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Morphology of Large ZSM-5 Crystals Unraveled by Fluorescence Microscopy

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Department of Microbial and Molecular Systems, Centre for Surface Chemistry and Catalysis, Katholieke Universiteit Leuven, Kasteelpark Arenberg 23, B-3001 Leuven, Belgium, Department of Chemistry, Katholieke Universiteit Leuven, Celestijnenlaan 200F, B-3001, Leuven, Belgium, and BASF AG, GCC/Z M 301, 67056 Ludwigshafen, Germany
[email protected]; [email protected]
†Department of Microbial and Molecular Systems, Katholieke Universiteit Leuven.
‡Department of Chemistry, Katholieke Universiteit Leuven.
§BASF AG.
Cite this: J. Am. Chem. Soc. 2008, 130, 17, 5763–5772
Publication Date (Web):April 3, 2008
https://doi.org/10.1021/ja7113147
Copyright © 2008 American Chemical Society
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    Abstract

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    Understanding the internal structure of ZSM-5 crystallites is essential for improving catalyst performance. In this work, a combination of fluorescence microscopy, AFM, SEM, and optical observations is employed to study intergrowth phenomena and pore accessibility in a set of five ZSM-5 samples with different crystal morphologies. An amine-functionalized perylene dye is used to probe acid sites on the external crystal surface, while DAMPI (4-(4-diethylaminostyryl)-N-methylpyridinium iodide) is used to map access to the straight channels in MFI from the outer surface. The use of these dyes is validated by studying the well-understood rounded-boat type ZSM-5 crystals. Next coffin-shaped ZSM-5 crystals are considered; we critically evaluate the seemingly conflicting 2-component and 3-component models that have been proposed to account for the hourglass structure in these crystals. The data prove that observation of an hourglass structure is essentially unrelated to a 90° rotation of the pyramidal crystal components under the (010) face. Hence, in perfectly formed coffin-shaped crystals, the straight channels can be accessed from (010). However, in other crystal batches, sections with a 90° rotation can be found; they are indeed located inside the crystal sections under (010) but often only partially occupy these pyramidal components. In such a case, both straight and sinusoidal pores surface at the hexagonal face. The results largely support the 3-component model, but with the added notion that 90° rotated sections (as proposed in the 2-component model) are most likely to be formed inside the defect-rich, pyramidal crystal sections under the (010) faces.

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