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Issue 24, 2016
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Understanding the Zr and Si interdispersion in Zr1−xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy

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Abstract

Zr–Si mixed mesoporous oxides were obtained in a wide range of proportions, from 0 to 30% and from 70 to 100% of Si, using Si(OEt)4 and ZrCl4 as precursors and Pluronic F127 as a template. The oxide mesostructure was characterized by transmission electron microscopy and 2D-small angle X-ray scattering. Fourier transform infrared spectroscopy measurements suggested a local homogeneous interdispersion of both cations. Further selective studies using X-ray Absorption Near Edge Structure (XANES) spectroscopy for separately Zr and Si local environments, allowed for demonstrating that the Zr coordination varies from close to 7 to 6, when its concentration in the mixed oxide is reduced. In addition, it was possible to determine that in mixed oxides with low Zr concentrations, Zr can fit into the spaces occupied by Si in SiO2 pure oxide. An equivalent XANES result was obtained for Si, which is also compatible with the information obtained by FTIR. Furthermore, the Zr–O distance varied from close to 2.2 Å to 1.7 Å when the Zr concentration decreased. Finally, our study also demonstrates the usefulness of XANES to selectively assess the local structure (coordination, symmetry and chemical state) of specific atoms in nanostructured systems.

Graphical abstract: Understanding the Zr and Si interdispersion in Zr1−xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy

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Supplementary files

Article information


Submitted
15 Jan 2016
Accepted
03 Mar 2016
First published
07 Mar 2016

Dalton Trans., 2016,45, 9977-9987
Article type
Paper

Understanding the Zr and Si interdispersion in Zr1−xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy

L. Andrini, P. C. Angelomé, G. J. A. A. Soler-Illia and F. G. Requejo, Dalton Trans., 2016, 45, 9977
DOI: 10.1039/C6DT00203J

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