Using oxalic acid and stoichiometrically mixed solution of NiCl 2 , CoCl 2 , and MnCl 2 as starting materials, the triple oxalate precursor of nickel, cobalt, and manganese was synthesized by liquid-phase co-precipitation method. And then the LiNi 1/3 Co 1/3 Mn 1/3 O 2 cathode materials for Li-ion battery were prepared from the precursor and LiOH·H 2 O by solid-state reaction. The precursor and LiNi 1/3 Co 1/3 Mn 1/3 O 2 were characterized by chemical analysis, XRD, EDX, SEM and TG-DTA. The results show that the composition of precursor is Ni 1/3 Co 1/3 Mn 1/3 C 2 O 4 ·2H 2 O. The product LiNi 1/3 Co 1/3 Mn 1/3 O 2 , in which nickel, cobalt and manganese are uniformly distributed, is well crystallized with a-NaFeO 2 layered structure. Sintering temperature has a remarkable influence on the electrochemical performance of obtained samples. LiNi 1/3 Co 1/3 Mn 1/3 O 2 synthesized at 900 °C has the best electrochemical properties. At 0.1C rate, its first specific discharge capacity is 159.7 mA·h/g in the voltage range of 2.75–4.30 V and 196.9 mA·h/g in the voltage range of 2.75–4.50 V; at 2C rate, its specific discharge capacity is 121.8 mA·h/g and still 119.7 mA·h/g after 40 cycles. The capacity retention ratio is 98.27%.