In Situ Neutron and Synchrotron X-Ray Analysis of Structural Evolution on Plastically Deformed Metals During Annealing

This review highlights the significance of modern quantum-beam techniques, particularly neutron and synchrotron radiation sources, for advanced microstructural characterization of metallic systems. Following a brief introduction to neutron and synchrotron diffraction, selected studies demonstrate their application in probing thermally induced structural evolution in plastically deformed metals. Additively manufactured CoCrFeNi alloys and 316L stainless steels subjected to high-pressure torsion (HPT) were investigated by in situ neutron diffraction during heating, revealing the sequential regimes of recovery, recrystallization, and grain growth. Coupled with mechanical measurements, the results show that HPT followed by controlled thermal treatment improves the mechanical performance, offering strategies for designing engineering materials with enhanced properties. The thermal anisotropy behavior of Ti-45Al-7.5Nb alloys under in situ neutron diffraction is defined as anisotropic ordering upon heating, while the HPT-processed alloy displayed isotropic recovery of order at earlier temperatures. Complementary in situ synchrotron studies in rolled-sheet magnesium alloys unveiled microstructural rearrangement, grain rotation, recovery, and precipitate dissolution during annealing. And phase transformation, recovery, and recrystallization processes were detected in steel using HEXRD. This work emphasizes the complementary strengths of the neutron and synchrotron methods and recommends their broader application as powerful tools to unravel microstructure–property relationships in plastically deformed metals.