The solution combustion method (SCS) is demonstrated as an easy and fast alternative method allowing the synthesis of mixed oxides with thermally sensitive metals, still keeping a good control on their stoichiometry and phase composition. Bismuth molybdates with different theoretical Bi/Mo atomic ratios, namely alpha-Bi2Mo3O12, beta-Bi2Mo2O9, and gamma-Bi2MoO6 were synthesized by the SCS, fully characterized by XRD, Raman, SEM/EDX, BET and XPS analyses, and tested in the partial oxidation of propene to acrolein. The SCS method allowed obtaining crystalline catalysts with Bi/Mo atomic ratios close to the theoretical values and very good catalytic properties namely high propene conversion (from 13.4 to 23.4%) and acrolein selectivity (from 71.5 to 80.0%) at 425 degrees C. A high purity of the SCS prepared bismuth molybdates was obtained by means of a subsequent calcination treatment. Such treatment did not alter the high catalytic activity of the catalysts, which slightly increased (from 12.3 to 25.5%), but induced a marked loss of acrolein selectivity (from 66.2 to 48.4%) at 425 degrees C. This effect is due to a strong increase of the oxidation states of Mo and Bi and reduction of the specific surface area during the calcination. (C) 2015 Elsevier B.V. All rights reserved.