Three amorphous alloy powders in the Ti‐Fe system with the ratios of Ti:Fe at 1:2, 1:1, and 2:1 were prepared by mechanical alloying of the elemental powders in a high‐energy ball mill. The amorphous powders were characterized by x‐ray diffraction and high‐resolution transmission electron microscopy. A complete amorphization of Ti1Fe1was achieved, whereas a remaining crystalline portion besides the amorphous phase was present in Ti2Fe1and Ti1Fe2. The crystallization temperatures for these alloys detected by differential scanning calorimetry varied from 714 to 791 K, which were corresponding to half of their melting points.