In this work electrodeposited Ni-Cu/Cu metallic multilayered films with different thicknesses of Ni and Cu were prepared on (100) polycrystalline Cu substrates. The nanostructure of the multilayers was studied using XRD. The existence of satellite peaks in the XRD patterns showed that the multilayered films have superlattice structures. The difference between the intensity of ML(200) and ML(111) peaks showed that the multilayers have a strong texture of (100) as their substrate structures which confirms the epitaxial growth. The morphology of the films was studied by SEM. The SEM images showed that the surface of the films is rough. The samples were also analyzed using EDX and the results showed that the real content of Ni is less than its nominal content this refers to the current efficiency which is less than unity due to hydrogen evolution. In the second stage of the work some identical samples which have the highest order of satellite peaks were electrodeposited. The samples were annealed at different temperatures and times. Their structures were then studied by XRD. The XRD patterns of the annealed samples showed that if the temperature and time of annealing increase, the satellite peaks begin to disappear. It means by increasing these two parameters, the sharpness of the bilayer interface decreases and the multilayered structure tends to become alloy structure. The morphology of the samples was also studied by SEM. The SEM images showed that the surface of the annealed films becomes approximately uniform due to the diffusion of Ni and Cu atoms to Cu and Ni layers, respectively.


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