The synthesis of zinc and nickel alternate multilayer coatings produced by successive deposition from dual baths containing a revised zinc sulphate electrolyte and a new developed nickel bath has been investigated. Smooth and uniform zinc-nickel compositionally modulated multilayered (CMM) coatings with different multilayer configurations were obtained. The surface and cross-sectional morphologies of samples were examined using scanning electron microscopy (SEM). Cross-sectional morphology showed the layered structure of the coatings clearly. The synthesis of zinc and nickel alternate multilayer coatings produced by successive deposition from dual baths containing a revised zinc sulphate electrolyte and a newly developed nickel bath has been investigated. Smooth and uniform zinc-nickel compositionally modulated multilayered (CMM) coatings with different multilayer configurations were obtained. The surface and cross-sectional morphologies of samples were examined using scanning electron microscopy (SEM). Cross-sectional morphology showed the layered structure of the coating clearly.