Fe–Ni nano-particles were synthesized by mechanical alloying and subsequent low-temperature hydrogen reduction of oxide mixtures. First, single-phase nickel ferrite was mechanically synthesized for 30 h with steel balls to powder weight ratio of 20 while the milling was operated at 300 rpm. The as-milled powder was then placed in contact with hydrogen at 600 °C for 1 h. Reduction reactions resulted in production of Fe–Ni nano-particles. Phase identification, morphological and microstructural studies, chemical analysis and magnetic property determination were carried out by X-ray diffraction (XRD), scanning electron microscopy (SEM), transition electron microscopy (TEM), energy dispersive spectrometry (EDS) and vibration sample magnetometry (VSM) on the samples. Results are described in the paper.