Nickel oxide（NiO）as a semiconductor using as active catalysts for electrochemical CH4 activation at room temperature has attracted considerable attention. In this study, series of NiO with diverse morphologies including nanoparticle(NP),nanoflower(NF),nanoslice(NS) have been successfully synthesized to inquire their electrocatalysic performance in CH4 oxidation. Physicochemical properties of these materials were characterized by several techniques, like BET,XRD,TEM,CV,LSV,EIS. The NF and NS of samples possess much better low-temperature reducibility and higher CH4 conversion comparing with other samples. This proposal of low temperature electrochemical oxidation of methane may provide a method for the complex organic compounds of carbon and syngas.