<p>Nickel-based alloys are widely employed in high-temperature applications due to their excellent mechanical strength and oxidation resistance; however, the maximum operating temperature of these materials remains limited. This study aims to enhance the high-temperature oxidation resistance of nickel–chromium (NiCr, 80-20) alloys by incorporating a refractory molybdenum disilicide (MoSi₂) and fabricating composites using the spark plasma sintering (SPS) technique. The alloy microstructure, phase composition, hardness, and oxidation behavior were systematically characterized using scanning electron microscope-energy-dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), micro-Vickers and cyclic oxidation testing at 1000&#xa0;°C. The addition of MoSi₂ led to the formation of ternary Laves phase and ternary silicide, significantly increasing the Vickers hardness from 204.46 HV to 1038.22 HV, as well as suppressing the mass gain of NiCr alloy due to the formation of oxide scale consisting mainly of chromia (Cr₂O₃). The incorporation of MoSi₂ into NiCr composites, despite resulting in a reduction in mass gain, as well as observable oxide peeling and/or cracking of the formed oxide layer, demonstrates a notable enhancement in the thermal stability of the composites. The findings underscore the potential of MoSi₂ as an additive to improve the performance characteristics of NiCr materials in high-temperature applications. For the first time, this study demonstrates the successful integration of MoSi₂ into NiCr alloys via SPS, thereby opening opportunities for developing advanced structural materials for high-temperature applications.</p>