The redoxactivity (Li-ion intercalation/deintercalation) of as eries of individual LiMn 2 O 4 particles of known geometry and (nano)structure,w ithin an array, is determined using acorrelative electrochemical microscopystrategy.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 microscopyt hat enables the corresponding particle size, morphology,c rystallinity,a nd other factors to be visualized. This study identifies aw ide spectrum of activity of nominally similar particles and highlights hows ubtle changes in particle form can greatly impact electrochemical properties. SECCM is well-suited for assessing single particles and constitutes acombinatorial method that will enable the rational design and optimization of battery electrode materials.