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Structural and phase stability of the Pd-plated Ti3(Al, Si)C2–TiC composite at elevated temperatures was analyzed by the in situ X-ray diffraction method using synchrotron radiation. Porous Ti3(Al, Si)C2–TiC composite was prepared by spark plasma sintering of preceramic paper with 90 wt % of a Ti3(Al, Si)C2 powder filler at 1000°C and 20 MPa. The sintered composite was covered with a Pd film via electroless plating. During in situ investigation, the Pd-plated composite was linearly heated from 25 to 1000°C and annealed for 1 h at a maximum temperature. Structural and phase analysis reveals a formation of new Pd2Si, PdAl, and PdCx phases. It was noted that the newly formed phases began to be formed during heating at ~750°C. Scanning electron microscopy showed that the obtained Ti3AlSiC2–TiC composite had a well-developed porous structure where some pores were filled with Pd. After high-temperature treatment, Pd could be detected at depths up to 5 μm into the Ti3AlSiC2–TiC composite. [ABSTRACT FROM AUTHOR]