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This work presents a multi-scale microstructural characterization of aluminum alloys processed by high-pressure torsion (HPT) and cold angular rolling process (CARP) to improve their mechanical properties. Mechanical properties such as microhardness and tensile strength were correlated with microstructural features. To understand the processing-structure-property relationships, characterization methods spanning nano- to millimeter scales were used, including X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), and scanning transmission electron microscopy (STEM) EDS. TEM and STEM EDS were used to show that HPT of a Mg sheet sandwiched between Al sheets successfully produced a supersaturated solid solution (SSSS) of Mg in Al and several Al-Mg intermetallic phases, leading to significant grain refinement and increases in microhardness over pure Al. Although CARP has potential to induce the severe plastic deformation (SPD), the CARP system used in this work was not able to achieve SPD aluminum alloys. However, SEM EBSD characterization shows that CARP achieves an increase of the low-angle grain boundaries (LAGBs) and geometrically necessary dislocation (GND) density in Al-1043,which improves the mechanical properties. Moreover, a preliminary study was conducted on CAPR processed Al-6061 alloys to understand the synergistic effects precipitation and CARP-processing on the microstructure and properties. This research provides the critical insights into the capabilities and current limitations of CARP as a continuous SPD technique for aluminum alloys, and demonstrate the importance of integrated multi-scale characterization in understanding advanced materials processing. 

Al-Mg alloy disks were produced from Mg sandwiched between Al through 100 turns of high-pressure torsion (HPT) at 6.0 GPa at room temperature, resulting in high microhardness of Hv 300–350 in regions experiencing a nominal shear strain >  ~ 390. While compositional mapping using scanning electron microscopy energy-dispersive spectroscopy (EDS) showed a uniform distribution of Mg through the disk thickness at 1.5 mm and 3.0 mm from the disk center, transmission electron microscopy EDS showed a heterogeneous distribution of Mg remained on the nanoscale. Although HPT induces enough mixing to result in face-center-cubic Al with supersaturations of Mg of up to ~ 20 at.% near the disk surfaces, β-Al3Mg2, γ-Al12Mg17 and Al2Mg intermetallic phases were identified by electron diffraction throughout the disk thickness even in regions experiencing high shear strain. This study visually captures detailed compositional heterogeneity throughout the sample thickness following intense mechanical alloying, nanoscale re-structuring and phase transformations. 

The cold angular rolling process (CARP) is being developed as a continuous severe plastic deformation technique, which can process metal sheets without any length limitations at room temperature. CARP contains cold rolling and equal‐channel angular process components. The sheet thickness is kept consistent before and after CARP, allowing multiple passes of the sheet. The desired microstructure and mechanical properties can be achieved in the processed metallic sheets. The current study is aimed to evaluate the capability of CARP by processing copper sheets with different sheet widths for repetitive passes. The CARP‐treated sheets are examined by lab‐scale X‐ray and high‐energy synchrotron X‐ray diffraction to investigate the evolution in dislocation density, texture, and strain anisotropy, and by tensile testing to identify the bulk mechanical properties. The digital image correlation method is applied to tensile testing so that strain localization within the sample gauge is visualized and deformation behavior is evaluated after yielding till postnecking by estimating the hardening exponent and strain hardening rate of the CARP‐treated sheet. Comparing the reported continuous and multiple‐step processes on Cu and its alloys, the present study confirms that the CARP is potentially a useful sheet process for strengthening ductile metals.