Composite LiFePO4/C cathode materials were prepared with a novel solution method followed by heat-treating at various temperatures. The compositions, crystalline structure, and morphology of the prepared powders were investigated with AA, EA, XRD, SEM, and EPMA. The electrochemical properties as cathode material for lithium batteries were studied by capacity retention study. Among the prepared composite cathode materials, the sample heat-treated at 700°C for 12h shows better cycling performance than those of others. It shows initial specific discharge capacities of 165 and 130mAhg−1 at 30°C with C rates of C/10 and 1C, respectively.