The effects of excess lithium and aluminum doping in nickel oxide were investigated in an attempt to improve electrochemical properties of the layered LiNiO2. Li1+x NiO2 (x=0–0.02) and LiAl y Ni1−y O2 (y=0–0.3) powders were synthesized by a sol–gel method using adipic acid as a chelating agent. The electrochemical properties of the synthesized materials were explored at room and high temperatures. Gas analysis during decomposition of gel precursors revealed that oxygen might play an important role in the synthesis of highly crystallized LiNiO2. Although the electrochemical test of the Al-doped samples showed a low initial discharge capacity of about 140 mAh g−1, the capacity loss with repeated cycling was very small at room temperature. Furthermore the fade in capacity of this cell at high temperature (50°C) was almost negligible. The Al-doping of the LiNiO2 cathode material was very effective in improving cycle performance at high temperature due to the enhanced stability of LiNiO2 structure.