Ni foam supporting-NiCo 2 O 4 nanosheet arrays (NiCo 2 O 4 /Ni foam) are successfully prepared by electrodeposition of the hydroxide precursor, followed by a thermal treatment in air without any template and surfactant. The morphology of NiCo 2 O 4 nanosheet arrays is characterized by scanning electron microscope and transmission electron microscopy. The structure is analyzed using X-ray diffractometer, X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy.