Refractory high-entropy alloys (RHEAs) are promising candidates for those applications requiring of strong materials at high temperatures with elevated thermal stability and excellent oxidation, irradiation, and corrosion resistance. Particularly, RHEAs synthesized using mechanical alloying (MA) followed by spark plasma sintering (SPS) has proven to be a successful path to produce stronger alloys than those produced by casting techniques. This superior behavior, at both room and high temperature, can be attributed to the microstructural features resultant from this powder metallurgy route, that include the presence of homogeneously distributed non-metallic particles, fine- and ultrafine-grained microstructures, and higher content of interstitial solutes. Nevertheless, the powder metallurgy fabrication relies over a complex balance of several operational variables, and the process is no exempt of certain challenges, such as contamination or the presence of pores in the bulk parts. This review aims to cover all the peculiarities of the MA + SPS route, the resultant microstructures, their mechanical properties, and the strengthening and deformation mechanisms behind their superior performance, as well as a brief description of their oxidation resistance.

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In situ composite manufacture is an approach to improve interfacial adhesion between matrix and reinforcements, in which reinforcements are synthesized along composite processing itself. In situ powder metallurgy route, in particular, offers alternatives to some shortcomings found in other techniques. This work aims not only to review the state of the art on metal matrix composites (MMCs)—including cermets—obtained in situ by powder metallurgy, but also to dissect key aspects related to the development of such materials in order to establish theoretical criteria for decision making before and along experiments. Aspects regarding the design, raw material selection, and processing of such composites were observed and divided between concept, intrinsic, and extrinsic parameters. That way, by means of material databases and computational thermodynamics applied to examples of the reviewed literature, we aim at providing tools in both conducting leaner experiments and richer discussion in this field.@en

Four titanium alloys (Ti-Ta, Ti-Ta-Sn, Ti-Ta-Mn, and Ti-Nb-Sn) were synthesized by mechanical alloying (MA) in a planetary mill in different times between 2 h and 100 h. The microstructure characterization was made by X-ray diffraction (XRD), in which the Rietveld method was applied to analyze the diffraction patterns. The study demonstrated that after short milling times between 2 h and 30 h, the fraction of hexagonal close-packed (hcp) phase decreases; at the same time, the formation of body-centered cubic (bcc) and face-centered cubic (fcc) Ti phases are promoted. Additionally, after 30 h of MA, the full transformation of hcp-Ti was observed, and the bcc-Ti to fcc-Ti phase transformation took place until 50 h. The results suggest that the addition of Ta and Sn promotes the fcc-Ti phase formation, obtaining 100% of this phase at 50 h onwards, whereas Nb and Mn show the opposite effect.

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