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The presented paper concerns the technological aspects of the interface evolution in the nickel-silicon carbide composite during the sintering process. The goal of our investigation was to analyse the material changes occurring due to the violent reaction between nickel and silicon carbide at elevated temperatures. The nickel matrix composite with 20 vol pct SiC particles as the reinforcing phase was fabricated by the spark plasma sintering technique. The sintering tests were conducted with variable process conditions (temperature, time, and pressure). It was revealed that the strong interaction between the individual components and the scale of the observed changes depends on the sintering parameters. To identify the microstructural evolution, scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, X-ray diffraction, and Raman spectroscopy were used. The silicon carbide decomposition process progresses with the extension of the sintering time. As the final product of the observed reaction, new phases from the Ni-Si system and free carbon were detected. The step-by-step materials evolution allowed us to reveal the course of the reaction and the creation of the new structure, especially in the reaction zone. The detailed analysis of the SiC decomposition and formation of new components was the main achievement of the presented paper.