Severe plastic deformation Compositionally complex alloys 3 dimensional atom probe tomography Microstructure a b s t r a c t An equiatomic CoCrFeMnNi high-entropy alloy (HEA), produced by arc melting and drop casting, was subjected to severe plastic deformation (SPD) using high-pressure torsion. This process induced substantial grain refinement in the coarse-grained casting leading to a grain size of approximately 50 nm. As a result, strength increased significantly to 1950 MPa, and hardness to 520 HV. Analyses using transmission electron microscopy (TEM) and 3-dimensional atom probe tomography (3D-APT) showed that, after SPD, the alloy remained a true single-phase solid solution down to the atomic scale. Subsequent investigations characterized the evolution of mechanical properties and microstructure of this nanocrystalline HEA upon annealing. Isochronal (for 1 h) and isothermal heat treatments were performed followed by microhardness and tensile tests. The isochronal anneals led to a marked hardness increase with a maximum hardness of 630 HV at about 450°C before softening set in at higher temperatures. The isothermal anneals, performed at this peak hardness temperature, revealed an additional hardness rise to a maximum of about 910 HV after 100 h. To clarify this unexpected annealing response, comprehensive microstructural analyses were performed using TEM and 3D-APT. New nano-scale phases were observed to form in the originally single-phase HEA. After times as short as 5 min at 450°C, a NiMn phase and Cr-rich phase formed. With increasing annealing time, their volume fractions increased and a third phase, FeCo, also formed. It appears that the surfeit of grain boundaries in the nanocrystalline HEA offer many fast diffusion pathways and nucleation sites to facilitate this phase decomposition. The hardness increase, especially for the longer annealing times, can be attributed to these nano-scaled phases embedded in the HEA matrix. The present results give new valuable insights into the phase stability of single-phase high-entropy alloys as well as the mechanisms controlling the mechanical properties of nanostructured multiphase composites.

In this review, we focus on the saturation microstructure that evolves during severe plastic deformation (SPD). These nanocrystalline or ultrafine-grained microstructures consist predominantly of high-angle boundaries, although low-angle boundaries are also present. Deformation temperature, alloying, and strain path are the dominant factors controlling the saturation grain size in single-phase materials. The saturation grain size decreases significantly with decreasing deformation temperature, although the dependency is stronger at medium homologous temperatures and less in the low-temperature regime. The saturation microstructure is sensitive to strain rate at medium temperatures and less so at low temperatures. The addition of alloying elements to pure metals also reduces the saturation grain size. The results indicate that grain boundary migration is the dominant process responsible for the limitation in refinement by SPD. Therefore, second-phase particles of the nanometer scale can stabilize even finer microstructures. This mechanism of stabilization of the microstructure is an effective tool for overcoming the limit in refinement of single-phase materials by SPD. The improved thermal stability of the obtained nanostructures is another benefit of the introduction of second-phase particles.

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