Preprint of "A Multimodal Correlative SPM-SEM Approach For Tracking Electro-Structural Nanoscale Connectivity In NMC Cathodes"

This work presents a correlative AFM-in-SEM methodology for multiscale structural, elemental, and electronic characterization of NMC cathodes. By integrating SEM imaging, EDS elemental mapping, and conductive AFM within a unified vacuum environment, the workflow enables precise spatial correlation of morphology and local conductivity while minimizing contamination and misalignment. Large-area stitched datasets are processed using an automated computational pipeline to extract statistically significant particle-level descriptors. Application to cathodes at different states of health reveals a deterministic relationship between particle size, intergranular cracking, and electronic isolation, directly quantifying particle contact loss. The proposed approach establishes a robust diagnostic platform for resolving electronic decoupling mechanisms in lithium-ion battery cathodes.