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Instruments / Technical Area	Publication Details	Published	Actions
I13-2-Diamond Manchester Imaging	Non-linear cracking response to voltage revealed by operando X-ray tomography in polycrystalline NMC811 Huw C. W. Parks , Matthew Jones , Aaron Wade , Alice Llewellyn , Chun Tan , Hamish Reid , Ralf Ziesche , Thomas M. M. Heenan , Shashidhara Marathe , Christoph Rau , Paul R. Shearing , Rhodri Jervis Ees Batteries 526 DOI: 10.1039/D5EB00008D Diamond Proposal Number(s): [28650] Open Access Show Abstract ▼ Abstract: To understand fracture behaviour in battery materials, X-ray computed tomography (X-ray CT) has become the primary technique for non-destructive particle and crack analysis. Cracking causes performance decline in polycrystalline NMC811 by exposing new surfaces for parasitic electrolyte reactions and disconnecting active material from the electrode matrix. First cycle crack formation has been documented, but definitive electrochemically induced particle fracture is challenging to assess due to complex sample preparation and high-resolution X-ray imaging requirements. Presented here is an operando X-ray CT technique that enables accurate observation of fracture behaviour during de-/lithiation. A non-linear relationship between fracture behaviour and cell voltage was uncovered, and evidence of particle reformation during re-lithiation. Using a grey level analysis algorithm for fracture detection, we expedite damage evaluation in several thousands of particles throughout the electrochemical process, understanding crack initiation, propagation, and closure on a large, statistical scale and give the ability to track any one of the thousands of particles through its individual electrochemical history. Additionally, we explore the effects of continued volumetric hysteresis on particle damage. For the first time, we demonstrate the complex plurality of fracture behaviour in commercial lithium-ion battery materials, aiding in designing mitigation strategies against particle fracture.	Mar 2025
I14-Hard X-ray Nanoprobe	Identifying the origins of microstructural defects such as cracking within Ni‐rich NMC811 cathode particles for lithium‐ion batteries Thomas M. M. Heenan , Aaron Wade , Chun Tan , Julia E. Parker , Dorota Matras , Andrew S. Leach , James B. Robinson , Alice Llewellyn , Alexander Dimitrijevic , Rhodri Jervis , Paul D. Quinn , Dan J. L. Brett , Paul R. Shearing Advanced Energy Materials 1 DOI: 10.1002/aenm.202002655 Diamond Proposal Number(s): [20841, 23858] Open Access Show Abstract ▼ Abstract: The next generation of automotive lithium‐ion batteries may employ NMC811 materials; however, defective particles are of significant interest due to their links to performance loss. Here, it is demonstrated that even before operation, on average, one‐third of NMC811 particles experience some form of defect, increasing in severity near the separator interface. It is determined that defective particles can be detected and quantified using low resolution imaging, presenting a significant improvement for material statistics. Fluorescence and diffraction data reveal that the variation of Mn content within the NMC particles may correlate to crystallographic disordering, indicating that the mobility and dissolution of Mn may be a key aspect of degradation during initial cycling. This, however, does not appear to correlate with the severity of particle cracking, which when analyzed at high spatial resolutions, reveals cracking structures similar to lower Ni content NMC, suggesting that the disconnection and separation of neighboring primary particles may be due to electrochemical expansion/contraction, exacerbated by other factors such as grain orientation that are inherent in such polycrystalline materials. These findings can guide research directions toward mitigating degradation at each respective length‐scale: electrode sheets, secondary and primary particles, and individual crystals, ultimately leading to improved automotive ranges and lifetimes.	Nov 2020

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