Operando/in-situ liquid cell transmission electron microscopy (LCTEM) permits for actual time imaging of dynamic nanoscale liquid-based processes. Nonetheless, because of the thick liquid cell of conventional LCTEM holders and thus scattering of the electron beam passing by the cell, the achievable spatial and chemical decision is restricted. Cryogenic atom probe tomography (cryo-APT) overcomes these limitations by providing (near-)atomic scale compositional evaluation of frozen liquid-solid interfaces. Nonetheless, APT gives restricted structural evaluation and has no capability for dynamic or operando liquid cell research. This work presents a novel workflow for site-specific cryo-APT pattern preparation of liquid-solid interfaces from in-situ electrochemical LCTEM Micro-Electro-Mechanical Programs (MEMS) chips. Utilizing cryogenic inert fuel switch suitcase and a cryogenic plasma-focused ion beam (PFIB), a MEMs nanochip containing a Li electrolyte from an electrochemistry LCTEM holder was efficiently frozen, transferred to the cryo stage of a PFIB and ready into APT needle samples containing the electrolyte-electrode interface at cryogenic temperatures, adopted by cryogenic switch to an atom probe for nanoscale compositional evaluation. This correlative method gives dynamic nanoscale imaging and close to atomic scale compositional evaluation of liquid-solid interfaces. This technique permits dependable and reproducible APT pattern preparation of those frozen interfaces from MEMs based mostly nanochips and may therefore be used throughout supplies programs and energy-conversion or storage units.
