Ti3SiC2/20vol%SiC composite was synthesized by spark plasma sintering (SPS) under a pressure of 50MPa at 1350°C using Ti, Si and C as starting powders. The phase constituents and microstructures of the composite were investigated. X-ray diffraction (XRD) results demonstrated that Ti reacted with C to form TiC firstly, then TiSi2 formed from Ti and Si. The formation of Ti3SiC2 might come from two reactions. One was that TiSi2, Ti and TiC reacted directly to form monolithic Ti3SiC2. The other one was that TiSi 2, Ti and C reacted to form Ti3SiC2 and SiC. The EPMA results showed that the main phases were Ti3SiC2 and SiC with a minor content of TiC as impurity. TiC particles less than 1μm in diameter distributed in SiC phase.
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