Spherical LiMnPO4/C composite microparticles were prepared by a combination of spray pyrolysis and spray drying followed by heat treatment and examined as a cathode material for lithium batteries. The structure, morphology and electrochemical performance of the resulting spherical LiMnPO4/C microparticles were characterized by X-ray diffraction, field-emission scanning electron microscopy. transmission electronic microscopy and standard electrochemical techniques. The final sample was identified as a single phase orthorhombic structure of LiMnPO4 and spherical powders with a geometric mean diameter of 3.65 mu m and a geometric standard deviation of 1.34. The electrochemical cells contained the spherical LiMnPO4/C microparticles exhibited first discharge capacities of 112 and 130 mAh g(-1) at 0.05 degrees C at room temperature and 55 degrees C, respectively. These also showed a good rate capability up to 5 C at room temperature and 55 degrees C. (C) 2011 Elsevier Ltd. All rights reserved.