Elemental mixtures of Al, Cu, Fe powders with the nominal composition of Al 70 Cu 20 Fe 10 were mechanically alloyed in a planetary ball mill for 80 h. Subsequent annealing of the as-milled powders were performed at 600-800 • C temperature range for 4 h. Structural characteristics of the mechanically alloyed Al 70 Cu 20 Fe 10 powders with the milling time and the heat treatment were investigated by X-ray diffraction (XRD), differential scanning calorimeter (DSC) and differential thermal analysis (DTA). Mechanical alloying of the Al 70 Cu 20 Fe 10 did not result in the formation of icosahedral quasicrystalline phase (i-phase) and a long time milling resulted in the formation of β-Al(Cu,Fe) solid solution phase (β-phase). The i-phase was observed only for short-time milled powders after heat treatment above 600 • C. The β-phase was one of the major phases in the Al 70 Cu 20 Fe 10 alloy. The w-Al 7 Cu 2 Fe 1 phase (w-phase) was obtained only after heat treatment of the short-time milled and unmilled samples. The present investigation indicated that a suitable technique to obtain a large amount of quasicrystalline powders is to use a combination of short-time milling and subsequent annealing.