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Alloy films of Ni-Co and Ni-Cr of compositional ratios 1:1, 1:3, and 3:1 deposited by vapor deposition were studied by Transmission Electron Microscopy (TEM) and X-Ray Diffraction (XRD). Results of TEM analysis on the Ni-Co alloy films indicated that the films were face-centered cubic (fee) in structure. XRD results confirmed the TEM observations. TEM analysis of Ni-Cr alloy films showed that the films were bodycentered cubic (bec) in structure. With increase in the Cr content more than 25%, the material contained a higher fraction of an amorphous phase. XRD studies provide limited information owing to the quasi-amorphous structure of the films of high Cr content.