Preparation of tin oxide by sol-gel method and its characterization 1, Importance of the experiment: ‘Nano tin oxide (Sn0:) 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 cell, anti-reflection coatings in solar cells, gas sensors, optoelectronic devices and resistors. SnO; 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. Principle of sol-gel method’: Three approaches are used to make sol-gel = { ‘monoliths: method 1, gelation of 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 Sn; nanoparticles: Tin oxide (SnO,), cassitrite , 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 erystal displays (LCDs); solid-state optoelectronic devices; catalysts for methanol conversion and CO/O, COMNO 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 SnOp for the above mentioned applications depend on several factors, mainly crystallite size and specific surface area. For example, inthe 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. sont Scanned with CamScanner2BCEZLES SHREYA SINGH Expt.Noz O07 Date: o7/12]2021 Experiment Preparation of tin oxide by sol-gel method and its characterization Tin oxide (SnO,) nanoparticles find application in various fields. Hence, itis of great importance to synthesize SnO, nanoparticles. ‘SnOz nanoparticles were prepared by sol-gel method and characterized by powder X-ray diffraction (powder XRD) Solution Preparation of SnO; nanoparticles Problem definition Methodology Students will learn to 4) prepare metal oxide nanoparticles by sol-gel method b) analyze the nanoparticles by powder XRD Student learning outcomes Prineipl Tin oxide (SnOz) nanoparticles were prepared by sol-gel method! starting from tin tetrachloride pentahydrate,(SqC}s,SH20), preeurspr? Tin tetrachloride pentahydrate, (SnCls.5H120),was dissolved in methanol. The above solution undergoes hydrolysis with the addition of aquesous ammonia results tin turbid colloidal solution called sol. fi i se qe ye alton elcsemet + ANOH to-go Sol is Gonvéited ito el by polycondensation of td ijdrokide (Sn(OH] into a condensed polymere network (sot get) Condens: HO~o-OH # HO" Ho dp-0- don 0 POS Gy enatoesten NO=ty- Odeon # # Wo ie ok 2, Principle of sol-gel n Pee Matai) On dtyitig, condensed ‘polymeric’ network was converted into a three dimensional network reddnbaigen™ msttens 2s Dole ‘Cotidensed polymeric network (gel ) > Dried form (Three ©“ atiinersfonal network) (gel) igell S80» 4 les were formed. SiO; :nanoparticles. were characterized by’ powder XRD techitique.”" “ Requirement sions of eailondal p. fin tetrachloride, pentahydrate (SnCly.SH,O), methanol, aqueous ammonia. Reagents and solution: Apparatus, equipment“and Instruments: Round bottom ask, Buchmann funnel, hot air oven, powder XRD i sient. A simplified chat of various manostiustates is shawn in Fig Be lraportance of SuO), nanoparticles: A 35 eV Ins prominin Scanned with CamScannerProcedure: perimental procedure: In.8 100 mL. round bottom Mask, 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 stiring, The dropping rate must be well controlled for the chemical homogencity. ‘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 $ h at 80 °C. The obtained gel powder was finally calcined in ‘A muMMe furnace at 400 °C for 2 h to get SnO nanoparticles. Characterlzation: ‘The powder XRD pater of the collected powder sample was recorded on a Bruker D8 advance (Germany) with Cu Ka radiation source (operating Voltage and current 30K V, 40MA respectively) in the scan range 10-80° (20), ‘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)? Analysis: ‘The powder XRD peak positions for the prepared SnO: 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 calewlation using Scherrer’s equation: Scherrer equation Schorrer’s equation Grain size = k*2,/ cos(0)*(FWHM) Nes FN) k= 0.9, 2= 1.0506 A, and “O" and FWHM ie will be obtained from powder XRD data ee asin Aero waelreh wnt fa wy tho smoxmon (nada) :peck postion Scanned with CamScannerResult: () The powder XRD peak positions for the prepared by SnO; nanoparticles are ‘ (ii) Particle size_5-O86 nm Qua 4528 nm__. References: 1. Hench, L. Li; West J. K. Chem. Rey., 1990, 90, 33-72. 2, Gnanam, $.; Rajendran, V. J. Sol-Gel Sei. Technol, 2010, 53, 555-559. CALCULATION ©) For Wo ptous , 20= 26.9169" oO 4619591 Hs ere Cuystaluite Be oxo HOS ee 104619537 UGX °. 5472 534 159 5086 nm SF the ti) Fo ot 28= 33-9167 B* 16:958u" C038 = 0956 516182 FWUN = 1'9302° FOrosIgyyIEIA caddaus ~ SS OMTIEIS AOASESICTED. : » equation Scanned with CamScanner