To improve the electrochemical characteristics of positive electrode in lithium secondary battery, synthesized LiNi1-xCoxO2 by sol-gel method and emulsion-drying method. The optimal synthesis conditions and the electrochemical characteristics of LiNi1-xCoxO2 with variation of x were studied. Synthesized by sol-gel and emulsion-drying method at the optimal conditions, the hexagonal lattice parameter c increased with increasement of x. Therefore, Ni rich samples showed good cycle-life characteristics and high coulomb efficiency than Co rich samples and Co rich samples showed higher initial discharge capacity than Ni rich sample.