Spherical C/LiFePO4 cathode materials were successfully prepared by spray pyrolysis. The saccharides such as monosaccharide and disaccharide or organic acid were used as carbon source. SEM observation showed that they had spherical morphology with particle size of about 1m. XRD analysis revealed that the olivine phase was obtained by heating at 700 °C under the atmosphere of argon/hydrogen (5 %). Electrochemical measurement revealed that the rechargeable capacity of LiFePO4 was significantly improved by the addition of carbon. The use of sucrose was most effective for the high rechargeable capacity and cycle stability.