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(Mo1‐xNix) (Si1‐xAlx)2 (x = 0.025, 0.05, and 0.1) alloys were prepared using self‐propagating combustion synthesis from Mo, Si, Al, and Ni powders and subsequently hot‐pressed to achieve a high density of above 96.2%. The combustion products were composed of C11b MoSi2 and C40 Mo(Si,Al)2. A systematic shift of diffraction peaks of C11b MoSi2 toward low angles was observed, and C40 Mo(Si,Al)2 diffraction...