Segregation-enhanced grain boundary embrittlement of recrystallised tungsten evidenced by site-specific microcantilever fracture

Tungsten stands a prime candidate for plasma-facing applications in fusion reactors, attributed to its capacity to withstand high temperatures and intensive particle fluxes. The operational heat flux, however, can induce recrystallisation of the initial microstructure, increasing the brittle-to-ductile transition temperature. Although such a phenomenon is thought to result from impurity segregation to grain boundaries, direct evidence of impurity-induced grain boundary embrittlement has not yet been reported. Addressing this, our study employs microcantilever testing, coupled with local chemical analysis via atom probe tomography, to unveil the impact of impurity segregation on the fracture toughness of recrystallised tungsten with a purity of 99.98 at.%. The in situ fracture toughness measurements were performed with the notch placed directly at random high-angle grain boundaries, revealing brittle failure regardless of grain boundary misorientation or grain orientation. Notably, both single-crystalline microcantilevers and the as-received material exhibited significant plasticity before failure, with instances without crack propagation. In contrast, recrystallised grain boundaries displayed a fracture toughness of 4.7 ± 0.4 MPa·√m, determined using a linear elastic approach - notably lower than for cleavage plane fracture in tungsten microcantilevers. Local atom probe analysis of the high-angle grain boundaries exposed phosphorous segregation exceeding 2 at.% at the recrystallised interfaces, stemming from recrystallisation. Atomistic simulations confirmed the role of phosphorous in embrittling high-angle grain boundaries in tungsten, while additionally revealing mechanisms of crack-grain boundary interactions and their dependence on phosphorous segregation.