Metal alloys has been extensively studied to light upon applications where differentiated physical and chemical properties are required. In this context, its value highlighting the alloys for the coating of metallic substrates with the objective of protecting the substrate in corrosive environments. The present work proposes to approach a method of synthesis of Cu-Ni alloys in copper substrates through the thermal decomposition of nickel nitrate and subsequently to discount the NiO oxide formed by reduction with H2 at 350 degrees Celsius and heat treatment in the same atmosphere at 800 degrees Celsius with (3, 4 and 5h) to stimulate the diffusion of the nickel produced inside the Cu matrix. The films were then characterized by scanning electron microscopy (SEM) in both cross-sectional and panoramic sessions, in addition to X-ray diffraction (XRD) with low incidence, aiming to identify Cu-Ni alloy produced. The results suggest that the proposed process was successful, allowing a wide coating of the substrate and subsequent diffusion of Ni produced, which allowed the identification in all samples of the alloy of interest. Selected samples will be used in the future for microhardness tests, as well as for electro-corrosion, and the measured behavior is compared to that observed for pure substrate. The presence of the coating is expected to raise the abrasion resistance as well as to hinder the corrosion of the copper present.