Experiment: Synthesis of ZnO nanoparticles by Sol-gel method.
Objective: Synthesis of ZnO nanoparticles by Sol-gel method
Apparatus (Materials Required):
• Zinc acetate dihydrate (Zn(CH₃COO)₂·2H₂O)
• Ethanol or methanol
• Sodium hydroxide (NaOH) or ammonium hydroxide (NH₄OH)
• Distilled water
• Glassware (beakers, Measuring cylinder etc.)
• Magnetic stirrer
• Heating equipment (oven)
• Muffle Furnace
Theory:
Sol-gel is broadly defined as the production of solid materials like metallic oxides from the solution
reactants or precursors (starting materials). The precursors usually are metal alkoxides which crosslink
forming metal-oxane gels, or metal ion-chelate complex or metal containing organic polymeric gels. The
choice of precursor strongly affects the composition and structure of the end product. Sol-gel processing,
or sol-gel chemistry as it is often termed, can be used for producing solid material from chemically
homogenous precursor. By exploiting the arbitrariness involved in the solution state, it ensures atomic
level mixing of reagents, and therefore, it can form complicate inorganic materials at low temperatures
in short processing times. Moreover, sol-gel chemistry also enables better control over the particle size
and morphology. In this module, the participants will learn the basics of sol-gel technique for
nanomaterials synthesis.
In a conventional sol-gel method, the precursor goes through reactions of hydrolysis and polymerization
topro duce a colloidal suspension (or sol). Complete polymerization along with subsequent loss of
solvent directs conversion from sol (liquid phase) to gel (solid phase). A wet gel is formed once sol is
casted into a pattern. Further drying and sintering convert the wet gel to dense ceramic. An extremely
porous and very low-density material, termed aerogel, can be formed by removal of solvent from the wet
gel at some supercritical conditions. Homogeneous and ultrafine ceramic powder can be produced by
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employing spray pyrolysis, precipitation, or emulsion techniques. The following subsections elaborate
the various stages in the sol-gel processing.
Introduction to ZnO Nanoparticles:
a) ZnO is a wide-band gap semiconductor with promising applications in opto-electronic devices due to
its unique electronic and optical properties.
b) Nano-scale ZnO particles exhibit size-dependent characteristics that can be tailored for specific
applications.
Procedure / Experimental Approach:
Here are the detailed steps from the experimental method for synthesizing ZnO nanoparticles via the
Sol-gel method.
1. Chemical Precursor Preparation:
a) Dissolve 0.2M zinc acetate dihydrate [Zn(CH₃COO)₂·2H₂O] in 200ml methanol (CH₃OH) at room
temperature to obtain a clear solution.
b) Stir the solution for 2 hours until a clear solution is achieved.
c) Titrate 1.0 M NaOH into the solution until the pH reaches 9, resulting in the formation of a milky
white slurry.
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d) Stir the white slurry for an additional 1 hour to ensure homogeneous mixing.
2. Gel Formation:
a) Allow the homogeneous mixture to age for 12 and 24 hours to complete hydrolysis and gelation.
b) After aging, observe the separation between a clear solution and white precipitate at the bottom of the
storage container.
3. Isolation and Drying:
a) Filter the aged samples to separate the white precipitate.
b) Dry the white precipitate in an oven at 100°C for a specific duration.
c) Grind the dried samples into a fine powder using a mortar and pestle.
4. Calcination: Calcine the powdered samples at 300°C in normal air to produce well-crystallized ZnO
nanoparticles.
5. Characterization: The synthesized ZnO nanoparticles can be characterized using techniques such as
X-ray diffraction (XRD) to determine crystallinity, scanning electron microscopy (SEM) for
morphology, and UV-Vis spectroscopy for optical properties. (It is Part of Advance Studies)
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Dissolve 0.2M zinc acetate dihydrate [Zn(CH₃COO)₂·2H₂O] in 200ml methanol (CH₃OH). + Stir the solution
for 2 hours until a clear solution is achieved.
Titrate 1.0 M NaOH into the solution until the pH reaches 9, resulting in the formation of a milky white
slurry. + Stir the white slurry for an additional 1 hour to ensure homogeneous mixing.
Allow the homogeneous mixture to age for 12 and 24 hours to complete hydrolysis and gelation. + After
aging, observe the separation between a clear solution and white precipitate at the bottom.
Filter the aged samples to separate the white precipitate.
Dry the white precipitate in an oven at 100°C for a specific duration. + Grind the dried samples into a fine
powder using a mortar and pestle.
Calcine the powdered samples at 300°C in normal air to produce well-crystallized ZnO nanoparticles.
Precautions:
• Purity of Reagents: Use high-purity reagents to minimize impurities in the final product.
• Control of pH: Carefully control the pH during the addition of the hydroxide solution to avoid
agglomeration.
• Stirring: Continuous and uniform stirring is crucial for the homogeneity of the sol and gel.
• Calcination Temperature: Optimize the calcination temperature to achieve the desired
nanoparticle size and crystallinity.
