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Stacking disorders in zeolites and open-frameworks - structure elucidation and analysis by electron crystallography and X-ray diffraction
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
2013 (English)In: Zeitschrift fur Kristallographie, ISSN 0044-2968, Vol. 228, no 1, 11-27 p.Article, review/survey (Refereed) Published
Abstract [en]

Intergrowth and stacking disorders are often found in minerals and synthetic zeolites and inorganic open-frameworks. Structure elucidation of stacking disorders in these materials have been difficult and structure solution of stacking disorders in unknown zeolites and open-frameworks has been challenging. There exist no standard methods for structure analysis of such disordered materials. In this review we present various stacking disorders and intergrowth in a number of representative zeolite families containing stacking disorders. These include zeolite beta, SSZ-26/SSZ-33, ITQ-39, ABC-6, ZSM-48, SSZ-31, UTD-1, faujasite FAU/EMT, pentasil ZSM-5/ZSM-11, ITQ-13/ITQ-34, ITQ-22/ITQ-38 etc. Stacking disorders in open-frameworks containing mixed coordinations, including titanosilicates ETS-10 and ETS-4, and the silicogermanate SU-JU-14 are also described. Various crystallographic methods used for solving disordered structures are summarized. The methods include powder X-ray diffraction (PXRD), electron diffraction, high resolution transmission electron microscopy (HRTEM), and single-crystal X-ray diffraction. Examples of model building combined with simulations of PXRD and single crystal X-ray diffraction to verify the structure models are given.

Place, publisher, year, edition, pages
2013. Vol. 228, no 1, 11-27 p.
Keyword [en]
Zeolites, Open-frameworks, Stacking disorders, Electron crystallography, Structure analysis
National Category
Chemical Sciences
URN: urn:nbn:se:su:diva-88953DOI: 10.1524/zkri.2012.1564ISI: 000315475900003OAI: diva2:616562


Available from: 2013-04-17 Created: 2013-04-08 Last updated: 2013-11-05Bibliographically approved
In thesis
1. Structural study of zeolites utilizing novel electron crystallographic methods: A voyage into the world of zeolite structures
Open this publication in new window or tab >>Structural study of zeolites utilizing novel electron crystallographic methods: A voyage into the world of zeolite structures
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Electron crystallography has evolved as a powerful method for structural characterization of a wide range of materials. It has two significant advantages over other methods for structure determination, e.g. X-ray diffraction. Electrons interact much more strongly with matter compared to X-rays and they can be focused by electromagnetic lenses to form images with atomic resolution. These advantages make electron crystallography a unique tool for characterization of crystalline materials suffering from small crystal size and complex or disordered structures.

     Zeolites are a class of microporous materials with significance in several applications. They often possess complex and disordered structures, which demand large efforts in the structure determination.

     Over the last years, two new electron crystallographic methods have been developed; the rotation electron diffraction (RED) and the structure projection reconstruction from a through-focus series of high resolution transmission electron microscopy (HRTEM) images. In this thesis, they will be applied for structure determination of four new zeolite structures, including EMM-25 and EMM-23 with two ordered structures, and ITQ-39 and ITQ-38 with disordered structures. Each of the structure solutions have different challenges to overcome. The high silica borosilicate EMM-25 was solved by the RED method. The aluminosilicate EMM-23 was solved by a combination of HRTEM and RED. The structure solution of two materials with disordered structures, ITQ-39 and ITQ-38, will be described. For materials containing disorders, structure projection images are of utmost importance.

     Furthermore, the mesoporosity inside hierarchically porous ZSM-5 crystals was studied by a combination of focused ion beam (FIB) and HRTEM imaging. The last part of this thesis explores STEM imaging for use in structure determination from 3D reconstruction.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2013. 104 p.
Electron crystallography, zeolites, structure determination, disorder, electron microscopy
National Category
Inorganic Chemistry
Research subject
Structural Chemistry
urn:nbn:se:su:diva-95870 (URN)978-91-7447-810-5 (ISBN)
Public defence
2013-12-16, Nordenskiöldsalen, Geovetenskapens hus, Svante Arrhenius väg 12, Stockholm, 10:00 (English)

At the time of the doctoral defence the following papers were unpublished and had a status as follows: Papers 4 and 5: Manuscipts; Paper 10: Manuscript

Available from: 2013-11-24 Created: 2013-11-05 Last updated: 2013-11-26Bibliographically approved

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Zou, Xiaodong
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