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An investigation of the properties of large crystals of the zeolites dodecasil-3C and ferrierite by high-temperature birefringence microscopy and X-ray diffraction

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Lethbridge, Zoe A. D., Keeble, Dean Samuel, Walker, David, Thomas, Pam A. and Walton, Richard I. (2010) An investigation of the properties of large crystals of the zeolites dodecasil-3C and ferrierite by high-temperature birefringence microscopy and X-ray diffraction. Journal of Applied Crystallography, Vol.43 (No.1). pp. 168-175. doi:10.1107/S0021889809052753

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Official URL: http://dx.doi.org/10.1107/S0021889809052753

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Abstract

Optical birefringence has been measured as a function of temperature for two types of siliceous zeolite crystals that contain organic template molecules. The specimens were prepared using modified solvothermal synthesis to produce large (similar to 1 mm dimension) crystals. In the case of the clathrasil dodecasil-3C the material undergoes a first-order phase transition at similar to 433 K that is reversible after heating to 873 K and cooling to room temperature. Comparison with powder X-ray diffraction data from a bulk sample shows that this is a ferroelastic tetragonal (I (4) over bar 2d) to cubic (Fd (3) over barm) transition, which is supported by the functional form of temperature variation of the birefringence. There is apparently no loss of the organic template involved in this transition. For the zeolite ferrierite, the plate-like crystals show a pronounced domain-like structure, which, although not due to twinning, shows a distinctive optical birefringence change on heating, suggesting that variable concentrations of organic template might be present in different domain-like regions. In this material there is no evidence for a change in crystal symmetry up to 873 K (Pnnm), despite apparent loss of some organic template from the material which, in turn, gives rise to strain birefringence at the edges parallel to the [010] direction.

Item Type: Journal Article
Subjects: Q Science > QC Physics
Q Science > QD Chemistry
Divisions: Faculty of Science > Chemistry
Faculty of Science > Physics
Library of Congress Subject Headings (LCSH): Zeolites, X-rays -- Diffraction, Refraction, Double
Journal or Publication Title: Journal of Applied Crystallography
Publisher: Wiley-Blackwell Publishing Ltd.
ISSN: 0021-8898
Official Date: February 2010
Dates:
DateEvent
February 2010Published
Volume: Vol.43
Number: No.1
Number of Pages: 8
Page Range: pp. 168-175
DOI: 10.1107/S0021889809052753
Status: Peer Reviewed
Publication Status: Published
Funder: Engineering and Physical Sciences Research Council (EPSRC), Advantage West Midlands (AWM), European Regional Development Fund (ERDF)

Data sourced from Thomson Reuters' Web of Knowledge

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