In the present work, an elemental powder mixture of Al60Fe20Ti15Ni5 (at.%) was mechanically alloyed in a high-energy ball mill. The phase transformations occurring in the material during milling were studied with the use of X-ray diffraction. The results obtained show that an amorphous phase was formed during performed mechanical alloying process. Thermal behaviour of the milling product was examined by differential scanning calorimetry. It was found that amorphous phase crystallised above 540 °C when a heating rate of 40 °C/min was applied. On the basis of X-ray diffraction results, crystallisation product was identified as a cubic phase with the lattice parameter a0 = 11.856 Å, isomorphic with the 2 (Al2FeTi, fcc structure D8a) phase. The mean crystallite size of the crystallised 2 phase was 19 nm.