The high-surface-area Ce x Ba 12x MnAl 11 O y (x 5 0, 0.1, 0.2, 0.3) catalysts were synthesized in the nonionic reverse microemulsion (ME), using the inorganic salts as the reactants. The supercritical drying (SCD) and conventional oven drying (CD) methods were used to remove the water in hydrogels, respectively. The Ce x Ba 12x MnAl 11 O y samples were characterized by N 2 -adsorption, transmission electron microscopy (TEM), TGA-DTA, and X-ray powder diffraction (XRD). The effects of the microemulsion composition, the drying method, the calcination temperature and the introduction of Ce on the catalysts were investigated. The results showed that the morphology of the catalyst was controlled by the microemulsion microstructure; and the homogeneity of the precursor was improved effectively by the reverse microemulsion method and the supercritical drying method. Due to the high homogeneity of the precursors, the initial formation temperature of the hexaaluminate phase decreased to lower than 1100 uC. The BaMnAl 11 O 19 catalyst had high surface area (72.4 m 2 g
21) and high catalytic activity (T 10 5 445 uC) for methane combustion. When Ce was introduced, the Ce x Ba 12x MnAl 11 O y catalyst (x 5 1) had the higher activity (T 10 5 430 uC) than that of the BaMnAl 11 O 19 one due to a synergetic effect between Ce and Mn.