Bulk Al materials with average grain sizes of 0.47 and 2.4µm, were fabricated by quasi-isostatic forging consolidation of two types of Al powders with average particle sizes of 1.3 and 8.9μm, respectively. By utilizing the native amorphous Al2O3 (am-Al2O3) film on the Al powders surfaces, a continuous, ∼7nm thick, am-Al2O3 network was formed in situ in the Al specimens. Systematic investigation of the changes to the am-Al2O3 network embedded in the Al matrix upon heating and annealing up to 600°C was performed by transmission electron microscopy (TEM). At the same time, the stability of the Al grain structure was studied by transmission Kikuchi diffraction (TKD), electron back-scatter diffraction (EBSD), and TEM. The am-Al2O3 network remained stable after annealing at 400°C for 24h. In-situ TEM studies revealed that at temperatures ≥450°C, phase transformation of the am-Al2O3 network to crystalline γ-Al2O3 particles occurred. After annealing at 600°C for 24h the transformation was completed, whereby only nanometric γ-Al2O3 particles with an average size of 28nm resided on the high angle grain boundaries of Al. Due to the pinning effect of γ-Al2O3, the Al grain and subgrain structures remained unchanged during annealing up to 600°C for 24h. The effect of the am-Al2O3→γ-Al2O3 transformation on the mechanical properties of ultrafine- and fine-grained Al is discussed from the standpoint of the underlying mechanisms.
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