A rapidly solidified Al-2.5Ti-2.5Fe-2.5Cr (mass fraction in %) alloy was prepared by melt spinning. Asquenched and as-annealed microstructures were studied by X-ray diffractometry (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HREM) and energy dispersive spectrum (EDS) analysis.The microhardness of the alloy at different annealing temperatures was measured. The results obtained indicate that the microhardness of the rapidly solidified Al-2.5Ti-2.5Fe-2.5Cr alloy does not vary with different annealing temperatures.The as-quenched microstructure of the alloy includes two kinds of dispersed primary phases: Al3Ti and Al13(Cr, Fe)2. After annealing at 400 ℃ for 10 h, the stable phase Al13Fe4 appears in the microstructure.