Correlative Analysis of Ion Concentration Profile and Surface Nanoscale Topography Changes using Operando Scanning Ion Conductance Microscopy

Although various spectroscopic methods have been developed to capture the ion concentration profile changes, it is still difficult to visualize the ion concentration profile and surface topographical changes simultaneously during the charging/discharging of LIBs. To tackle this issue, we have developed an operando scanning ion-conductance microscopy (SICM) method that can directly visualize an ion concentration profile and surface topography using a SICM nanopipette whilst controlling sample potential or current by potentiostat for characterizing the polarization state during charging/discharging. Using operando SICM on the negative electrode (anode) of LIBs, we have characterized ion concentration profile changes and the reversible volume changes related to the phase transition during cyclic voltammetry (CV) and charge/discharge of the hard carbon anode. Operando SICM is a versatile technique that is likely to be of major value for evaluating correlation of the electrolyte concentration profile and nanoscale surface topography changes.