Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution

Kulkarni, Devashish; Normile, Stanley J.; Connolly, Liam G.; Zenyuk, Iryna V.

doi:10.1088/2515-7655/abb783

Title: Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution

Journal Article · 07 October 2020 · JPhys Energy

DOI: https://doi.org/10.1088/2515-7655/abb783 · OSTI ID:1670807

Kulkarni, Devashish; Normile, Stanley J.; Connolly, Liam G.;

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).

View Journal Article

Cite

Export

Save

Sponsoring Organization:: USDOE

Grant/Contract Number:: EE0007270

OSTI ID:: 1670807

Journal Information:: JPhys Energy, Journal Name: JPhys Energy Vol. 2 Journal Issue: 4; ISSN 2515-7655

Publisher:: IOP PublishingCopyright Statement

Country of Publication:: United Kingdom

Language:: English

References (46)

3D Printed Flow Field and Fixture for Visualization of Water Distribution in Fuel Cells by X-ray Computed Tomography White, Robin T.; Orfino, Francesco P.; Hannach, Mohamed El Journal of The Electrochemical Society, Vol. 163, Issue 13 https://doi.org/10.1149/2.0461613jes	journal	January 2016
Multi‐Scale Imaging of Polymer Electrolyte Fuel Cells using X‐ray Micro‐ and Nano‐Computed Tomography, Transmission Electron Microscopy and Helium‐Ion Microscopy Meyer, Q.; Hack, J.; Mansor, N. Fuel Cells, Vol. 19, Issue 1 https://doi.org/10.1002/fuce.201800047	journal	January 2019
Direct observations of liquid water formation at nano- and micro-scale in platinum group metal-free electrodes by operando X-ray computed tomography Normile, Stanley J.; Sabarirajan, Dinesh C.; Calzada, Osvaldo Materials Today Energy, Vol. 9 https://doi.org/10.1016/j.mtener.2018.05.011	journal	September 2018
Understanding Liquid-Water Management in PEFCs Using X-Ray Computed Tomography and Modeling Zenyuk, I. V.; Weber, A. Z. ECS Transactions, Vol. 69, Issue 17 https://doi.org/10.1149/06917.1253ecst	journal	September 2015
Investigation of water evolution and transport in fuel cells with high resolution synchrotron x-ray radiography Manke, I.; Hartnig, Ch.; Grünerbel, M. Applied Physics Letters, Vol. 90, Issue 17 https://doi.org/10.1063/1.2731440	journal	April 2007
Multi-scale 3D investigations of a commercial 18650 Li-ion battery with correlative electron- and X-ray microscopy Gelb, Jeff; Finegan, Donal P.; Brett, Dan J. L. Journal of Power Sources, Vol. 357 https://doi.org/10.1016/j.jpowsour.2017.04.102	journal	July 2017
X-ray microtomography of materials Stock, S. R. International Materials Reviews, Vol. 44, Issue 4 https://doi.org/10.1179/095066099101528261	journal	April 1999
Fast in situ 3D nanoimaging: a new tool for dynamic characterization in materials science Villanova, Julie; Daudin, Rémi; Lhuissier, Pierre Materials Today, Vol. 20, Issue 7 https://doi.org/10.1016/j.mattod.2017.06.001	journal	September 2017
Optimum energies for x-ray transmission tomography of small samples Grodzins, L. Nuclear Instruments and Methods in Physics Research, Vol. 206, Issue 3 https://doi.org/10.1016/0167-5087(83)90393-9	journal	March 1983
Investigating Phase‐Change‐Induced Flow in Gas Diffusion Layers in Fuel Cells with X‐ray Computed Tomography Shum, Andrew D.; Parkinson, Dilworth Y.; Xiao, Xianghui Electrochimica Acta, Vol. 256 https://doi.org/10.1016/j.electacta.2017.10.012	journal	December 2017
Electrocatalyst approaches and challenges for automotive fuel cells Debe, Mark K. Nature, Vol. 486, Issue 7401 https://doi.org/10.1038/nature11115	journal	June 2012
Enhanced Water Management of Polymer Electrolyte Fuel Cells with Additive-Containing Microporous Layers Spernjak, Dusan; Mukundan, Rangachary; Borup, Rodney L. ACS Applied Energy Materials, Vol. 1, Issue 11 https://doi.org/10.1021/acsaem.8b01059	journal	September 2018
Probing water distribution in compressed fuel-cell gas-diffusion layers using X-ray computed tomography Zenyuk, Iryna V.; Parkinson, Dilworth Y.; Hwang, Gisuk Electrochemistry Communications, Vol. 53 https://doi.org/10.1016/j.elecom.2015.02.005	journal	April 2015
Review of Advances in Thermal Spreading Resistance Problems Razavi, M.; Muzychka, Y. S.; Kocabiyik, S. Journal of Thermophysics and Heat Transfer, Vol. 30, Issue 4 https://doi.org/10.2514/1.T4801	journal	October 2016
Coupled Thermal and Water Management in Polymer Electrolyte Fuel Cells Weber, Adam Z.; Newman, John Journal of The Electrochemical Society, Vol. 153, Issue 12 https://doi.org/10.1149/1.2352039	journal	January 2006
Three-Dimensional Microstructural Imaging of Sulfur Poisoning-Induced Degradation in a Ni-YSZ Anode of Solid Oxide Fuel Cells Harris, William M.; Lombardo, Jeffrey J.; Nelson, George J. Scientific Reports, Vol. 4, Issue 1 https://doi.org/10.1038/srep05246	journal	June 2014
Improving water management in fuel cells through microporous layer modifications: Fast operando tomographic imaging of liquid water Nagai, Yasutaka; Eller, Jens; Hatanaka, Tatsuya Journal of Power Sources, Vol. 435 https://doi.org/10.1016/j.jpowsour.2019.226809	journal	September 2019
Operando Spectroscopic Microscopy of LiCoO2 Cathodes Outside Standard Operating Potentials Nelson Weker, Johanna; Wise, Anna M.; Lim, Kipil Electrochimica Acta, Vol. 247 https://doi.org/10.1016/j.electacta.2017.06.173	journal	September 2017
4D in situ visualization of electrode morphology changes during accelerated degradation in fuel cells by X-ray computed tomography White, Robin T.; Wu, Alex; Najm, Marina Journal of Power Sources, Vol. 350 https://doi.org/10.1016/j.jpowsour.2017.03.058	journal	May 2017
Imaging ionomer in fuel cell catalyst layers with synchrotron nano transmission x-ray microscopy Normile, Stanley J.; Zenyuk, Iryna V. Solid State Ionics, Vol. 335 https://doi.org/10.1016/j.ssi.2019.02.017	journal	July 2019
Direct three-dimensional reconstruction of a nanoporous catalyst layer for a polymer electrolyte fuel cell Ziegler, Christoph; Thiele, Simon; Zengerle, Roland Journal of Power Sources, Vol. 196, Issue 4 https://doi.org/10.1016/j.jpowsour.2010.09.044	journal	February 2011
Low-dose x-ray tomography through a deep convolutional neural network Yang, Xiaogang; De Andrade, Vincent; Scullin, William Scientific Reports, Vol. 8, Issue 1 https://doi.org/10.1038/s41598-018-19426-7	journal	February 2018
Fundamental limits to imaging resolution for focused ion beams Orloff, Jon Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, Vol. 14, Issue 6 https://doi.org/10.1116/1.588663	journal	November 1996
Modeling and high-resolution-imaging studies of water-content profiles in a polymer-electrolyte-fuel-cell membrane-electrode assembly Weber, A. Z.; Hickner, M. A. Electrochimica Acta, Vol. 53, Issue 26 https://doi.org/10.1016/j.electacta.2008.05.018	journal	November 2008
New Insights into Perfluorinated Sulfonic-Acid Ionomers Kusoglu, Ahmet; Weber, Adam Z. Chemical Reviews, Vol. 117, Issue 3 https://doi.org/10.1021/acs.chemrev.6b00159	journal	January 2017
X-ray nanotomography Withers, Philip J. Materials Today, Vol. 10, Issue 12 https://doi.org/10.1016/S1369-7021(07)70305-X	journal	December 2007
Mechanisms and effects of mechanical compression and dimensional change in polymer electrolyte fuel cells – A review Millichamp, Jason; Mason, Thomas J.; Neville, Tobias P. Journal of Power Sources, Vol. 284 https://doi.org/10.1016/j.jpowsour.2015.02.111	journal	June 2015
Impact of synchrotron radiation on fuel cell operation in imaging experiments Schneider, Armin; Wieser, Christian; Roth, Jörg Journal of Power Sources, Vol. 195, Issue 19 https://doi.org/10.1016/j.jpowsour.2010.04.032	journal	October 2010
Materials research and development focus areas for low cost automotive proton-exchange membrane fuel cells Gittleman, Craig S.; Kongkanand, Anusorn; Masten, David Current Opinion in Electrochemistry, Vol. 18 https://doi.org/10.1016/j.coelec.2019.10.009	journal	December 2019
Progress in In Situ X-Ray Tomographic Microscopy of Liquid Water in Gas Diffusion Layers of PEFC Eller, Jens; Rosén, Tomas; Marone, Federica Journal of The Electrochemical Society, Vol. 158, Issue 8 https://doi.org/10.1149/1.3596556	journal	January 2011
Designing the 3D Architecture of PGM-Free Cathodes for H ₂ /Air Proton Exchange Membrane Fuel Cells Li, Jingkun; Brüller, Sebastian; Sabarirajan, Dinesh C. ACS Applied Energy Materials, Vol. 2, Issue 10 https://doi.org/10.1021/acsaem.9b01181	journal	September 2019
X-Ray Tomography for Lithium Ion Battery Research: A Practical Guide Pietsch, Patrick; Wood, Vanessa Annual Review of Materials Research, Vol. 47, Issue 1 https://doi.org/10.1146/annurev-matsci-070616-123957	journal	July 2017
Interfacial analysis of a PEM electrolyzer using X-ray computed tomography Leonard, Emily; Shum, Andrew D.; Danilovic, Nemanja Sustainable Energy & Fuels, Vol. 4, Issue 2 https://doi.org/10.1039/C9SE00364A	journal	January 2020
Radiation damage in polymer films from grazing-incidence X-ray scattering measurements Vaselabadi, Saeed Ahmadi; Shakarisaz, David; Ruchhoeft, Paul Journal of Polymer Science Part B: Polymer Physics, Vol. 54, Issue 11 https://doi.org/10.1002/polb.24006	journal	February 2016
Progress and perspectives for atomic-resolution electron microscopy Smith, David J. Ultramicroscopy, Vol. 108, Issue 3 https://doi.org/10.1016/j.ultramic.2007.08.015	journal	February 2008
Understanding the Role of Interfaces for Water Management in Platinum Group Metal-Free Electrodes in Polymer Electrolyte Fuel Cells Liu, Jiangjin; Talarposhti, Morteza Rezaei; Asset, Tristan ACS Applied Energy Materials, Vol. 2, Issue 5 https://doi.org/10.1021/acsaem.9b00292	journal	April 2019
X-Ray Tomographic Microscopy (XTM) Using Synchrotron Radiation Kinney, J. H.; Nichols, M. C. Annual Review of Materials Science, Vol. 22, Issue 1 https://doi.org/10.1146/annurev.ms.22.080192.001005	journal	August 1992
Operando Sub-Second Tomographic Imaging of Water in PEFC Gas Diffusion Layers Eller, J.; Marone, F.; Buchi, F. N. ECS Transactions, Vol. 69, Issue 17 https://doi.org/10.1149/06917.0523ecst	journal	September 2015
Nano-structured platinum group metal-free catalysts and their integration in fuel cell electrode architectures Serov, Alexey; Shum, Andrew D.; Xiao, Xianghui Applied Catalysis B: Environmental, Vol. 237 https://doi.org/10.1016/j.apcatb.2017.08.067	journal	December 2018
X-ray transparent proton-exchange membrane fuel cell design for in situ wide and small angle scattering tomography Martens, Isaac; Vamvakeros, Antonis; Chattot, Raphael Journal of Power Sources, Vol. 437 https://doi.org/10.1016/j.jpowsour.2019.226906	journal	October 2019
Using operando techniques to understand and design high performance and stable alkaline membrane fuel cells Peng, Xiong; Kulkarni, Devashish; Huang, Ying Nature Communications, Vol. 11, Issue 1 https://doi.org/10.1038/s41467-020-17370-7	journal	July 2020
Design of a miniature flow cell for in situ x-ray imaging of redox flow batteries Jervis, Rhodri; Brown, Leon D.; Neville, Tobias P. Journal of Physics D: Applied Physics, Vol. 49, Issue 43 https://doi.org/10.1088/0022-3727/49/43/434002	journal	October 2016
Understanding water management in platinum group metal-free electrodes using neutron imaging Komini Babu, Siddharth; Spernjak, Dusan; Mukundan, Rangachary Journal of Power Sources, Vol. 472 https://doi.org/10.1016/j.jpowsour.2020.228442	journal	October 2020
Operando X-ray tomography and sub-second radiography for characterizing transport in polymer electrolyte membrane electrolyzer Leonard, Emily; Shum, Andrew D.; Normile, Stanley Electrochimica Acta, Vol. 276 https://doi.org/10.1016/j.electacta.2018.04.144	journal	June 2018
Hard X-ray-induced damage on carbon–binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent Journal of Synchrotron Radiation, Vol. 24, Issue 3 https://doi.org/10.1107/S1600577517003046	journal	March 2017
Bridging X-ray computed tomography and computational modeling for electrochemical energy-conversion and –storage Zenyuk, Iryna V. Current Opinion in Electrochemistry, Vol. 13 https://doi.org/10.1016/j.coelec.2018.10.016	journal	February 2019

Similar Records

Interfacial analysis of a PEM electrolyzer using X-ray computed tomography

Journal Article · 2019 · Sustainable Energy & Fuels · OSTI ID:1763359

Leonard, Emily; Shum, Andrew D.; Danilovic, Nemanja; +7 more

IN-SITU CORRELATIVE ELECTRON AND X-RAY OPTICAL-ENVIRONMENTAL CELL SAMPLE HOLDER FOR ELECTROCHEMICAL IMAGING AND SPECTROSCOPY. FINAL TECHNICAL REPORT

Technical Report · 2020 · OSTI ID:1616654

Alsem, Daan Hein

Operando X-ray tomography and sub-second radiography for characterizing transport in polymer electrolyte membrane electrolyzer

Journal Article · 2018 · Electrochimica Acta · OSTI ID:1480988

Leonard, Emily; Shum, Andrew D.; Normile, Stanley; +4 more

Title: Development of low temperature fuel cell holders for Operando x-ray micro and nano computed tomography to visualize water distribution

Citation Formats

References (46)

Similar Records

Related Subjects