The low-heating solid-state method has been adopted to synthesize LiNi 1/3 Co 1/3 Mn 1/3 O 2 materials. The final product, with homogeneous phase and smooth crystals indicated by XRD and SEM results, can be synthesized at 700°C, much lower than the synthesis temperatures of co-precipitation method. The reaction process and microstructure of precursor has been investigated by IR spectrum. By comparative studies with the mixture of CH 3 COOLi and (Ni, Co, Mn)(C 2 O 4 ), it is testified that the precursor is homogeneous, rather than a mixture. The decomposition process and the reaction energy have been studied to investigate the reaction mechanism of the precursor when heated at high temperature. The as-synthesized LiNi 1/3 Co 1/3 Mn 1/3 O 2 exhibits excellent electrochemical properties, exhibiting initial specific capacity of 167mAhg −1 with stable cyclic performance.