The materials of Ni nanoparticles/carbon nanofibers (Ni NPs/CNFs) and carbon nanofibers (CNFs) were prepared by electrospinning the Ni doped precursor solutions. The Ni doped nanofibers with the diameter of 200-300 nm possess the uniform morphology and smooth surface. These nanofibers were carbonized at 600 degrees C for 2 h. The Ni NPs/CNFs composite was characterized with SEM (scanning electro microscope), XRD (X-ray diffraction) and FT-IR (Infrared spectroscopy). The Ni NPs/CNFs electrode was investigated through the cyclic voltammetry measurement. The average specific capacity was calculated to be 113 F.g(-1) at the scan rate of 2 mV.s(-1). The high specific capacity was larger than the CNFs owing to the Ni NPs. The specific capacity retention also maintains 72% after 5 cycles, suggesting that the electrode possess good reversibility. The Ni NPs/CNFs composite material with excellent electrochemical properties will be a promising material which can be used for energy storage.