Pyrolytic Conversion of Spherical Organo-silica Powder to Silicon Nitride under Nitrogen

Monodisperse, spherical Si₃N₄ powder composed of fine particulates was synthesized by pyrolyzing spherical organo-silica powder under nitrogen. The organo-silica powder was prepared by hydrolyzing a mixture of phenyltrimethoxysilane (PTMS) and tetraethoxysilane (TEOS) in a methanol solution of water and ammonia. The organo-silica powder consisted of 81.3 at.% silicon units derived from PTMS and 18.7 at.% silicon units derived from TEOS. During the pyrolysis under nitrogen, the organo-silica powder decomposed to a mixture of free carbon and silica, with an increase of the surface area, at 500°-600°C, followed by the formation of alpha-Si₃N₄, with ß-Si₃N₄ as a minor phase, at 1450° and 1500°C and ß-SiC at 1550°C. The pyrolyzed powders, which retained the spherical shape and monodispersity of the organo-silica powders, with a reduction in mean particle diameter, were composed of fine particulates that were ~40 nm in size.