The ultrafine titanium carbonitride () particles below 100 nm in mean size, including various carbon and nitrogen contents (x=0.55~0.9, y=0.1~0.5), were successfully synthesized by new Mg-thermal reduction process. Nanostructured sub-stoichiometric titanium carbide () particles were initially produced by the magnesium reduction of gaseous at and post heat treatments in vacuum were performed for 2 hrs to remove residual magnesium and magnesium chloride mixed with . Finally, well C/N-controled phases were successfully produced by nitrification heat treatment under normal gas atmosphere at for 2 hrs. The values of purity, mean particle size and oxygen content of produced particles were about 99.3%, 100 nm and 0.2 wt.%, respectively.