Journal
JOURNAL OF SOLID STATE CHEMISTRY
Volume 249, Issue -, Pages 114-123Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jssc.2017.02.023
Keywords
Electron diffraction; Aluminum borate; Crystal structure determination; Superstructure; Disorder
Funding
- Carl-Zeiss-Stiftung
- Stipendienstiftung Rheinland-Pfalz
- Deutsche Forschungsgemeinschaft [GE1981/5-1, FI442/19-1, DFG/INST163/2951]
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The crystal structure and disorder phenomena of Al4B2O9, 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. Al4B2O9, 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 AlO6 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 1/2a and 1/2c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns.
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