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Exploring cycling induced crystallographic change in NMC with X-ray diffraction computed tomography.

Sohrab R Daemi1, Chun Tan2, Antonis Vamvakeros3

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X-ray diffraction computed tomography revealed that cycling lithium nickel manganese cobalt oxide (LiNi0.33Mn0.33Co0.33O2) electrodes to higher voltages causes unit cell volume reduction and particle cracking. This advanced technique maps crystal dimension changes and electrode heterogeneities.

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Area of Science:

  • Materials Science
  • Electrochemistry
  • Crystallography

Background:

  • Lithium-ion battery performance relies on electrode material stability during cycling.
  • Understanding crystal structure changes at the microscale is crucial for improving battery longevity.
  • High-voltage cycling can induce significant stress and degradation in cathode materials.

Purpose of the Study:

  • To apply X-ray diffraction computed tomography for analyzing crystal dimension changes in LiNi0.33Mn0.33Co0.33O2 electrodes.
  • To spatially map heterogeneities and degradation at the electrode and particle level.
  • To correlate electrochemical cycling conditions with changes in unit cell dimensions and material integrity.

Main Methods:

  • X-ray diffraction computed tomography (XRD-CT) at 1 μm spatial resolution.
  • Electrochemical cycling of LiNi0.33Mn0.33Co0.33O2 electrodes in full cells with graphite anodes.
  • Focused ion beam-scanning electron microscopy (FIB-SEM) for cross-section analysis.

Main Results:

  • Unit cell volume decreased by 0.4% (4.2 V) and 0.6% (4.7 V) after 100 cycles.
  • Extensive particle cracking was observed with increasing upper cut-off voltage.
  • XRD-CT detected inhomogeneous lattice parameters within the electrode structure.

Conclusions:

  • Electrochemical cycling, especially at higher voltages, induces significant lattice parameter changes and physical degradation (cracking) in LiNi0.33Mn0.33Co0.33O2 electrodes.
  • XRD-CT is an effective diagnostic tool for correlating crystal structure evolution with electrochemical performance and identifying localized degradation.
  • The technique bridges the gap between crystal structure analysis and battery performance, aiding in the development of more stable electrode materials.