CuV2O6 is a very promising cathode material for rechargeable lithium batteries. By a soft chemistry method, CuV2O6 is successfully synthesized from V2O5 hydrogel and Cu2O powder. CuV2O6 with different degrees of crystallinity are obtained by heating CuV2O6 precursor at various temperatures. XRD, TG-DTA, TEM and SEM experiments are conducted to characterize its physical properties, and the electrochemical properties have been investigated by galvanostatic charge-discharge experiments. As a result, CuV2O6 annealed at 550 degrees C has smaller crystal lattice constants and better electrochemical properties compared to the sample synthesized by the conventional solid-state method. (c) 2006 Published by Elsevier B.V.