1D to 2D Transition in Tellurium Observed by 4D Electron Microscopy

Abstract A new microwave‐enhanced synthesis method for the production of tellurium nanostructures is reported—with control over products from the 1D regime (sub‐5 nm diameter nanowires), to nanoribbons, to the 2D tellurene regime—along with a new methodology for local statistical quantification of the crystallographic parameters of these materials at the nanometer scale. Using a direct electron detector and image‐corrected microscope, large and robust 4D scanning transmission electron microscopy datasets for accurate structural analysis are obtained. These datasets allow the adaptation of quantitative techniques originally developed for X‐ray diffraction (XRD) refinement analyses to transmission electron microscopy, enabling the first demonstration of sub‐picometer accuracy lattice parameter extraction while also obtaining both the size of the coherent crystallite domains and the nanostrain, which is observed to decrease as nanowires transition to tellurene. This new local analysis is commensurate with global powder XRD results, indicating the robustness of both the new synthesis approach and new structural analysis methodology for future scalable production of 2D tellurene and characterization of nanomaterials.