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Structure analysis of zeolites by rotation electron diffraction (RED)
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).ORCID-id: 0000-0001-9800-3370
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).
Vise andre og tillknytning
2014 (engelsk)Inngår i: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 189, s. 115-125Artikkel i tidsskrift (Fagfellevurdert) Published
Abstract [en]

Single crystal X-ray diffraction and powder X-ray diffraction (PXRD) are powerful methods for determination of unknown crystal structures including zeolites. However, these techniques have some limitations. For instance, single crystal X-ray diffraction requires large enough crystals which are often difficult to synthesize. For powder X-ray diffraction, peak indexing and intensity extraction become difficult if there exist peak broadening caused by small crystal sizes and peak overlap due to large unit cell and high symmetry. This becomes even more complicated for samples that contain more than one phase. We developed a new rotation electron diffraction (RED) method that can overcome these limitations. Almost complete three-dimensional electron diffraction datasets can be collected from micron- or nano-sized single crystals in a transmission electron microscope by combining electron beam tilt and goniometer tilt. Here, we demonstrate the power and limitations of the RED method for ab initio structure determination of four sub-micron sized zeolites, including a calcined silicalite-1, an EUO-type germanosilicate, an FER-type aluminogermanosilicate and an AST-type aluminogermanosilicate. The latter three zeolites were found in multiphasic samples. We show how the tilt range, tilt step and resolution affect the unit cell determination, structure solution and structure refinement. The EUO-, FER- and AST-type zeolites were found in two multiphasic samples in the Al-Ge-Si system, which were also characterized by PXRD and N-2 sorption.

sted, utgiver, år, opplag, sider
2014. Vol. 189, s. 115-125
Emneord [en]
Electron crystallography, Electron diffraction, Unit cell determination, Zeolites, Structure determination
HSV kategori
Identifikatorer
URN: urn:nbn:se:su:diva-103268DOI: 10.1016/j.micromeso.2013.10.014ISI: 000333853200014OAI: oai:DiVA.org:su-103268DiVA, id: diva2:719261
Konferanse
17th International Zeolite Conference (IZC), JUL 07-12, 2013, Moscow, RUSSIA
Merknad

AuthorCount:9;

Tilgjengelig fra: 2014-05-23 Laget: 2014-05-12 Sist oppdatert: 2019-12-04bibliografisk kontrollert

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Su, JieKapaca, ElinaLiu, LeifengWan, WeiHovmöller, SvenZou, Xiaodong
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