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Formation of the Ti 3 (Al,Sn)C 2 solid solutions with a broad substitutional range was investigated by combustion synthesis from elemental powder compacts with Al 4 C 3 and TiC additions. High combustion temperatures of 1590–1700 °C and rapid flame-front speeds of 14.2–18.8 mm/s were measured for the Al 4 C 3 -adopted samples. Due to the dilution effect of TiC, the combustion temperature and velocity were significantly reduced for the TiC-added samples and approximated to 1220–1280 °C and 7.1–9.6 mm/s, respectively. The XRD analysis indicated that Ti 3 (Al 1– x Sn x )C 2 solid solutions with x = 0.2, 0.4, and 0.6 were produced from the Al 4 C 3 -adopted samples. Further increase of Sn to x = 0.8 led to the formation of a large amount of Ti 2 SnC and TiC. Because of the low reaction temperature for the TiC-based reaction scheme, the effective substitution of Sn for Al in Ti 3 (Al 1– y Sn y )C 2 was only achieved at y = 0.2 and 0.4. Incomplete phase formation at y = 0.6 and 0.8 yielded Sn-lean Ti 3 (Al,Sn)C 2 along with Ti 2 SnC, TiC, and free Sn. The as-synthesized Ti 3 (Al,Sn)C 2 grains were formed into the shape of platelets and most of them were closely stacked into a laminated microstructure. [ABSTRACT FROM AUTHOR]