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Currently, metal–matrix composite materials are some of the most promising types of materials, and they combine the advantages of a metal matrix and reinforcing particles/fibres. Within the framework of this article, the high-temperature synthesis of metal–matrix composite materials based on the (Ni-Ti)-TiB2 system was studied. The selected approaches make it possible to obtain composite materials of various compositions without contamination and with a high degree of energy efficiency during production processes. Combustion processes in the samples of a 63.5 wt.% NiB + 36.5 wt.% Ti mixture and the phase composition and structure of the synthesis products were researched. It has been established that the synthesis process in the samples proceeds via the spin combustion mechanism. It has been shown that self-propagating high-temperature synthesis (SHS) powder particles have a composite structure and consist of a Ni-Ti matrix and TiB2 reinforcement inclusions that are uniformly distributed inside it. The inclusion size lies in the range between 0.1 and 4 μm, and the average particle size is 0.57 μm. The obtained metal-matrix composite materials can be used in additive manufacturing technologies as ligatures for heat-resistant alloys, as well as for the synthesis of composites using traditional methods of powder metallurgy.