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HfB2–15 vol% MoSi2 composites were produced from powder mixtures and densified through different techniques, namely hot pressing and spark plasma sintering. Dense materials were obtained at 1900 °C by hot pressing and at 1750 °C by spark plasma sintering. Microstructure and mechanical properties were compared. The most relevant result was for high-temperature strength: independent of the processing technique, the flexural strength in air at 1500 °C was higher than 500 MPa.

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Fully dense HfC and TaC-based composites containing 15 vol% TaSi2 or MoSi2 were produced by hot pressing at 1750–1900 °C. TaSi2 enhanced the sinterability of the composites and nearly fully dense materials were obtained at lower temperatures than in the case of MoSi2-containing ones. The TaC-based composites performed better than HfC composites at room temperature, showing values of mechanical strength up to 900 MPa and a fracture toughness of 4.7 MPa·m1/2. However, preliminary oxidation tests carried out in air at 1600 °C revealed that HfC-based composites have a superior high temperature stability compared to TaC-based materials.

Ceramics based on group IV-V transition metal borides and carbides possess melting points above 3000 °C, are ablation resistant and are, therefore, candidates for the design of components of next generation space vehicles, rocket nozzle inserts, and nose cones or leading edges for hypersonic aerospace vehicles. As such, they will have to bear high thermo-mechanical loads, which makes strength at high temperature of great importance. While testing of these materials above 2000 °C is necessary to prove their capabilities at anticipated operating temperatures, literature reports are quite limited. Reported strength values for zirconium diboride (ZrB2) ceramics can exceed 1 GPa at room temperature, but these values rapidly decrease, with all previously reported strengths being less than 340 MPa at 1500 °C or above. Here, we show how the strength of ZrB2 ceramics can be increased to more than 800 MPa at temperatures in the range of 1500–2100 °C. These exceptional strengths are due to a core-shell microstructure, which leads to in-situ toughening and sub-grain refinement at elevated temperatures. Our findings promise to open a new avenue to designing materials that are super-strong at ultra-high temperatures.

Starting from a ZrB2 matrix, composites containing 10, 20 vol% of SiC whiskers and 20 vol% of SiC‐chopped fibers were sintered by spark plasma sintering at 1500°C. The addition of whiskers allowed both strengthening (740–770 MPa) and toughening (5.1–5.7 MPa·m1/2) compared with the reference material. In the fiber‐reinforced composite, the increase in fracture toughness (5.5 MPa·m1/2) was accompanied by a decrease of strength (370 MPa). Toughening mechanisms were explored through the analysis of crack propagation. Crack deflection, crack pinning, and thermal residual stresses were the most important mechanisms identified. The experimental toughness increase was successfully compared with the values predicted by theoretical models. Compared with the baseline material, the reinforced composites showed an increased strength at 1200°C in air. The highest value, 450 MPa, was for the fiber‐reinforced composite.

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