Abstract: The mechanism of electrodeposition of Cu/Ni multilayer thin films from citrate salt electrolyte has been studied by means of potentodynamic sweep, cyclic voltammetry sweep and AC impendence.The results indicated that the copper deposition is mass transfer controlled process and nickel deposition is related to the absorbed intermediate species such as Ni(OH)_ads. The nickel ions first form Ni(OH)_ads,then was deoxygenated to nickel on the electrode surface.