Abstract: Ti(C, N) powders were synthesized by the hydrolysis precipitation-carbothemal reduction and nitridation method, using TiCl₄ and carbon black as the raw materials. The effects of synthesis technology on the Ti(C, N) powders were characterized by the differential thermal analysis, X-ray diffraction analysis, and scanning electron microscopy. In the results, after baking the precursor powders at 350 ℃ for 2 h, the titanium atoms can only exist in a compound of TiO₂, and a uniformly mixed aggregate of TiO₂ and carbon black forms. The titanium oxide transforms into a complex compound of TiC_xN_yO_z during the carbothermal reduction and nitridation process at 1200~1400 ℃. The nitrogen atoms accelerate the transformation processes from TiO₂ to TiC_xN_yO_z. As the reaction goes on, the oxygen atoms are gradually replaced by carbon and nitrogen atoms to form the solid solution of TiC_xN_y. The Ti(C, N) powders as the chemical formula of TiC_0.547N_0.453 are synthesized at 1530 ℃ for 4 h with the oxygen mass fraction of 0.3% and the powder size of ~300 nm.