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Title: Elucidating structural order and disorder phenomena in mullite-type Al{sub 4}B{sub 2}O{sub 9} by automated electron diffraction tomography

Journal Article · · Journal of Solid State Chemistry
;  [1];  [2];  [1];  [3];  [4];  [3];  [5];  [2];  [2];
  1. Institute of Inorganic Chemistry and Analytical Chemistry, Jakob-Welder-Weg 11, Johannes Gutenberg-University Mainz, 55128 Mainz (Germany)
  2. Crystallography, Department of Geosciences, Klagenfurter Str. 2, GEO, University of Bremen, 28359 Bremen (Germany)
  3. Department of Materials and Geoscience, Technische Universität Darmstadt, Petersenstr. 23, 64287 Darmstadt (Germany)
  4. Department of Physics, Lehrstuhl für Kristallographie und Strukturphysik, Friedrich-Alexander University Erlangen-Nürnberg, Staudtstr.3, 91058 Erlangen (Germany)
  5. Institute of Inorganic Chemistry and Crystallography, Leobener Str. NW2, University of Bremen, 28359 Bremen (Germany)

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along the b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.

OSTI ID:
22658267
Journal Information:
Journal of Solid State Chemistry, Vol. 249; Other Information: Copyright (c) 2017 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
Country of Publication:
United States
Language:
English