Key insights on the structural characterization of textured Er2O3–ZrO2 nano-oxides prepared by a surfactant-free solvothermal route
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Otros documentos de la autoría: Julian-Lopez, Beatriz; De la Luz, Verónica; Gonell, Francisco; Cordoncillo, Eloisa; López-Haro, Miguel; Calvino, Jose J.; Escribano López, Purificación
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Título
Key insights on the structural characterization of textured Er2O3–ZrO2 nano-oxides prepared by a surfactant-free solvothermal routeAutoría
Fecha de publicación
2012Editor
ElsevierISSN
0925-8388; 1873-4669Cita bibliográfica
Journal of Alloys and Compounds Volume 519, 5 April 2012, Pages 29–36Tipo de documento
info:eu-repo/semantics/articleVersión de la editorial
http://www.sciencedirect.com/science/article/pii/S0925838811021864Palabras clave / Materias
Resumen
Zirconia-mixed oxides can exhibit cubic fluorite and pyrochlore structure. Their discrimination is not easy in nanooxides with a crystal size close to that of a few unit cells. In this work, high resolution transmission ... [+]
Zirconia-mixed oxides can exhibit cubic fluorite and pyrochlore structure. Their discrimination is not easy in nanooxides with a crystal size close to that of a few unit cells. In this work, high resolution transmission electron microscopy (HRTEM) has been employed to provide key insights on the structural characterization of a nanometric and porous mixed Er2O3–ZrO2 oxide. The material was prepared by a simple template-free solvothermal route that provided nanocrystalline powders at low temperature (170 °C) with spherical morphology, and high surface area (∼280 m2 g−1). The porosity was mainly originated from the assembling of organic complexing agents used in the synthesis to limit the crystal growth and to control hydrolysis and condensation reaction rates. The samples were characterized by thermal analysis, X-ray diffraction, scanning electron microscopy and N2 adsorption measurements.
A detailed study by HRTEM was conducted on microtomed samples. It was observed that the material was made of nanocrystals packed into spherical agglomerates. HRTEM simulations indicated that it is not possible to identify the pyrochlore phase in nanoparticles with diameter below 2 nm. In our samples, the analysis of the HRTEM lattice images by means of fast Fourier transform (FFT) techniques revealed well defined spots that can be assigned to different planes of a cubic fluorite-type phase, even in the raw material. Raman spectroscopy was also a powerful technique to elucidate the crystalline phase of the materials with the smallest nanoparticles. HREM and Raman results evidenced that the material is constituted, irrespective of the temperature of the final calcination step, by an ensemble of randomly oriented nanocrystals with fluorite structure. This study opens new perspectives for the design of synthetic approaches to prepare nanooxides (fluorites and pyrochlores) and the analysis of their crystalline structure. [-]
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Journal of Alloys and Compounds, 2012, vol. 519, num. 5Derechos de acceso
Copyright © 2013 Elsevier B.V. All rights reserved. SciVerse® is a registered trademark of Elsevier Properties S.A., used under license. ScienceDirect® is a registered trademark of Elsevier B.V. This is the author’s version of a work that was accepted for publication in Journal of Alloys and Compounds. Changes resulting from the publishing process, such as peer review, editing, corrections, structural formatting, and other quality control mechanisms may not be reflected in this document. Changes may have been made to this work since it was submitted for publication. A definitive version was subsequently published in Journal of Alloys and Compounds, VOL 519, ISSUE 5, (April 2012) DOIhttp://dx.doi.org/10.1016/j.jallcom.2011.11.099
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