Layered materials are of high importance because of their anisotropyand as asource of 2D materials.Whilst there is aplethora of multi-elemental 2D materials,the number monoelemental 2D materials is rather limited. Herein, we demonstrate that aqueous shear exfoliation can be used to obtain As, Sb,and Bi exfoliated nanosheets.Morphological and chemical characterization of the exfoliated materials shows adecrease in thickness,sheet-to-nanosheet scale,and partial oxidation owing to ah igher surface area. The electrochemical performance is tested in terms of inherent electrochemistry,e lectron transfer, and sensing applications as demonstrated with ascorbic acid. Potential energy-related applications are evaluated in the hydrogen evolution reaction (HER), oxygen evolution reaction (OER), and oxygen reduction reaction (ORR), with shearexfoliated Sb having the best electrochemical performance overall. These findings will have ap rofound impact on the preparation and application of 2D mono-elemental materials.Supportinginformation and the ORCID identification number(s) for the author(s) of this article can be found under: https://doi.