A process for producing substantially oxygen-free titanium. carbide, nitride or carbonitride in powder form comprises treating a gas phase reaction mixture of titanium. halide, desirably TiC4, a reductant vapor, desirably sodium or magnesium, and a reactive gas capable of furnishing carbon, nitrogen or mixtures thereof at the reaction temperature, desirably nitrogen, methane or ammonia, to a temperature in the range from 500 degrees to 1250 degrees C., preferably 800 degrees to 1100 degrees C., whereby the titanium. halide is substantially simultaneously reduced and carbided, nitrided or carbonitrided. The process may also be practiced using volatile metal halides of metals such as zironium, hafnium, vanadium, niobium, tantalum and silicon for forming substantially oxygen-free carbides, nitrides or carbonitrides thereof in powder form.