A series of Ni-Co oxide nano-composites were prepared by thermal decomposition of the precursors obtained via coordination homogeneous co-precipitation method. Thermogravimetric analysis (TGA), powder X-ray diffraction (XRD), and transition electron microscopy (TEM) tests were applied to investigate the thermal behavior, crystalline. and morphology of the Ni-Co oxide composites. The electrochemical properties of Ni-Co oxide electrodes were evaluated by cyclic voltammetry, galvanostatic charge-discharge, and electrochemical impedance measurements. Results showed that the calcination temperature had great effect on morphology and specific capacitance of product. The effect of the molar ratios of Ni2+/Co2+ in the reaction system on the electrochemical properties of Ni-Co oxide electrodes was also discussed.