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Severe plastic deformation (SPD) has been known for decades to provide microstructural refinement under a hydrostatic stress state by introducing a tremendous quantity of lattice defects, including vacancies, dislocations, and grain boundaries, leading to enhanced mechanical properties. Many SPD processes have been well studied and utilized for the processing of ultrafine-grained (UFG) metals and materials. One major challenge with SPD-processed UFG materials is their limited applicability, primarily due to their microstructural stability at elevated temperatures and the difficulty of scaling up to larger sizes or volumes. To first understand the thermal stability of UFG material, a copper prepared by high-pressure torsion, a technique that can achieve true nano-scale grains in bulk samples, was evaluated using two novel in situ techniques of micro-beam high-energy synchrotron X-ray diffraction. These are, namely, monochromatic X-ray beams that yield changes in microstructure with time and temperature, and a polychromatic X-ray beam that determines grain reorientation behavior during microstructural relaxation. Furthermore, a new processing technique named cold angular rolling process (CARP) demonstrated some promise as an SPD technique for producing theoretically unlimited lengths of strength-enhanced copper sheets at room temperature with a relatively low energy consumption. Additional miniature tensile testing incorporating digital image correlation (DIC) method and microstructural analysis utilizing high-energy X-ray diffraction determined the influence of CARP having higher shear strain hardening in comparison with other established techniques. This study highlights the significance of lattice-defect influenced mechanical properties and microstructure of UFG obtained across multi-length scales and volumes, which are critical for guiding the control and scalable production of advanced materials for commercialization.
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Defect-driven relaxation of nanostructured Cu examined by in situ heating high-energy synchrotron X-ray microbeam diffraction
Bulk nanostructured metals introduced by severe plastic deformation contain an excess of lattice defects. A nanostructured copper (Cu) processed by a high-pressure torsion technique was examined during in situ heating to investigate microstructural relaxation and quantify the evolution of microstructural parameters using high-energy synchrotron microbeam X-ray diffraction. While general microstructural relaxations, such as recovery, recrystallization, and subsequent grain growth, were observed, the key microstructural parameters, including grain size, microstrain, dislocation density, and thermal expansion coefficient, and their changes at critical temperatures were uniquely described and quantified through diffraction data. Based on this analysis, the stored energies driving thermally activated microstructural changes were estimated for individual defect types — grain boundaries, dislocations, and vacancies — that are expected to significantly influence the relaxation behavior of nanostructured Cu. This study demonstrates the effectiveness of diffraction characterization techniques for gaining a comprehensive understanding of the thermal stability of bulk nanostructured materials.
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- Award ID(s):
- 2051205
- PAR ID:
- 10643561
- Publisher / Repository:
- ELSEVIER
- Date Published:
- Journal Name:
- Journal of alloys and compounds
- Volume:
- 1028
- ISSN:
- 0925-8388
- Page Range / eLocation ID:
- 180599
- Subject(s) / Keyword(s):
- Copper High-pressure torsion Line broadening Nanocrystalline metal Recrystallization Synchrotron radiation
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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- Free Publicly Accessible Full Text
-
Accepted Manuscript
- Journal Article:
- https://doi.org/10.1016/j.jallcom.2025.180599
