Spherical C/LiMn1-XMXPO4 (M=Mg, Zn) cathode materials were successfully prepared by spray pyrolysis. An olivine structure was obtained by heating at 973 K under argon/hydrogen (5%) atmosphere. Citric acid was used as the carbon source. Scanning electron microscopy (SEM) showed that the materials had spherical morphology. The electrochemical properties of the cathode were also estimated by the rechargeable capacity and cycle performance. The first discharge capacity of C/LiMn1-XZnXPO4 (X = 0.1) was approximately 60 mAh/g at 0.1 C.