The LiCoxNi1-xO2 (x-0.2, 0.5 and 0.8) cathode materials were synthesized by sintering the mixtures of lithium salt and Cox Ni1-x (OH)2 (x= 0.2, 0.5 and 0.8) which were achieved from corresponding Cox Ni1-x alloys by electrolysis technique. The structure and electrochemical characteristics of the obtained LiCoxNi1-xO2 were studied by XRD, SEM, PSCA and charge-discharge cycling test. The results show that the electrochemical capacities of the LiCoxNi1-xO2 (x=0.2, 0.5 and 0.8) materials are improved with the increase of the Ni content. The electrochemical performance of LiCo0.2 Ni0.8 O2 made in oxygen atmosphere has higher charge-discharge capacity and better cycleability compared with the one made in air atmosphere.