溶胶凝胶法的机理以及其在合成碳化硅中的应用.pptVIP

The Mechanism of Sol-Gel Method and its Application on the Preparation of Silicon Carbide 张玉强 迟晓伟 罗 涛 谢滨欢 周 遥 弓 娟 SiC on nano-scale A sol-gel process is a colloidal route used to synthesize materials with an intermediate stage including a sol and/or a gel state. Advantages Any oxide composition Pure products Low temperature Structure can be easily controlled Avoiding pollution Simplified chart of sol-gel processes Colloidal: Solvent = alcohol (or water) Precipitation: [alkoxide][water] Polymer: Solvent = alcohol Sol--gel kick-off: [water]/[alkoxide]=1-4 Influences Precursors Solvent(organic/inorganic) pH Electrolyte Additives n(H2O): n [M (OR)n] …… Acid： C2H5 Si O C2H5OH Si H+ Si(OC2H5)4 HOSi(OC2H5)3 H3O+ Electrophilic reaction，tend to be chains Base: OH- C2H5 Si O H+ in aq Si C2H5OH Si(OC2H5)4 HOSi(OC2H5)3 Nucleophilic reaction , tend to be conglobation SiC nanorod 1 SiC nanofiber 2 SiC nanowire 3 TEOS: water: CH2Cl2=1:4:4 Stirred at room temperature for 7-8h polysiloxane Add kraft lignin For impregnation of Silica into the lignin matrix Take out over a night Precursor pyrolyzed at 1400℃ In Argon gas for 1h Grey-black product Cool down to room temerature And then at 800℃ for 1h Grey-white product Preparation Materials Letters 63 (2009)2449–2451 Formation between lignin and polysiloxane Discussion SEM image of SiC nanorods. XRD spectra of SiC nanorod β-SiC SiO2 HRTEM image of pyrolyzed sample of SiC nanorods. Pyrolyzed-oxidised sample of SiC nanorod Discussion TEOS、ethanol La(NO3)3 phenolic resin (酚醛树脂) Add HCl Stirring 24h Add HMTA(35.8%) To rapid gelation Drying at 110℃ for 12h Xerogel Materials Letters60(2006)1334–1337 Carbothermal reduction xerogel Al2O3 tubular furnace Al2O3 Boat Ar gas (50cm3/min) To 1000℃(10℃/min) To 1300℃(2℃/min) keep for 5h Then cool down to the room temperature Product containing SiC Heated in air at 700℃ for 3h Treated with HNO3 and HF Light-green powder Discussion TEM image and corresponding SAED pattern of the co