Transition metal dichalcogenides (TMDs) are attractive materials for a variety of applications in solar energy conversion and electrocatalysis, due to their favorable optical and electrical properties and their unique two-dimensional structures which facilitate the fabrication of wide-area, ultrathin layers. Unfortunately, the basal planes which make up the majority of these materials are relatively inert, and thus a great deal of effort has been directed to engineering favorable, catalytically active defects into these materials. Here, we demonstrate how probe-based electrochemical techniques can be employed as multifunctional tools for locally modifying TMD materials and probing the electrochemical behavior of the resulting defects. Scanning Electrochemical Cell Microscopy (SECCM) was employed to locally anodize exfoliated p-type WSe2 nanosheets, creating hole-like defects within individual basal planes in a highly controllable fashion. Photoelectrochemical SECCM imaging was then employed to characterize the chemical behavior of these engineered defects, revealing significantly enhanced activity toward the Hydrogen Evolution Reaction (HER). Atomic force microscopy studies are presented which suggest these enhancements result from an increased density of monolayer-high step features within the anodized defects. Analysis of the SECCM data in the context of finite element simulations revealed that these enhancements increased with increasing anodization time, with local kinetic rates over 2 orders of magnitude higher than unaltered basal planes.

Recently, a newly discovered VIB group transition metal dichalcogenide (TMD) material, 2M-WS2, has attracted extensive attention due to its interesting physical properties such as topological superconductivity, nodeless superconductivity, and anisotropic Majorana bound states. However, the techniques to grow high-quality 2M-WS2 bulk crystals and the study of their physical properties at the nanometer scale are still limited. In this work, we report a new route to grow high-quality 2M-WS2 single crystals and the observation of superconductivity in its thin layers. The crystal structure of the as-grown 2M-WS2 crystals was determined by X-ray diffraction (XRD) and scanning tunneling microscopy (STM). The chemical composition of the 2M-WS2 crystals was determined by energy dispersive X-ray spectroscopy (EDS) analysis. At 77 K, we observed the spatial variation of the local tunneling conductance (dI/dV) of the 2M-WS2 thin flakes by scanning tunneling spectroscopy (STS). Our low temperature transport measurements demonstrate clear signatures of superconductivity of a 25 nm-thick 2M-WS2 flake with a critical temperature (T C) of ∼8.5 K and an upper critical field of ∼2.5 T at T = 1.5 K. Our work may pave new opportunities in studying the topological superconductivity at the atomic scale in simple 2D TMD materials.

Transition metal dichalcogenide (TMD) heterostructures are promising for a variety of applications in photovoltaics and photosensing. Successfully exploiting these heterostructures will require an understanding of their layer-dependent electronic structures. However, there is no experimental data demonstrating the layer-number dependence of photovoltaic effects (PVEs) in vertical TMD heterojunctions. Here, by combining scanning electrochemical cell microscopy (SECCM) with optical probes, we report the first layer-dependence of photocurrents in WSe2/WS2 vertical heterostructures as well as in pristine WS2 and WSe2 layers. For WS2, we find that photocurrents increase with increasing layer thickness, whereas for WSe2 the layer dependence is more complex and depends on both the layer number and applied bias (Vb). We further find that photocurrents in the WS2/WSe2 heterostructures exhibit anomalous layer and material-type dependent behaviors. Our results advance the understanding of photoresponse in atomically thin WSe2/WS2 heterostructures and pave the way to novel nanoelectronic and optoelectronic devices.

Using scanning tunneling spectroscopy (dI/dV) measurements, small energy gap was revealed in CrBr3 flakes.