Ni3Fe powder has been obtained by high energy ball milling from elemental powders. We used two extreme conditions for milling: “friction mode” – friction between powder and ball/vial– and “shock mode” – direct impact of ball to powders. The influence of milling mode - friction and shock – was investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). It was observed that the Ni3Fe grain size obtained by “friction mode” after 30 hours of milling was around 10 nm. For “shock mode” milling the average grain sizes was around 17 nm after 20 hours. The grain size was calculated using Williamson-Hall formula for both, “shock mode” and “friction mode” of milled powders and Scherrer formula for annealed powders. The powders were subjected to an annealing (30 min. at 350 °C) in order to eliminate the internal stress accumulated to the milling process and to finish the Ni3Fe phase formation.