On the basis of X-ray diffraction analysis result, technological parameters in the preparation of nanocrystalline Ti(C1-x,Nx) via carbothermal reduction of nano TiO2 in close nitrogen atmosphere was studied. The results showed on condition that other technological parameters are fixed, nitrogen content of Ti(C1-x,Nx) decreases with the increment of reaction temperature, isothermal treatment time, starting powders weight, or C/Ti value except for nitrogen pressure. Reaction temperature and isothermal treatment time have a crucial effect on crystallite size of nanocrystalline Ti(C1-x,Nx). When the temperature exceeds 1600 ℃ or isothermal treatment time exceeds 4 h, the grain growth of nanocrystalline Ti(C1-x,Nx) accelerates.