This study synthesized FeNiCuAlX high-entropy alloys (HEAs) (where X = Cr, Co, Mn) using arc melting and investigated their high-temperature oxidation behavior in air at 900 °C. The oxidation kinetics of all alloys followed a parabolic rate, with the oxidation rate constants (kp) of FeNiCuAlCr, FeNiCuAlCo, and FeNiCuAlMn being approximately two to three orders of magnitude lower than that of the FeNiCu alloy. Specifically, FeNiCuAlCr exhibited the lowest kp value of 1.72 × 10⁻⁶ mg²·cm⁴/s, which is significantly lower than those of FeNiCuAlCo (3.29 × 10⁻⁶ mg²·cm⁴/s) and FeNiCuAlMn (1.71 × 10⁻⁵ mg²·cm⁴/s). This suggests that the addition of chromium promotes the formation of a dense Al₂O₃/Cr₂O₃ oxide layer, significantly enhancing the oxidation resistance. Furthermore, corrosion resistance was assessed through potentiodynamic polarization and electrochemical impedance spectroscopy in a 3.5% NaCl solution. FeNiCuAlCr demonstrated exceptional resistance to localized corrosion, as indicated by its low corrosion current density (45.7 μA/cm²) and high pitting potential (−0.21 V), highlighting its superior corrosion performance.

Boron carbide (B₄C) holds significant application potential in the fields of lightweight, high-hardness protective and high-end wear-resistant components due to its low density and exceptional hardness. However, its strong covalent bonding leads to low sintering activity and weak grain-boundary cohesion, resulting in high brittleness and crack sensitivity. These inherent properties make it difficult to achieve simultaneous full densification and toughness enhancement, severely limiting the reliability of B₄C under complex service conditions. Although diamond is an attractive reinforcement because of its high elastic modulus and low coefficient of thermal expansion, the simultaneous realization of densification, graphitization suppression, and fracture-resistance improvement in diamond/B₄C composites remains insufficiently understood. In this study, diamond particles were introduced into the B₄C matrix and consolidated by rapid high-temperature and high-pressure (HTHP) sintering to synergistically promote densification and fracture toughening. The effects of sintering temperature and diamond content on phase evolution, densification, microstructure, and mechanical properties were systematically investigated, and the associated toughening mechanisms were analyzed. The results indicate that the hardness generally increases with rising sintering temperature and diamond content. The primary toughening mechanisms are identified as the pull-out of diamond particles and crack deflection induced by residual stresses generated during the cooling process. Although the composite with 20 wt.% diamond exhibits higher hardness, it also experiences severe macroscopic cracking. The composite with 10 wt.% diamond sintered at 1450 °C under 5.3 GPa for 4 min exhibits the optimal balance of properties, achieving a relative density of 98.85%, a Vickers hardness of 40.72 GPa, and a fracture toughness of 9.20 MPa·m^1/2. This work confirms the effectiveness of combining diamond reinforcement with HTHP sintering in simultaneously achieving densification and toughening of B₄C-based composites, providing a new pathway for developing high-performance lightweight protective ceramics.