Nanostructures made of Co metal and Fe-Co-Ni alloys were successfully prepared by means of cyclic voltammetry (CV) and pulse-reverse (PR) plating techniques in simple chloride deposition solutions. Cobalt nanoparticles without whiskers or nanowires could be prepared by using CV plating without the anodic dissolution process under a scan rate of 50 mV/s. The diameter of each Co nanoparticle decreased as the scan rate of CV plating increased. The Co nanoparticles were found to homogeneously disperse on the electrode surface when a pre-deposited film composed of Co provided nucleation islands for the growth of these particles. The diameter of the Co particles ranged from 60 to 110 nm as the CV scan rate varied from 50 to 20 mV/s. The anodic dissolution process of PR and CV plating was found to be the key factor promoting the formation of Fe-Co nanowires on Fe-Co-Ni nanoparticles. The diameter of the Fe-Co-Ni nanowires varied between 20 and 40 nm, while the diameter of the Fe-Co-Ni nanoparticles varied from 110 to 130 rim. The morphologies and crystalline information of these iron-group deposits, prepared using CV and PR plating techniques, were examined through field-emission scanning, electron microscopic (FE-SEM), atomic force microscopic (AFM), and X-ray diffraction (XRD) analyses.