Pure LiFePO4 was synthesized by heating an amorphous LiFePO4. The amorphous LiFePO4 obtained through lithiation of FePO4·xH2O by using oxalic acid as a novel reducing agent at room temperature. FePO4·xH2O was prepared through co-precipitation by employing FeSO4·7H2O and H3PO4 as raw materials. X-ray diffraction (XRD), scanning electron microscopy (SEM) observations showed that LiFePO4 composites with fine particle sizes between 100nm and 200nm, and with homogenous sizes distribution. The electrochemical performance of LiFePO4 powder synthesized at 500°C were evaluated using coin cells by galvanostatic charge/discharge. The synthesized LiFePO4 composites showed a high electrochemical capacity of 166mAhg−1 at the 0.1C rate, and possessed a favorable capacity cycling maintenance at the 0.1C, 0.2C, 0.5C and 1C rate.