Correlative Electrochemical Microscopy of Li-Ion (De)intercalation at a Series of Individual LiMn2 O4 Particles.

The redox activity (Li-ion intercalation/deintercalation) of a series of individual LiMn2 O4 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.