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A method for determination of angular accuracy of the goniometer on a transmission electron microscope
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).ORCID iD: 0000-0002-4327-6424
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
(English)Manuscript (preprint) (Other academic)
Abstract [en]

For collection and reconstruction of 3D electron diffraction or electron tomography data, it is essential to have reliable goniometer tilt angles. Thus, it is important to know the accuracy of tilt angles a goniometer can provide on a transmission electron microscope (TEM).  In this paper, a method to determine the angular accuracy of a goniometer is presented, which is based on the orientation determination of rotation electron diffraction (RED) data from a crystal with known unit cell. The method was demonstrated on a JEOL JEM 2100 LaB6 TEM. The result showed that the uncertainty for the goniometer was 1.75% from the expected rotation angle. Meanwhile, the readout error from the TEM hardware followed a combination of sinusoidal and linear components, indicating a more complicated readout error source than only linear errors. A quality assessment method for general TEM goniometers is proposed.

National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-168151OAI: oai:DiVA.org:su-168151DiVA, id: diva2:1306100
Available from: 2019-04-23 Created: 2019-04-23 Last updated: 2019-05-08Bibliographically approved
In thesis
1. Development of rotation electron diffraction as a fully automated and accurate method for structure determination
Open this publication in new window or tab >>Development of rotation electron diffraction as a fully automated and accurate method for structure determination
2019 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Over the past decade, electron diffraction methods have aroused more and more interest for micro-crystal structure determination. Compared to traditional X-ray diffraction, electron diffraction breaks the size limitation of the crystals studied, but at the same time it also suffers from much stronger dynamical effects. While X-ray crystallography has been almost thoroughly developed, electron crystallography is still under active development. To be able to perform electron diffraction experiments, adequate skills for using a TEM are usually required, which makes ED experiments less accessible to average users than X-ray diffraction. Moreover, the relatively poor data statistics from ED data prevented electron crystallography from being widely accepted in the crystallography community.

The thesis focused on both application and method development of continuous rotation electron diffraction (cRED) technique. The cRED method was first applied to a beam sensitive metal-organic framework sample, Co-CAU-36, and the structure was determined and refined within one working day. More importantly, the guest molecules in the pores were also located using only electron diffraction data. To facilitate general users to perform cRED data collection for useful data, software was developed to automate the overall data collection procedure. Through combination of hierarchical cluster analysis tools, the automatically collected data showed comparable quality to those from recent publications, and thus were useful for structure determination and even phase identification. To deal with dynamical refinement for ED data, a frame orientation refinement algorithm was designed to calculate accurate frame orientations for rotation data. Accuracy for the method was validated and compared to an existing software, and the behavior of TEM goniometer was studied by applying the method to an experimental data set.

Place, publisher, year, edition, pages
Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2019. p. 81
Keywords
electron crystallography, structure determination, structure refinement, metal-organic framework, guest molecules, software development, automation, hierarchical cluster analyses, high-throughput data processing, data merging, frame orientations, least-squares optimization, data processing, TEM goniometer
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-168157 (URN)978-91-7797-646-2 (ISBN)978-91-7797-647-9 (ISBN)
Public defence
2019-06-10, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Note

At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 2: Submitted. Paper 4: Manuscript. Paper 5: Manuscript.

Available from: 2019-05-16 Created: 2019-04-23 Last updated: 2019-05-08Bibliographically approved

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Wang, BinHovmöller, SvenZou, Xiaodong
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