Publication date: 10th April 2024
Graphite is the dominant anode material for lithium-ion batteries which has been studied for decades. The structure of lithium graphite intercalated compounds have been studied in-situ and in-operando using a range of techniques, including Raman spectroscopy, synchrotron x-ray and neutron diffraction, and NMR. However, while these techniques are powerful, they lack the time and space resolution for understanding fast intercalation in single particles. This is especially important for the dilute stages of graphite, the structure of which are still debated, and are believed to be heterogeneous at a single particle level. Here we use operando optical microscopy on temperature controlled cells, observing fast intercalation events in the dilute stages of graphite.
Optical microscopy has shown to be a powerful and flexible technique for resolving fast intercalation in single particles. We combine this with a temperature-controlled coin cell to observe dynamic intercalation events in the dilute stages of graphite. Surprisingly, we find that the intercalation proceeds discontinuously throughout all of the dilute stages, with fast intercalation events affecting separated domains within a single particle. These domains often act independently, and undergo multiple intercalation events per cycle. This behaviour does not continue in the dense stages, where the domain-by-domain behaviour is not distinct, and the particle undergoes biphasic transitions as expected. This is unlike the solid-solution like behaviour predicted for the 4L-3L transition, as true solid-solutions in materials such as LiCoO2 and LiNixMnyCozO2 do not show discontinuity in their optical scattering signal. We corroborate these findings with SEM and EBSD, and correlate the optically resolved domains.
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