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Electrodeposition is being investigated as a novel and low-cost method to prepare magneto-optic thin film and nanostructured materials. This deposition method allows precise control over thin-film properties and permits deposition of novel magnetic geometries. Multilayers and alloys can be deposited and controlled by adjusting deposition potentials and ion concentrations in the bath. Nickel/cobalt alloys have been electrodeposited from sulfamate, sulfate, and chloride solutions onto Au substrates. The optical properties were monitored in situ with a real-time spectroscopic ellipsometer measuring simultaneously at 44 wavelengths in the 410–750 nm spectral range. In situ measurements have the advantage of determining the material microstructural properties (thickness, density, and roughness) before the films are oxidized in the air ambient. Ex situ variable angle spectroscopic ellipsometry measurements were taken over the spectral range from 205 to 1000 nm.