Simultaneously hard and tough nitride ceramics open new venues for a variety of advanced applications. To produce such materials, attention is focused on the development of high-entropy ceramics, containing four or more metallic components distributed homogeneously in the metallic sublattice. While the fabrication of bulk high-entropy carbides and borides is well established, high-entropy nitrides have only been produced as thin films. Herein, we report on a newel three-step process to fabricate bulk high-entropy nitrides. The high-entropy nitride phase was obtained by exothermic combustion of mechanically-activated nanostructured metallic precursors in nitrogen and consolidated by spark plasma sintering. The fabricated bulk high-entropy nitride (Hf0.2Nb0.2Ta0.2Ti0.2Zr0.2)N demonstrates outstanding hardness (up to 33 GPa) and fracture toughness (up to 5.2 MPa∙m1/2), significantly surpassing expected values from mixture rules, as well as all other reported binary and high-entropy ceramics and can be used for super-hard coatings, structural materials, optics, and others. The obtained results illustrate the scalable method to produce bulk high-entropy nitrides with the new benchmark properties.

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The influence of different SPS‐based methods, that is, conventional spark plasma sintering (SPS), flash SPS (FSPS), and reactive SPS (RSPS) on the properties of Al2O3/SiC composite was investigated. It was shown that the application of preliminary high energy ball milling of the powders significantly enhances the sinterability of the ceramics. It was also demonstrated that FSPS provides unique conditions for rapid, that is, less than a minute, consolidation of refractory ceramics. The Al2O3‐20 wt% SiC composite produced by FSPS possesses the highest relative density (~99%), fracture toughness (7.5 MPa m1/2), hardness (20.3 GPa) and wear resistance among all ceramics produced by other SPS‐based approaches with dwelling time 10 minutes. The RSPS ceramics hold the highest Young's modulus (390 GPa). Substitution of micron‐sized Al2O3 particles by nano alumina does not lead to measurable enhancement of the mechanical properties.

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