Gold nanoparticles of various sizes, supported onto ceria, were synthesized using both deposition-precipitation and coprecipitation methods. Whatever the size, the study of the Au/CeO 2 interface confirms the existence of two preferential orientation relationships with a dislocation network which compensates the 25% interfacial lattice mismatch. Behaviors of supported gold nanostructures under the electron beam were examined by high-resolution transmission electron microscopy (HRTEM). The thermal stability of the gold nanostructures was found to be strongly affected by the particle size. For small nanostructures (<5 nm), reversible shrinkage of gold layer by layer onto ceria surface was observed. For larger ones, a progressive and irreversible encapsulation by a CeO 2-x layer was found and a four-step process was experimentally underlined.
New Pr1-xZrxO2-y oxides with x < 0.5 have been prepared by co-precipitation in basic medium and annealed under air at high temperatures (T≤ 1200 °C). Defined compositions with x = 0.02, 0.1, 0.2, 0.35, 0.40 and 0.5 have been characterized by XRD, Zr-K-edge EXAFS for the local structure, magnetic susceptibility measurements, and Pr LIII-edge XANES in order to identify the variation of the cell parameter and Zr local environment versus Zr content and Pr(n+) (4 < n < 3) oxidation states. The higher the Zr content, the lower the Pr valence state. The Zr amount stabilized in the distorted octahedral site is at the origin of the formation of defined compositions as discovered by Leroy Eyring et al. in the PrnO2n-2m series and the generation of oxygen vacancies stabilized in the fluorite-type network. TGA and TPR analyses help to follow the reduction properties under Ar/5% H2 and show high Pr reducible rates at low temperatures (T < 250 °C). The identification of the fluorite-type superstructure (SG: Ia3[combining macron]) of reduced compositions annealed at T = 900 °C under Ar/5% H2 shows the cationic and oxygen vacancy ordering. This feature plays a key role with Zr(4+) cations stabilized in flattened octahedral sites for the generation of oxygen vacancies and the stabilization of Pr(3+) in the reduced states.
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