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The dependence of MAX-phase synthesis on phase composition of the initial mixture and heat treatment terms in the electric furnace was investigated. Using Ti and AlN powders with the molecular ratio 2:1 as an example, the sequence of phase composition changes with increasing exposure temperature was tracked. It was established that the maximum amount of Ti2AlN MAX-phase in the end products is obtained at 1400°C. At this temperature a single phase product (100% wt Ti2AlN) was obtained for the initial mixture Ti:Al:TiN = 1:1:1. The principal possibility of scaling for obtaining a single-phase product of Ti2AlN by vacuum sintering was experimentally shown on the example of the mixture of this composition weighing 500 g at a certain mode of thermal vacuum treatment.