New single phase undoped LiCoO2 and doped LiCo0.8M0.2O2 (M = Mg, Ca, Ba) layered oxide materials have been synthesized by a low temperature solid-state reaction. The phase purity and cation environment of the synthesized oxides were characterized using XRD and FT-IR. The particle size, nature, morphological properties and the composition of the synthesized oxides were examined by TEM and SEM with EDAX analysis. Finally, the electrochemical behaviour of the prepared layered materials was studied using cyclic voltammetry and charge-discharge cycling. LiCo0.8Mg0.2O2 has better cycling results compared to all other materials. These results have also been supported by cyclic voltammograms. (C) 2007 Published by Elsevier Ltd.