Title
Direct spectroscopic detection of framework-incorporated vanadium in mesoporous silica materials
Author
Faculty/Department
Faculty of Sciences. Chemistry
Faculty of Sciences. Physics
Publication type
article
Publication
Cambridge ,
Subject
Physics
Chemistry
Source (journal)
Physical chemistry, chemical physics / Royal Society of Chemistry [London] - Cambridge, 1999, currens
Volume/pages
11(2009) :27 , p. 5823-5832
ISSN
1463-9076
1463-9084
ISI
000267727500033
Carrier
E
Target language
English (eng)
Full text (Publishers DOI)
Affiliation
University of Antwerp
Abstract
Framework-incorporated vanadium mesoporous silica materials with different contents in vanadium were obtained by a facile, direct synthesis at room temperature, using VOSO4·5H2O as the vanadium precursor. The porous characteristics of the samples and the coordination environment of the vanadia in the structure were studied by a combination of techniques: X-ray diffraction, N2-adsorption/desorption, FT-Raman, FTIR-PAS and UV-Vis-DR, electron paramagnetic resonance (EPR) and electron nuclear double resonance (ENDOR) spectroscopy. A structural comparison is made using pulsed EPR and ENDOR spectroscopic techniques between vanadia deposited on the surface of MCM-41 by the Molecular Designed Dispersion method and as-synthesised samples of vanadia incorporated in the mesoporous silica framework using the above-mentioned synthesis method. The EPR study on the non-calcined samples proves the incorporation of a high amount of vanadium in the silica framework by the observation of a strong hyperfine coupling of the unpaired electron with 29Si. It demonstrates the feasibility for EPR to reveal structural information on true incorporation of metal ions in framework positions leading to metal oxides.
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