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The first zeolite with a tri-directional extra-large 14-ring pore system derived using a phosphonium-based organic molecule
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
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(English)Manuscript (preprint) (Other academic)
Abstract [en]

A new germanosilicate zeolite (denoted as ITQ-53) with extra-large 14-ring pores has been synthesized using tri-tertbutylmethylphosphonium cation as the organic structure directing agent (OSDA). The new rotation electron diffraction (RED) method was used to both identify and solve the structure of ITQ-53 from an initially synthesized sample containing impurities, which facilitated the synthesis optimization that led to pure ITQ-53. The structure was refined against PXRD data. ITQ-53 is the first example of extra-large pore zeolites with tri-directional interconnected 14 × 14 × 14-ring channels. It is built from double 3-rings (D3Rs), double 4-rings (D4Rs), and a new composite building unit [42.54.63]. D3Rs are very rare, previously only found in two zeolitic silicogermanates. ITQ-53 is stable up to at least 450 °C. The structure of ITQ-53 was changed from monoclinic to orthorhombic up on calcination.

National Category
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-108927OAI: oai:DiVA.org:su-108927DiVA: diva2:761514
Available from: 2014-11-06 Created: 2014-11-06 Last updated: 2014-11-07
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)
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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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