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Severe plastic deformation (SPD) is an effective route for the nanocrystallization of multi-principal element alloys (MPEAs). The stability of the refined microstructure is important, considering the high temperature applications of these materials. In the present study, the effect of SPD on the stability of a body-centered cubic (bcc) HfNbTiZr MPEA was investigated. SPD was performed using a high-pressure torsion (HPT) technique by varying the number of turns between ½ and 10. The evolution of phase composition and microstructure was studied near the disk centers and edges where the imposed strain values were the lowest and highest, respectively. Thus, the shear strain caused by HPT varies between 3 (½ turn, near the center) and 340 (10 turns, near the edge). It was found that during annealing up to 1000 K, the bcc HfNbTiZr alloy decomposed into two bcc phases with different lattice constants at 740 K. In addition, at high strains a hexagonal close packed (hcp) phase was formed above 890 K. An inhomogeneous elemental distribution was developed at temperatures higher than 890 K due to the phase decomposition. The scale of the chemical heterogeneities decreased from about 10 µm to 30 nm where the shear strain increased from 3 to 340, which is similar to the magnitude of grain refinement. Anneal-induced hardening was observed in the MPEA after HPT for both low and high strains at 740 K, i.e., the hardness of the HPT-processed samples increased due to heat treatment. At low strain, the hardness remained practically unchanged between 740 and 1000 K, while for the alloy receiving high strains there was a softening in this temperature range. 

Herein, lab‐scale X‐ray diffraction and in situ heating neutron diffraction analyses for evaluating the structural changes at postprinting nanostructuring and structural relaxation upon heating, respectively, in an additive‐manufactured (AM) 316L stainless steel are conducted. The nanostructured AM steel after nanostructuring by high‐pressure torsion reached crystallite sizes of 23–26 nm, a dislocation density of ≈45 × 10¹⁴ m⁻²and a microstrain of >0.008. A limited amount of deformation‐inducedε‐martensite was observed at a local region in the nanostructured AM steel. The time‐resolved neutron diffraction experiment upon heating successfully visualizes the sequential structural relaxation and linear thermal lattice expansion in the nanostructured AM steel. In practice, by calculating the changes in crystallite sizes, microstrains, and dislocation densities, the relaxation behaviors of the nanocrystalline AM steel is observed: 1) recovery with slow stress relaxation with increasing hardness up to 873 K, 2) recrystallization with accelerated stress relaxation at 873–973 K; and 3) grain growth above 973 K with (iii′) total stress relaxation in lattices up to 1023 K. In addition, this manuscript makes connections between the critical subjects in materials science of advanced manufacturing, metal processing and properties, and novel time‐resolved characterization techniques.