Langmuir, Vol.20, No.25, 11223-11233, 2004
Microemulsion-based synthesis of CeO2 powders with high surface area and high-temperature stabilities
Pure ceria powders, CeO2, were synthesized in heptane-microemulsified aqueous solutions of CeCl3 or Ce(NO3)(3) stabilized by AOT (sodium bis(2-ethylhexyl) sulfosuccinate), DDAB (di-n-didodecyldimethylammonium bromide), or DDAB + Brij 35 surfactant mixtures. Micellar DTAB (n-dodecyltrimethylammonium bromide) and vesicular DDAB systems were also used as media for generating CeO2. Characterization of the powders by X-ray powder diffractometry, laser-Raman spectroscopy, and Fourier transform infrared spectroscopy revealed that in the presence of surfactants almost-agglomerate-free nanosized crystallites (6-13 nm) of anionic vacancy-free cubic CeO2 were produced. In the absence of surfactants 21-nm-sized crystallites were formed, comparing with the 85-nm-sized crystallites when cubic CeO2 was created via thermal decomposition of cerium oxalate. Surface characterization, by X-ray photoelectron spectroscopy, N-2 sorptiometry, and high-resolution electron microscopy showed AOT- or (DDAB + Brij 35)-stabilized microemulsions to assist in formation of crystallites exposing surfaces of large specific areas (up to ca. 250 m(2)/g) but of low stability to high-temperature calcination (28-13 m(2)/g at 800 degreesC). In contrast, the double-chained DDAB was found to generate cubic CeO2 crystallites of lower initial surface areas (144 (microemulsion) to 125 (vesicles) m(2)/g)) but of higher thermal stability (55-45 m(2)/g at 800 degreesC). Hence, the latter cerias could be considered as appropriate components for total oxidation (combustion) catalysts.