Morphology of large ZSM-5 crystals unraveled by fluorescence microscopy

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...

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Published in:	Journal of the American Chemical Society Vol. 130; no. 17; pp. 5763 - 5772
Main Authors:	Roeffaers, Maarten B. J., Ameloot, Rob, Baruah, Mukulesh, Uji-i, Hiroshi, Bulut, Metin, De Cremer, Gert, Mueller, Ulrich, Jacobs, Pierre A., Hofkens, Johan, Sels, Bert F., De Vos, Dirk E.
Format:	Journal Article
Language:	English
Published:	WASHINGTON Amer Chemical Soc 30.04.2008
Subjects:	Chemistry Chemistry, Multidisciplinary Physical Sciences Science & Technology SILICALITE CATALYSIS H-ZSM-5 KINETICS GROWTH SORPTION MOLECULAR-SIEVES SINGLE MOLECULES ZEOLITE CRYSTALS INTERGROWTH
ISSN:	0002-7863, 1520-5126, 1520-5126
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Abstract	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 901 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 degrees 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 900 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.
AbstractList	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 degree 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 degrees 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 degree 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. 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 901 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 degrees 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 900 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. 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 degree 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 degrees 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 degree 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.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 degree 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 degrees 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 degree 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.
Author	Bulut, Metin De Cremer, Gert Hofkens, Johan Sels, Bert F. Ameloot, Rob Uji-i, Hiroshi Roeffaers, Maarten B. J. Baruah, Mukulesh Jacobs, Pierre A. Mueller, Ulrich De Vos, Dirk E.
Author_xml	– sequence: 1 givenname: Maarten B. J. orcidid: 0000-0001-6582-6514 surname: Roeffaers fullname: Roeffaers, Maarten B. J. organization: Katholieke Univ Leuven, Ctr Surface Chem & Catalysis, Dept Microbial & Mol Syst, B-3001 Heverlee, Belgium – sequence: 2 givenname: Rob orcidid: 0000-0003-3178-5480 surname: Ameloot fullname: Ameloot, Rob organization: Katholieke Univ Leuven, Ctr Surface Chem & Catalysis, Dept Microbial & Mol Syst, B-3001 Heverlee, Belgium – sequence: 3 givenname: Mukulesh surname: Baruah fullname: Baruah, Mukulesh organization: Katholieke Univ Leuven, Dept Chem, B-3001 Heverlee, Belgium – sequence: 4 givenname: Hiroshi orcidid: 0000-0002-0463-9659 surname: Uji-i fullname: Uji-i, Hiroshi organization: Katholieke Univ Leuven, Dept Chem, B-3001 Heverlee, Belgium – sequence: 5 givenname: Metin surname: Bulut fullname: Bulut, Metin organization: Katholieke Univ Leuven, Ctr Surface Chem & Catalysis, Dept Microbial & Mol Syst, B-3001 Heverlee, Belgium – sequence: 6 givenname: Gert surname: De Cremer fullname: De Cremer, Gert organization: Katholieke Univ Leuven, Ctr Surface Chem & Catalysis, Dept Microbial & Mol Syst, B-3001 Heverlee, Belgium – sequence: 7 givenname: Ulrich surname: Mueller fullname: Mueller, Ulrich organization: BASF AG, D-67056 Ludwigshafen, Germany – sequence: 8 givenname: Pierre A. surname: Jacobs fullname: Jacobs, Pierre A. organization: Katholieke Univ Leuven, Ctr Surface Chem & Catalysis, Dept Microbial & Mol Syst, B-3001 Heverlee, Belgium – sequence: 9 givenname: Johan orcidid: 0000-0002-9101-0567 surname: Hofkens fullname: Hofkens, Johan email: johan.hofkens@chem.kuleuven.be organization: Katholieke Univ Leuven, Dept Chem, B-3001 Heverlee, Belgium – sequence: 10 givenname: Bert F. surname: Sels fullname: Sels, Bert F. organization: Katholieke Univ Leuven, Ctr Surface Chem & Catalysis, Dept Microbial & Mol Syst, B-3001 Heverlee, Belgium – sequence: 11 givenname: Dirk E. surname: De Vos fullname: De Vos, Dirk E. email: dirk.devos@biw.kuleuven.be organization: Katholieke Univ Leuven, Ctr Surface Chem & Catalysis, Dept Microbial & Mol Syst, B-3001 Heverlee, Belgium
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Keywords	SILICALITE CATALYSIS H-ZSM-5 KINETICS GROWTH SORPTION MOLECULAR-SIEVES SINGLE MOLECULES ZEOLITE CRYSTALS INTERGROWTH
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Snippet	Understanding the internal structure of ZSM-5 crystallites is essential for improving catalyst performance. In this work, a combination of fluorescence...
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SubjectTerms	Chemistry Chemistry, Multidisciplinary Physical Sciences Science & Technology
Title	Morphology of large ZSM-5 crystals unraveled by fluorescence microscopy
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