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An Extra-Large-Pore Zeolite with 24 x 8 x 8-Ring Channels Using a Structure-Directing Agent Derived from Traditional Chinese Medicine
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
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Number of Authors: 92018 (English)In: Angewandte Chemie International Edition, ISSN 1433-7851, E-ISSN 1521-3773, Vol. 57, no 22, p. 6486-6490Article in journal (Refereed) Published
Abstract [en]

Extra-large-pore zeolites have attracted much interest because of their important applications for processing larger molecules. Although great progress has been made in academic science and industry, it is challenging to synthesize these materials. A new extra-large-pore zeolite SYSU-3 (Sun Yat-sen University no?) has been synthesized by using a novel sophoridine derivative as an organic structure-directing agent (OSDA). The framework structure was solved and refined using continuous rotation electron diffraction (cRED) data from nanosized crystals. SYSU-3 exhibits a new zeolite framework topology, which has the first 24 x 8 x 8-ring extra-large pore system and a framework density (FD) as low as 11.4 T/1000 angstrom(3). The unique skeleton of the OSDA plays an essential role in the formation of the distinctive zeolite structure. This work provides a new perspective for developing new zeolilic materials by using alkaloids as cost-effective OSDAs.

Place, publisher, year, edition, pages
2018. Vol. 57, no 22, p. 6486-6490
Keywords [en]
alkaloids, extra-large pores, organic structure-directing agents, structure elucidation zeolites
National Category
Chemical Sciences
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-158153DOI: 10.1002/anie.201801386ISI: 000434041700011PubMedID: 29532573OAI: oai:DiVA.org:su-158153DiVA, id: diva2:1235286
Available from: 2018-07-25 Created: 2018-07-25 Last updated: 2020-01-15Bibliographically approved
In thesis
1. A journey towards complete structure determination of zeolites by electron crystallography methods
Open this publication in new window or tab >>A journey towards complete structure determination of zeolites by electron crystallography methods
2020 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Electron crystallography has recently become very successful for structural studies of materials with sub-micrometer sized crystals. In this thesis two major techniques have been applied for structure elucidation – 3-dimensional electron diffraction (3D ED) and high-resolution transmission electron microscopy (HRTEM) imaging. Both can provide information about the structure at the atomic level and have been used for structure determination. During the last decade, two 3D ED methods have been used in our group; the stepwise rotation electron diffraction (RED) method developed in our lab and continuous rotation electron diffraction (cRED) where improvements on the already existing RED method were implemented. Both 3D ED methods can be used for fast structure determination of ordered crystalline materials. HRTEM imaging is very useful for structure determination of more complex and severely disordered materials. For complex structures it is often necessary to combine several methods including powder X-ray diffraction (PXRD).

   Zeolites are microporous crystalline materials. They have complex structures and often synthesized as polycrystalline powders. The aforementioned electron crystallography methods have unique advantages in elucidation of atomic structures of such zeolites. In this thesis, the development of 3D ED methods, especially from RED to cRED, is described through the journey of structure determination of four zeolites; a known pure silicate silicalite-1 for testing the RED method, and three new zeolites. The new zeolites include two extra-large pore germanosilicates ITQ-56 and SYSU-3 and one small-pore aluminosilicate EMM-37. The thesis shows the limitations and advantages of the RED and cRED methods and how different challenges in the structure determination of zeolites are tackled by the advances of 3D ED methods. Finally the thesis presents a detailed structural study of disorders in an aluminosilicate zeolite ITQ-39 by combining HRTEM, RED with sample preparation by ultramicrotomy. The structure of ITQ-39 was determined in 2012 by our group. Here three new zeolite polytypes of ITQ-39 were identified from the HRTEM images and their structure models are proposed.

   A complete structure determination of zeolites includes elucidation of the framework structure, guest species such as structure directing agent (SDA) molecules and ions in the pores, and any structural disorder in the crystal. This thesis reflects to all of these structural characteristics of zeolites, presenting the power of electron crystallography.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry, Stockholm University, 2020. p. 87
Keywords
Electron crystallography, Zeolites, Structure determination, Rotation electron diffraction, Continuous rotation electron diffraction, Disorder
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-177988 (URN)978-91-7797-964-7 (ISBN)978-91-7797-965-4 (ISBN)
Public defence
2020-02-28, 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 paper was unpublished and had a status as follows: Paper 2: Manuscript.

Available from: 2020-02-05 Created: 2020-01-15 Last updated: 2020-05-25Bibliographically approved

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