The powders of pure Al, Fe, and Zr for preparing Al_(78)Fe_(20)Zr_2 were subject to a high-energy planetary ball milling. The microstructure evolution of the mixtures at the different intervals of milling was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). It was found that a nearly complete amorphization could be achieved in the mixtures after ball milling for 23 h. Further ball milling led to the crystallization of the amorphous powders. A long time ball milling, e.g., 160 h, led to a complete crystallization of the amorphous powders and the formation of Al_3Zr and Al_(13)Fe_4. The crystallization products caused by ball milling are almost the same as that produced by isothermal annealing of the amorphous powders in vacuum at 800 K for 1 h.
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