This book describes the experimental details of the electrochemical process for the synthesis of Ni nanoparticles. We have used commercially available metal foils for the synthesis of Ni, nanoparticles respectively. The variation in the particles size with respect to stabilizers has also studied. The Ni nanoparticles thus obtained were characterized by UV-Visible Spectroscopy, FTIR, SEM, EDS, TEM, FE-SEM and HR-TEM.Here, we present nanostructured particles of NiO have been successfully synthesized by electrochemical reduction method using TBAB as capping agent at 16mA/cm2. The NiNPs were crystalline in nature and the average crystallite size was found to be 18.22 nm and 21.96 nm respectively. SEM confirms that the particles are in nano size and the appearances of particles are in irregular polygonal and spherical in shape. FE-SEM clearly indicates that particles are spherical and bucky ball like shape.TEM and FE-TEM confirms the cubic structure of synthesized nickel nanoparticles. From TEM images the Ni nanoparticles average size obtained was 22nm and 50nm. In NiO nanoparticles, inter planner spacing from SEAD pattern was in good agreement with XRD pattern.