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ITQ-54: a multi-dimensional extra-large pore zeolite with 20 [times] 14 [times] 12-ring channels
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK), Inorganic and Structural Chemistry.
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK), Inorganic and Structural Chemistry.
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2015 (English)In: Chemical Science, ISSN 2041-6520, E-ISSN 2041-6539, Vol. 6, 480-485 p.Article in journal (Refereed) Published
Abstract [en]

A multi-dimensional extra-large pore silicogermanate zeolite, named ITQ-54, has been synthesised by in situ decomposition of the N,N-dicyclohexylisoindolinium cation into the N-cyclohexylisoindolinium cation. Its structure was solved by 3D rotation electron diffraction (RED) from crystals of ca. 1 [small mu ]m in size. The structure of ITQ-54 contains straight intersecting 20 [times] 14 [times] 12-ring channels along the three crystallographic axes and it is one of the few zeolites with extra-large channels in more than one direction. ITQ-54 has a framework density of 11.1 T atoms per 1000 A3, which is one of the lowest among the known zeolites. ITQ-54 was obtained together with GeO2 as an impurity. A heavy liquid separation method was developed and successfully applied to remove this impurity from the zeolite. ITQ-54 is stable up to 600 [degree]C and exhibits permanent porosity. The structure was further refined using powder X-ray diffraction (PXRD) data for both as-made and calcined samples.

Place, publisher, year, edition, pages
2015. Vol. 6, 480-485 p.
National Category
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-108918DOI: 10.1039/C4SC02577FISI: 000345901600055OAI: oai:DiVA.org:su-108918DiVA: diva2:761498
Available from: 2014-11-06 Created: 2014-11-06 Last updated: 2017-12-05Bibliographically approved
In thesis
1. Characterization of crystalline materials by rotation electron diffraction: Phase identification and structure determination
Open this publication in new window or tab >>Characterization of crystalline materials by rotation electron diffraction: Phase identification and structure determination
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Electron crystallography is powerful for determination of complex structures. The newly-developed 3D electron diffraction (ED) methods make structure determination from nano- and micron-sized crystals much easier than using other methods, for example X-ray diffraction. Almost complete 3D ED data can be collected easily and fast from crystals at any arbitrary orientations. Dynamical effects are largely reduced compared to zonal ED patterns. 3D ED is powerful for phase identification and structure solution from individual nano- and micron-sized crystals, while powder X-ray diffraction (PXRD) provides information from all phases present in the samples. 3D ED methods and PXRD are complementary and their combinations are promising for studying multiphasic samples and complicated crystal structures.

In this thesis, the feasibility and capability of 3D ED methods, specifically rotation electron diffraction (RED), in phase identification and structure determination of different kinds of crystalline materials with nano- or submicrometer-sized crystals are investigated. Experimental conditions for RED data collection and data processing in relation to data quality, as well as the challenges in the applications of RED are discussed.

RED was combined with PXRD to identify phases from as-synthesized samples and to characterize atomic structures of eleven crystalline compounds. It was shown to be possible to identify as many as four distinct compounds within one sample containing submicron-sized crystals in a Ni-Se-O-Cl system. RED was also used to determine unit cell and symmetry of isoreticular metal-organic frameworks (SUMOF-7) and solve five zeolite structures with new frameworks, ITQ-51, ITQ-53, ITQ-54, EMM-23 and EMM-25 and that of a metal-organic framework (MOF), SUMOF-7I. The structure of an open-framework germanate SU-77 was solved by combining RED with PXRD. The structures of the zeolites and SU-77 were confirmed by Rietveld refinement against PXRD. High-resolution transmission electron microscopy was used to confirm the structure models of ITQ-51, EMM-25 and SUMOF-7I.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2014. 102 p.
Keyword
electron microscopy, phase identification, rotation electron diffraction, structure determination, three-dimensional electron diffraction
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-108930 (URN)978-91-7649-017-4 (ISBN)
Public defence
2014-12-17, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (English)
Opponent
Supervisors
Note

At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 2: Submitted. Paper 4: Accepted. Paper 6: Manuscript. Paper 7: Epub ahead of print. Paper 9: Manuscript. Paper 11: Manuscript.

Available from: 2014-11-25 Created: 2014-11-06 Last updated: 2015-10-27Bibliographically approved

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