Fast-ADT: A fast and automated electron diffraction tomography setup for structure determination and refinement

•New EDT acquisition routine for fast and systematic crystallography analyses.•Module designed for universal application both in TEM or STEM mode.•External optical CCD camera used for analysis of disordered structures.•New polymorph of DRED1 organic dye solved ab initio in P1¯. Electron crystallogra...

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Veröffentlicht in:Ultramicroscopy 2020-04, Vol.211, p.112951, Article 112951
Hauptverfasser: Plana-Ruiz, S, Krysiak, Y, Portillo, J, Alig, E, Estradé, S, Peiró, F, Kolb, U
Format: Artikel
Sprache:eng
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Zusammenfassung:•New EDT acquisition routine for fast and systematic crystallography analyses.•Module designed for universal application both in TEM or STEM mode.•External optical CCD camera used for analysis of disordered structures.•New polymorph of DRED1 organic dye solved ab initio in P1¯. Electron crystallography has focused in the last few years on the analyses of microcrystals, mainly organic compounds, triggered by recent publications on acquisition methods based on direct detection cameras and continuous stage tilting. However, the main capability of a transmission electron microscope is the access to features at the nanometre scale. In this context, a new acquisition method, called fast and automated diffraction tomography (Fast-ADT), has been developed in form of a general application in order to get the most of the diffraction space from a TEM. It consists of two subsequent tilt scans of the goniometric stage; one to obtain a crystal tracking file and a second one to acquire an electron diffraction tomography. This setup has been implemented on both TEM and STEM modes of the microscope, thus it can be installed on any TEM regardless of the availability of a scanning unit. BaSO4 crystals have been measured to demonstrate the validity of the technique for structure determination and refinement. A recently solved layered silicate, RUB-5, has been used to prove the method advantages for fine identification of disorder details. Last, a new polymorph of a DRED1 organic molecule has been solved ab initio and refined by X-ray powder diffraction to show the full application of the presented method.
ISSN:0304-3991
1879-2723
DOI:10.1016/j.ultramic.2020.112951