LiCo0.3Ni0.7O2 has been prepared at 700 degrees C for 8 h in air by using beta-Co0.3Ni0.7OOH and (LiOHH2O)-H-. as starting materials. The sample was characterized by XRD, ICP, SEM, XPS, valence analysis and electrochemical performance. The results show that the sample has a good layered structure and the average oxidation value of (Co, Ni) in the sample is +3. Moreover, the sample has a good electrochemical performance with an initial discharge capacity of 145 mAh g(-1) and a good capacity retention of 97.79% after 50 cycles. The good cycle performance is attributed to the limited structural disorder and the non-occurrences of any structural transition from hexagonal to monoclinic during the charge and discharge processes. (c) 2005 Published by Elsevier B.V.