A series of nano-crystalline Ni/NiO particles was synthesized by a combustion route depending upon the glycine-nitrate process. The as prepared samples were characterized by X-ray diffraction (XRD), scanning electron micrograph (SEM), transmission electron micrograph (TEM), nitrogen adsorption isothems at 77 K and vibrating sample magnetometer (VSM) techniques. The XRD results revealed that the Ni powder crystallizes was formed with the cubic phase when the molar ratio of glycine to nitrate is 1.5. Above or below that molar ratio, NiO phase coexists as an impurity along with the Ni phase. The SEM and TEM measurements of the as synthesized powders showed that the particles are irregular in shapes and have porous morphology. Increasing the ratio between glycine and Ni-nitrate resulted in slightly agglomeration and grain growth of nano-particles with subsequent decrease in the value of surface area depending upon high combustion heat. The magnetization value of Ni measured at room temperature is very close to the value observed for commercial Ni powder. (C) 2011 Elsevier B.V. All rights reserved.