This article shows a new conceptional design of an experimental setup for in situ visualization of the lyophilization process using neutron radiography and computed tomography and its validation. The setup is designed for the neutron imaging beam line ANTARES at FRM II, considering all the requirements for this method. Neutrons are ideally suited to detect water in a sample because of the high neutron attenuation of hydrogen, whereas other materials like aluminum have a low absorption of neutrons resulting in an image where the drying fronts in bulk materials are observable. Consisting of a freeze-drying cell and a sample-stick, the setup is basically inspired by a common freeze-drying unit. The cell is axial symmetrical to allow computed tomography measurements. The developed sample stick connects the vacuum cell with the measurement devices and the vacuum pump. Experiments were performed at FRM II, showing that the setup is functional. In addition, the experiments discovered some possibilities for improvements, which can be used in further measurements.
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January 2020
Research Article|
January 03 2020
Development of an experimental setup for in situ visualization of lyophilization using neutron radiography and computed tomography
Mathias Hilmer
;
Mathias Hilmer
a)
1
Institute of Process Systems Engineering, Technical University of Munich
, Gregor-Mendel Straße 4, 85354 Freising, Germany
a)Author to whom correspondence should be addressed: [email protected]
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Jürgen Peters;
Jürgen Peters
2
Heinz Maier-Leibnitz Zentrum, Technical University of Munich
, Lichtenbergstraße 1, 85748 Garching bei München, Germany
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Michael Schulz
;
Michael Schulz
2
Heinz Maier-Leibnitz Zentrum, Technical University of Munich
, Lichtenbergstraße 1, 85748 Garching bei München, Germany
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Sebastian Gruber;
Sebastian Gruber
1
Institute of Process Systems Engineering, Technical University of Munich
, Gregor-Mendel Straße 4, 85354 Freising, Germany
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Nicole Vorhauer;
Nicole Vorhauer
3
Institute of Process Engineering, Otto von Guericke University Magdeburg
, Universitätsplatz 2, 39106 Magdeburg, Germany
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Evangelos Tsotsas
;
Evangelos Tsotsas
3
Institute of Process Engineering, Otto von Guericke University Magdeburg
, Universitätsplatz 2, 39106 Magdeburg, Germany
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Petra Foerst
Petra Foerst
1
Institute of Process Systems Engineering, Technical University of Munich
, Gregor-Mendel Straße 4, 85354 Freising, Germany
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a)Author to whom correspondence should be addressed: [email protected]
Rev. Sci. Instrum. 91, 014102 (2020)
Article history
Received:
September 09 2019
Accepted:
December 16 2019
Citation
Mathias Hilmer, Jürgen Peters, Michael Schulz, Sebastian Gruber, Nicole Vorhauer, Evangelos Tsotsas, Petra Foerst; Development of an experimental setup for in situ visualization of lyophilization using neutron radiography and computed tomography. Rev. Sci. Instrum. 1 January 2020; 91 (1): 014102. https://doi.org/10.1063/1.5126927
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