Preparation of Silicon Nitride‐Titanium Nitride and Titanium‐Titanium Nitride Composites from (CH ₃ ) ₃ SiNHTiCl ₃ ‐Coated Si ₃ N ₄ and Ti Particles

Abstract

[(Trimethylsilyl)amino]titanium trichloride, (CH 3 ) 3 ‐SiNHTiClj, was isolated as a red‐orange crystalline solid in 58% yield from the reaction of TiCl 4 with [(CH 3 ) 3 Si] 2 NH in 1:1 molar ratio in dichloromethane at —78°C. Pyrolysis of (CH 3 ) 3 SiNHTiCl 3 at 600°C furnished titanium nitride. This precursor is suitable for the preparation of composites and was employed to prepare Si 3 N 4 ‐TiN and Ti‐TiN powders by adding Si 3 N 4 particles or titanium powders to a solution of (CH 3 ), SiNHTiCl 3 in dichloromethane, drying and pyrolyzing the resulting solid. This precursor also has been used as a binder to prepare Si 3 N 4 ‐TiN and Ti‐TiN bodies. High‐resolution transmission electron microscopic studies of the Si 3 N 4 ‐TiN composite showed that titanium nitride is concentrated on the surface of the Si 3 N 4 particles.