Nanostructured nickel and cobalt deposits were obtained on Cu substrates, using electrodeposition method, with different operating conditions such as: current density id, temperature C, time min, PH, Concentration of Ni/Co c and organic additive contents in the deposition bath. The obtained coatings were characterized using X-ray diffractometr (X RD), Scanning Electron microscope (SEM) and Energy Dispersive X-ray (EDX). Results indicated the formation of nanostructured Face centered cubic (fcc) and Hexagonal close packed (hcp) This is, due to the presence of Ni, and Co in the composite, respectively. The optimum conditions results from the presence bath is of anomalies type.