NH 2 NH 2 ·H 2 O which was used as controlling agent was applied to prepare the precursor Ni 1/3 Co 1/3 Mn 1/3 (OH) 2 in the hydroxide co-precipitation method. The precursor was used to synthesize LiNi 1/3 Co 1/3 Mn 1/3 O 2 . The samples were characterized by XRD, XPS and SEM. It has been found that sintered sample at 800°C for 16h is considered as the optimal synthetic condition. The LiNi 1/3 Co 1/3 Mn 1/3 O 2 was used as positive electrode and the activated carbon as negative electrode of the asymmetric supercapacitor. The electrochemical capacitance performance was tested by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge/discharge. The results indicate that species of aqueous electrolyte, current density, scan rate and potential limit, etc. have influence on the capacitance property of AC/LiNi 1/3 Co 1/3 Mn 1/3 O 2 supercapacitor. The initial discharge specific capacitance of 298Fg −1 was obtained in 1molL −1 Li 2 SO 4 solution within potential range 0–1.4V at the current density of 100mAg −1 and was cut down less than 0.058Fg −1 per cycling period in 1000 cycles. The asymmetric supercapacitor exhibited a good cycling performance.