Revealing Nanoscale Ni-Oxidation State Variations in Single-Crystal NMC811 via 2D and 3D Spectro-Ptychography

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Main Authors: Ziesche, Ralf F., Johnson, Michael J., Manke, Ingo, Cruddos, Joshua H., Llewellyn, Alice V., Tan, Chun, Jervis, Rhodri, Shearing, Paul R., Rau, Christoph, Rettie, Alexander J. E., Cipiccia, Silvia, Batey, Darren
Format: Preprint
Published: 2025
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author Ziesche, Ralf F.
Johnson, Michael J.
Manke, Ingo
Cruddos, Joshua H.
Llewellyn, Alice V.
Tan, Chun
Jervis, Rhodri
Shearing, Paul R.
Rau, Christoph
Rettie, Alexander J. E.
Cipiccia, Silvia
Batey, Darren
author_facet Ziesche, Ralf F.
Johnson, Michael J.
Manke, Ingo
Cruddos, Joshua H.
Llewellyn, Alice V.
Tan, Chun
Jervis, Rhodri
Shearing, Paul R.
Rau, Christoph
Rettie, Alexander J. E.
Cipiccia, Silvia
Batey, Darren
contents Enabling lithium (Li)-ion batteries with higher energy densities, longer cycle life, and lower costs will underpin the widespread electrification of the transportation and large-scale energy storage industries. Nickel (Ni)-rich layered oxide cathodes, such as LiNi$_{x}$Mn$_{y}$Co$_{z}$O$_{2}$ (NMC, x > 0.8), have gained popularity due to their high specific capacities and lower cobalt content. However, the standard polycrystalline morphology suffers from accelerated degradation at voltages above 4.2 V versus graphite, due to its increased mechanical and chemical instability. Single-crystal NMC (SC-NMC) has emerged as a promising morphology for suppressing the mechanical instability by preventing intergranular cracking; however, robust methods of understanding its chemical degradation pathways are required. We demonstrate how a high-throughput data collection strategy unlocks the ability to perform 2D and 3D ptychography in minutes, where it currently requires hours, and combine this with X-ray absorption near edge spectroscopy (XANES) to visualise the local Ni oxidation state behaviour in SC-NMC811, with nanometre-scale spatial resolution, and use this as a proxy for state-of-charge. By employing this technique at various stages during lifetime cycling to high voltages (>4.2 V), direct mapping of chemical degradation along the Li channels, identification of nucleation sites, and observation of Ni oxidation state heterogeneities across both electrode and particle scales can be achieved. We further correlate these heterogeneities with the formation and growth of the rocksalt phase and oxygen-induced planar gliding. This methodology will advance the fundamental understanding of how high-Ni layered oxide materials chemically degrade during high-voltage operation, guiding the design of more durable battery materials.
format Preprint
id arxiv_https___arxiv_org_abs_2507_22834
institution arXiv
publishDate 2025
record_format arxiv
spellingShingle Revealing Nanoscale Ni-Oxidation State Variations in Single-Crystal NMC811 via 2D and 3D Spectro-Ptychography
Ziesche, Ralf F.
Johnson, Michael J.
Manke, Ingo
Cruddos, Joshua H.
Llewellyn, Alice V.
Tan, Chun
Jervis, Rhodri
Shearing, Paul R.
Rau, Christoph
Rettie, Alexander J. E.
Cipiccia, Silvia
Batey, Darren
Materials Science
Chemical Physics
Enabling lithium (Li)-ion batteries with higher energy densities, longer cycle life, and lower costs will underpin the widespread electrification of the transportation and large-scale energy storage industries. Nickel (Ni)-rich layered oxide cathodes, such as LiNi$_{x}$Mn$_{y}$Co$_{z}$O$_{2}$ (NMC, x > 0.8), have gained popularity due to their high specific capacities and lower cobalt content. However, the standard polycrystalline morphology suffers from accelerated degradation at voltages above 4.2 V versus graphite, due to its increased mechanical and chemical instability. Single-crystal NMC (SC-NMC) has emerged as a promising morphology for suppressing the mechanical instability by preventing intergranular cracking; however, robust methods of understanding its chemical degradation pathways are required. We demonstrate how a high-throughput data collection strategy unlocks the ability to perform 2D and 3D ptychography in minutes, where it currently requires hours, and combine this with X-ray absorption near edge spectroscopy (XANES) to visualise the local Ni oxidation state behaviour in SC-NMC811, with nanometre-scale spatial resolution, and use this as a proxy for state-of-charge. By employing this technique at various stages during lifetime cycling to high voltages (>4.2 V), direct mapping of chemical degradation along the Li channels, identification of nucleation sites, and observation of Ni oxidation state heterogeneities across both electrode and particle scales can be achieved. We further correlate these heterogeneities with the formation and growth of the rocksalt phase and oxygen-induced planar gliding. This methodology will advance the fundamental understanding of how high-Ni layered oxide materials chemically degrade during high-voltage operation, guiding the design of more durable battery materials.
title Revealing Nanoscale Ni-Oxidation State Variations in Single-Crystal NMC811 via 2D and 3D Spectro-Ptychography
topic Materials Science
Chemical Physics
url https://arxiv.org/abs/2507.22834