Control of Nanoscale Precipitation and Elimination of Intermediate-Temperature Embrittlement in Multicomponent High-Entropy Alloys

Thermally stable high-entropy alloys (HEAs) consisting of a high density of coherent precipitates show a great potential for high-temperature applications. In this work, we systematically investigated the phase stability and coarsening kinetics of L1₂-type coherent precipitates in a Ni-Co-Fe-Cr-Al-Ti-based HEA isothermally aged at 800, 900 and 1000 °C. Aged microstructures in the grain interiors under this temperature range were essentially dominated by the uniform precipitation of multicomponent L1₂ (Ni, Co, Fe, Cr)₃(Ti, Al)-type precipitates. The coarsening kinetics of these intragranular L1₂ precipitates were quantitatively determined, which were adequately characterized by the classical Lifshitz-Slyozov-Wagner model. The activation energy for coarsening was determined to be 378 kJ/mol, which is relatively higher than that of conventional Ni or Co-based superalloys, suggesting a slow elemental diffusion in the HEA matrix. More importantly, the heterogeneous precipitation and the associated metastable phase transformation mechanism along grain boundaries (GBs) were carefully analyzed. Localized chemical heterogeneity was identified within the discontinuous L1₂ phase at the GBs, which thermodynamically destabilizes the L1₂ structure and encourages the formation of brittle Heusler phase. Finally, we establish a unique duplex-aging strategy that can be efficiently utilized for GB stabilization, by which these detrimental intergranular heterostructures can be greatly eliminated, leading to an exceptional resistance to intermediate-temperature embrittlement, along with enhanced tensile strengths. These findings will not only shed light on the precipitation mechanisms in compositionally complex HEAs but also generate new opportunities to the interfacial design of HEAs for advanced high-temperature applications with superior properties.