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Langmuir : the ACS journal of surfaces and colloids

Direct synthesis of zirconia aerogel nanoarchitecture in supercritical CO2.


PMID 16618192

Abstract

The objective of the present study was to synthesize porous ZrO2 aerogels with a nanostructure via a direct sol-gel route in the green solvent supercritical carbon dioxide (scCO2). The synthesis involved the coordination and polycondensation of a zirconium alkoxide using acetic acid in CO2, followed by scCO2 drying and calcination. Either a translucent or opaque monolith was obtained, which was subsequently characterized by electron microscopy, X-ray diffraction, thermal analysis, N2 physisorption, and infrared spectroscopy analysis. The electron microscopy results showed that the translucent monolithic ZrO2 exhibited a well-defined mesoporous structure, while the opaque monolith, formed using added alcohol as a cosolvent, was composed of loosely compacted nanospherical particles with a diameter of ca. 20 nm. After calcination at 400 and 500 degrees C, X-ray diffraction results indicated that the ZrO2 exhibited tetragonal and/or monoclinic phases. In situ infrared spectroscopy results showed the formation of a Zr-acetate coordinate complex at the initial stage of the polycondensation, followed by further condensation of the complex into macromolecules.

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