In this work, the Ni/Co/Si system was annealed at temperatures ranging from 300 °C to 800 °C. The samples were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, Rutherford backscattering spectroscopy (RBS), atomic force microscopy (AFM) and sheet resistance measurement. The XRD and Raman spectroscopy results showed that the formation of nickel and cobalt silicides (CoSi, Co2Si, Ni2Si, NiSi, NiSi2, CoSi2) is an annealing temperature dependent diffusion process. The diffusion phenomenon was evidenced by RBS. The low values of the sheet resistance which were correlated with the films surface roughness were attributed to the formation of both CoSi and NiSi phases.