Spherical Li[Li0.2Ni0.2Mn0.6]O-2 has been synthesized by a carbonate co-precipitation method. The Li[Li0.2Ni0.2Mn0.6]O-2 with a phase-pure and well-ordered layered structure was synthesized by heat-treatment of a spherical (Ni0.25Mn0.75)(3)O-4 precursor with (LiOHH2O)-H-.. The average particle size of the Li[Li0.2Ni0.2Mn0.6]O-2 powders was approximately 20 mu m and the size distribution was quite narrow due to the homogeneity of the (Ni0.25Mn0.75)CO3. The Li[Li0.2Ni0.2Mn0.6]O-2 electrode calcined at 900 degrees C delivered an initial discharge capacity of approximately 270 mAh g(-1) in the voltage range of 2.0-4.6 V The differential scanning calorimetry (DSC) results for the Li[Li0.2Ni0.2Mn0.6]O-2 prepared at 900 degrees C showed a major exothermic reaction at 270 degrees C. (c) 2006 Elsevier B.V. All rights reserved.