Mechanically alloyed Fe 100−x Al x powders, with 20≤x≤90, have been studied by X-ray diffraction and room temperature 57 Fe Mössbauer spectroscopy. The milling time was chosen such that complete alloying does not take place. For a fixed milling time of 10 h, the rate of alloying was seen to increase exponentially with increase in Fe content. Mössbauer spectra of all the samples consist of a broad magnetic sextet and a quadrupole doublet. The isomer shifts and quadrupole splitting of the doublets are typical of Al-rich, Fe-Al alloys. The area under the quadrupole doublet is a maximum for x=66. Analysis of the Mössbauer spectra indicates the formation off-stoichiometric Fe 3 Al phase for x<66, while the formation of Fe clusters is largely responsible for the magnetic hyperfine component in x≥66 compositions.