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2D materials are emerging as promising nanomaterials for applications inenergy storage and catalysis. In the wet chemical synthesis of MXenes, these 2Dtransition metal carbides and nitrides are terminated with a variety offunctional groups, and cations such as Li+ are often used to intercalate intothe structure to obtain exfoliated nanosheets. Given the various elementsinvolved in their synthesis, it is crucial to determine the detailed chemicalcomposition of the final product, in order to better assess and understand therelationships between composition and properties of these materials. Tofacilitate atom probe tomography analysis of these materials, a revisedspecimen preparation method is presented in this study. A colloidal Ti3C2TzMXene solution was processed into an additive-free free-standing film andspecimens were prepared using a dual beam scanning electron microscope /focused ion beam. To mechanically stabilize the fragile specimens, they werecoated using an in situ sputtering technique. As various 2D material inks canbe processed into such free-standing films, the presented approach is pivotalfor enabling atom probe analysis of other 2D materials.

Facilitating Atom Probe Tomography of 2D MXene Films by In Situ Sputtering