X-ray Nanocomputed Tomography in Zernike Phase Contrast for Studying 3D Morphology of Li–O2 Battery Electrode
Abstract
In this work, we investigated the lithium peroxide (Li2O2) and pore size distribution in lithium-O2 battery electrodes at different states of charge using transmission X-ray microscopy coupled with Zernike phase contrast to carry out nano-Computed Tomography. We report that such technique enables, at the nanoscale, to distinguish light elements such as carbon and Li2O2 in Li-O2 battery cathode electrodes. We verified by wave-propagation simulation that this approach efficiently improves the contrast of images in comparison with the pure absorption. The Li2O2 distribution and thickness, interphases, and pore network are visualized and quantified, which give a valuable insight into our cathode architecture. From this 3D analysis, we highlight modifications of the air-cathode morphology and the Li2O2 spatial organization as well as their potential implication in terms of carbon surface passivation and pore-clogging. After the full recharge process, this technique can also reveal the spatial distribution of the residual Li2O2 and other byproducts.
- Authors:
-
- Univ. de Picardie Jules Verne, Amiens (France). Lab. de Reactivite et Chimie des Solides (LRCS); Reseau sur le Stockage Electrochimique de l'Energie (RS2E), Amiens (France)
- Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
- Univ. de Picardie Jules Verne, Amiens (France). Lab. de Reactivite et Chimie des Solides (LRCS); Nanyang Technological Univ. (Singapore)
- Univ. de Picardie Jules Verne, Amiens (France). Lab. de Reactivite et Chimie des Solides (LRCS); Reseau sur le Stockage Electrochimique de l'Energie (RS2E), Amiens (France); Inst. Univ. de France, Paris (France); ALISTORE-European Research Inst., Amiens (France)
- Univ. de Picardie Jules Verne, Amiens (France). Lab. de Reactivite et Chimie des Solides (LRCS); Reseau sur le Stockage Electrochimique de l'Energie (RS2E), Amiens (France); ALISTORE-European Research Inst., Amiens (France)
- Publication Date:
- Research Org.:
- Argonne National Lab. (ANL), Argonne, IL (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES)
- OSTI Identifier:
- 1785721
- Grant/Contract Number:
- AC02-06CH11357
- Resource Type:
- Accepted Manuscript
- Journal Name:
- ACS Applied Energy Materials
- Additional Journal Information:
- Journal Volume: 3; Journal Issue: 5; Journal ID: ISSN 2574-0962
- Publisher:
- American Chemical Society (ACS)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 25 ENERGY STORAGE; Li-O2 battery; Li2O2 spatial organization; x-ray nanocomputed tomography; Zernike phase contrast; electrode architecture characterization; x-rays; oxides; electrodes; batteries; tomography
Citation Formats
Su, Zeliang, De Andrade, Vincent, Cretu, Sorina, Yin, Yinghui, Wojcik, Michael J., Franco, Alejandro A., and Demortière, Arnaud. X-ray Nanocomputed Tomography in Zernike Phase Contrast for Studying 3D Morphology of Li–O2 Battery Electrode. United States: N. p., 2020.
Web. doi:10.1021/acsaem.9b02236.
Su, Zeliang, De Andrade, Vincent, Cretu, Sorina, Yin, Yinghui, Wojcik, Michael J., Franco, Alejandro A., & Demortière, Arnaud. X-ray Nanocomputed Tomography in Zernike Phase Contrast for Studying 3D Morphology of Li–O2 Battery Electrode. United States. https://doi.org/10.1021/acsaem.9b02236
Su, Zeliang, De Andrade, Vincent, Cretu, Sorina, Yin, Yinghui, Wojcik, Michael J., Franco, Alejandro A., and Demortière, Arnaud. Tue .
"X-ray Nanocomputed Tomography in Zernike Phase Contrast for Studying 3D Morphology of Li–O2 Battery Electrode". United States. https://doi.org/10.1021/acsaem.9b02236. https://www.osti.gov/servlets/purl/1785721.
@article{osti_1785721,
title = {X-ray Nanocomputed Tomography in Zernike Phase Contrast for Studying 3D Morphology of Li–O2 Battery Electrode},
author = {Su, Zeliang and De Andrade, Vincent and Cretu, Sorina and Yin, Yinghui and Wojcik, Michael J. and Franco, Alejandro A. and Demortière, Arnaud},
abstractNote = {In this work, we investigated the lithium peroxide (Li2O2) and pore size distribution in lithium-O2 battery electrodes at different states of charge using transmission X-ray microscopy coupled with Zernike phase contrast to carry out nano-Computed Tomography. We report that such technique enables, at the nanoscale, to distinguish light elements such as carbon and Li2O2 in Li-O2 battery cathode electrodes. We verified by wave-propagation simulation that this approach efficiently improves the contrast of images in comparison with the pure absorption. The Li2O2 distribution and thickness, interphases, and pore network are visualized and quantified, which give a valuable insight into our cathode architecture. From this 3D analysis, we highlight modifications of the air-cathode morphology and the Li2O2 spatial organization as well as their potential implication in terms of carbon surface passivation and pore-clogging. After the full recharge process, this technique can also reveal the spatial distribution of the residual Li2O2 and other byproducts.},
doi = {10.1021/acsaem.9b02236},
journal = {ACS Applied Energy Materials},
number = 5,
volume = 3,
place = {United States},
year = {Tue Mar 24 00:00:00 EDT 2020},
month = {Tue Mar 24 00:00:00 EDT 2020}
}
Works referenced in this record:
Erratum: Li–O2 and Li–S batteries with high energy storage
journal, December 2011
- Bruce, Peter G.; Freunberger, Stefan A.; Hardwick, Laurence J.
- Nature Materials, Vol. 11, Issue 2
Redox Mediators for Li-O 2 Batteries: Status and Perspectives
journal, November 2017
- Park, Jin-Bum; Lee, Seon Hwa; Jung, Hun-Gi
- Advanced Materials, Vol. 30, Issue 1
TomoPy: a framework for the analysis of synchrotron tomographic data
journal, August 2014
- Gürsoy, Dogˇa; De Carlo, Francesco; Xiao, Xianghui
- Journal of Synchrotron Radiation, Vol. 21, Issue 5
Free-standing, hierarchically porous carbon nanotube film as a binder-free electrode for high-energy Li–O2 batteries
journal, January 2013
- Liu, Shaohong; Wang, Zhiyu; Yu, Chang
- Journal of Materials Chemistry A, Vol. 1, Issue 39
Full-field transmission x-ray microscopy for bio-imaging
journal, September 2009
- Andrews, J. C.; Brennan, S.; Liu, Y.
- Journal of Physics: Conference Series, Vol. 186
Four-Dimensional Studies of Morphology Evolution in Lithium–Sulfur Batteries
journal, August 2018
- Tan, Chun; Heenan, Thomas M. M.; Ziesche, Ralf F.
- ACS Applied Energy Materials, Vol. 1, Issue 9
Investigation of bi-porous electrodes for lithium oxygen batteries
journal, July 2018
- Gaya, Caroline; Yin, Yinghui; Torayev, Amangeldi
- Electrochimica Acta, Vol. 279
Decoupling Energy Storage from Electrochemical Reactions in Li–Air Batteries toward Achieving Continuous Discharge
journal, February 2017
- Takechi, Kensuke; Singh, Nikhilendra; Arthur, Timothy S.
- ACS Energy Letters, Vol. 2, Issue 3
Stochasticity of Pores Interconnectivity in Li–O 2 Batteries and its Impact on the Variations in Electrochemical Performance
journal, February 2018
- Torayev, Amangeldi; Rucci, Alexis; Magusin, Pieter C. M. M.
- The Journal of Physical Chemistry Letters, Vol. 9, Issue 4
Quantification of Heterogeneous Degradation in Li‐Ion Batteries
journal, May 2019
- Yang, Yang; Xu, Rong; Zhang, Kai
- Advanced Energy Materials, Vol. 9, Issue 25
The Carbon Electrode in Nonaqueous Li–O2 Cells
journal, December 2012
- Ottakam Thotiyl, Muhammed M.; Freunberger, Stefan A.; Peng, Zhangquan
- Journal of the American Chemical Society, Vol. 135, Issue 1, p. 494-500
Impact of the Cathode Microstructure on the Discharge Performance of Lithium Air Batteries: A Multiscale Model
journal, January 2014
- Xue, Kan-Hao; Nguyen, Trong-Khoa; Franco, Alejandro A.
- Journal of The Electrochemical Society, Vol. 161, Issue 8
Direct Detection of Discharge Products in Lithium-Oxygen Batteries by Solid-State NMR Spectroscopy
journal, July 2012
- Leskes, Michal; Drewett, Nicholas E.; Hardwick, Laurence J.
- Angewandte Chemie International Edition, Vol. 51, Issue 34
Thick Binder-Free Electrodes for Li-Ion Battery Fabricated Using Templating Approach and Spark Plasma Sintering Reveals High Areal Capacity
journal, January 2018
- Elango, Rakesh; Demortière, Arnaud; De Andrade, Vincent
- Advanced Energy Materials, Vol. 8, Issue 15
Aprotic and Aqueous Li–O2 Batteries
journal, April 2014
- Lu, Jun; Li, Li; Park, Jin-Bum
- Chemical Reviews, Vol. 114, Issue 11, p. 5611-5640
Three-dimensional phase segregation of micro-porous layers for fuel cells by nano-scale X-ray computed tomography
journal, April 2016
- Andisheh-Tadbir, Mehdi; Orfino, Francesco P.; Kjeang, Erik
- Journal of Power Sources, Vol. 310
Tortuosity Anisotropy in Lithium-Ion Battery Electrodes
journal, October 2013
- Ebner, Martin; Chung, Ding-Wen; García, R. Edwin
- Advanced Energy Materials, Vol. 4, Issue 5
Enhanced Cyclability of Li–O 2 Batteries Based on TiO 2 Supported Cathodes with No Carbon or Binder
journal, April 2014
- Zhao, Guangyu; Mo, Runwei; Wang, Baoyu
- Chemistry of Materials, Vol. 26, Issue 8
The application of phase contrast X-ray techniques for imaging Li-ion battery electrodes
journal, April 2014
- Eastwood, D. S.; Bradley, R. S.; Tariq, F.
- Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, Vol. 324
Probing the Reaction Kinetics of the Charge Reactions of Nonaqueous Li–O 2 Batteries
journal, December 2012
- Lu, Yi-Chun; Shao-Horn, Yang
- The Journal of Physical Chemistry Letters, Vol. 4, Issue 1
Identifying Reactive Sites and Transport Limitations of Oxygen Reactions in Aprotic Lithium-O 2 Batteries at the Stage of Sudden Death
journal, March 2016
- Wang, Jiawei; Zhang, Yelong; Guo, Limin
- Angewandte Chemie International Edition, Vol. 55, Issue 17
Defect Chemistry in Discharge Products of Li-O 2 Batteries
journal, November 2018
- Dai, Wenrui; Cui, Xinhang; Zhou, Yin
- Small Methods, Vol. 3, Issue 3
Superior Rechargeability and Efficiency of Lithium-Oxygen Batteries: Hierarchical Air Electrode Architecture Combined with a Soluble Catalyst
journal, March 2014
- Lim, Hee-Dae; Song, Hyelynn; Kim, Jinsoo
- Angewandte Chemie International Edition, Vol. 53, Issue 15
Reaction chemistry in rechargeable Li–O 2 batteries
journal, January 2017
- Lim, Hee-Dae; Lee, Byungju; Bae, Youngjoon
- Chemical Society Reviews, Vol. 46, Issue 10
Discharge Performance of Li–O 2 Batteries Using a Multiscale Modeling Approach
journal, June 2015
- Bao, Jie; Xu, Wu; Bhattacharya, Priyanka
- The Journal of Physical Chemistry C, Vol. 119, Issue 27
In situ investigation of pore clogging during discharge of a Li/O2 battery by electrochemical impedance spectroscopy
journal, March 2015
- Bardenhagen, Ingo; Yezerska, Olga; Augustin, Matthias
- Journal of Power Sources, Vol. 278
Anomalous Discharge Product Distribution in Lithium-Air Cathodes
journal, April 2012
- Nanda, Jagjit; Bilheux, Hassina; Voisin, Sophie
- The Journal of Physical Chemistry C, Vol. 116, Issue 15
Lithium−Air Battery: Promise and Challenges
journal, June 2010
- Girishkumar, G.; McCloskey, B.; Luntz, A. C.
- The Journal of Physical Chemistry Letters, Vol. 1, Issue 14
Current density dependence of peroxide formation in the Li–O2 battery and its effect on charge
journal, January 2013
- Adams, Brian D.; Radtke, Claudio; Black, Robert
- Energy & Environmental Science, Vol. 6, Issue 6
Quantification and modeling of mechanical degradation in lithium-ion batteries based on nanoscale imaging
journal, June 2018
- Müller, Simon; Pietsch, Patrick; Brandt, Ben-Elias
- Nature Communications, Vol. 9, Issue 1
Three-dimensional localization of nanoscale battery reactions using soft X-ray tomography
journal, March 2018
- Yu, Young-Sang; Farmand, Maryam; Kim, Chunjoong
- Nature Communications, Vol. 9, Issue 1
Relative merits and limiting factors for x-ray and electron microscopy of thick, hydrated organic materials
journal, January 2018
- Du, Ming; Jacobsen, Chris
- Ultramicroscopy, Vol. 184
In situ characterization of Si-based anodes by coupling synchrotron X-ray tomography and diffraction
journal, February 2019
- Vanpeene, V.; King, A.; Maire, E.
- Nano Energy, Vol. 56
In Situ Transmission Electron Microscopy Observations of Electrochemical Oxidation of Li 2 O 2
journal, April 2013
- Zhong, Li; Mitchell, Robert R.; Liu, Yang
- Nano Letters, Vol. 13, Issue 5
Integration of TomoPy and the ASTRA toolbox for advanced processing and reconstruction of tomographic synchrotron data
journal, April 2016
- Pelt, Daniël M.; Gürsoy, Dogˇa; Palenstijn, Willem Jan
- Journal of Synchrotron Radiation, Vol. 23, Issue 3
Operando liquid cell electron microscopy of discharge and charge kinetics in lithium-oxygen batteries
journal, July 2018
- He, Kun; Bi, Xuanxuan; Yuan, Yifei
- Nano Energy, Vol. 49