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9th Conference on Industrial Computed Tomography, Padova, Italy (iCT 2019) Synchrotron based absorption edge tomography for the analysis of 3D printed polymer embedded MOF Christian Gollwitzer 1 , Philipp Scholz 1 , Alexander Ulbricht 1 , Yogita Joshi 1 , Steffen Weidner 1 1 Bundesanstalt für Materialforschung und -prüfung, Unter den Eichen 87, 12205 Berlin, Germany e-mail: [email protected], [email protected], [email protected], [email protected] Abstract Absorption edge tomography (AET), also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element [1]. Synchrotron radiation is the best source for absorption edge tomo- graphy, because of its small bandwidth, high intensity and easily adjustable photon energy [2]. The syn- chrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer mono- chromator is used [3]. Together with the microtomography setup, this enables differential tomography with submicron resolution at the K edge of the elements [4] from chromium up to the lanthanides, and up to uranium, when the L edges are used as well. In this work, mechanochemically synthesized metal-organic framework (MOF) material HKUST-1 in com- bination with acrylonitrile-butadiene styrene (ABS) polymer was used to form a polymer MOF composite material by a simple extruder. This composite filament was used for 3D printing. Absorption edge tomo- graphy facilitated the evaluation of the 3D distribution of the MOF material both in the filament and the resultant printed sample up to μm resolution. Our very first data indicate, that HKUST-1 is mainly homo- geneously dispersed in both polymer bulk materials. In addition, a few clusters having significantly higher Cu concentration were found. AET in combination with data fusion also allows for the calculation of the MOF amount located on the external polymer surface. Keywords: Absorption edge tomography, metal organic framework, synchrotron CT, additive manufacturing References [1] R. Cesareo, Principles and applications of differential tomography, Nucl. Instr. Meth. A 270 (2) (1988) 572–577. doi:10.1016/0168-9002(88)90731-0. [2] K. G. Scheckel, R. Hamon, L. Jassogne, M. Rivers, E. Lombi, Synchrotron X-ray absorption-edge computed microtomography imaging of thallium compartmentalization in Iberis intermedia, Plant and Soil 290 (1-2) (2007) 51–60. doi:10.1007/s11104-006-9102-7. [3] W. Görner, M. P. Hentschel, B. R. Müller, H. Riesemeier, M. Krumrey, G. Ulm, W. Diete, U. Klein, R. Frahm, BAMline: the first hard X-ray beamline at BESSY II, Nucl. Instr. Meth. A 467-468 (2001) 703–706. doi:10.1016/S0168-9002(01)00466-1. [4] T. Arlt, I. Manke, K. Wippermann, H. Riesemeier, J. Mergel, J. Banhart, Investigation of the local catalyst distribution in an aged direct methanol fuel cell MEA by means of differential synchrotron X-ray absorption edge imaging with high energy resolution, Journal of Power Sources 221 (2013) 210– 216. doi:10.1016/j.jpowsour.2012.08.038.

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Page 1: Synchrotron based absorption edge tomography for the analysis … · Synchrotron based absorption edge tomography for the analysis of 3D printed polymer embedded MOF Christian Gollwitzer1,

9th Conference on Industrial Computed Tomography, Padova, Italy (iCT 2019)

Synchrotron based absorption edge tomographyfor the analysis of 3D printed polymer embedded MOF

Christian Gollwitzer1, Philipp Scholz1, Alexander Ulbricht1, Yogita Joshi1, Steffen Weidner1

1Bundesanstalt für Materialforschung und -prüfung, Unter den Eichen 87, 12205 Berlin, Germanye-mail: [email protected], [email protected], [email protected],

[email protected]

AbstractAbsorption edge tomography (AET), also known as differential tomography at absorption edges, is amethod which exploits the sudden change of the attenuation coefficient, when the photon energy crossesthe absorption edge of an element [1]. Synchrotron radiation is the best source for absorption edge tomo-graphy, because of its small bandwidth, high intensity and easily adjustable photon energy [2]. The syn-chrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operatedby the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in aphoton energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer mono-chromator is used [3]. Together with the microtomography setup, this enables differential tomography withsubmicron resolution at the K edge of the elements [4] from chromium up to the lanthanides, and up touranium, when the L edges are used as well.In this work, mechanochemically synthesized metal-organic framework (MOF) material HKUST-1 in com-bination with acrylonitrile-butadiene styrene (ABS) polymer was used to form a polymer MOF compositematerial by a simple extruder. This composite filament was used for 3D printing. Absorption edge tomo-graphy facilitated the evaluation of the 3D distribution of the MOF material both in the filament and theresultant printed sample up to µm resolution. Our very first data indicate, that HKUST-1 is mainly homo-geneously dispersed in both polymer bulk materials. In addition, a few clusters having significantly higherCu concentration were found. AET in combination with data fusion also allows for the calculation of theMOF amount located on the external polymer surface.

Keywords: Absorption edge tomography, metal organic framework, synchrotron CT,additive manufacturing

References[1] R. Cesareo, Principles and applications of differential tomography, Nucl. Instr. Meth. A 270 (2) (1988)

572–577. doi:10.1016/0168-9002(88)90731-0.[2] K. G. Scheckel, R. Hamon, L. Jassogne, M. Rivers, E. Lombi, Synchrotron X-ray absorption-edge

computed microtomography imaging of thallium compartmentalization in Iberis intermedia, Plant andSoil 290 (1-2) (2007) 51–60. doi:10.1007/s11104-006-9102-7.

[3] W. Görner, M. P. Hentschel, B. R. Müller, H. Riesemeier, M. Krumrey, G. Ulm, W. Diete, U. Klein,R. Frahm, BAMline: the first hard X-ray beamline at BESSY II, Nucl. Instr. Meth. A 467-468 (2001)703–706. doi:10.1016/S0168-9002(01)00466-1.

[4] T. Arlt, I. Manke, K. Wippermann, H. Riesemeier, J. Mergel, J. Banhart, Investigation of the localcatalyst distribution in an aged direct methanol fuel cell MEA by means of differential synchrotronX-ray absorption edge imaging with high energy resolution, Journal of Power Sources 221 (2013) 210–216. doi:10.1016/j.jpowsour.2012.08.038.

Page 2: Synchrotron based absorption edge tomography for the analysis … · Synchrotron based absorption edge tomography for the analysis of 3D printed polymer embedded MOF Christian Gollwitzer1,