LiFCPO4/C nanoparticles were prepared using raw Fe2O3 and Fe materials by rheological phase reaction under nitrogen atmosphere. Thermogravimetric analysis (TGA) was employed to analyze the precursor. The effect of the sintering temperature on its structure was investigated by X-ray diffraction (XRD). The chemical composition, surface morphology and valance states of the as-prepared product sintered at 700 degrees C has been characterized by X-ray photoelectron spectrometry (XPS), transmission electron microscopy (TEM). The content of carbon in LiFePO4/C was determined by the elemental analyzer. The cyclic voltammogram(CV) and the charge-discharge test are adopted to study the electrochemical performance of the LiFePO4/C prepared at 700 degrees C. The initial discharge capacity was 162.4 mAh g(-1), and the discharge capacity was 166.6 mAh g(-1) after the 30th cycle at a rate of 240 mA g(-1) in a potential range of 2.0 and 4.4 V. (C) 2008 Elsevier B.V. All rights reserved.