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B4C‐TiB2 ceramics (TiB2 ranging 5~70 vol%) with Mo‐Co‐WC as the sintering additive were prepared by spark plasma sintering. In comparison with B4C‐TiB2 without additive, the enhanced densification was evident in the sintered specimen with Mo‐Co‐WC additive. Core‐rim structured grain was observed around TiB2 grains. The interface of the rim between TiB2 and B4C phases demonstrated different feature: the inner borderline of the rim exhibited a smooth feature, whereas a sharp curved grain boundary was observed between the rim and the B4C grain. The formation mechanism is discussed: the epitaxial growth of (Ti,Mo,W)B2 rim around the TiB2 core may occur as a result of the solid solution and dissolution‐precipitation between TiB2 phase and the sintering additive. It was revealed that the fracture toughness increased as the content of TiB2 content increased, alongside the decreased hardness. B4C‐30 vol% TiB2 specimen demonstrated the optimal combination of mechanical properties, reaching Vickers hardness of 24.3 GPa and fracture toughness of 3.33 MPa·m1/2.

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