We report the implementation of energy dispersive X-ray spectroscopy for layered semiconductors in the form of atomically thin transition metal dichalcogenides. The technique is based on a scanning electron microscope equipped with a silicon drift detector for energy dispersive X-ray analysis. By optimizing operational parameters in numerical simulations and experiments, we achieve layer-resolving sensitivity for few-layer crystals down to the monolayer limit and demonstrate elemental composition profiling in vertical and lateral heterobilayers of transition metal dichalcogenides. The technique can be straight-forwardly applied to other layered two-dimensional materials and van der Waals heterostructures, thus expanding the experimental toolbox for quantitative characterization of layer number, atomic composition, or alloy gradients for atomically thin materials and devices.

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