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Operando/in-situ liquid cell transmission electron microscopy (LCTEM) allowsfor real time imaging of dynamic nanoscale liquid-based processes. However, dueto the thick liquid cell of traditional LCTEM holders and thus scattering ofthe electron beam passing through the cell, the achievable spatial and chemicalresolution is limited. Cryogenic atom probe tomography (cryo-APT) overcomesthese limitations by offering (near-)atomic scale compositional analysis offrozen liquid-solid interfaces. However, APT provides limited structuralanalysis and has no capacity for dynamic or operando liquid cell studies. Thiswork presents a novel workflow for site-specific cryo-APT sample preparation ofliquid-solid interfaces from in-situ electrochemical LCTEMMicro-Electro-Mechanical Systems (MEMS) chips. Using cryogenic inert gastransfer suitcase and a cryogenic plasma-focused ion beam (PFIB), a MEMsnanochip containing a Li electrolyte from an electrochemistry LCTEM holder wassuccessfully frozen, transferred to the cryo stage of a PFIB and prepared intoAPT needle samples containing the electrolyte-electrode interface at cryogenictemperatures, followed by cryogenic transfer to an atom probe for nanoscalecompositional analysis. This correlative approach provides dynamic nanoscaleimaging and near atomic scale compositional analysis of liquid-solidinterfaces. This method enables reliable and reproducible APT samplepreparation of these frozen interfaces from MEMs based nanochips and can hencebe used across materials systems and energy-conversion or storage devices.

A Workflow for Correlative in-situ Nano-chip Liquid Cell Transmission  Electron Microscopy and Atom Probe Tomography Enabled by Cryogenic Plasma  Focused Ion Beam