The ribbon of Al 85 Y 4Nd 4Ni 7 amorphous alloy was prepared by rapid solidification in melt-spinning. The alloy obtained was analyzed by means of DSC and X-ray diffractometry （XRD） as well as the micro-hardness measurement （Hv）. The results showed that the amorphous crystal and supersaturated α-Al phase coexisted in the chilled alloy. The amorphous crystal transformed into nano-Al crystal and ternary metastable AlNiY and AlNdNi during annealing at 310 ℃. The metastable phases partially transformed into binary equilibrium phases Al 3Ni and Al 3Nd duringr annealing at 340 ℃ and 400 ℃. The micro-hardness values of the alloy were almost the same during annealing at 310 ℃ and 340 ℃

which were much higher than that of the alloy in chilled state

while decreased dramatically during annealing at 400 ℃

owing to the growth of the crystal.