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Bulk Ta4AlC3 ceramic was prepared by an in situ reaction synthesis/hot‐pressing method using Ta, Al, and C powders as the starting materials. The lattice parameter and a new set of X‐ray diffraction data were obtained. The physical and mechanical properties of Ta4AlC3 ceramic were investigated. Ta4AlC3 is a good electrical and thermal conductor. The flexural strength and fracture toughness are 372 MPa and 7.7 MPa·m1/2, respectively. Typically, plate‐like layered grains contribute to the damage tolerance of Ta4AlC3. After indentation up to a 200 N load, no obvious degradation of the residual flexural strength of Ta4AlC3 was observed, demonstrating the damage tolerance of this ceramic. Even at above 1200°C in air, Ta4AlC3 still retains a high strength and shows excellent thermal shock resistance, which renders it a promising high‐temperature structural material.

In this work, a bulk Nb4AlC3 ceramic was prepared by an in situ reaction/hot pressing method using Nb, Al, and C as the starting materials. The reaction path, microstructure, physical, and mechanical properties of Nb4AlC3 were systematically investigated. The thermal expansion coefficient was determined as 7.2 × 10−6 K−1 in the temperature range of 200°–1100°C. The thermal conductivity of Nb4AlC3 increased from 13.5 W·(m·K)−1 at room temperature to 21.2 W·(m·K)−1 at 1227°C, and the electrical conductivity decreased from 3.35 × 106 to 1.13 × 106Ω−1·m−1 in a temperature range of 5–300 K. Nb4AlC3 possessed a low hardness of 2.6 GPa, high flexural strength of 346 MPa, and high fracture toughness of 7.1 MPa·m1/2. Most significantly, Nb4AlC3 could retain high modulus and strength up to very high temperatures. The Young's modulus at 1580°C was 241 GPa (79% of that at room temperature), and the flexural strength could retain the ambient strength value without any degradation up to the maximum measured temperature of 1400°C.

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An in situ reactive hot‐pressing process using zirconium (zirconium hydride), aluminum, and graphite as staring materials and Si and Y2O3 as additives was used to synthesize bulk Zr3Al3C5 ceramics. This method demonstrates the advantages of easy synthesis, lower sintering temperature, high purity and density, and improved mechanical properties of synthesized Zr3Al3C5. Its electrical and thermal properties were measured. Compared with ZrC, Zr3Al3C5 has a relatively low hardness (Vickers hardness of 12.5 GPa), comparable stiffness (Young's modulus of 374 GPa), but superior strength (flexural strength of 488 GPa) and toughness (fracture toughness of 4.68 MPa·m1/2). In addition, the stiffness decreases slowly with increasing temperature and at 1600°C remains 78% of that at ambient temperature, indicating that Zr3Al3C5 is a potential high‐temperature structural ceramic.