Mechanical milling of a mixture of pure iron and chromium powders with a nominal composition of 28 at. % of Fe and 72 at. % of Cr was performed using two kinds of tools. The alloying process was followed by X ray diffraction and57Fe Mössbauer spectroscopy. The room temperature Mössbauer spectra revealed the formation of a broad single line at the expense of the area of α-Fe sextet. At 4.2 °K most of the singlet still remains unsplit. This behavior may be due to some metastable structure induced by the preparation method. © 1991 J.C. Baltzer A.G., Scientific Publishing Company.