Invar 36 (Fe64Ni36) nanocrystalline powders were successfully obtained by the mechanical alloying process. The mechanically alloyed Invar 36 powders were obtained from both, Fe–Ni elemental and Fe–Ni3Fe prealloyed powders. XRD, DSC and magnetic measurements were used to characterise the Invar 36 powders. The lattice parameter evolution versus temperature of Invar 36 powders was investigated by in-situ high-temperature X-ray diffraction (HT-XRD). For both, Invar 36 (Fe, Ni) and Invar 36 (Fe, Ni3Fe) powders, the lattice parameter values are constant up to about 350°C. The magnetic measurement also indicated that the Invar 36-type alloys are formed after 16 h of milling.
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