TiN/Al2O3 composite material was prepared by aluminothermic reduction of TiO2 in coke bed. The phase composition, lattice parameter and microstructure of products treated at 1300℃, 1400℃, 1500℃ for 3h were analyzed by XRD, SEM, TEM. The results showed that TiN/Al2O3 composite material can be prepared in coke bed via aluminothermic reduction method. However, the treatment temperatures affect the evolution of aluminothermic reaction and morphology of the materials obviously. The content, grain size and lattice parameter of TiN in materials in coke bed increased with the increase of treatment temperature. Thermodynamic calculation confirmed that metal Al reacteds with O2 in coke bed while it was involved in aluminothermic reduction reaction, causing the lack of Al and surplus rutile in the products.