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Increasing the strength of Al-based alloys is an important issue of physical metallurgy and industrial processing. Severe plastic deformation and related extension of solid solubility during mechanical alloying provide an opportunity for significant strengthening due to grain refinement, solid solution, and precipitation strengthening mechanisms. During mechanical alloying, an anomalous increase in the solid-state solubility of alloying elements occurs. The present study focuses on the investigation of the pre-milling treatment to the microstructure, phase composition, and solubility in Al-7.7 Mn-3.5 Cu (wt%) alloy processed by a high-energy ball milling of Al-14.3 Mn-6.5 Cu (wt%) master alloy diluted with Al powder. During milling, the mean granular size decreased to ~5 µm, and a strong grain refinement occurred. According to our TEM and XRD data, ball milling provided a mean grain size of 13–14 nm and a microhardness of 490–540 HV. The lattice parameter of the Al-based solid solution decreased with an increase in the milling time to 7.5–10 h, which suggested the dissolution of the alloying elements, and the lattice parameter increased at a higher milling time of 12.5–40 h, which suggested the decomposition of the solid solution. The XRD data revealed the dissolution of the Al6Mn and Al20Cu2Mn3 solidification-originated phases with a further precipitation of the Al6Mn dispersoids. Pre-milling of the master alloy entailed a significant decrease in the minimal lattice parameter value from 0.4029 nm to 0.4023 nm due to an increase in the Mn solute content from 6.2 wt% (3.3 at%) to 7.5 wt % (4.0 at%) in the studied alloy during high-energy ball milling.

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