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The Cu/Ni, Ni/Cu and Cu/Ni/Si film/substrate and film/film/substrate systems were prepared by magnetron sputtering method to investigate the surface segregation. The chemical composition of film was analyzed by Auger Electron Spectroscopy (AES). The microtopographies of the Cu/Ni surface and the cross section of the film were observed by Transmission Electron Microscope (TEM), where the blocky distribution of Ni-rich area on surface of Cu film and columnar grains was observed in the specimen. It is found that the thickness of sputtered film has stronger effect on the composition of segregation layer near the surface than that of the annealing time. The surface segregation could be ascribed to the fast vertical diffusion of the substrate atoms through the columnar grain boundaries and the subsequent lateral surface diffusion.

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