Synthesis of porous silicon nitride using silica/carbon composite derived from phenol–resorcinol–formaldehyde gel

Mesoporous silicon nitride (Si3N4), which is one of the most promising structural materials for applications in high-temperature filtration, was synthesized from the carbothermal reduction and nitridation of a pyrolyzed silica-containing phenol-resorcinol-formaldehyde (PRF) gel. The PRF gel was synthesized by combining sol–gel and polymerization of phenol, resorcinol and formaldehyde using sodium carbonate as a catalyst. Silica was incorporated into the gel by addition of 3-aminopropyl trimethoxysilane (APTMS) as a silica precursor. After aging and being freeze-dried, the silica/PRF composite was pyrolyzed under nitrogen gas to convert it into porous silica/carbon composite. The combination of phenol-formaldehyde (PF) and resorcinol-formaldehyde (RF) gels into PRF gel, allows further enhancement in porosity of the silica/carbon composite via pre-calcination in the range of 400–500 °C, since carbon derived from PF gel and that from RF gel have different thermal stability. The final product obtained after final calcination to remove residual carbon has a surface area as high as 194 m2/g, which is significantly much higher than the conventional Si3N4 granules. Specific surface area of the product is affected by molar ratio of phenol-to-resorcinol, molar ratio of silica-to-carbon, and the pre-calcination temperature.