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Multidimensional Disorder in Zeolite IM-18 Revealed by Combining Transmission Electron Microscopy and X-ray Powder Diffraction Analyses
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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Number of Authors: 102018 (English)In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 18, no 4, p. 2441-2451Article in journal (Refereed) Published
Abstract [en]

A new medium-pore germanosilicate, denoted IM-18, with a three-dimensional 8 x 8 x 10-ring channel system, has been prepared hydrothermally using 4-dimethylaminopyridine as an organic structure-directing agent (OSDA). Due to the presence of stacking disorder, the structure elucidation of IM-18 was challenging, and a combination of different techniques, including electron diffraction, high-resolution transmission electron microscopy (HRTEM), and Rietveld refinement using synchrotron powder diffraction data, was necessary to elucidate the details of the structure and to understand the nature of the disorder. Rotation electron diffraction data were used to determine the average structure of IM-18, HRTEM images to characterize the stacking disorder, and Rietveld refinement to locate the Ge in the framework and the OSDA occluded in the channels.

Place, publisher, year, edition, pages
2018. Vol. 18, no 4, p. 2441-2451
National Category
Chemical Sciences Materials Engineering
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-155967DOI: 10.1021/acs.cgd.8b00078ISI: 000429508200057OAI: oai:DiVA.org:su-155967DiVA, id: diva2:1206225
Available from: 2018-05-16 Created: 2018-05-16 Last updated: 2018-12-17Bibliographically approved
In thesis
1. Unraveling the structures of complex nanocrystalline materials by combining TEM and XRPD – development and application
Open this publication in new window or tab >>Unraveling the structures of complex nanocrystalline materials by combining TEM and XRPD – development and application
2019 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Knowledge of the three-dimensional (3D) atomic structure of materials is essential to a fundamental understanding of their properties. The key to understanding the functionality of many materials, particularly those of commercial and industrial interest, is often hidden in the details at the nanoscale. For this reason, it is very important to choose the right strategy to analyze the structure of challenging materials with complex disordered framework structures, or of the layered materials that are the subject of this thesis. Structure analysis of beam-sensitive or uniquely disordered materials can be complicated. Although there are already existing methods such as X-ray powder diffraction (XRPD), the data may exhibit reflection overlap or other problems that make structure determination difficult. To overcome these limitations for nanocrystalline materials, complementary characterization techniques can be used. Here, I will focus on 3D electron crystallography (continuous rotation electron diffraction and high-resolution electron microscopy) methods that have grown during the past years as hybrid methods for structure determination. Based on the presented materials, I will also emphasize that any kind of challenges can be a driving force for method development.  Furthermore, some of the insights gained lead to better understanding of how to collect and process 3D electron diffraction data, which could be applied to make data collection of challenging samples easier and obtain higher quality structure refinements from the data. Finally, I will try to describe the general procedures for ab initio structure elucidation of disordered nanocrystals and layered materials.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2019. p. 82
Keywords
Structure determination, 3D electron diffraction, Complex materials, X-ray powder diffraction, Transmission electron microscopy
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-162710 (URN)978-91-7797-532-8 (ISBN)978-91-7797-533-5 (ISBN)
Public defence
2019-02-08, 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 3: Manuscript. Paper 4: Manuscript.

Available from: 2019-01-16 Created: 2018-12-07 Last updated: 2019-01-15Bibliographically approved

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