Abstract: The powder mixture of Al, Ti and graphite has been mechanically alloyed in a planetary ball mill.The structural evolution of as-milled powder sample has been characterized by XRD, DTA. The results show that the amorphous phase is formed first at an early milling stage, then crystallization occurs during further milling, leading to formation of a nanocrystalline fcc metastable phase. In contrast, during annealing the amorphous phase is crystallized to the equilibrium phase instead of the fcc phase. This indicates that crystallization during ball milling is different from that induced by annealing