Subscript textThe Co3O4 nanocubes were synthesized by hydrothermal process. The products are characterized in detail by multiform techniques: scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and energy-dispersive X-ray analysis. The results show that the products are uniform nanocubes with an average crystallite size about 20-40 nm. Electrocatalytic property of the prepared Co3O4 nanocubes was characterized by linear sweep voltammetry. LSV results indicate that Co3O4 nanocubes exhibit a remarkable electrocatalytic activity for the H2O2 reduction.