NiO/Ni nanocomposites were prepared by chemically reduction-oxidation process in tetra-ethylene glycol (TEG) solution. The structure and morphology of the samples were examined by XRD and SEM. The results indicated the composite consisted of NiO and Ni and exhibited spherical morphology with diameter of 50-200 nm. The electrochemical performances of composite electrodes used in electrochemical capacitors were studied. The electrochemical measurements were carried out using cyclic voltammetry, galvanostatic charge/discharge and impedance spectroscopy in 6M KOH aqueous electrolyte using three-electrode Swagelok systems. The results showed that the composite had a high specific capacitance and excellent capacitive behavior. The specific capacitance of the composite decreased to 192F/g after 500 cycles. Due to the existance of Ni, the charge transfer resistance is lower than 1Ω. It revealed that the composite exhibited good cycling performance.