The cathode materials LiNixCo1-xO2 (0≤x≤1) for lithium ion battery were prepared in solid phase . The effects of synthesis temperature , the time of heat treatment and also the ratio of raw materials on products were discussed . The residts showed that the products preheated under 600℃ and then sintered under constant, temperature 75017 were better than those sintered under constant temperature 650℃ or 850℃ , and their layer structures were more obvious and their initial capacity was higher . The longer the heat-treating time is , the stronger the products ’ XRD peaks intensity and the better their structures and electrochemical performance are. The samples LiN-ix Co 1-xO2(0≤x≤1) with a perfect structure and electrochemical performance were synthesized. And the products initial capacity was perfect when n(Li) : n( Ni) : n( Co) ℃ 1.15:0.3:0.7,viz. 156.l46mAh/g.