To determine optimum conditions for the synthesis of LiNiO2 by the combustion method, syntheses were carried out in air and under oxygen at various calcination temperatures and for different times. The electrochemical properties of the prepared samples were then investigated. The optimum conditions are preheating at 400 °C for 30 min in air in the mole ratio of urea to nitrate 3.6 and calcination at 750 °C for 36 h under O2. The LiNiO2 synthesized under these conditions had a first discharge capacity of 189 mAh g−1 at 0.1 C-rate and relatively good cycling performance. This sample has a larger value of I003/I104 (smaller cation mixing) and a smaller R-factor (larger hexagonal ordering). Cycling performance was investigated in various voltage ranges. The first discharge capacity increased as the upper limit of the voltage range rose. The first discharge capacity was small but cycling performance was good when the sample was cycled in the voltage range with the lowest upper limit.
