Ingots of alloys Al-Cu-Fe were obtained by casting in a graphite mold. Mechanical milling of alloy particles in the as-cast state and after homogenization annealing was carried out in planetary ball mill Retsch PM400 in an argon atmosphere. As a result of mechanical milling granules with an average size of 35-40 μm and fine internal microstructure are formed. The size of coherent scattering regions in quasicrystalline phase after mechanical milling was about 10-15 nm. Mechanical milling after homogenization heat treatment allows much refines the quasicrystalline phase than in the case of mechanical milling of cast alloy.