Submicron-sized NiV3O8 powder was prepared by solid-state reaction method. A mixture of NiO, V2O5 and home-made VO2 (B) was used as starting material. The phase purity, structures, morphologies of the prepared powders were characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and X-ray photo-electron spectrometry (XPS), respectively. The results show that the as-prepared NiV3O8 material is highly crystalline and a single phase. The charge-discharge experiments were performed to investigate the electrochemical properties of NiV3O8 powder. NiV3O8 cathode delivers an initial discharge capacity of 286.6mAhg−1 and still remains at 241mAhg−1 after 30 cycles in the voltage of 1.5–4.2V. The rate performance and EIS results indicate that the as-prepared electrode material has very good structural stability upon cycling after electrode conditioning by an initial charge and discharge.