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Through its capability for 3D mapping of Li at the nanoscale, atom probetomography (APT) is poised to play a key role in understanding themicrostructural degradation of lithium-ion batteries (LIB) during successivecharge and discharge cycles. However, APT application to materials for LIB isplagued by the field induced delithiation (deintercalation) of Li-ions duringthe analysis itself that prevents the precise assessment of the Lidistribution. Here, we showcase how a thin Cr-coating, in-situ formed on APTspecimens of NMC811 in the focused-ion beam (FIB), preserves the sample'sintegrity and circumvent this deleterious delithiation. Cr-coated specimensdemonstrated remarkable improvements in data quality and virtually eliminatedpremature specimen failures, allowing for more precise measurements via.improved statistics. Through improved data analysis, we reveal substantialcation fluctuations in commercial grade NMC811, including complete grains ofLiMnO. The current methodology stands out for its simplicity andcost-effectiveness and is a viable approach to prepare battery cathodes andanodes for systematic APT studies.

Facilitating the systematic nanoscale study of battery materials by atom probe tomography through in-situ metal coating