TiN/Al2O3 composite material was prepared by aluminothermic reduction of TiO2 in coke bed from mixtures of TiO2 powder and metal Al powder. The phase composition, lattice parameter and microstructure of products after treatment in different temperatures were analyzed by XRD, SEM. The results show that TiN/Al2O3 composite material can be produced in coke bed via aluminothermic reduction reaction. Moreover, the treatment temperature affects the evolution of aluminothermic reaction and morphology of products obviously. The content, grain size and lattice parameter of TiN in products in coke bed increase with the increasing of treatment temperature. Thermodynamically it confirms that metal Al reacts with oxygen in coke bed while it is involved in aluminothermic reduction reaction, and then it causes the lack of Al, which takes part in the aluminothermic reaction leading to a surplus rutile in the products.