In order to get homogeneous layered oxide Li[Ni1/3Mn1/3Co1/3]O2 as a lithium insertion positive electrode material, we applied carbonate co-precipitation. The oxide compounds were synthesized under different annealing temperature. XRD experiment revealed that the layered Li[Ni1/3Mn1/3Co1/3]O2 material can be synthesized at lower temperature of 750°C, and the oxidation state of Ni, Mn and Co in the cathode confirmed by XPS were 2+, 4+ and 3+, respectively. SEM observation shows that the synthesized materials have spherical particle morphology and the morphology could be controlled by carbonate co-precipitation method. The cathode synthesized at 800°C showed small irreversible capacity loss of 10.72% and high discharge capacity of 186.7mAhg−1 as well as stable cycling performance in the voltage range 2.8–4.5 V Li / L i + . In spite of difference in specific surface area, rate capability of the samples synthesized in the temperature range 750–900°C showed similar rate capability and all these cathodes delivered high discharge capacity of over than 143mAhg−1 at 2.5C (450mAg−1).