Stabilized lithium nickelate is receiving increased attention as a low-cost alternative to the LiCoO2 cathode now used in rechargeable lithium batteries. Layered LiNi1-x-yMxMyO2 samples (M-x = Al3+ and My = Mg2+, where x = 0.05, 0.10 and y = 0.02, 0.05) are prepared by the refluxing method using acetic acid at 750 degrees C under an oxygen stream, and are subsequently subjected to powder X-ray diffraction analysis and coin-cell tests. The co-doped LiNi1-x-yAlxMgyO2 samples show good structural stability and electrochemical performance. The LiNiAl0.05Mg0.05O2, cathode material exhibits a reversible capacity of 180 mA h g(-1) after extended cycling. These results suggest that the threshold concentration for aluminum and magnesium substitution is of the order of 5%. The co-substitution of magnesium and aluminium into lithium nickelate is considered to yield a promising cathode material. (c) 2005 Elsevier B.V. All rights reserved.