Phospho-olivine LiFCPO4 cathode materials were prepared by hydrothermal reaction at different temperatures. The structural and morphological performance of LiFePO4 powders were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and high-resolution transmission electron microscope (HR-TEM), LiFePO4/Li batteries were characterized electrochemically by cyclic voltammetry (CV) and charge/ discharge experiments. The XRD results demonstrate that LiFePO4 powder has an orthorhombic olivine-type structure with a space group of Puma. Among the synthesized cathode materials, LiFePO4 synthesized at 170 degrees C and subsequent 500 degrees C shows the best electrochemical properties with an initial discharge capacity of 167 mAh g(-1) (98% of theoretical capacity) close to the theoretical capacity of LiFePO4 (170 mAh g(-1)) at 0.1 C rate. (c) 2007 Elsevier B.V. All rights reserved.