CuV2O6 was prepared by a precipitation method followed by heat treatment at 600 C. The material showed an initial discharge capacity of 379 mAh g(-1), which decreased to 160 mAh g(-1) after 30 cycles. X-ray diffraction showed an irreversible structural change of the material from crystalline to amorphous phase after the first cycle. Contrarily, Raman scattering showed the reversible change of the material's local structure in the first cycle. Further, Raman scattering confirmed the gradual increase of irreversible LixCuV(2)O(6) phase in the cathode material, which was responsible for the poor cycling performance of CuV2O6. (c) 2006 The Electrochemical Society.