Abstract: The Ti(C_1-xN_x) powder was synthesized by utilization of tetrabutyl titanate (Ti(OC₄H₉)₄) and nano carbon black (C) as raw materials, with their theory mass ratio of 9.4:1. Tetrabutyl titanate and carbon black with their mass ratio of m(Ti(OC₄H₉)₄):m(C)=9:1, were mixed to prepare the sintering precursor through sol-gel process. Ultrafine Ti(C_1-xN_x) powder was obtained after calcination at various temperatures and N₂ atmospheres for 1 h with the help of high temperature carbon thermal reductive reaction. The results show that, with increasing temperature, x values of Ti(C_1-xN_x) gradually reduce and range from 0.19 to 0.72. The content of total carbon(C_t) in the products increases from 14.23wt% to 18.66wt%, the contents of free carbon (C_f) and oxygen (C_o) all remain below 0.5wt%. In addition, the particle sizes also show a trend of increase, in the range of 220 nm to 275 nm.