4D nano-tomography of electrochemical energy devices using lab-based X-ray imaging

Heenan, T. M. M.; Finegan, D. P.; Tjaden, B.; Lu, X.; Iacoviello, F.; Millichamp, J.; Brett, D. J. L.; Shearing, P. R.

doi:10.1016/j.nanoen.2018.03.001

4D nano-tomography of electrochemical energy devices using lab-based X-ray imaging

Journal Article · Sat Mar 03 00:00:00 EST 2018 · Nano Energy

DOI:https://doi.org/10.1016/j.nanoen.2018.03.001· OSTI ID:1432607

Heenan, T. M. M. ^[1]; Finegan, D. P. ^[2]; Tjaden, B. ^[1]; Lu, X. ^[1]; Iacoviello, F. ^[1]; Millichamp, J. ^[1]; Brett, D. J. L. ^[1]; Shearing, P. R. ^[1]

UCL, London, London (United Kingdom)
UCL, London, London (United Kingdom); National Renewable Energy Lab. (NREL), Lakewood, CO (United States)

Electrochemical energy devices offer a variety of alternate means for low-carbon, multi-scale energy conversion and storage. Reactions in these devices are supported by electrodes with characteristically complex microstructures. To meet the increasing capacity and lifetime demands across a range of applications, it is essential to understand microstructural evolutions at a cell and electrode level which are thought to be critical aspects influencing material and device lifetime and performance. X-ray computed tomography (CT) has become a highly employed method for non-destructive characterisation of such microstructures with high spatial resolution. However, sub-micron resolutions present significant challenges for sample preparation and handling particularly in 4D studies, (three spatial dimensions plus time). Here, microstructural information is collected from the same region of interest within two electrode materials: a solid oxide fuel cell and the positive electrode from a lithium-ion battery. Using a lab-based X-ray instrument, tomograms with sub-micron resolutions were obtained between thermal cycling. The intricate microstructural evolutions captured within these two materials provide model examples of 4D X-ray nano-CT capabilities in tracking challenging degradation mechanisms. Furthermore, this technique is valuable in the advancement of electrochemical research as well as broader applications for materials characterisation.

View Accepted Manuscript (DOE)

Research Organization:: National Renewable Energy Laboratory (NREL), Golden, CO (United States)

Sponsoring Organization:: USDOE Office of Energy Efficiency and Renewable Energy (EERE)

Grant/Contract Number:: AC36-08GO28308

OSTI ID:: 1432607

Report Number(s):: NREL/JA--5400-71275

Journal Information:: Nano Energy, Journal Name: Nano Energy Journal Issue: C Vol. 47; ISSN 2211-2855

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

References (45)

Quantifying Bulk Electrode Strain and Material Displacement within Lithium Batteries via High-Speed Operando Tomography and Digital Volume Correlation Finegan, Donal P.; Tudisco, Erika; Scheel, Mario Advanced Science, Vol. 3, Issue 3 https://doi.org/10.1002/advs.201500332	journal	December 2015
In Situ Three-Dimensional Synchrotron X-Ray Nanotomography of the (De)lithiation Processes in Tin Anodes Wang, Jiajun; Chen-Wiegart, Yu-chen Karen; Wang, Jun Angewandte Chemie International Edition, Vol. 53, Issue 17 https://doi.org/10.1002/anie.201310402	journal	March 2014
Simulating the Impact of Particle Size Distribution on the Performance of Graphite Electrodes in Lithium-Ion Batteries Röder, Fridolin; Sonntag, Sören; Schröder, Daniel Energy Technology, Vol. 4, Issue 12 https://doi.org/10.1002/ente.201600232	journal	September 2016
Redox Cycling of Ni-Based Solid Oxide Fuel Cell Anodes: A Review Sarantaridis, D.; Atkinson, A. Fuel Cells, Vol. 7, Issue 3 https://doi.org/10.1002/fuce.200600028	journal	June 2007
Experimental and Theoretical Investigation of Degradation Mechanisms by Particle Coarsening in SOFC Electrodes Tanasini, P.; Cannarozzo, M.; Costamagna, P. Fuel Cells, Vol. 9, Issue 5 https://doi.org/10.1002/fuce.200800192	journal	October 2009
Three-Phase Segmentation of Solid Oxide Fuel Cell Anode Materials Using Lab Based X-ray Nano-Computed Tomography Heenan, T. M. M.; Bailey, J. J.; Lu, X. Fuel Cells, Vol. 17, Issue 1 https://doi.org/10.1002/fuce.201600176	journal	February 2017
Prevent thermal runaway of lithium-ion batteries with minichannel cooling Xu, Jian; Lan, Chuanjin; Qiao, Yu Applied Thermal Engineering, Vol. 110 https://doi.org/10.1016/j.applthermaleng.2016.08.151	journal	January 2017
3D reconstruction of SOFC anodes using a focused ion beam lift-out technique Shearing, P. R.; Golbert, J.; Chater, R. J. Chemical Engineering Science, Vol. 64, Issue 17 https://doi.org/10.1016/j.ces.2009.05.038	journal	September 2009
On the origin and application of the Bruggeman correlation for analysing transport phenomena in electrochemical systems Tjaden, Bernhard; Cooper, Samuel J.; Brett, Daniel JL Current Opinion in Chemical Engineering, Vol. 12 https://doi.org/10.1016/j.coche.2016.02.006	journal	May 2016
In situ synchrotron X-ray micro-tomography study of pitting corrosion in stainless steel Ghahari, S. Majid; Davenport, Alison J.; Rayment, Trevor Corrosion Science, Vol. 53, Issue 9 https://doi.org/10.1016/j.corsci.2011.05.040	journal	September 2011
Characterization of the 3-dimensional microstructure of a graphite negative electrode from a Li-ion battery Shearing, P. R.; Howard, L. E.; Jørgensen, P. S. Electrochemistry Communications, Vol. 12, Issue 3 https://doi.org/10.1016/j.elecom.2009.12.038	journal	March 2010
Investigation of 3D water transport paths in gas diffusion layers by combined in-situ synchrotron X-ray radiography and tomography Markötter, H.; Manke, I.; Krüger, Ph. Electrochemistry Communications, Vol. 13, Issue 9 https://doi.org/10.1016/j.elecom.2011.06.023	journal	September 2011
Morphology of nanoporous carbon-binder domains in Li-ion batteries—A FIB-SEM study Vierrath, Severin; Zielke, Lukas; Moroni, Riko Electrochemistry Communications, Vol. 60 https://doi.org/10.1016/j.elecom.2015.09.010	journal	November 2015
A 3D thermal runaway propagation model for a large format lithium ion battery module Feng, Xuning; Lu, Languang; Ouyang, Minggao Energy, Vol. 115 https://doi.org/10.1016/j.energy.2016.08.094	journal	November 2016
Three dimensional stress analysis of solid oxide fuel cell anode micro structure Celik, Selahattin; Ibrahimoglu, Beycan; Toros, Serkan International Journal of Hydrogen Energy, Vol. 39, Issue 33 https://doi.org/10.1016/j.ijhydene.2014.09.110	journal	November 2014
Hydrogen and fuel cell technologies for heating: A review Dodds, Paul E.; Staffell, Iain; Hawkes, Adam D. International Journal of Hydrogen Energy, Vol. 40, Issue 5 https://doi.org/10.1016/j.ijhydene.2014.11.059	journal	February 2015
X-ray nano computerised tomography of SOFC electrodes using a focused ion beam sample-preparation technique Shearing, P. R.; Gelb, J.; Brandon, N. P. Journal of the European Ceramic Society, Vol. 30, Issue 8 https://doi.org/10.1016/j.jeurceramsoc.2010.02.004	journal	June 2010
Understanding and approaches for the durability issues of Pt-based catalysts for PEM fuel cell Shao, Yuyan; Yin, Geping; Gao, Yunzhi Journal of Power Sources, Vol. 171, Issue 2, p. 558-566 https://doi.org/10.1016/j.jpowsour.2007.07.004	journal	September 2007
Fundamental mechanisms limiting solid oxide fuel cell durability Yokokawa, Harumi; Tu, Hengyong; Iwanschitz, Boris Journal of Power Sources, Vol. 182, Issue 2 https://doi.org/10.1016/j.jpowsour.2008.02.016	journal	August 2008
Quantification of SOFC anode microstructure based on dual beam FIB-SEM technique Iwai, Hiroshi; Shikazono, Naoki; Matsui, Toshiaki Journal of Power Sources, Vol. 195, Issue 4 https://doi.org/10.1016/j.jpowsour.2009.09.005	journal	February 2010
Analysis of the three-dimensional microstructure of a solid-oxide fuel cell anode using nano X-ray tomography Guan, Yong; Li, Wenjie; Gong, Yunhui Journal of Power Sources, Vol. 196, Issue 4 https://doi.org/10.1016/j.jpowsour.2010.09.059	journal	February 2011
Stress analysis of solid oxide fuel cell anode microstructure reconstructed from focused ion beam tomography Clague, R.; Shearing, P. R.; Lee, P. D. Journal of Power Sources, Vol. 196, Issue 21 https://doi.org/10.1016/j.jpowsour.2010.12.097	journal	November 2011
Investigating the effect of thermal gradients on stress in solid oxide fuel cell anodes using combined synchrotron radiation and thermal imaging Robinson, James B.; Brown, Leon D.; Jervis, Rhodri Journal of Power Sources, Vol. 288 https://doi.org/10.1016/j.jpowsour.2015.04.104	journal	August 2015
Energy distributions exhibited during thermal runaway of commercial lithium ion batteries used for human spaceflight applications Yayathi, Sandeep; Walker, William; Doughty, Daniel Journal of Power Sources, Vol. 329 https://doi.org/10.1016/j.jpowsour.2016.08.078	journal	October 2016
Experimental and theoretical analysis of a method to predict thermal runaway in Li-ion cells Shah, Krishna; Chalise, Divya; Jain, Ankur Journal of Power Sources, Vol. 330 https://doi.org/10.1016/j.jpowsour.2016.08.133	journal	October 2016
Microstructural degradation of silicon electrodes during lithiation observed via operando X-ray tomographic imaging Taiwo, Oluwadamilola O.; Paz-García, Juan M.; Hall, Stephen A. Journal of Power Sources, Vol. 342 https://doi.org/10.1016/j.jpowsour.2016.12.070	journal	February 2017
Correlation between triple phase boundary and the microstructure of Solid Oxide Fuel Cell anodes: The role of composition, porosity and Ni densification Lu, Xuekun; Heenan, Thomas M. M.; Bailey, Josh J. Journal of Power Sources, Vol. 365 https://doi.org/10.1016/j.jpowsour.2017.08.095	journal	October 2017
Li-ion battery materials: present and future Nitta, Naoki; Wu, Feixiang; Lee, Jung Tae Materials Today, Vol. 18, Issue 5 https://doi.org/10.1016/j.mattod.2014.10.040	journal	June 2015
Nanoscale chemical mapping of Li-ion battery cathode material by FIB-SEM and TOF-SIMS multi-modal microscopy Sui, Tan; Song, Bohang; Dluhos, Jiri Nano Energy, Vol. 17 https://doi.org/10.1016/j.nanoen.2015.08.013	journal	October 2015
TauFactor: An open-source application for calculating tortuosity factors from tomographic data Cooper, S. J.; Bertei, A.; Shearing, P. R. SoftwareX, Vol. 5 https://doi.org/10.1016/j.softx.2016.09.002	journal	January 2016
Exploring microstructural changes associated with oxidation in Ni–YSZ SOFC electrodes using high resolution X-ray computed tomography Shearing, P. R.; Bradley, R. S.; Gelb, J. Solid State Ionics, Vol. 216 https://doi.org/10.1016/j.ssi.2011.10.015	journal	May 2012
Three-dimensional reconstruction of a solid-oxide fuel-cell anode Wilson, James R.; Kobsiriphat, Worawarit; Mendoza, Roberto Nature Materials, Vol. 5, Issue 7 https://doi.org/10.1038/nmat1668	journal	June 2006
Investigating lithium-ion battery materials during overcharge-induced thermal runaway: an operando and multi-scale X-ray CT study Finegan, Donal P.; Scheel, Mario; Robinson, James B. Physical Chemistry Chemical Physics, Vol. 18, Issue 45 https://doi.org/10.1039/C6CP04251A	journal	January 2016
Characterising thermal runaway within lithium-ion cells by inducing and monitoring internal short circuits Finegan, Donal P.; Darcy, Eric; Keyser, Matthew Energy & Environmental Science, Vol. 10, Issue 6 https://doi.org/10.1039/C7EE00385D	journal	January 2017
Oxidation kinetics of nickel nanoparticles Karmhag, Richard; Niklasson, Gunnar A.; Nygren, Mats Journal of Applied Physics, Vol. 89, Issue 5 https://doi.org/10.1063/1.1325002	journal	March 2001
Electrical Properties of NiO Morin, F. J. Physical Review, Vol. 93, Issue 6 https://doi.org/10.1103/PhysRev.93.1199	journal	March 1954
High-pressure and high-temperature electrical resistivity of ferromagnetic transition metals: Nickel and iron Yousuf, Mohammad; Sahu, P. Ch.; Rajan, K. Govinda Physical Review B, Vol. 34, Issue 11 https://doi.org/10.1103/PhysRevB.34.8086	journal	December 1986
Laser-preparation of geometrically optimised samples for X-ray nano-CT: LASER-PREPARATION OF GEOMETRICALLY OPTIMISED SAMPLES FOR X-RAY NANO-CT Bailey, J. J.; Heenan, T. M. M.; Finegan, D. P. Journal of Microscopy, Vol. 267, Issue 3 https://doi.org/10.1111/jmi.12577	journal	May 2017
A Review of Image Denoising Algorithms, with a New One Buades, A.; Coll, B.; Morel, J. M. Multiscale Modeling & Simulation, Vol. 4, Issue 2 https://doi.org/10.1137/040616024	journal	January 2005
Diffusion Limitations in the Porous Anodes of SOFCs Williford, R. E.; Chick, L. A.; Maupin, G. D. Journal of The Electrochemical Society, Vol. 150, Issue 8 https://doi.org/10.1149/1.1586300	journal	January 2003
Thermal Expansion of Nickel-Zirconia Anodes in Solid Oxide Fuel Cells during Fabrication and Operation Mori, Masashi Journal of The Electrochemical Society, Vol. 145, Issue 4 https://doi.org/10.1149/1.1838468	journal	January 1998
On the Mechanism of Low-Temperature Oxidation (23°–450°C) of Polycrystalline Nickel Graham, M. J.; Cohen, M. Journal of The Electrochemical Society, Vol. 119, Issue 7 https://doi.org/10.1149/1.2404360	journal	January 1972
Nondestructive Reconstruction and Analysis of SOFC Anodes Using X-ray Computed Tomography at Sub-50 nm Resolution Izzo, John R.; Joshi, Abhijit S.; Grew, Kyle N. Journal of The Electrochemical Society, Vol. 155, Issue 5 https://doi.org/10.1149/1.2895067	journal	January 2008
Intercalation-Induced Stress and Heat Generation within Single Lithium-Ion Battery Cathode Particles Zhang, Xiangchun; Sastry, Ann Marie; Shyy, Wei Journal of The Electrochemical Society, Vol. 155, Issue 7 https://doi.org/10.1149/1.2926617	journal	January 2008
3D Characterization of Diffusivities and Its Impact on Mass Flux and Concentration Overpotential in SOFC Anode Lu, Xuekun; Tjaden, Benhard; Bertei, Antonio Journal of The Electrochemical Society, Vol. 164, Issue 4 https://doi.org/10.1149/2.0111704jes	journal	January 2017

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4D imaging of lithium-batteries using correlative neutron and X-ray tomography with a virtual unrolling technique Ziesche, Ralf F.; Arlt, Tobias; Finegan, Donal P. Nature Communications, Vol. 11, Issue 1 https://doi.org/10.1038/s41467-019-13943-3	journal	February 2020
Evaluating microstructure evolution in an SOFC electrode using digital volume correlation Heenan, T. M. M.; Lu, X.; Finegan, D. P. Sustainable Energy & Fuels, Vol. 2, Issue 12 https://doi.org/10.1039/c8se00292d	journal	January 2018
Thermally Driven SOFC Degradation in 4D: Part II. Macroscale Heenan, T. M. M.; Lu, X.; Robinson, J. B. Journal of The Electrochemical Society, Vol. 165, Issue 11 https://doi.org/10.1149/2.0061811jes	journal	January 2018
Thermally Driven SOFC Degradation in 4D: Part I. Microscale Heenan, T. M. M.; Lu, X.; Iacoviello, F. Journal of The Electrochemical Society, Vol. 165, Issue 11 https://doi.org/10.1149/2.0151811jes	journal	January 2018
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