MoSi₂–ZrB₂–SiC ceramics were synthesized using Mo, Zr, Si and B₄C powders by self-propagating high-temperature synthesis and densifying by spark plasma sintering. The effects of MoSi₂ content on the combustion synthesis process, microstructure, and mechanical properties of the ceramics were investigated. The results showed that combustion synthesis is an unstable mode, spiral combustion. The Gibbs calculations and combustion temperature curves indicate there are two reactions occurring at the same time. The volume fraction of the four different phases and their relative densities were also measured and calculated. Compared to pure MoSi₂, the 1.0MoSi₂–0.2ZrB₂–0.1SiC (M10) ceramic exhibits excellent mechanical properties with its maximum Vickers hardness and fracture toughness being 14.0 GPa and of 5.5 MPa m^1/2, respectively. The hardness is in agreement with the rule of mixture. The morphology of indentation cracks reveals that the fracture toughness improves as a result of toughening mechanisms such as crack bridge, crack deflection, and microcracks.