Li+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteries

Irregular Li heterostructure growth at the interphase between the solid electrolyte and anode reduces solid-state Li metal battery (SSLMB) performance, but the fundamental cause is still elusive. Measuring and imaging Li ^+ ion diffusion in operando inside an SSLMB using a commercially standard cell...

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Main Authors: Chun Huang, Matthew D Wilson, Ben Cline, Abeiram Sivarajah, Wiebe Stolp, Matthieu N Boone, Thomas Connolley, Chu Lun Alex Leung
Format: Article
Language:English
Published: IOP Publishing 2025-01-01
Series:JPhys Energy
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Online Access:https://doi.org/10.1088/2515-7655/adafda
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author Chun Huang
Matthew D Wilson
Ben Cline
Abeiram Sivarajah
Wiebe Stolp
Matthieu N Boone
Thomas Connolley
Chu Lun Alex Leung
author_facet Chun Huang
Matthew D Wilson
Ben Cline
Abeiram Sivarajah
Wiebe Stolp
Matthieu N Boone
Thomas Connolley
Chu Lun Alex Leung
author_sort Chun Huang
collection DOAJ
description Irregular Li heterostructure growth at the interphase between the solid electrolyte and anode reduces solid-state Li metal battery (SSLMB) performance, but the fundamental cause is still elusive. Measuring and imaging Li ^+ ion diffusion in operando inside an SSLMB using a commercially standard cell configuration are extremely challenging because the ultra-light Li element exhibits a minute signal-to-noise ratio using most x-ray-related characterization methods, and the weak x-ray signals of Li ^+ are buried by strong signals of other heavy transition metal elements in the cathode and battery enclosure. Here, we pioneer novel operando correlative imaging of coupling x-ray Compton scattering with computed tomography (XCS-CT), which is able to quantify the interplay between spatially resolved Li ^+ ion diffusion kinetics and Li ^0 metal structure growth at the interphases of both the anode and cathode sides inside a full-cell SSLMB using a solid polymer electrolyte (SPE) and commercially standard cell configuration during (dis)charging. We show a 61% increase in the efficiency of extracting Li ^+ ions from the cathode LiNi _0.6 Mn _0.2 Co _0.2 O _2 to the anode during charging at 0.1 C compared with at 1 C due to restricted Li ^+ ion diffusion at the higher rate inside SSLMB. However, this led to the formation of a more irregular interfacial morphology, consisting not only of Li ^0 dendrites, but also sub-surface pore formation at the anode/SPE interphase. We find that surprisingly, the irregular Li ^0 structure initiation and growth are accelerated during the first Li stripping step, not the Li plating step, and the root cause is the onset imbalance of Li ^+ ion diffusion and redox reactions between the anode and cathode. These insights highlight the benefits of asymmetric charging and discharging rates as a promising solution to improving SSLMB performance with SPEs. The operando correlative XCS-CT imaging technique has the potential to study the relationship between active ion concentrations and buried morphological changes for a variety of battery chemistries.
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spelling doaj-art-59cc3719a6534d95b3003e9b23e913fe2025-08-20T02:12:50ZengIOP PublishingJPhys Energy2515-76552025-01-017202500910.1088/2515-7655/adafdaLi+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteriesChun Huang0https://orcid.org/0000-0001-6548-2977Matthew D Wilson1Ben Cline2Abeiram Sivarajah3https://orcid.org/0009-0005-2330-6138Wiebe Stolp4https://orcid.org/0000-0003-0282-4401Matthieu N Boone5Thomas Connolley6https://orcid.org/0000-0002-1851-3467Chu Lun Alex Leung7https://orcid.org/0000-0002-4153-7512Department of Materials, Imperial College London , London SW7 2AZ, United Kingdom; The Faraday Institution , Didcot OX11 0RA, United Kingdom; Research Complex at Harwell , Rutherford Appleton Laboratory, Didcot OX11 0FA, United KingdomSTFC-UKRI , Rutherford Appleton Laboratory, Didcot OX11 0QX, United KingdomSTFC-UKRI , Rutherford Appleton Laboratory, Didcot OX11 0QX, United KingdomDepartment of Materials, Imperial College London , London SW7 2AZ, United KingdomRadiation Physics, Department of Physics and Astronomy, Ghent University , Proeftuinstraat 86/N12, 9000 Gent, BelgiumRadiation Physics, Department of Physics and Astronomy, Ghent University , Proeftuinstraat 86/N12, 9000 Gent, BelgiumDiamond Light Source , Didcot OX11 0QX, United KingdomResearch Complex at Harwell , Rutherford Appleton Laboratory, Didcot OX11 0FA, United Kingdom; Department of Mechanical Engineering, University College London , London WC1E 7JE, United KingdomIrregular Li heterostructure growth at the interphase between the solid electrolyte and anode reduces solid-state Li metal battery (SSLMB) performance, but the fundamental cause is still elusive. Measuring and imaging Li ^+ ion diffusion in operando inside an SSLMB using a commercially standard cell configuration are extremely challenging because the ultra-light Li element exhibits a minute signal-to-noise ratio using most x-ray-related characterization methods, and the weak x-ray signals of Li ^+ are buried by strong signals of other heavy transition metal elements in the cathode and battery enclosure. Here, we pioneer novel operando correlative imaging of coupling x-ray Compton scattering with computed tomography (XCS-CT), which is able to quantify the interplay between spatially resolved Li ^+ ion diffusion kinetics and Li ^0 metal structure growth at the interphases of both the anode and cathode sides inside a full-cell SSLMB using a solid polymer electrolyte (SPE) and commercially standard cell configuration during (dis)charging. We show a 61% increase in the efficiency of extracting Li ^+ ions from the cathode LiNi _0.6 Mn _0.2 Co _0.2 O _2 to the anode during charging at 0.1 C compared with at 1 C due to restricted Li ^+ ion diffusion at the higher rate inside SSLMB. However, this led to the formation of a more irregular interfacial morphology, consisting not only of Li ^0 dendrites, but also sub-surface pore formation at the anode/SPE interphase. We find that surprisingly, the irregular Li ^0 structure initiation and growth are accelerated during the first Li stripping step, not the Li plating step, and the root cause is the onset imbalance of Li ^+ ion diffusion and redox reactions between the anode and cathode. These insights highlight the benefits of asymmetric charging and discharging rates as a promising solution to improving SSLMB performance with SPEs. The operando correlative XCS-CT imaging technique has the potential to study the relationship between active ion concentrations and buried morphological changes for a variety of battery chemistries.https://doi.org/10.1088/2515-7655/adafdasolid-state batteriescorrelative imaginglithium ion concentrationmicrostructurex-ray Compton scatteringmass transport
spellingShingle Chun Huang
Matthew D Wilson
Ben Cline
Abeiram Sivarajah
Wiebe Stolp
Matthieu N Boone
Thomas Connolley
Chu Lun Alex Leung
Li+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteries
JPhys Energy
solid-state batteries
correlative imaging
lithium ion concentration
microstructure
x-ray Compton scattering
mass transport
title Li+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteries
title_full Li+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteries
title_fullStr Li+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteries
title_full_unstemmed Li+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteries
title_short Li+ concentration and morphological changes at the anode and cathode interphases inside solid-state lithium metal batteries
title_sort li concentration and morphological changes at the anode and cathode interphases inside solid state lithium metal batteries
topic solid-state batteries
correlative imaging
lithium ion concentration
microstructure
x-ray Compton scattering
mass transport
url https://doi.org/10.1088/2515-7655/adafda
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