An Al-3% Mg solid solution alloy was subjected to intense plastic deformation, using either equal-channel angular (ECA) pressing or torsion straining, to produce grain sizes in the submicrometer range. Static annealing at elevated temperatures led to grain growth and average grain sizes of up to > 100 μm. As-fabricated and statically annealed specimens were used to determine the variation in microhardness with grain size, and results confirm that the Hall-Petch relationship persists down to at least the finest grain size examined experimentally (~90 nm). The results provide no evidence to support the claims of a negative Hall-Petch slope when the average grain size is very small, but there is evidence of a decrease in the slope of the Hall-Petch plot at the very finest grain sizes (< 150 nm); this is attributed to the increased participation of mobile extrinsic dislocations in the boundary regions when taking the hardness measurements.
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