Compounds LiCo1-xNixO2 with different x values were prepared by sol-gel synthetic method, in which citric acid was used as chelating agent and the chelate was calcined at 800 V in air, environment. When x is less than 0.5, the products have good layered structures. Their charge and discharge capacities increase with the increment of Ni amount. When x is 0.5, the first charge and discharge capacities of product are 169 and 148 mA.h/g respectively, and the tenth discharge capacity of product is 129 mA.h/g. When x is more than 0.5, non-stoichiometric products with impefect structures are produced due to decomposing reaction, and their electrochemical properties become worse.