Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution
Abstract
Abstract Synchrotron x-ray imaging techniques, like x-ray computed tomography (CT) and radiography have proven instrumental in expanding the communities knowledge of complex transport and reaction kinetics in electrochemical devices such as fuel cells and electrolyzers. This work presents the development of novel x-ray CT imaging techniques for operando visualization of water within low temperature fuel cells at spatial resolutions spanning the micro and nano scales. The design of operando sample holders, for both micro x-ray CT and nano CT experiments is described in depth, and prototypes of these sample holders were evaluated across a set of requirements, the most important of which are x-ray transmissibility, electrical conductivity and mechanical stability. Water segmentation from micro x-ray CT data was enabled by an image subtraction method, where the image without water is subtracted from the one with water. Through iterative experimentations, the operando nano CT cell was developed to optimize mechanical compression, electric conductivity and gas flow. While three-dimensional fuel cell reconstructions were shown possible, there remain challenges to overcome at typical lower energies (8 keV) due to beam damage, whereas it is not as significant for higher energies (>17.5 keV).
- Authors:
- Publication Date:
- Sponsoring Org.:
- USDOE
- OSTI Identifier:
- 1670807
- Grant/Contract Number:
- EE0007270
- Resource Type:
- Published Article
- Journal Name:
- JPhys Energy
- Additional Journal Information:
- Journal Name: JPhys Energy Journal Volume: 2 Journal Issue: 4; Journal ID: ISSN 2515-7655
- Publisher:
- IOP Publishing
- Country of Publication:
- United Kingdom
- Language:
- English
Citation Formats
Kulkarni, Devashish, Normile, Stanley J., Connolly, Liam G., and Zenyuk, Iryna V. Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution. United Kingdom: N. p., 2020.
Web. doi:10.1088/2515-7655/abb783.
Kulkarni, Devashish, Normile, Stanley J., Connolly, Liam G., & Zenyuk, Iryna V. Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution. United Kingdom. https://doi.org/10.1088/2515-7655/abb783
Kulkarni, Devashish, Normile, Stanley J., Connolly, Liam G., and Zenyuk, Iryna V. Wed .
"Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution". United Kingdom. https://doi.org/10.1088/2515-7655/abb783.
@article{osti_1670807,
title = {Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution},
author = {Kulkarni, Devashish and Normile, Stanley J. and Connolly, Liam G. and Zenyuk, Iryna V.},
abstractNote = {Abstract Synchrotron x-ray imaging techniques, like x-ray computed tomography (CT) and radiography have proven instrumental in expanding the communities knowledge of complex transport and reaction kinetics in electrochemical devices such as fuel cells and electrolyzers. This work presents the development of novel x-ray CT imaging techniques for operando visualization of water within low temperature fuel cells at spatial resolutions spanning the micro and nano scales. The design of operando sample holders, for both micro x-ray CT and nano CT experiments is described in depth, and prototypes of these sample holders were evaluated across a set of requirements, the most important of which are x-ray transmissibility, electrical conductivity and mechanical stability. Water segmentation from micro x-ray CT data was enabled by an image subtraction method, where the image without water is subtracted from the one with water. Through iterative experimentations, the operando nano CT cell was developed to optimize mechanical compression, electric conductivity and gas flow. While three-dimensional fuel cell reconstructions were shown possible, there remain challenges to overcome at typical lower energies (8 keV) due to beam damage, whereas it is not as significant for higher energies (>17.5 keV).},
doi = {10.1088/2515-7655/abb783},
journal = {JPhys Energy},
number = 4,
volume = 2,
place = {United Kingdom},
year = {2020},
month = {10}
}
https://doi.org/10.1088/2515-7655/abb783
Works referenced in this record:
3D Printed Flow Field and Fixture for Visualization of Water Distribution in Fuel Cells by X-ray Computed Tomography
journal, January 2016
- White, Robin T.; Orfino, Francesco P.; Hannach, Mohamed El
- Journal of The Electrochemical Society, Vol. 163, Issue 13
Multi‐Scale Imaging of Polymer Electrolyte Fuel Cells using X‐ray Micro‐ and Nano‐Computed Tomography, Transmission Electron Microscopy and Helium‐Ion Microscopy
journal, January 2019
- Meyer, Q.; Hack, J.; Mansor, N.
- Fuel Cells, Vol. 19, Issue 1
Direct observations of liquid water formation at nano- and micro-scale in platinum group metal-free electrodes by operando X-ray computed tomography
journal, September 2018
- Normile, Stanley J.; Sabarirajan, Dinesh C.; Calzada, Osvaldo
- Materials Today Energy, Vol. 9
Understanding Liquid-Water Management in PEFCs Using X-Ray Computed Tomography and Modeling
journal, September 2015
- Zenyuk, I. V.; Weber, A. Z.
- ECS Transactions, Vol. 69, Issue 17
Investigation of water evolution and transport in fuel cells with high resolution synchrotron x-ray radiography
journal, April 2007
- Manke, I.; Hartnig, Ch.; Grünerbel, M.
- Applied Physics Letters, Vol. 90, Issue 17
Multi-scale 3D investigations of a commercial 18650 Li-ion battery with correlative electron- and X-ray microscopy
journal, July 2017
- Gelb, Jeff; Finegan, Donal P.; Brett, Dan J. L.
- Journal of Power Sources, Vol. 357
X-ray microtomography of materials
journal, April 1999
- Stock, S. R.
- International Materials Reviews, Vol. 44, Issue 4
Fast in situ 3D nanoimaging: a new tool for dynamic characterization in materials science
journal, September 2017
- Villanova, Julie; Daudin, Rémi; Lhuissier, Pierre
- Materials Today, Vol. 20, Issue 7
Optimum energies for x-ray transmission tomography of small samples
journal, March 1983
- Grodzins, L.
- Nuclear Instruments and Methods in Physics Research, Vol. 206, Issue 3
Investigating Phase‐Change‐Induced Flow in Gas Diffusion Layers in Fuel Cells with X‐ray Computed Tomography
journal, December 2017
- Shum, Andrew D.; Parkinson, Dilworth Y.; Xiao, Xianghui
- Electrochimica Acta, Vol. 256
Electrocatalyst approaches and challenges for automotive fuel cells
journal, June 2012
- Debe, Mark K.
- Nature, Vol. 486, Issue 7401
Enhanced Water Management of Polymer Electrolyte Fuel Cells with Additive-Containing Microporous Layers
journal, September 2018
- Spernjak, Dusan; Mukundan, Rangachary; Borup, Rodney L.
- ACS Applied Energy Materials, Vol. 1, Issue 11
Probing water distribution in compressed fuel-cell gas-diffusion layers using X-ray computed tomography
journal, April 2015
- Zenyuk, Iryna V.; Parkinson, Dilworth Y.; Hwang, Gisuk
- Electrochemistry Communications, Vol. 53
Review of Advances in Thermal Spreading Resistance Problems
journal, October 2016
- Razavi, M.; Muzychka, Y. S.; Kocabiyik, S.
- Journal of Thermophysics and Heat Transfer, Vol. 30, Issue 4
Coupled Thermal and Water Management in Polymer Electrolyte Fuel Cells
journal, January 2006
- Weber, Adam Z.; Newman, John
- Journal of The Electrochemical Society, Vol. 153, Issue 12
Three-Dimensional Microstructural Imaging of Sulfur Poisoning-Induced Degradation in a Ni-YSZ Anode of Solid Oxide Fuel Cells
journal, June 2014
- Harris, William M.; Lombardo, Jeffrey J.; Nelson, George J.
- Scientific Reports, Vol. 4, Issue 1
Improving water management in fuel cells through microporous layer modifications: Fast operando tomographic imaging of liquid water
journal, September 2019
- Nagai, Yasutaka; Eller, Jens; Hatanaka, Tatsuya
- Journal of Power Sources, Vol. 435
Operando Spectroscopic Microscopy of LiCoO2 Cathodes Outside Standard Operating Potentials
journal, September 2017
- Nelson Weker, Johanna; Wise, Anna M.; Lim, Kipil
- Electrochimica Acta, Vol. 247
4D in situ visualization of electrode morphology changes during accelerated degradation in fuel cells by X-ray computed tomography
journal, May 2017
- White, Robin T.; Wu, Alex; Najm, Marina
- Journal of Power Sources, Vol. 350
Imaging ionomer in fuel cell catalyst layers with synchrotron nano transmission x-ray microscopy
journal, July 2019
- Normile, Stanley J.; Zenyuk, Iryna V.
- Solid State Ionics, Vol. 335
Direct three-dimensional reconstruction of a nanoporous catalyst layer for a polymer electrolyte fuel cell
journal, February 2011
- Ziegler, Christoph; Thiele, Simon; Zengerle, Roland
- Journal of Power Sources, Vol. 196, Issue 4
Low-dose x-ray tomography through a deep convolutional neural network
journal, February 2018
- Yang, Xiaogang; De Andrade, Vincent; Scullin, William
- Scientific Reports, Vol. 8, Issue 1
Fundamental limits to imaging resolution for focused ion beams
journal, November 1996
- Orloff, Jon
- Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, Vol. 14, Issue 6
Modeling and high-resolution-imaging studies of water-content profiles in a polymer-electrolyte-fuel-cell membrane-electrode assembly
journal, November 2008
- Weber, A. Z.; Hickner, M. A.
- Electrochimica Acta, Vol. 53, Issue 26
New Insights into Perfluorinated Sulfonic-Acid Ionomers
journal, January 2017
- Kusoglu, Ahmet; Weber, Adam Z.
- Chemical Reviews, Vol. 117, Issue 3
Mechanisms and effects of mechanical compression and dimensional change in polymer electrolyte fuel cells – A review
journal, June 2015
- Millichamp, Jason; Mason, Thomas J.; Neville, Tobias P.
- Journal of Power Sources, Vol. 284
Impact of synchrotron radiation on fuel cell operation in imaging experiments
journal, October 2010
- Schneider, Armin; Wieser, Christian; Roth, Jörg
- Journal of Power Sources, Vol. 195, Issue 19
Materials research and development focus areas for low cost automotive proton-exchange membrane fuel cells
journal, December 2019
- Gittleman, Craig S.; Kongkanand, Anusorn; Masten, David
- Current Opinion in Electrochemistry, Vol. 18
Progress in In Situ X-Ray Tomographic Microscopy of Liquid Water in Gas Diffusion Layers of PEFC
journal, January 2011
- Eller, Jens; Rosén, Tomas; Marone, Federica
- Journal of The Electrochemical Society, Vol. 158, Issue 8
Designing the 3D Architecture of PGM-Free Cathodes for H 2 /Air Proton Exchange Membrane Fuel Cells
journal, September 2019
- Li, Jingkun; Brüller, Sebastian; Sabarirajan, Dinesh C.
- ACS Applied Energy Materials, Vol. 2, Issue 10
X-Ray Tomography for Lithium Ion Battery Research: A Practical Guide
journal, July 2017
- Pietsch, Patrick; Wood, Vanessa
- Annual Review of Materials Research, Vol. 47, Issue 1
Interfacial analysis of a PEM electrolyzer using X-ray computed tomography
journal, January 2020
- Leonard, Emily; Shum, Andrew D.; Danilovic, Nemanja
- Sustainable Energy & Fuels, Vol. 4, Issue 2
Radiation damage in polymer films from grazing-incidence X-ray scattering measurements
journal, February 2016
- Vaselabadi, Saeed Ahmadi; Shakarisaz, David; Ruchhoeft, Paul
- Journal of Polymer Science Part B: Polymer Physics, Vol. 54, Issue 11
Progress and perspectives for atomic-resolution electron microscopy
journal, February 2008
- Smith, David J.
- Ultramicroscopy, Vol. 108, Issue 3
Understanding the Role of Interfaces for Water Management in Platinum Group Metal-Free Electrodes in Polymer Electrolyte Fuel Cells
journal, April 2019
- Liu, Jiangjin; Talarposhti, Morteza Rezaei; Asset, Tristan
- ACS Applied Energy Materials, Vol. 2, Issue 5
X-Ray Tomographic Microscopy (XTM) Using Synchrotron Radiation
journal, August 1992
- Kinney, J. H.; Nichols, M. C.
- Annual Review of Materials Science, Vol. 22, Issue 1
Operando Sub-Second Tomographic Imaging of Water in PEFC Gas Diffusion Layers
journal, September 2015
- Eller, J.; Marone, F.; Buchi, F. N.
- ECS Transactions, Vol. 69, Issue 17
Nano-structured platinum group metal-free catalysts and their integration in fuel cell electrode architectures
journal, December 2018
- Serov, Alexey; Shum, Andrew D.; Xiao, Xianghui
- Applied Catalysis B: Environmental, Vol. 237
X-ray transparent proton-exchange membrane fuel cell design for in situ wide and small angle scattering tomography
journal, October 2019
- Martens, Isaac; Vamvakeros, Antonis; Chattot, Raphael
- Journal of Power Sources, Vol. 437
Design of a miniature flow cell for in situ x-ray imaging of redox flow batteries
journal, October 2016
- Jervis, Rhodri; Brown, Leon D.; Neville, Tobias P.
- Journal of Physics D: Applied Physics, Vol. 49, Issue 43
Understanding water management in platinum group metal-free electrodes using neutron imaging
journal, October 2020
- Komini Babu, Siddharth; Spernjak, Dusan; Mukundan, Rangachary
- Journal of Power Sources, Vol. 472
Operando X-ray tomography and sub-second radiography for characterizing transport in polymer electrolyte membrane electrolyzer
journal, June 2018
- Leonard, Emily; Shum, Andrew D.; Normile, Stanley
- Electrochimica Acta, Vol. 276
Hard X-ray-induced damage on carbon–binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries
journal, March 2017
- Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent
- Journal of Synchrotron Radiation, Vol. 24, Issue 3
Bridging X-ray computed tomography and computational modeling for electrochemical energy-conversion and –storage
journal, February 2019
- Zenyuk, Iryna V.
- Current Opinion in Electrochemistry, Vol. 13