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Effect of preparation and metal content on the introduction of Fe in BEA zeolite, studied by DR UV-vis, EPR and Mössbauer spectroscopy
Authors:Stanislaw Dzwigaj  Lorenzo Stievano  Michel Che
Affiliation:a Laboratoire de Réactivité de Surface, UMR 7609-CNRS, Université Pierre et Marie Curie, Case 178, 4 Place Jussieu, 75252 Paris Cedex 05, France
b Physik-Department E15, Technische Universität München, James-Franck Strasse, 85747 Garching, Germany
c Institut Universitaire de France, France
Abstract:
Fe-containing SiBEA zeolites were prepared by a two-step postsynthesis method: creation of vacant T-sites by dealumination of tetraethylammonium BEA zeolite with nitric acid and then impregnation of the resulting SiBEA zeolite with an aqueous solution of Fe(NO3)3. X-ray diffraction shows that iron is incorporated in SiBEA at lattice sites. The presence of Fe in its oxidation state +3 and at isolated tetrahedral sites for low metal content, was demonstrated by diffuse reflectance UV-vis, EPR and Mössbauer spectroscopy. For high iron content, diffuse reflectance UV-vis and Mössbauer spectra revealed the additional presence of extra-lattice FeOx oligomers and superparamagnetic Fe-oxyhydroxide. Mössbauer spectroscopy identified superparamagnetic Fe-oxyhydroxide as the main phase when basic conditions are used for the preparation.
Keywords:A. Microporous materials   B. Chemical synthesis   C. Mö  ssbauer spectroscopy   D. Electron paramagnetic resonance   D. Microstructure
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