ZrB
2–SiC composite ceramics were fabricated by spark plasma sintering SiC powders with various mixtures of ZrB
2, Zr, Al and graphite components, toughening the ceramics through the in-situ synthesis of Zr–Al–C microstructures. Different microstructures of Zr–Al–C toughened ZrB
2–SiC (ZSA) composite ceramics were formed during the sintering process by varying the components ball milled with the ZrB
2 powders prior to sintering. When the milled ZrB
2-based powders contained Al, the major Zr–Al–C phase changed into Zr
3Al
4C
6 from the designed Zr
2Al
4C
5, and the layered Zr–Al–C grains formed with a large aspect ratio in the ZSA ceramics due to the formation of an Al-based coating layer covering the ZrB
2 powders during milling process. The Zr and Al co-milled ZrB
2-based powders further improved the toughness of composite ceramics through a more uniform distribution and the larger aspect ratio of Zr–Al–C grains. As a result, the ZSA ceramic made using the milled powders of ZrB
2, Zr and Al showed the highest fracture toughness of 5.96 MPa·m
1/2, about 10% higher than that of the ceramic made using milled ZrB
2 and Zr powders. The toughening mechanisms are shown to be crack deflection and bridging caused by Zr–Al–C grains. This work points to a possible pathway to control the microstructure of Zr–Al–C grains for toughening ZrB
2–SiC composite ceramics.
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