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The influence of basic high-temperature synthesis parameters on the process of structure formation in the mechanically activated powder mixture 3Ti+Al was investigated in the study. The synthesis was realized by the method of induction heating in the thermal explosion mode. The heating temperature of the mixture reached 1500°C during the solid state reaction. This temperature exceeded the adiabatic combustion temperature. The investigations of the phase structure formation processes were conducted by XRD methods. In order to obtain a Ti3Al single-phase compound, the optimal time-temperature parameters of the synthesis were determined.