Single-phase YAlO 3 was obtained by combustion synthesis using a fuel mixture of urea and glycine. Temperature-time profile recorded by infrared thermal imaging indicates that an aqueous solution of Y(NO 3 ) 3 :-Al(NO 3 ) 3 :urea:glycine (molar ratio of 6:6:15:10) ignites at 315°C, leading to the formation of a white nanocrystalline YAlO 3 powder (51 nm) having a BET surface area of 3 m 2 /g. No additional annealing was required, as the formation of YAlO 3 structure took place at the expense of the heat generated in situ by the highly exothermal, selfpropagated combustion reaction. In this case, the maximum combustion temperature recorded during the combustion reaction was 1661°C. Powders prepared under the same conditions but using the classical version of the combustion method, involving the use of a single fuel (urea or glycine), were amorphous. The absence of YAlO 3 from these samples was caused by the lower temperature achieved during the combustion processes: 414°C in the case of urea and 829°C in the case of glycine.