LiFePO4/C composite materials were synthesized at 700 degrees C by an in situ solid-state reaction. The effect of the sintering time on its structure, surface morphology and electrochemical performance was investigated by X-ray diffraction (XRD), field-emission scanning electron microscope (FESEM), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), Raman spectroscopy analyses, cyclic voltammogram (CV), and galvanostatically charge-discharge techniques. It was found that, all prepared materials for various sintering time show the single olivine structure. The powder morphology change is negligible with extending sintering time from 5 to 40 h. Moreover, the I-D/I-G ratio of carbon in Raman shift remains almost invariant (similar to 0.96) with the increase of sintering time. Electrochemical tests show that the discharge capacity remains at 153 mA h g(-1) with medium-rate (0.5 C), while increases from about 120 to 130 mA h g(-1) at high-rate (1 C) with increasing sintering time, and the possible reasons are discussed. The LiFePO4/C composite synthesized at 700 degrees C for 30 It demonstrates a best electrochemical performance, delivering a discharge capacity of 110 mA h g(-1) (1.5 C) after 50 cycles. (c) 2005 Elsevier B.V.. All rights reserved.