X-ray diffraction using focused-ion-beam-prepared single crystals

Journal of Applied Crystallography
Tina WeigelDirk C Meyer

Abstract

High-quality single-crystal X-ray diffraction measurements are a prerequisite for obtaining precise and reliable structure data and electron densities. The single crystal should therefore fulfill several conditions, of which a regular defined shape is of particularly high importance for compounds consisting of heavy elements with high X-ray absorption coefficients. The absorption of X-rays passing through a 50 µm-thick LiNbO3 crystal can reduce the transmission of Mo Kα radiation by several tens of percent, which makes an absorption correction of the reflection intensities necessary. In order to reduce ambiguities concerning the shape of a crystal, used for the necessary absorption correction, a method for preparation of regularly shaped single crystals out of large samples is presented and evaluated. This method utilizes a focused ion beam to cut crystals with defined size and shape reproducibly and carefully without splintering. For evaluation, a single-crystal X-ray diffraction study using a laboratory diffractometer is presented, comparing differently prepared LiNbO3 crystals originating from the same macroscopic crystal plate. Results of the data reduction, structure refinement and electron density reconstruction indicate ...Continue Reading

References

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Oct 22, 2002·Acta Crystallographica. Section A, Foundations of Crystallography·Lukás Palatinus, Sander van Smaalen
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Jan 9, 2015·Acta Crystallographica. Section C, Structural Chemistry·George M Sheldrick

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Citations

Sep 30, 2021·IUCrJ·Uriel VakninSemën Gorfman

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Methods Mentioned

BETA
X-ray
electron microscopy
scanning electron microscopy
transmission electron microscopy

Software Mentioned

APEX2
BayMEM
VASP
EDMA
JANA2006
SHAPE

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