Abstract Ni-Fe-TiO2 ccomposite coating was deposited potentiostatically on the rotating disk electrode by adding inert particle TiO2 into Ni-Fe plating bath. We study the variations Ni,Fe and TiO2 within coatings at different TiO2 bulk concentrations, pH values and disk rotation speeds. Generally,the surface charge of the particle in the plating solution affectsthe plating process. We studied the zeta potential of the particles in various plating solutions using Zeta Meter. To obtain significant amount of TiO2 within the deposite and improve the stability of the composite coating,we add the promoting agent-Tl2SO4 into thesolution. It was found that the partial current densities of Ni,Fe are increased whenadding a slight amount of TiO2. However the current densities of Ni,Fe are inhibited when adding large amounts of TiO2. Content of TiO2 in the deposit is higher when the disk rotation is decreased.The partial current densities of Ni,Fe are increased at a higher solution pH value,but the TiO2 content is decreased. The TiO2 content is increased significantly by adding Tl+ to the platingsolution.The deposited rate of Fe is inhibited while Ni is enhanced at the adding of Tl+. The surface morphology of composite coating was studied by scaning electronmicrograph.