Nanoscale Lithium Quantification in Li_XNi_yCo_wMn_ZO₂ as Cathode for Rechargeable Batteries

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) using a focused ion-beam scanning electron microscope (FIB-SEM) is a promising and economical technique for lithium detection and quantification in battery materials because it overcomes the limitations with detecting low Li content by energy dispersive spectroscopy (EDS). In this work, an experimental calibration curve was produced, which to our best knowledge allowed for the first time, the quantification of lithium in standard nickel manganese cobalt oxide (NMC-532) cathodes using 20 nm resolution. The technique overcomes matrix effects and edges effects that makes quantification complex. This work shows the high potential of TOF-SIMS tool for analytical characterization of battery materials, and demonstrates its tremendous capabilities towards identification of various chemical or electrochemical phenomena in the cathodes via high-resolution ion distributions. Various phenomena in the ion distributions are also assessed, such as edge effects or measurement artifacts from real signal variations.