Electrochemical performances of substituted layered oxides (LiM1-yMyO2)-O-' (M = Ni, Co and M' = Mg, Al, B) as cathode materials in lithium batteries have been investigated. These materials have been made through a solid state reaction of precursors in an oxygen rich atmosphere. X-ray diffraction and infrared measurements have been carried out. Structural data have shown that a single phase, impurity free, can be made through careful selection of precursors, except for the B substituted compounds, for which residual impurity phases were observed due to a more glassy nature of the products. The voltage profiles of the layered oxides and substituted oxides were monitored against a lithium electrode. The overall capacity of the oxides have been reduced due to the sp metal substitution, however, a more stable charge-discharge cycling performance has been observed when electrodes are charged to 4.3 V as compared to the performances of the native oxides. At the cut-off voltage of 4.4 V, the charge capacity of the Li//LiNi0.95Al0.05O2 cell is ca. 165 mAh/g. Boron doped LiCoO2 also provides very low polarization during charge-discharge cycling, with a capacity over 130 mAh/g when charged up to 4.3 V versus a Lithium anode. A sample of LiNiO2 with 5% Mg substitution delivers a capacity of 168 mAh/g. (C) 2000 Elsevier Science B.V. All rights reserved.