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This study reports the densification behavior and novel design of core-rim microstructure for different ZrB2–MoSi2-SiCw (ZMSw) composites. Four ZrB2–MoSi2 composites containing various amounts of SiCw (0, 5, 10, and 20 vol%) were densified by multistage spark plasma sintering. Optimal combinations of sintering schedule, temperature, and composition are recognized for producing dense ZrB2-based ceramic-matrix composite with core-rim grain structure in the boride matrix, where ZrB2 core is surrounded by a solid solution of (Mo,W)Si2. Fragmentation, rearrangement, plastic deformation, and grain boundary diffusion mechanisms are responsible for densification of composites sintered by multistage SPS conditions at 1700 °C. Addition of SiCw significantly improves the density and mechanical properties of ZrB2–MoSi2–SiCw composites due to the formation of a core-rim structure.

The effect of SiC content, additives, and process parameters on densification and structure–property relations of pressureless sintered ZrB2–(10–40 vol%) SiC particulate composites have been studied. The ZrB2–SiC composite powders mixed by ball-milling with 1.2 wt% C (added as phenolic resin) and 3 wt% B4C have been uniaxially cold-compacted and sintered in argon environment at 1950–2050 °C for 2 h, or at 2000 °C for durations between 1/2 and 3 h. The amount of densification is found to increase with sintering duration, and by prior holding at 1250 and 1600 °C for reduction of oxide impurities (ZrO2, B2O3 and SiO2) on powder particle surfaces by the aforementioned additives. Presence of SiC with average size smaller than that of ZrB2 appears to aid in densification by enhancing green density, increasing WC content by erosion of milling media, and inhibiting matrix grain growth. Both SiC and WC appear to aid in reduction of oxide impurities. Furthermore, the impurities enriched in W, Fe and Co obtained from milling media are found to be segregated at ZrB2 grain boundaries, and appear to assist in densification by forming liquid phase, which completely wets the ZrB2 grains. Hardness increases with SiC content or with sintering duration till 1 h, but decreases for periods ≥2 h due to grain growth. The experimentally measured elastic moduli approaches corresponding theoretically predicted values with increasing SiC content due to reduction in porosity.