Correlative Electrochemical Microscopy of Li‐Ion (De)intercalation at a Series of Individual LiMn2O4 Particles

Each one an individual! The electrochemistry of a series of LiMn₂O₄ battery cathode materials is investigated at the single particle level. A wide variety of distinctive characteristics are revealed that can be assigned to the structure and morphology of the same particle as observed by microscopy.

Abstract

The redox activity (Li‐ion intercalation/deintercalation) of a series of individual LiMn₂O₄ particles of known geometry and (nano)structure, within an array, is determined using a correlative electrochemical microscopy strategy. Cyclic voltammetry (current–voltage curve, I–E) and galvanostatic charge/discharge (voltage–time curve, E–t) are applied at the single particle level, using scanning electrochemical cell microscopy (SECCM), together with co‐location scanning electron microscopy that enables the corresponding particle size, morphology, crystallinity, and other factors to be visualized. This study identifies a wide spectrum of activity of nominally similar particles and highlights how subtle changes in particle form can greatly impact electrochemical properties. SECCM is well‐suited for assessing single particles and constitutes a combinatorial method that will enable the rational design and optimization of battery electrode materials.

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