Preparation of tin oxide by sol-gel method and its characterization

Name: Srisudharshan Manikandan

Register Number: 21BEC2104

1. Importance of the experiment:

Nano tin oxide (SnO2) is a promising nano phase metal oxide to find applications in various fields (vide
infra). They are used in magnetic data storage, magnetic resonance imaging, as catalysts, energy-saving
coatings and anti-static coatings, as electrodes in solar cells, anti-reflection coatings in solar cells, gas
sensors, optoelectronic devices and resistors.

SnO2 nanoparticles can be achieved by various wet chemical methods such as precipitation,
hydrothermal, solvothermal, sol-gel, combustion, spray pyrolysis, polymerized complex (PC) and
amorphous citrate method. Each method has its merits and demerits. Sol-gel method is one of the
promising methods in the preparation of SnO2 nanoparticles.

2. Principle of sol-gel method1:

Three approaches are used to make sol-gel

monoliths: method 1, gelation of a solution of
colloidal powders; method 2, hydrolysis and
polycondensation of alkoxide or nitrate precursors
followed by hypercritical drying of gels; method 3,
hydrolysis and polycondensation of alkoxide
precursors followed by aging and drying under
ambient atmospheres.

Sols are dispersions of colloidal particles (with

diameters 1-100 nm) in a solvent. A gel is
interconnected, rigid network with pores of sub-
micrometer dimensions and polymeric chains
whose average length is greater than a micrometer.

A simplified chart of sol-gel method for preparation Fig. 1. Simplified chart of sol-gel method for
of various nanostructures is shown in Fig. 1. preparation of various nanostructures.

3. Importance of SnO2 nanoparticles:

Tin oxide (SnO2), cassiterite , is a n-type semiconductor having a wide bandgap 3.8 eV. Its promising
chemical and mechanical stabilities made it suitable and most widely used semiconductor oxide for
various energy related applications. It is used as transparent electrodes for solar cells; liquid crystal
displays (LCDs); solid-state optoelectronic devices; catalysts for methanol conversion and CO/O2,
CO/NO reaction in the control of noxious emissions; antistatic coatings and gas sensors; anodes for
lithium ion batteries; transistors; catalyst supports; nano and ultrafiltration membranes and
anticorrosion coatings and gas sensors. The use of of SnO2 for the above mentioned applications depend
on several factors, mainly crystallite size and specific surface area. For example, in the field of lithium-
ion battery, very fine tin oxide particles are needed to obtain high capacity. So it is of great importance
to synthesize nanoscale tin oxide particles.

Expt. No.: Date:

Experiment Preparation of tin oxide by sol-gel method and its characterization

Tin oxide (SnO2) nanoparticles find application in various fields. Hence, it is of

Problem definition
great importance to synthesize SnO2 nanoparticles.
SnO2 nanoparticles were prepared by sol-gel method and characterized by powder
Methodology
X-ray diffraction (powder XRD)
Solution Preparation of SnO2 nanoparticles
Students will learn to
Student learning
a) prepare metal oxide nanoparticles by sol-gel method
outcomes
b) analyze the nanoparticles by powder XRD

Principle:
Tin oxide (SnO2) nanoparticles were prepared by sol-gel method1 starting from tin tetrachloride
pentahydrate (SnCl4.5H2O) precursor.2 Tin tetrachloride pentahydrate (SnCl4.5H2O) was dissolved in
methanol. The above solution undergoes hydrolysis with the addition of aquesous ammonia results tin
hydroxide [Sn(OH)4], turbid colloidal solution called sol.

Sol is converted into gel by polycondensation of tin hydroxide [Sn(OH)4] into a condensed
polymeric network (sol → gel).

On drying, condensed polymeric network was converted into a three dimensional network
result a gel.
Colloidal solution (sol) → Condensed polymeric network (gel ) → Dried form (Three
dimensional network) (gel)
On calcination of the gel, SnO2 nanoparticles were formed. SnO2 nanoparticles were
characterized by powder XRD technique.
Requirements:
Reagents and solutions: Tin tetrachloride pentahydrate (SnCl4.5H2O), methanol, aqueous ammonia.
Apparatus, equipment and Instruments: Round bottom flask, Buchmann funnel, hot air oven, muffle
furnace, powder XRD instrument.

Procedure:
Experimental procedure:
In a 100 mL round bottom flask, tin tetrachloride pentahydrate (1 g) was dissolved in 30 mL methanol
under vigorous stirring. To the above solution, aqueous ammonia (1.2 mL) was added drop wise under
stirring. The dropping rate must be well controlled for the chemical homogeneity.
The resulting opal gel was filtered using Buchmann funnel fitted with a Whatmann filter paper.
The gel was washed with methanol to remove impurities. Gel was transferred carefully into a petri dish
and kept in a hot air oven for 5 h at 80 C. The obtained gel powder was finally calcined in a muffle
furnace at 400 C for 2 h to get SnO2 nanoparticles.
Characterization:
The powder XRD pattern of the collected powder sample was recorded on a Bruker D8 advance
(Germany) with Cu Kα radiation source (operating Voltage and current 30KV, 40MA respectively) in
the scan range 10-80 (2). The expected pattern is given in Fig. 1 for reference.

Fig. 1. XRD pattern of SnO2 nanoparticles mediated in methanol (a), ethanol (b), and water (c).2

Analysis:
The powder XRD peak positions for the prepared SnO2 nanoparticles by sol-gel method are identified
based on standard JCPDS file #__88-0287. This shows the tin oxide crystallizes in tetragonal crystal
system __________________________________________.
Particle size calculation using Scherrer’s equation:
Scherrer equation

Grain size = k* / cos(θ)*(FWHM)

k = 0.9,  = 1.0506 Å, and “” and FWHM

will be obtained from powder XRD data.

Result: (i) The powder XRD peak positions for the prepared by SnO2 nanoparticles are:
110,101 .
(ii) Particle size: 3.086nm, 4.538 nm.

References:
1. Hench, L. L.; West J. K. Chem. Rev., 1990, 90, 33-72.
2. Gnanam, S.; Rajendran, V. J. Sol-Gel Sci. Technol., 2010, 53, 555-559.