Elemental aluminum, titanium and iron powders with compositions of Fe 25 Al 75Àx Ti x (x ¼ 0, 3.75, 7.5, 11.25 and 15) were mechanical alloyed in a planetary ball mill. The transformations and thermal stabilities of milled powders were characterized by X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Supersaturated solid solutions were found in low Ti concentration (x = 0-7.5). The addition of Ti shortened the milling time for the formation of solid solution. The amorphous phases were obtained with high Ti concentration (x ¼ 11:25 and 15). The activation enthalpies of crystallization for amorphous phases increased with Ti. The crystallization temperatures of amorphous alloys were calculated, which are in good agreement with the experimental values.