Local chemical ordering (LCO) in the CrCoNi medium-entropy alloy was investigated by transmission electron microscopy (TEM) after different annealing treatments and their corresponding mechanical properties by bulk tensile tests and nanoindentation. A cold-rolled alloy was annealed at 1000°C for 0.5 h followed by ice water quenching and then aged at a number of different temperatures (600°C, 700°C, 800°C, 900°C, and 1000°C) under vacuum for 240 h to generate different degrees of chemical ordering. A splat-quenched sample rapidly cooled from the liquid phase was also examined. While bulk mechanical properties did not vary among samples with equivalent grain sizes, nanoindentation tests revealed notable differences. As indicated by the load at first pop-in using a Berkovich tip or the indentation yield strength via continuous stiffness measurements using a 10 μm spherical tip, the nanoindentation tests revealed that the stress for onset of plasticity during indentation varied with heat treatment and peaked in the 900°C aged sample. Energy-filtered TEM characterization indicated the presence of ordering in all specimens, with a higher degree of LCO in the aged samples relative to the splat-quenched and 1000°C-quenched samples. The evolution of LCO during aging was determined to occur on the time scale similar to those of bulk diffusion. The difference in nanoindentation strength was attributed to the difference in dislocation nucleation barriers imposed by different degrees of LCO.

CrCoNi-based medium- and high-entropy alloys display outstanding damage tolerance, especially at cryogenic temperatures. In this study, we examined the fracture toughness values of the equiatomic CrCoNi and CrMnFeCoNi alloys at 20 kelvin (K). We found exceptionally high crack-initiation fracture toughnesses of 262 and 459 megapascal-meters^½ (MPa·m^½) for CrMnFeCoNi and CrCoNi, respectively; CrCoNi displayed a crack-growth toughness exceeding 540 MPa·m^½ after 2.25 millimeters of stable cracking. Crack-tip deformation structures at 20 K are quite distinct from those at higher temperatures. They involve nucleation and restricted growth of stacking faults, fine nanotwins, and transformed epsilon martensite, with coherent interfaces that can promote both arrest and transmission of dislocations to generate strength and ductility. We believe that these alloys develop fracture resistance through a progressive synergy of deformation mechanisms, dislocation glide, stacking-fault formation, nanotwinning, and phase transformation, which act in concert to prolong strain hardening that simultaneously elevates strength and ductility, leading to exceptional toughness.