The lithium cobalt vanadate (LiCoVO4) cathode material has been synthesized by sol-gel method. Rietveld refinement analysis of powder X-ray diffraction pattern confirmed that the prepared LiCoVO4 crystalline sample had a cubic structure and showed no evidence of secondary phase peaks. FESEM and TEM images of LiCoVO4 identified that the particle ranged from 1 mu m to 200 nm. The XPS results showed that the oxidation states of cobalt and vanadium was +3 and +5, respectively. The conductivity is found to be 1.16 x 10(-5) S cm(-1) at 60 degrees C. The variation of sigma(DC) with temperature indicates that electrical conduction in the material is a thermally activated process. Cyclic voltammetry (CV) studies performed on the synthesized LiCoVO4 cathode revealed the reversibility and structural stability during cycling. Crown Copyright (C) 2012 Published by Elsevier B.V. All rights reserved.