Seven equimolar, five-component, metal diborides were fabricated via high-energy ball milling and spark plasma sintering. Six of them, including (Hf0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2, (Hf0.2Zr0.2Ta0.2Mo0.2Ti0.2)B2, (Hf0.2Zr0.2Mo0.2Nb0.2Ti0.2)B2, (Hf0.2Mo0.2Ta0.2Nb0.2Ti0.2)B2, (Mo0.2Zr0.2Ta0.2Nb0.2Ti0.2)B2, and (Hf0.2Zr0.2Ta0.2Cr0.2Ti0.2)B2, possess virtually one solid-solution boride phase of the hexagonal AlB2 structure. Revised Hume-Rothery size-difference factors are used to rationalize the formation of high-entropy solid solutions in these metal diborides. Greater than 92% of the theoretical densities have been generally achieved with largely uniform compositions from nanoscale to microscale. Aberration-corrected scanning transmission electron microscopy (AC STEM), with high-angle annular dark-field and annular bright-field (HAADF and ABF) imaging and nanoscale compositional mapping, has been conducted to confirm the formation of 2-D high-entropy metal layers, separated by rigid 2-D boron nets, without any detectable layered segregation along the c-axis. These materials represent a new type of ultra-high temperature ceramics (UHTCs) as well as a new class of high-entropy materials, which not only exemplify the first high-entropy non-oxide ceramics (borides) fabricated but also possess a unique non-cubic (hexagonal) and layered (quasi-2D) high-entropy crystal structure that markedly differs from all those reported in prior studies. Initial property assessments show that both the hardness and the oxidation resistance of these high-entropy metal diborides are generally higher/better than the average performances of five individual metal diborides made by identical fabrication processing.

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Twelve different equiatomic five-metal carbides of group IVB, VB, and VIB refractory transition metals are synthesized via high-energy ball milling and spark plasma sintering. Implementation of a newly developed ab initio entropy descriptor aids in selection of candidate compositions for synthesis of high entropy and entropy stabilized carbides. Phase formation and composition uniformity are analyzed via XRD, EDS, S/TEM-EDS, and EXAFS. Nine of the twelve candidates form true single-phase materials with the rocksalt (B1) structure when sintered at 2473 K and can therefore be investigated as high entropy carbides (HECs). The composition (V 0.2 Nb 0.2 Ta 0.2 Mo 0.2 W 0.2)C is presented as a likely candidate for further investigation as an entropy stabilized carbide. Seven of the carbides are examined for mechanical properties via nanoindentation. The HECs show significantly enhanced hardness when compared to a rule of mixtures average of the constituent binary carbides and to the highest hardness of the binary constituents. The mechanical properties are correlated to the electronic structure of the solid solutions, offering a future route to tunability of the mechanical properties of carbide ceramics via exploration of a new complex composition space.

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