In this paper we have shown the feasibility of ion beam assisted deposition to produce iron–nickel nitride thin films of various compositions. We have carried out their compositional and structural characterization by means of Rutherford backscattering spectroscopy (RBS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and integral conversion electron Mössbauer spectroscopy (ICEMS). The results have shown that Ni is incorporated within the films and that the temperature of the substrate has a large influence both in the phase composition obtained as well as in the degree of crystallinity of the thin films produced.