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In the present investigation, the synthesis of nanocrystalline Zn-22 pct Al by ball milling was studied. The microstructural evolution during cryomilling and subsequent annealing was characterized using transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction (XRD). Observations made during the cryomilling of the alloy reveal three findings. First, minimum average grain sizes of about 33 nm for the Al phase and 41 nm for the Zn phase are reached as cryomilling time increases to 16 hours. Second, the morphology of the powders changes from spherical (as-sprayed) to flaky (milled 8 hours) and then back to spherical again (milled 16 hours). Third, the microstructure transforms from two-phase coarse structure (0.8 m, as-sprayed) to bimodal structure (milled 8 hours) and then to a uniform fine-grained structure (milled 16 hours). The minimum grain size characterized by the peak broadening of the XRD patterns is much larger than that reported in previous work on Al and Zn but agrees well with those predicted from the approximate linear relationship between the minimum grain size and the critical equilibrium distance between two edge dislocations in a pileup. The mechanism of grain size refinement is discussed at three different levels: macroscopic level (individual powders), mesoscopic level (individual small fragments), and microscopic level (individual grains). The excellent thermal stability of the milled powders during subsequent annealing has been attributed to three factors: the nature of the eutectoid structure, grain-boundary pining by dispersions, and microporosity in the particles.

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