C–Ni thin films have been obtained by dual sputtering of graphite and nickel targets. This configuration allows the synthesis of coatings with high carbon content and an accurate control of the composition and degree of dispersion of metallic particles within the coatings. The Ni/(Ni+C) ratio within the films, as determined by XPS (X-ray photoelectron spectroscopy) analysis, varied between 5.8% and 62%. The films were investigated by using Grazing Angle X-ray Diffraction (GXRD), Raman spectroscopy and Scanning Electron Microscopy (SEM).An evolution of the coatings morphology from a poor defined columnar structure to a well defined one with the increasing relative Ni content has been noticed. Depending on the chemical composition of the films, a large distribution of the electrical resistivity values of the films has been observed. The variation of the coating resistivity is related to a change from a structure consisting of metallic particles embedded in an amorphous carbon matrix to a metallic crystalline structure.