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57Fe Mössbauer spectroscopy and X-ray diffraction are used to study in detail the mechanism of mechanical alloying in a planetary ball mill of the Fe-Cr nanocrystalline system in the concentration range from 20 to 48 at.% Cr. It is established that mechanical alloying proceeds in one stage at a concentration of up to 30 at.% Cr and in three stages at higher concentrations. The change in the mechanical alloying mechanism occurs as iron is saturated with chromium and is caused by the inversion of the mixing energy sign from negative to positive.