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Fabrication of Dense Ultrafine-Grained MoW, MoWNb, and MoWNbTa Alloys: Influence of Cobalt Doping on Sintering and Grain Growth

Dense ultrafine-grained (UFG) refractory MoW, MoWNb, and MoWNbTa alloys were fabricated by combining high-energy ball milling (HEBM) and spark plasma sintering (SPS), achieving ~92-96% relative densities and ~70-180 nm grain sizes. The effects of 2 at.% cobalt (Co) addition on sintering behavior and high-temperature grain growth resistance were investigated as a function of compositional complexity. Activated sintering was observed, with 2 at.% Co addition increasing relative densities from ~92-96% to ~96-98%. Isothermal grain growth experiments at 1200 °C and 1300 °C showed that Co doping suppressed the relative grain growth rate, despite a modest initial grain size increase due to Co-activated sintering, with the effect becoming more pronounced in compositionally complex alloys. The observed trend is consistent with the recently proposed high-entropy grain boundary (HEGB) effect. Notably, Mo24.5W24.5Nb24.5Ta24.5Co2 achieved a 96.4% relative density and maintained an ultrafine grain size, increasing only slightly from ~122 nm to ~127 nm after 5 h annealing at 1200 °C. Scanning transmission electron microscopy (STEM and energy-dispersive X-ray spectroscopy (EDS) confirmed strong Co segregation at grain boundaries, accompanied by minor depletion of Ta and W, supporting a recently proposed grain boundary segregation model for high-entropy alloys and HEGBs.