Ferrites with (inverse) spinel structure display a large variety of electronic and magnetic properties, making some of them interesting for potential applications in spintronics. We investigate the thermally induced interdiffusion of Ni2+ ions out of NiO into Fe3O4 ultrathin films, resulting in off-stoichiometric nickel ferrite-like thin layers. We synthesized epitaxial Fe3O4/NiO bilayers on Nb-doped SrTiO3(001) substrates by means of reactive molecular beam epitaxy. Subsequently, we performed an annealing cycle comprising three steps at temperatures of 400 °C, 600 °C, and 800 °C under an oxygen background atmosphere. We studied the changes of the chemical and electronic properties as result of each annealing step with help of hard x-ray photoelectron spectroscopy and found a rather homogeneous distribution of Ni and Fe cations throughout the entire film after the overall annealing cycle. For one sample we observed a cationic distribution close to that of the spinel ferrite NiFe2O4. Further evidence comes from low-energy electron diffraction patterns indicating a spinel-type structure at the surface after annealing. Site- and element-specific hysteresis loops performed by x-ray magnetic circular dichroism uncovered the antiferrimagnetic alignment between the octahedral coordinated Ni2+ and Fe3+ ions and the Fe3+ ion in tetrahedral coordination. We find a quite low coercive field of 0.02 T, indicating a rather low defect concentration within the thin ferrite films.