LiNiO2 (R (3) over bar m) powders were synthesized by a sol-gel method using adiphic acid as a chelating agent. Highly crystallized LiNiO2 was synthesized in oxygen at a calcination temperature of 750 degrees C for 14 h when molar ratio of adiphic acid to total metal ions was 1.0. The intensity ratio of (003)/(104) peaks of XRD spectrum for the synthesized material was 1.67. The LiNiO2 powders were monodispersed particulate with the average size of approximately 1-2 mu m The electrochemical test of a half cell fabricated using the LiNiO2 powders revealed that the cell had a high initial discharge capacity of 158 mAh g(-1), but it showed very fast capacity fading just after several tens of charge/discharge cycles.