The effect of reaction temperature on the particles properties such as morphology and particle size are investigated in detail during the preparation of ultra-fine nickel powder by chemical vapor deposition (CVD), which takes NiCl2·6H2O as raw materials. Morphology, size and phase of the prepared samples are characterized by scanning electron microscope (SEM), Laser particle analysis and X-ray diffraction (XRD). The results indicate that reaction temperature has profound impact on the crystallinity and size distribution of particles. The obtained powders are pure nickel with spherical-like morphology, submiron size and high crystallinity.