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Ti2AlN was prepared by a self‐propagating high‐temperature synthesis (SHS) in nitrogen at 0.45 and 0.79 MPa. TiN and AlN were adopted as diluents in the Ti–Al powder compacts and their contents varied from 8.3 to 25 mol%. Formation of Ti2AlN along with intermediates like TiN, Ti3Al, and TiAl was identified. For the AlN‐added samples, the degree of dilution at 11.7 mol% brought about the optimum formation up to 81.8% Ti2AlN in nitrogen of 0.79 MPa. When the sample was diluted with 20 mol% TiN, the SHS process yielded the highest percentage of Ti2AlN reaching 84.3% in nitrogen of 0.45 MPa.