Electroactive lithium vanadyl phosphate, beta-LiVOPO4, was synthesized via a sol-gel route, and beta-LiVOPO4/RuO2 composite was subsequently prepared by heating RuCl3 in the network of beta-LiVOPO4 particles. X-ray diffraction patterns showed that beta-LiVOPO4 has an orthorhombic structure with space group of Pnma. Energy dispersive X-ray spectroscopy dot mappings revealed that ruthenium was homogeneously distributed among beta-LiVOPO4 particles. Compared with pristine beta-LiVOPO4, beta-LiVOPO4/RuO2 composite presented better electrochemical Li ion intercalation performances due to the enhanced electrical conductivity and Li ion diffusion. beta-LiVOPO4 may be prospective for the application to high-voltage Li ion batteries if the electrical conductivity is improved through a practical way. (C) 2008 Elsevier B.V. All rights reserved.