Nanoscale Elemental Mapping of Intact Solid–Liquid Interfaces and Reactive Materials in Energy Devices Enabled by Cryo-FIB/SEM

Many modern energy devices rely on solid-liquid interfaces, highly reactive materials, or both, for their operation and performance. The difficulty of characterizing such materials means these devices often lack high-resolution characterization in an unaltered state. \nHere, we demonstrate how cryogenic sample preparation and transfer can extend the capabilities of FIB/SEM techniques to the solid-liquid interfaces and reactive materials common to energy devices by preserving their integrity through all stages of preparation and characterization. We additionally show how cryo-FIB/SEM paired with energy dispersive X-ray spectroscopy enables nanoscale elemental mapping of cross-sections produced in these materials and discuss strategies to achieve optimal results. Finally, we consider current limitations of the technique and propose future developments that could enhance its capabilities. Our results illustrate that cryo-FIB/SEM will be a useful technique for fields where solid-liquid interfaces or reactive materials play an important role and could, thus far, not be characterized at high resolution.