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With good high temperature and corrosive resistance performance, ceramic based composites can be used as promising materials to replace metal thermocouple materials. In this study, Si3N4–MoSi2 composites were prepared via hot pressing technology. X-ray diffraction (XRD), optical microscopy (OM), and scanning electron microscopy (SEM) were used to analyze the microstructure of the composites. The mechanical properties and electrical conductivity were tested. The results showed that the composites were composed of β-Si3N4, MoSi2, a small amount of Mo5Si3, and an amorphous glassy phase. The MoSi2 phase was evenly distributed in the matrix. The percolation network was formed with increasing MoSi2 content. The strength of the composites reached its maximum value when the MoSi2 content reached a critical point. The electrical conductivity behaved like a typical percolation phenomenon. The percolation threshold was about 30% to 45%.