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  In situ synchrotron x-ray diffraction studies monitoring mechanochemical reactions of hard materials: Challenges and limitations

Rathmann, T., Petersen, H., Reichle, S., Schmidt, W., Amrute, A. P., Etter, M., et al. (2021). In situ synchrotron x-ray diffraction studies monitoring mechanochemical reactions of hard materials: Challenges and limitations. Review of Scientific Instruments, 92(11): 114102. doi:10.1063/5.0068627.

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 Creators:
Rathmann, Tobias1, Author              
Petersen, Hilke1, Author              
Reichle, Steffen2, Author              
Schmidt, Wolfgang3, Author              
Amrute, Amol P.2, Author              
Etter, Martin4, Author
Weidenthaler, Claudia1, Author              
Affiliations:
1Research Group Weidenthaler, Max-Planck-Institut für Kohlenforschung, Max Planck Society, ou_1950291              
2Research Department Schüth, Max-Planck-Institut für Kohlenforschung, Max Planck Society, ou_1445589              
3Research Group Schmidt, Max-Planck-Institut für Kohlenforschung, Max Planck Society, ou_1445618              
4Deutsches Elektronen Synchrotron (DESY) P02.1 PETRA III, Notkestr. 85, 22607 Hamburg, Germany, ou_persistent22              

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 Abstract: In situ monitoring of mechanochemical reactions of soft matter is feasible by synchrotron diffraction experiments. However, so far, reactions of hard materials in existing polymer milling vessels failed due to insufficient energy input. In this study, we present the development of a suitable setup for in situ diffraction experiments at a synchrotron facility. The mechanochemical transformation of boehmite, γ-AlOOH, to corundum, α-Al2O3, was chosen as a model system. The modifications of the mill’s clamping system and the vessels themselves were investigated separately. Starting from a commercially available Retsch MM 400 shaker mill, the influence of the geometrical adaptation of the setup on the milling process was investigated. Simply extending the specimen holder proved to be not sufficient because changes in mechanical forces need to be accounted for in the construction of optimized extensions. Milling vessels that are suitable for diffraction experiments and also guarantee the required energy input as well as mechanical stability were developed. The vessels consist of a steel body and modular polymer/steel rings as x-ray transparent windows. In addition, the vessels are equipped with a gas inlet and outlet system that is connectable to a gas analytics setup. Based on the respective modifications, the transformation of boehmite to corundum could be observed in an optimized setup.

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Language(s): eng - English
 Dates: 2021-08-262021-10-262021-11-08
 Publication Status: Published online
 Pages: 10
 Publishing info: -
 Table of Contents: -
 Rev. Type: Peer
 Identifiers: DOI: 10.1063/5.0068627
 Degree: -

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Title: Review of Scientific Instruments
  Abbreviation : Rev. Sci. Instrum.
Source Genre: Journal
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Publ. Info: Melville, NY : AIP Publishing
Pages: - Volume / Issue: 92 (11) Sequence Number: 114102 Start / End Page: - Identifier: ISSN: 0034-6748
CoNE: https://pure.mpg.de/cone/journals/resource/991042742033452