A chemical precipitation-thermal decomposition method was developed to synthesize Co3O4 nanoparticles using cobalt liquor obtained from the atmospheric pressure acid leaching process of nickel laterite ores. The effects of the precursor reaction temperature, the concentration of Co2+, and the calcination temperature on the specific surface area, morphology, and the electrochemical behavior of the obtained Co3O4 particles were investigated. The precursor basic cobaltous carbonate and cobaltosic oxide products were characterized and analyzed by Fourier transform infrared spectroscopy, thermogravimetric differential thermal analysis, X-ray diffraction, field-emission scanning electron microscopy, specific surface area analysis, and electrochemical analysis. The results indicate that the specific surface area of the Co3O4 particles with a diameter of 30 nm, which were obtained under the optimum conditions of a precursor reaction temperature of 30A degrees C, 0.25 mol/L Co2+, and a calcination temperature of 350A degrees C, was 48.89 m(2)/g. Electrodes fabricated using Co3O4 nanoparticles exhibited good electrochemical properties, with a specific capacitance of 216.3 F/g at a scan rate of 100 mV/s.