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This paper discusses the effects of the environment and temperature of the Ti₃C₂ (MXene) oxidation process. The MXene powders were annealed at temperatures of 1000, 1200, 1400, 1600, and 1800 °C in argon and vacuum using a Spark Plasma Sintering (SPS) furnace. The purpose of the applied annealing method was to determine the influence of a high heating rate on the MXene degradation scheme. Additionally, to determine the thermal stability of MXene during the sintering of SiC matrix composites, SiC–C–B–Ti₃C₂ powder mixtures were also annealed. The process parameters were as follows: Temperatures of 1400 and 1600 °C, and pressure of 30 MPa in a vacuum. Observations of the microstructure showed that, due to annealing of the SiC–C–B–Ti₃C₂ powder mixtures, porous particles are formed consisting of TiC, Ti₃C₂^sym, and amorphous carbon. The formation of porous particles is a transitional stage in the formation of disordered carbon structures.