Synthesis of porous silicon nitride via the carbothermal reduction and nitridation of silica/PRF gel composite
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Title Synthesis of porous silicon nitride via the carbothermal reduction and nitridation of silica/PRF gel composite
Creator Marisa Meechoonuck
Contributor Varong Pavarajarn
Publisher Chulalongkorn University
Publication Year 2554
Keyword Silicon nitride -- Synthesis
Abstract This research studied the synthesis of porous silicon nitride, one of the most promising structural materials for applications in filter at high-temperature, from silica/phenol-resorcinol-formaldehyde (PRF) gel composite which was prepared by combining sol-gel and polymerization of phenol, resorcinol and formaldehyde using sodium carbonate as catalyst and 3-aminopropyl trimethoxysilane (APTMS) as silica precursor. After aging of the silica/PRF gel for 72 hours, t-butanol was used in the solvent exchange process for 24 hours and repeated for 3 times. Then the sample was dried in freeze drying processes at -40°C for 3 days. Next, the silica/PRF composite was pyrolyzed under nitrogen gas and pre-calcined first under air at temperature in the range of 400-500°C for 2 hours to convert the PRF structure into porous carbon and partially remove carbon from the composite, respectively. Finally, the composite was subjected to the carbothermal reduction and nitridation at 1450°C for 10 hours followed by the removal of residual carbon by calcination at 800°C for 8 hours. From the results, differences in molar ratio of phenol-to-resorcinol, silica-to-carbon and pre-calcination temperature result in difference in porosity of both silica/carbon composite and that of silicon nitride product. The pre-calcination is the major effect to improve the porosity, which has an effect on porosity of silicon nitride product. Moreover, it was also found that the use of pre-formed silica sol, which is another way to decrease violent interaction between silica precursor and the PRF solution, has an effect on porosity and crystallite size of silicon nitride product.
URL Website cuir.car.chula.ac.th
Chulalongkorn University

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