LiCoO₂ cathode powders were prepared by the two different spray pyrolysis processes. The mean size of the post-treated LiCoO₂ powders prepared by the FEAG process was 1.6 μm when the excess amount of lithium component was 10 mol% of the stoichiometric value. The post-treated LiCoO₂ powders obtained by ultrasonic spray pyrolysis were finer than those prepared by the FEAG process. The initial discharge capacities of the LiCoO₂ powders prepared by the FEAG process changed from 119 to 156 mAh/g when the excess amounts of lithium component were changed from 3 to 20 mol% of the stoichiometric value. The maximum initial discharge capacity of the LiCoO₂ powders prepared by the ultrasonic spray pyroysis was 151 mAh/g obtained from the excess amount of lithium component of 3 mol% of the stoichiometric value.