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

被引:60
|
作者
Plana-Ruiz, S. [1 ,2 ,3 ]
Krysiak, Y. [1 ]
Portillo, J. [4 ,5 ]
Alig, E. [6 ]
Estrade, S. [2 ,3 ]
Peiro, F. [2 ,3 ]
Kolb, U. [1 ,7 ]
机构
[1] Tech Univ Darmstadt, Inst Angew Geowissensch, Petersenstr 23, D-64287 Darmstadt, Germany
[2] Univ Barcelona, Dept Engn Elect & Biomed, MIND IN2UB, LENS, Marti i Franques 1, E-08028 Barcelona, Spain
[3] Univ Barcelona, Inst Nanosci & Nanotechnol IN2UB, E-08028 Barcelona, Catalonia, Spain
[4] Univ Barcelona, Ctr Cient & Tecnol, Lluis Sole & Sabaris 1-3, E-08028 Barcelona, Catalonia, Spain
[5] NanoMegas SPRL, Blvd Edmond Machtens 79, B-1080 Brussels, Belgium
[6] Goethe Univ Frankfurt, Inst Anorgan & Analyt Chem, Max von Laue 7, D-60438 Frankfurt, Germany
[7] Johannes Guttenberg Univ Mainz, Inst Anorgan Chem & Analyt Chem, Duesbergweg 10-14, D-55128 Mainz, Germany
关键词
INITIO STRUCTURE DETERMINATION; DATA-COLLECTION; PRECESSION; CRYSTAL; PROGRAM; DYE; CRYSTALLOGRAPHY; NANOCRYSTALS; ORIENTATION; POSITIONS;
D O I
10.1016/j.ultramic.2020.112951
中图分类号
TH742 [显微镜];
学科分类号
摘要
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.
引用
收藏
页数:15
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