Best practices for operando depth-resolving battery experiments

Liu, Hao; Li, Zhuo; Grenier, Antonin; Kamm, Gabrielle E.; Yin, Liang; Mattei, Gerard S.; Cosby, Monty R.; Khalifah, Peter G.; Chupas, Peter J.; Chapman, Karena W.

doi:10.1107/S1600576719016315

Title: Best practices for operando depth-resolving battery experiments

Abstract

We report operando studies that probe how electrochemical reactions propagate through a battery provide valuable feedback for optimizing the electrode architecture and for mitigating reaction heterogeneity. Transmission-geometry depth-profiling measurements carried out with the beam directed parallel to the battery layers – in a radial geometry – can provide quantitative structural insights that resolve depth-dependent reaction heterogeneity which are not accessible from conventional transmission measurements that traverse all battery layers. However, these spatially resolved measurements are susceptible to aberrations that do not affect conventional perpendicular-beam studies. Key practical considerations that can impact the interpretation of synchrotron depth-profiling studies, which are related to the signal-to-noise ratio, cell alignment and lateral heterogeneity, are described. Finally, strategies to enable accurate quantification of state of charge during rapid depth-profiling studies are presented.

Authors:

Liu, Hao ^[1]; Li, Zhuo ^[2]; Grenier, Antonin ^[3]; Kamm, Gabrielle E. ^[2]; Yin, Liang ^[2]; Mattei, Gerard S. ^[2]; Cosby, Monty R. ^[2];

^[4]; Chupas, Peter J. ^[2]; Chapman, Karena W. ^[3]

Argonne National Lab. (ANL), Lemont, IL (United States). Advanced Photon Source (APS)
Stony Brook Univ., NY (United States)
Argonne National Lab. (ANL), Lemont, IL (United States). Advanced Photon Source (APS); Stony Brook Univ., NY (United States)
Stony Brook Univ., NY (United States); Brookhaven National Lab. (BNL), Upton, NY (United States)

Publication Date:: Sat Feb 01 00:00:00 EST 2020

Research Org.:: Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II); Energy Frontier Research Centers (EFRC) (United States). Northeastern Center for Chemical Energy Storage (NECCES); Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Binghamton Univ., NY (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Energy Efficiency and Renewable Energy (EERE), Transportation Office. Vehicle Technologies Office; USDOE Office of Energy Efficiency and Renewable Energy (EERE), Vehicle Technologies Office (EE-3V)

OSTI Identifier:: 1633033

Alternate Identifier(s):: OSTI ID: 1597017; OSTI ID: 1630920; OSTI ID: 1637478

Report Number(s):: BNL-216037-2020-JAAM; BNL-216108-2020-JAAM
Journal ID: ISSN 1600-5767; JACGAR

Grant/Contract Number:: SC0012704; SC0012583; AC02-05CH11231; AC02-06CH11357

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Applied Crystallography (Online)

Additional Journal Information:: Journal Name: Journal of Applied Crystallography (Online); Journal Volume: 53; Journal Issue: 1; Journal ID: ISSN 1600-5767

Publisher:: International Union of Crystallography

Country of Publication:: United States

Language:: English

Subject:: 25 ENERGY STORAGE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; operando; batteries; pair distribution function analysis; depth profiling

Citation Formats


                    Liu, Hao, Li, Zhuo, Grenier, Antonin, Kamm, Gabrielle E., Yin, Liang, Mattei, Gerard S., Cosby, Monty R., Khalifah, Peter G., Chupas, Peter J., and Chapman, Karena W. Best practices for operando depth-resolving battery experiments.  United States: N. p., 2020. 
Web.  doi:10.1107/S1600576719016315.

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                    Liu, Hao, Li, Zhuo, Grenier, Antonin, Kamm, Gabrielle E., Yin, Liang, Mattei, Gerard S., Cosby, Monty R., Khalifah, Peter G., Chupas, Peter J., & Chapman, Karena W. Best practices for operando depth-resolving battery experiments.  United States.  https://doi.org/10.1107/S1600576719016315

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                    Liu, Hao, Li, Zhuo, Grenier, Antonin, Kamm, Gabrielle E., Yin, Liang, Mattei, Gerard S., Cosby, Monty R., Khalifah, Peter G., Chupas, Peter J., and Chapman, Karena W. Sat .  
"Best practices for operando depth-resolving battery experiments".  United States.  https://doi.org/10.1107/S1600576719016315.  https://www.osti.gov/servlets/purl/1633033.

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@article{osti_1633033,

  title        = {Best practices for operando depth-resolving battery experiments},

  author       = {Liu, Hao and Li, Zhuo and Grenier, Antonin and Kamm, Gabrielle E. and Yin, Liang and Mattei, Gerard S. and Cosby, Monty R. and Khalifah, Peter G. and Chupas, Peter J. and Chapman, Karena W.},

  abstractNote = {We report operando studies that probe how electrochemical reactions propagate through a battery provide valuable feedback for optimizing the electrode architecture and for mitigating reaction heterogeneity. Transmission-geometry depth-profiling measurements carried out with the beam directed parallel to the battery layers – in a radial geometry – can provide quantitative structural insights that resolve depth-dependent reaction heterogeneity which are not accessible from conventional transmission measurements that traverse all battery layers. However, these spatially resolved measurements are susceptible to aberrations that do not affect conventional perpendicular-beam studies. Key practical considerations that can impact the interpretation of synchrotron depth-profiling studies, which are related to the signal-to-noise ratio, cell alignment and lateral heterogeneity, are described. Finally, strategies to enable accurate quantification of state of charge during rapid depth-profiling studies are presented.},

  doi          = {10.1107/S1600576719016315},

  journal      = {Journal of Applied Crystallography (Online)},

  number       = 1,

  volume       = 53,

  place        = {United States},

  year         = {Sat Feb 01 00:00:00 EST 2020},

  month        = {Sat Feb 01 00:00:00 EST 2020}

}

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Title: Best practices for operando depth-resolving battery experiments

Abstract

Citation Formats

Capturing metastable structures during high-rate cycling of LiFePO4 nanoparticle electrodes journal, June 2014

Capillary-based micro-battery cell for in situ X-ray powder diffraction studies of working batteries: a study of the initial intercalation and deintercalation of lithium into graphite journal, October 2013

In Situ Energy Dispersive X-ray Diffraction Study of LiNi 0.8 Co 0.2 O 2 Cathode Material for Lithium Batteries journal, February 2001

Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries journal, September 2017

Mapping spatially inhomogeneous electrochemical reactions in battery electrodes using high energy X-rays journal, January 2013

Best Practices for Operando Battery Experiments: Influences of X-ray Experiment Design on Observed Electrochemical Reactivity journal, May 2015

Reactivity-Guided Interface Design in Na Metal Solid-State Batteries journal, April 2019

Methods and Protocols for Electrochemical Energy Storage Materials Research journal, November 2016

Thermodynamics, Kinetics and Structural Evolution of ε-LiVOPO 4 over Multiple Lithium Intercalation journal, February 2016

A radially accessible tubular in situ X-ray cell for spatially resolved operando scattering and spectroscopic studies of electrochemical energy storage devices journal, September 2016

In situ visualization of Li/Ag2VP2O8 batteries revealing rate-dependent discharge mechanism journal, January 2015

In situ X-ray diffraction of prototype sodium metal halide cells: Time and space electrochemical profiling journal, February 2011

Rational synthesis and electrochemical performance of LiVOPO 4 polymorphs journal, January 2019

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Mapping the Inhomogeneous Electrochemical Reaction Through Porous LiFePO 4 -Electrodes in a Standard Coin Cell Battery journal, March 2015

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GSAS-II : the genesis of a modern open-source all purpose crystallography software package journal, March 2013

Structural Evolution of Li[sub x]Mn[sub 2]O[sub 4] in Lithium-Ion Battery Cells Measured In Situ Using Synchrotron X-Ray Diffraction Techniques journal, January 1998

In situ X-ray diffraction and X-ray absorption studies of high-rate lithium-ion batteries journal, January 2001

Chemical Structures of Specific Sodium Ion Battery Components Determined by Operando Pair Distribution Function and X-ray Diffraction Computed Tomography journal, August 2017

Visualization of Electrochemical Reactions in Battery Materials with X-ray Microscopy and Mapping journal, April 2017

Capturing metastable structures during high-rate cycling of LiFePO4 nanoparticle electrodes
journal, June 2014

Capillary-based micro-battery cell for in situ X-ray powder diffraction studies of working batteries: a study of the initial intercalation and deintercalation of lithium into graphite
journal, October 2013

In Situ Energy Dispersive X-ray Diffraction Study of LiNi _0.8 Co _0.2 O ₂ Cathode Material for Lithium Batteries
journal, February 2001

Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries
journal, September 2017

Mapping spatially inhomogeneous electrochemical reactions in battery electrodes using high energy X-rays
journal, January 2013

Best Practices for Operando Battery Experiments: Influences of X-ray Experiment Design on Observed Electrochemical Reactivity
journal, May 2015

Reactivity-Guided Interface Design in Na Metal Solid-State Batteries
journal, April 2019

Methods and Protocols for Electrochemical Energy Storage Materials Research
journal, November 2016

Thermodynamics, Kinetics and Structural Evolution of ε-LiVOPO ₄ over Multiple Lithium Intercalation
journal, February 2016

A radially accessible tubular in situ X-ray cell for spatially resolved operando scattering and spectroscopic studies of electrochemical energy storage devices
journal, September 2016

In situ visualization of Li/Ag2VP2O8 batteries revealing rate-dependent discharge mechanism
journal, January 2015

In situ X-ray diffraction of prototype sodium metal halide cells: Time and space electrochemical profiling
journal, February 2011

Rational synthesis and electrochemical performance of LiVOPO ₄ polymorphs
journal, January 2019

Quantifying Reaction and Rate Heterogeneity in Battery Electrodes in 3D through Operando X-ray Diffraction Computed Tomography
journal, April 2019

Mapping the Inhomogeneous Electrochemical Reaction Through Porous LiFePO ₄ -Electrodes in a Standard Coin Cell Battery
journal, March 2015

In Situ X-ray Absorption Spectroscopic Study on LiNi _0.5 Mn _0.5 O ₂ Cathode Material during Electrochemical Cycling
journal, August 2003

GSAS-II : the genesis of a modern open-source all purpose crystallography software package
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Structural Evolution of Li[sub x]Mn[sub 2]O[sub 4] in Lithium-Ion Battery Cells Measured In Situ Using Synchrotron X-Ray Diffraction Techniques
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In situ X-ray diffraction and X-ray absorption studies of high-rate lithium-ion batteries
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journal, August 2017

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