Ceria-zirconia nanostructured materials for catalytic applications: textural characteristics and redox properties

Highly dispersed solid solutions of ceria-zirconia with nominal composition Ce0.6Zr0.4O2 were prepared by sol-gel technique and the influence of the gel aging time (1 day-3 weeks) on the morphological and textural properties of the materials was investigated. The samples were calcined at 923 K for 8 h, then characterized by XRD, BET surface area and pore size measurements by gas adsorption and by mercury porosimetry. DTA, TEM and SEM analyses were also carried out. The aging of the gel seems to have a remarkable influence on the morphology of the materials, whose surface area and porosity increase by increasing aging time. The phase composition of the solid solutions of ceria-zirconia, as determined by XRD analysis, seems to be independent from the synthetic procedure; in any case a cubic phase (space group Fm-3m) was identified as the main component. XRD and TEM characterizations show the presence of highly dispersed crystallites, with diameters in the range 60-80 Å. The redox properties and hydrogen chemisorption capacity have been studied by TPR/TPD/TPO experiments. Oxygen storage capacity measurements were carried out by a pulse technique, to determine the overall reducibility of the solid, OSCC (Oxygen storage capacity complete). OBC (Oxygen buffering capacity) measurement were also performed to determine the ability of the ceria-zirconia oxides to attenuate fast oscillations (0.1 Hz) of oxygen partial pressure. The correlation between textural, structural and redox properties of the oxides is discussed.