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

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 scatteri...

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Autores principales: Andrini, L., Angelomé, P.C., Soler-Illia, G.J.A.A., Requejo, F.G.
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Acceso en línea:http://hdl.handle.net/20.500.12110/paper_14779226_v45_n24_p9977_Andrini
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spelling todo:paper_14779226_v45_n24_p9977_Andrini2023-10-03T16:19:18Z Understanding the Zr and Si interdispersion in Zr1-xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy Andrini, L. Angelomé, P.C. Soler-Illia, G.J.A.A. Requejo, F.G. Fourier transform infrared spectroscopy High resolution transmission electron microscopy Silicon Transmission electron microscopy X ray absorption X ray absorption near edge structure spectroscopy X ray scattering Chemical state Local environments Local structure Mesoporous oxides Mesoporous thin films Mesostructures Nanostructured systems Pluronic F-127 Crystal atomic structure 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. © 2016 The Royal Society of Chemistry. Fil:Angelomé, P.C. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales; Argentina. Fil:Soler-Illia, G.J.A.A. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales; Argentina. JOUR info:eu-repo/semantics/openAccess http://creativecommons.org/licenses/by/2.5/ar http://hdl.handle.net/20.500.12110/paper_14779226_v45_n24_p9977_Andrini
institution Universidad de Buenos Aires
institution_str I-28
repository_str R-134
collection Biblioteca Digital - Facultad de Ciencias Exactas y Naturales (UBA)
topic Fourier transform infrared spectroscopy
High resolution transmission electron microscopy
Silicon
Transmission electron microscopy
X ray absorption
X ray absorption near edge structure spectroscopy
X ray scattering
Chemical state
Local environments
Local structure
Mesoporous oxides
Mesoporous thin films
Mesostructures
Nanostructured systems
Pluronic F-127
Crystal atomic structure
spellingShingle Fourier transform infrared spectroscopy
High resolution transmission electron microscopy
Silicon
Transmission electron microscopy
X ray absorption
X ray absorption near edge structure spectroscopy
X ray scattering
Chemical state
Local environments
Local structure
Mesoporous oxides
Mesoporous thin films
Mesostructures
Nanostructured systems
Pluronic F-127
Crystal atomic structure
Andrini, L.
Angelomé, P.C.
Soler-Illia, G.J.A.A.
Requejo, F.G.
Understanding the Zr and Si interdispersion in Zr1-xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy
topic_facet Fourier transform infrared spectroscopy
High resolution transmission electron microscopy
Silicon
Transmission electron microscopy
X ray absorption
X ray absorption near edge structure spectroscopy
X ray scattering
Chemical state
Local environments
Local structure
Mesoporous oxides
Mesoporous thin films
Mesostructures
Nanostructured systems
Pluronic F-127
Crystal atomic structure
description 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. © 2016 The Royal Society of Chemistry.
format JOUR
author Andrini, L.
Angelomé, P.C.
Soler-Illia, G.J.A.A.
Requejo, F.G.
author_facet Andrini, L.
Angelomé, P.C.
Soler-Illia, G.J.A.A.
Requejo, F.G.
author_sort Andrini, L.
title Understanding the Zr and Si interdispersion in Zr1-xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy
title_short Understanding the Zr and Si interdispersion in Zr1-xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy
title_full Understanding the Zr and Si interdispersion in Zr1-xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy
title_fullStr Understanding the Zr and Si interdispersion in Zr1-xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy
title_full_unstemmed Understanding the Zr and Si interdispersion in Zr1-xSixO2 mesoporous thin films by using FTIR and XANES spectroscopy
title_sort understanding the zr and si interdispersion in zr1-xsixo2 mesoporous thin films by using ftir and xanes spectroscopy
url http://hdl.handle.net/20.500.12110/paper_14779226_v45_n24_p9977_Andrini
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