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The thickness-dependent optical properties of nickel metal and nickel monosilicide (NiSi) thin films, used for self-aligned silicidation process, were characterized using spectroscopic ellipsometry. The thickness-dependent complex dielectric function of nickel metal films is shown to be correlated with the change in Drude free electron relaxation time. The change in relaxation time can be traced to the change in grain boundary (GB) reflection coefficient and grain size. A resistivity based model was used as the complementary method to the thickness-dependent optical model to trace the change in GB reflection coefficient and grain size. After silicidation, the complex dielectric function of NiSi films exhibit non-Drude behavior due to superimposition of interband absorptions arising at lower frequencies. The Optical models of the complete film stack were refined using x-ray photoelectron spectroscopy, Rutherford backscattered spectroscopy, and x-ray reflectivity (XRR).