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MXenes are a family of 2D transition metal carbides and nitrides with remarkable properties, bearing great potential for energy storage and catalysis applications. However, their oxidation behavior is not yet fully understood, and there are still open questions regarding the spatial distribution and precise quantification of surface terminations, intercalated ions, and possible uncontrolled impurities incorporated during synthesis and processing. Here, atom probe tomography (APT) analysis of as‐synthesized Ti 3 C 2 T  x   MXenes reveals the presence of alkali (Li, Na) and halogen (Cl, F) elements as well as unetched Al. Following oxidation of the colloidal solution of MXenes, it is observed that the alkalis are enriched in TiO 2  nanowires. Although these elements are tolerated through the incorporation by wet chemical synthesis, they are often overlooked when the activity of these materials is considered, particularly during catalytic testing. This work demonstrates how the capability of APT to image these elements in 3D at the near‐atomic scale can help to better understand the activity and degradation of MXenes, in order to guide their synthesis for superior functional properties.

Near‐Atomic‐Scale Perspective on the Oxidation of Ti 3 C 2 T x MXenes: Insights from Atom Probe Tomography