Nano-structure TiN powders were prepared by using anatase-TiO2 and graphite mixtures as the precursor. Prior to thermal conversion, the mixture of TiO2 and graphite was milled in a high energy attritor to enhance the validity of carbothermic reduction. The nano-TiN powders were thermal converted by introducing N2 into a low pressure circulated fluidized-bed reactor which was previously evacuated to the pressure around 10-1 torr The formation of TiN compound is greatly enhanced by high-energy milling due to the reduced crystallite size, large grain boundary area, presence of amorphous phases and the increased defect concentration in the powder reactants given by the high-energy milling. Crystallites size of the powder mixtures decreased as increasing of milling time. The nano-TiN formation can be accomplished at a relatively low reaction temperatures and short reaction time via severe milling of TiO2 + graphite mixtures. The experiment results evidenced that the carbothermic reduction could not be occurred if the powder mixture of TiO2 + graphite had not been undergone a severe milling