In the present work the effect of the ball to powder relation (BPR) and the different milling media, for the initial stages of milling from 15 min to 5 tl, was studied for elemental powders of Fe- 27 at % Al. Long time milling periods were also carried out in order to obtain nanophase particles and further sintering was performed for the samples mechanically alloyed (MA) during 5 h and 50 h. The evolution of the phases formed, for the different stages of milling was followed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Mossbauer spectroscopy. The formation of the alloy was found to be more effective for BPR 8:1, in which case the complete formation of the alloy was achieved after 3 h of milling. Nanophases with particle size of 7 nm were obtained after 50 h of milling. The alpha -Fe solid solution was also obtained by sintering at the different temperatures.