Titanium oxide gel was preared from n-butyl titanate by a sol-gel method, The gel was then sintered to form TiO₂ ceramic. From the TiO₂ powder, titanium nitride formed through nitrifying by ammonia at the temperature above 900℃. The processes were intensely studied through thermal analysis, chromotography, scanning electronic microscopy and X-ray diffraction. Emphasis is placed on the chemical reations, the crystalliztion and polyamorphism in the sol-gel process of TiO₂. Thereafter, the dependence of the yield of TiN under the preparatory conditions of TiO₂ is established.