The in situ nano Ta4HfC5 reinforced SiBCN-Ta4HfC5 composite ceramics were prepared by a combination of two-step mechanical alloying and reactive hot-pressing sintering. The microstructural evolution and mechanical properties of the resulting SiBCN-Ta4HfC5 were studied. After the first-step milling of 30 h, the raw materials of TaC and HfC underwent crushing, cold sintering, and short-range interdiffusion to finally obtain the high pure nano Ta4HfC5. A hybrid structure of amorphous SiBCN and nano Ta4HfC5 was obtained by adopting a second-step ball-milling. After reactive hot-pressing sintering, amorphous SiBCN has crystallized to 3C-SiC, 6H-SiC, and turbostratic BN(C) phases and Ta4HfC5 retained the form of the nanostructure. With the in situ generations of 2.5 wt% Ta4HfC5, Ta4HfC5 is preferentially distributed within the turbostratic BN(C); however, as Ta4HfC5 content further raised to 10 wt%, it mainly distributed in the grain-boundary of BN(C) and SiC. The introduction of Ta4HfC5 nanocrystals can effectively improve the flexural strength and fracture toughness of SiBCN ceramics, reaching to 344.1 MPa and 4.52 MPa·m1/2, respectively. This work has solved the problems of uneven distribution of ultra-high temperature phases in the ceramic matrix, which is beneficial to the real applications of SiBCN ceramics.

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