloys
E2014: Metallographic Laboratory Safety
E381: Macroetch Testing Steel Bars, Billets,
E2015: Preparation of Plastics and Polymeric
Blooms, and Forgings
Specimens for Microstructural Examination
E384: Microindentation Hardness of Materials
F1854: Stereological Evaluation of Porous Coat-
E407: Microetching Metals and Alloys ings on Medical Implants
E562: Determining Volume Fraction by Systemat-
ic Manual Point Count

E766: Calibrating the Magnification of a Scanning

134
FULL LAB & SOLUTIONS
ASTM/ISO STANDARDS
ASTM Metallography Standards Determination of Depth of Decarburization

B578: Microhardness of Electroplated Coatings ISO4499: Hardmetals: Metallographic

Determination of Microstructure
B721: Microhardness and Case Depth of Powder
Metallurgy Parts ISO4524-1: Metallic Coatings – Test Methods for
Electrodeposited Gold and Gold Alloy Coatings –
C730: Knoop Indentation Hardness of Glass
Part 1: Determination of Coating Thickness
C849: Knoop Indentation Hardness of Ceramic
ISO4964: Steel – Hardness Conversions
Whitewares
ISO4967: Steel – Determination of Content of
C1326: Knoop Indentation Hardness of Ad-
Non-Metallic Inclusions – Micrographic Method
vanced Ceramics
Using Standard Diagrams
C1327: Vickers Indentation Hardness of Ad-
ISO4968: Steel – Macrographic Examination by
vanced Ceramics
Sulphur Print (Baumann Method)
E10: Brinell Hardness of Metallic Materials
ISO4970: Steel – Determination of Total or Effec-
E18: Rockwell Hardness and Rockwell Superficial tive Thickness of Thin Surface-Hardened Layers
Hardness of Metallic Materials
ISO5949: Tool Steels and Bearing Steels –
E92: Vickers Hardness of Metallic Materials Micrographic Method for Assessing the
Distribution of Carbides Using Reference
E140: Standard Hardness Conversion Tables for
Photomicrographs
Metals
ISO9042: Steels – Manual Point Counting Method
E448: Scleroscope Hardness Testing of Metallic
for Statistically Estimating the Volume Fraction of
Materials
a Constituent with a Point Grid
E1842: Macro-Rockwell Hardness Testing of
ISO9220: Metallic Coatings – Measurement of
Metallic Materials
Coating Thickness – Scanning Electron Micro-
scope Method
ISO Metallography Standards
ISO14250: Steel – Metallographic Characteriza-
ISO643: Steels – Micrographic Determination of
tion of Duplex Grain Size and Distribution
the Ferritic or Austenitic Grain Size

ISO945: Cast Iron: Designation of Microstructure

of Graphite

ISO1083: Spheroidal Graphite Cast Iron –

Classification

ISO1463: Metallic and Oxide Coatings –

Measurement of Coating Thickness – Microscop-
ical Method

ISO2624: Copper and Copper Alloys – Estimation

of Average Grain Size

ISO2639: Steel – Determination and Verification

of the Effective Depth of Carburized and Hard-
ened Cases

ISO3754: Steel – Determination of Effective

Depth of Hardening After Flame or Induction
Hardening

ISO3763: Wrought Steels – Macroscopic Methods

for Assessing the Content of Non-Metallic
Inclusions

ISO3887: Steel, Non-Alloy and Low Alloy –

135
ISO/OTHER NATIONAL STANDARDS
ISO Hardness Standards Other National Standards
ISO1355: Metallic Materials – Hardness Test –
France
Calibration of Standardized Blocks to be Used for
Rockwell Superficial Hardness Testing Machines NFA04-10: Determination of the Ferritic and
(Scales 15N, 30N, 45N, 15T, 30T and 45T) Austenitic Grain Size of Steels

ISO4516: Metallic and Related Coatings – Vickers Germany

and Knoop Microhardness Tests
DIN50150: Testing of Steel and Cast Steel;
ISO4545: Metallic Materials – Hardness Test – Conversion Table for Vickers Hardness, Brinell
Knoop Test Hardness, Rockwell Hardness and Tensile
Strength
ISO4546: Metallic Materials – Hardness Test –
Verification of Knoop Hardness Testing Machines DIN50192: Determination of the Depth of
Decarburization
ISO4547: Metallic Materials – Hardness Test –
Calibration of Standardized Blocks to be Used for DIN50600: Testing of Metallic Materials;
Knoop Hardness Testing Machines Metallographic Micrographs; Picture Scales
and Formats
ISO6441-1: Paints and Varnishes – Determination
of Microindentation Harness – Part 1: Knoop DIN50601: Metallographic Examination;
Hardness by Measurement of Indentation Length Determination of the Ferritic or Austenitic
Grain Size
ISO6441-1: Paints and Varnishes – Determination
of Microindentation Harness – Part 2: Knoop DIN50602: Metallographic Examination;
Hardness by Measurement of Indentation Depth Microscopic Examination of Special Steels Using
Under Load Standard Diagrams to Assess the Content of
Non-Metallic Inclusions
ISO6507-1: Metallic Materials – Hardness Test –
Vickers Test – Part I: HV 5 to HV 100 SEP1510: Microscopic Test of Steels for Grain Size
by Comparison with Standard Charts
ISO6507-2: Metallic Materials – Hardness Test –
Vickers Test – Part 2: HV 0, 2 to Less Than HV 5 SEP1570: Microscopical Examination of Special
Steels for Non-Metallic Inclusions Using Standard
ISO6508: Metallic Materials – Hardness Test –
Micrograph Charts
Rockwell Test (Scales A, B, C, D, E, F, G, H, K)
SEP1572: Microscopic Testing of Free-Cutting
ISO9385: Glass and Glass-Ceramics – Knoop
Steels for Non-Metallic Sulphide Inclusions by
Hardness Test
Means of a Series of Pictures
ISO10250: Metallic Materials – Hardness Testing –
Tables of Knoop Hardness Values for Use in Tests
Made on Flat Surfaces Italy
UNI3137: Extraction and Preparation of Samples
ISO14271: Vickers Hardness Testing of Resistance
Spot, Projection and Seam Welds (low load and UNI3138: Macrographic Analysis
microhardness) UNI3245: Microscopic Examination of Ferrous
Materials - Determination of Austenitic or Ferritic
Grain Size of Plain Carbon and Low-Alloy Steels

UNI4227: Determination of Metallographic

Structures

UNI4389: Nonferrous Metals and Their Alloys:

Determination of the Dimension of Their Crystal
Grains

136
FULL LAB & SOLUTIONS
OTHER NATIONAL STANDARDS
Japan PN-75/H-04512: Nonferrous Metals. Reagents for
JISB7724: Brinell Hardness – Verification of Test- Revealing Microstructure.
ing Machine PN-75/H-04661: Gray, Spheroidal Graphite and
JISB7725: Vickers Hardness – Verification of Test- Malleable Cast Iron. Metallographic Examination.
ing Machines Evaluation of Microstructure

JISB7730: Rockwell Hardness Test – Calibration of PN-76/H-04660: Cast Steel and Iron. Microscopic
Standardized Blocks Examination. Sampling and Preparation of Test
Pieces.
JISB7734: Knoop Hardness Test – Verification of
Testing Machines PN-84/H-04507/01: Metals. Metallographic Test-
ing of Grain Size. Microscopic Methods for
JISB7735: Vickers Hardness Test – Calibration of Determination of Grain Size.
the Reference Blocks
PN-84/H-04507/02: Metals. Metallographic Test-
JISB7736: Brinell Hardness Test – Calibration of ing of Grain Size. Methods of Revealing the
Standardized Blocks Prior-Austenitic Grains in Non-Austenitic Steels.
JISG0551: Methods of Austenite Grain Size Test PN-84/H-04507/03: Metals. Metallographic
for Steel Testing of Grain Size. Macroscopic Method of
JISG0552: Method of Ferrite Grain Size Test Revealing the Prior-Austenitic Grain Size by the
for Steel Fracture Method.

JISG0553: Macrostructure Detecting Method for PN-84/H-04507/04: Metals. Metallographic

Steel, Edition 1 Testing of Grain Size. A Method of Testing for
Overheating of Steel.
JISH0501: Methods for Estimating Average Grain
Size of Wrought Copper and Copper Alloys PN-87/H-04514: Steel, Cast Steel, Cast Iron.
Macrostructure Examination. Baumann’s Test.
JISR1610: Testing Method for Vickers Hardness
of High Performance Ceramics
Russia
JISR1623: Test Method for Vickers Hardness of
Fine Ceramics at Elevated Temperatures GOST801: Standard for Ball and Roller Bearing
Steel
JISZ2243: Brinell Hardness Test – Test Method
GOST1778: Metallographic Methods of
JISZ2244: Vickers Hardness Test – Test Method Determination of Nonmetallic Inclusions
JISZ2245: Rockwell Hardness Test – Test Method GOST5639: Grain Size Determination
JISZ2251: Knoop Hardness Test – Test Method

JISZ2252: Test Methods for Vickers Hardness at Sweden

Elevated Temperatures SIS111101: Estimating the Average Grain Size of
Metals
Poland SIS111102: Estimating the Austenitic Grain Size of
PN-57/H-04501: Macroscopic Examination of Ferritic and Martensitic Steels
Steel. The Deep Etching Test. SIS111111: Methods for Assessing the Slag
PN-61/H-04502: Reagents for Macrostructure Inclusion Content in Steel: Microscopic Methods
Tests of Iron Alloys SIS111114: Determination of Slag Inclusions –
PN-61/H-04503: Reagents for Microstructure Microscopic Methods – Manual Representation
Tests of Iron Alloys SIS111116: Steel – Method for Estimation of the
PN-63/H-04504: Microstructure Testing of Steel Content of Non-Metallic Inclusions – Microscopic
Products. Iron Carbide. Ghost Structure. Methods – Jernkontoret’s Inclusion Chart II for the
Widmanstätten’s Structure. Assessment of Non-Metallic Inclusions

PN-66/H-04505: Microstructure of Steel Products.

Templates and Evaluation.

137
OTHER NATIONAL STANDARDS
Sweden (continued)
SIS110340: Hardness Test – Vickers Test HV 0, 2 to
HV 100 – Direct Verification of Testing Machines

SIS1103 41: Hardness Test – Vickers Test HV 0,2 to

HV 100 – Indirect Verification of Testing Machines
Using Standardized Blocks

SIS1103 42: Hardness Test – Vickers Test HV 0,2 to

HV 100 – Direct Verification of Standardizing
Machine for Calibration of Standardized Blocks

SIS110343: Hardness Test – Vickers Test HV 0,2 to

HV 100 – Calibration of Standardized Blocks

SIS112516: Metallic Materials – Hardness Test –

Vickers Test HV 5 to HV 100

SIS112517: Metallic Materials – Hardness Test –

Vickers Test HV 0,2 to Less Than HV 5

SIS117020: Determination of the Depth of

Decarburization in Steel

United Kingdom
BS860: Tables for Comparison of Hardness
Scales.

BS4490: Methods for Micrographic Determina-

tion of the Grain Size of Steel

BS5710: Macroscopic Assessment of the

Non-Metallic Inclusion Content of Wrought Steels

BS6285: Macroscopic Assessment of Steel by

Sulphur Print

BS6286: Measurement of Total or Effective

Thickness of Thin Surface-Hardened Layers in
Steel

BS6479: Determination and Verification of Effec-

tive Depth of Carburized and Hardened Cases in
Steel

BS6481: Determination of Effective Depth of

Hardening of Steel after Flame or Induction
Hardening

BS6533: Macroscopic Examination of Steel by

Etching with Strong Mineral Acids

BS6617: Determination of Decarburisation in

Steel

138
INDEX
A exotherm, 13
Abrasive cutters: Flat Edge Filler particles, 12,15
chop cutters, 6 recommendations, 12, 130
minimum area of contact cutting, 6-8 Central force, 15, 20, 27
orbital cutting, 8 Ceramics:
planar or saw cutting, 7 etchants, 83
pulse cutting mode, 6, 8 preparation, 57-58
Y-Feed cutting, 7 Chemical polish, 38, 39, 40, 41, 42, 49, 50, 52
Abrasive wheels: Clamp mounting, 10
bond strength, 6 Cobalt and alloys:
recommendations, 6 etchants, 81
thickness, 5 preparation, 49-50
troubleshooting guide, 128 Colloidal silica, 21, 23, 26, 28, 133
Abrasive sectioning, 5-8, 128 “Comet tails,” 18, 19,121, 133
Acids, 115-118 Composites:
Acrylic resins, 11-12, 129-130 preparation, 62-64
Alumina, 2, 5, 8, 16, 21-23, 131 Compression mounting, 14-15, 17-19, 53, 117
Aluminum and alloys: Contra rotation, 28, 133
etchants, 72, 75-76, 78 Coolant, 3,6
preparation, 32-33 Copper and alloys:
ASTM Standards, 134-135 etchants, 81, 83
Attack polishing: preparation, 47
Au, 52 Cutting damage, 5, 28
Be, 35
Co, 49
D
Cu, 47
Damage, sectioning, 5, 28
Hf, 39-40
Dark field illumination, 90-91
Ni, 48
Diamond, 16, 18, 21
Nb, V and Ta, 41
Differential interference contrast, 90-91
safety, 119
Digital imaging:
Ti, 38-39
acquisition, 93
Zr, 41-42
calibration, 95
cameras, 93, 94, 95, 100
B clarification, 96
Bases, 118-119 color, 94
Beryllium pixels, 94, 95, 96, 98, 99, 100
preparation, 35 resolution, 88
Bright field illumination, 84, 85,90
Buehler trademarks, 129
E
EcoMet / AutoMet, 20
C Edge preservation, 13, 15
Castable resins:
Educational courses, 144
acrylic resins, 11-12, 129-130
Electronic materials:
Conductive Filler particles, 12, 129
epoxy resins, 11-12, 129-130

139
INDEX
E (cont.) measurements, 96, 99-100
preparation, 67-68 thresholding, 96, 99-100
Embedded abrasive, 16, 17, 18, 133 Individual force, 15

Epoxy resin, 11-13, 130 Iron and steel:

Etchants, 24, 26, 72-77 etchants, 80, 83

chemicals, 78-83 preparation, 43-46

dangerous solutions, 114 ISO standards, 135

mixing, 112-113
storage, 112 K-L
Etching, 24-26 Knoop hardness, 106-108
anodizing, 26 Light microscopy, 84-92
electrolytic, 24 Low-melting point metals:
heat tinting, 76 etchants, 78
interference layer method, 77 preparation, 36-37
procedure, 72
selective etching, 73-765
M
Magnesium and alloys:
F etchants, 78
Ferrous metals: preparation, 34
etchants, 80, 83 Magnesium oxide, 21
preparation, 43-46 Method Development, 7
Fluorescent dyes, 53 Microindentation hardness:
accuracy, precision, bias, 107-108
automation, 108-109
G indentation size effect, 108
Grain size measurement,99
Knoop test,106-108
Grinding:
Vickers test, 105-106
diamond, 16-17
Microscope, reflected light:
embedding, 69
condenser, 85
emery paper, 16
depth of field, 89
machines, 18
diaphragms, 90
planar, 16
“empty” magnification, 89
PlanarMet 300, 18
eye clearance, 87
SiC paper, 16
eye pieces, 87
filters, 86
H graticules, 81
Hafnium and alloys: illumination modes, 90-92
etchants, 79 Köhler illumination, 90
preparation, 39-40 light sources, 85
magnification, 87, 88
numerical aperture, 86, 88, 89
I
Image analysis objective lens, 84, 85, 86

binary operations, 96-99

feature-specific measurements, 99
field measurements, 99

140
INDEX
M (cont.) recommendations, 120
ray diagram, 90 Polymers:
resolution, 88-89 etchants, 83
reticles, 87 preparation, 70
Microscope, reflected light (cont): Precision cutters, 8-9
stage, 84, 87-88 Precious metals:
stand, 88 preparation, 51-52
working distance, 86, 87 Preparation method development:
Mounting: 2,4, 27, 28

castable resins, 11-13, 130 Preparation problems:

clamp mounting, 10 “comet tails,” 18, 19, 121, 133

compression mounting, 10-11, 129 disturbed metal, 18

conductive resins, 10 edge retention (preservation), 13, 15

embedded abrasive, 16, 17, 18, 133
edge retention (preservation), 13, 129
excessive relief, 18, 19, 28
phenolic resins, 10
pitting, 14, 18, 19, 24, 131
presses, 11
pull outs, 121
purposes, 10
scratches, 121, 133
recommendations, 10, 12
smear, 4, 22 ,121, 133
shrinkage gaps, 11, 14, 129
troubleshooting guide, 133
thermoplastic resins, 10, 129
water sensitivity, 59
thermosetting resins, 10, 129
Preparation procedures
troubleshooting guides, 129
contemporary methods, 28-29
Mount size, 30, 132
Al and alloys, 32-33
Be, 35
N ceramics, 57-58
Nickel and alloys:
Co and alloys, 49-50
etchants, 81
composites, 62-64
preparation, 48
Cu and alloys, 47
Nomarski DIC, 91
electronic devices, 67-69
Fe and alloys, 43-46
O-P glass, 60
Oblique illumination, 90 Hf and alloys, 39-40
Other National Standards, 136-38 low-melting point alloys, 36-37
Periodic table of the elements, 31 minerals, 59-60
Polarized light, 91-82 Mg and alloys, 34
Polishing: Ni and alloys, 48
abrasives, 21-22 polymers, 70-71
automated, 20 precious metals, 51-52
automet, 20 printed circuit boards, 65-66
cloths, 21, 22 Refractory metals, 38-42
ecomet, 20 Sintered carbides, 55-56
electrolytic, 24 Ti and alloys, 38-39
head position, 15, 30 TSC and TBC coated metals, 53-54
lubricants, 22 Zr and alloys, 39-40
manual, 24

141
INDEX
O-P (cont.) Smartcut, 8
specific procedures, 30-70 Solvents, 113, 114
development, 30 Sorby, Sir Henry Clifton, 84

load, 30 Specimen preparation:

platen size, 30 goals, 4

time, 30 Methods

“traditional” method, 27 Contemporary, 28-29

Printed circuit boards: Specific materials, 30-70

preparation, 65-66 traditional, 27

Pull outs, 131 (see: preparation procedures)

Stains, staining, 131, 133
Standards, metallography and hardness,
R 134-138
Refractory metals: Steels (see: Fe and alloys or Irons and steels)
etchants, 79
preparation, 38-42
Relief, 18, 19, 28
T
Thermally spray-coated metals
Rigid grinding discs, 15, 28
preparation, 53-54
Thermoplastic resins, 11, 122
S
Thermosetting resins, 11, 122
Safety:
Titanium and alloys:
acids, 115-118
etchants, 79
bases, 118-119
heat tinting, 76
chemical storage, 112
preparation, 38-39
dust, 111, 119
Trademarks, Buehler, 139
equipment operation, 111
fume hoods, 111, 117
MSDS, 110, 111 U-Z
personal protective equipment, 111 Ultrasonic cleaning, 20
publications, 127 Vacuum impregnation, 11, 15
safety plan, 110 Vickers hardness, 105-106
solvents, 113, 114 Water-sensitive materials, 21, 34, 35, 131
web sites, 127 Worldwide Sales Offices, 1346
Sampling, 3 Zirconium and alloys:
Sectioning, 5-9 etchants, 79
Sectioning damage, 5, 18, 27 preparation, 39-40
Shrinkage gaps, 10, 11, 12, 13, 14, 129, 133
Silicon
preparation, 67-69
Silicon carbide paper, 16-17
ANSI/CAMI grit size, 17
FEPA grit size, 17
Silicon dioxide, 21
Sintered carbides:
etchants, 82
preparation, 55-56

142
FULL LAB & SOLUTIONS
EDUCATIONAL COURSES
More thorough testing of increasingly complex materials, to include microstructural analysis, is being
driven by industry and consumer requirements for improved product quality and reliability. Existing
methods for specimen preparation can be insufficient to produce excellent results in higher through-
put environments. The desire for speed, consistency and quality have created demand for improved
preparation and analysis techniques. Besides offering solutions for this purpose, the training courses
offered by Buehler enable individuals to obtain or improve the necessary preparation skills.

Buehler® established the Institute for Microstructural Analysis in 1989, offering both general introductory
courses and specialized courses focused on the needs of specific industries or applications. All courses
include supervised, hands-on activities in the laboratory with classroom instruction to help students
understand the principles. Courses are offered at the Buehler headquarters in Lake Bluff, IL, United
States, Buehler ITW Test & Measurement GmbH in Esslingen, Germany, the University of Warwick in
the United Kingdom and other affiliated institutions.

SumMet™ Fundamentals of Metallographic Techniques (3 days)

A three day course designed for both metallographers without formal training or experienced metallographers
who want to learn the latest preparation techniques. The fundamentals of sectioning, mounting, grinding and
polishing are covered both in theory and practice in this course based on SumMet methods developed at
Buehler. Students will also be exposed to optical microscopy, etching, hardness testing, and microstructural
interpretation. Students are strongly encouraged to bring their own specimens.

On location training available upon request.

Visit www.buehler.com for more information on class dates and availability.

143
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Buehler Worldwide Locations

Lake Bluff, IL, US

Binghampton, NY, US
Norwood, MA, US
Coventry, UK
Dardilly, FR
Esslingen, DE
Ehsan, MY
Shanghai, CN
Tokyo, JP

Solutions for Materials Preparation, Testing and Analysis

BUEHLER
41 Waukegan Road, Lake Bluff, Illinois 60044 Asia-Pacific Offices
P: +1 847 295 6500 | 800 BUEHLER (800 283 4537) BUEHLER China - Shanghai
W: www.buehler.com | E: [email protected] ITW Test & Measurement (Shanghai) Co., Ltd.
Asia Headquarters
North America-South America Offices P: +86 400 111 8683
BUEHLER Worldwide Headquarters E: [email protected]
P: +1 847 295 6500 | 800 BUEHLER (800 283 4537)
W: www.buehler.com | E: [email protected] BUEHLER Japan
P: +81 3 5439 5077
Europe Offices E: [email protected]
BUEHLER Germany - Esslingen
ITW Test & Measurement GmbH BUEHLER Asia-Pacific Region
European Headquarters P: +86 400 111 8683
P: +49 (0) 711 4904690-0 E: [email protected]
E: [email protected]
Visit www.buehler.com for more information
BUEHLER France - Dardilly on a Buehler location near you.
P: +33 (0) 800 89 73 71
E: [email protected]
ISBN 0-9752898-0-2 FN01255
BUEHLER United Kingdom - Coventry
P: +44 (0) 800 707 6273
USA $149.00
Canada $159.00

E: [email protected]

© 2018 BUEHLER, a division of Illinois Tool Works Inc. FN01533