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MSssbauer spectroscopy, X-ray diffraction, Auger spectroscopy, secondary ion massspectrometry and chemical analysis were used to study mechanical alloying of Fe and Mg powder mixture with the atomic ratio of 93:7. It has been shown that the process of mechanical alloying involves the formation of nanostructure in a-Fe particles, penetration and segregation of Mg atoms along the a-Fe grain boundaries, formation of the a-Fe(Mg) supersaturated solid solution.PACS: 76.80.+y