Impact of structural heterogeneities in hierarchically grown microribbons on 2D WS2 monolayer on the measured local hydrogen evolution activity on Au substrate

This dataset contains all raw data supporting the study investigating the local electrocatalytic activity of two-dimensional WS₂ monolayers and microribbons toward the hydrogen evolution reaction (HER) and the influence of structural and electronic heterogeneity on the measured electrochemical current. CVD-grown WS₂ flakes comprising monolayer regions and microribbon features were locally characterized using scanning electrochemical cell microscopy (SECCM). The spatially resolved electrochemical measurements were correlated with Raman spectroscopy, photoluminescence (PL) mapping, atomic force microscopy (AFM), and Kelvin probe force microscopy (KPFM) to establish direct structure–property–activity relationships. Differences in HER activity were observed between monolayer domains and microribbon regions, revealing pronounced spatial heterogeneity across the WS₂ surface. All raw and processed SECCM, Raman, PL, AFM, KPFM, and SEM data, together with associated metadata and custom MATLAB post-processing scripts, are included to enable full reproducibility of the analysis and to facilitate further quantitative investigation of local electrocatalytic behavior in 2D WS₂ systems.