Grazing-Incidence SEM Characterization of MoS2 Nanosheet Coatings Prepared by Liquid-Phase Exfoliation

Ultrathin two-dimensional (2D) coatings exhibit functional properties that are strongly defined by morphological features such as sheet edges, fracture sites, overlaps, folds, and local thickness variations, which are often difficult to resolve using conventional scanning electron microscopy (SEM) configurations. Here, we introduce a grazing-incidence SEM approach based on controlled sample tilting close to 90° for enhancing surface sensitivity and morphological feature detectability in ultrathin coatings. The method is proved on colloidal MoS2 nanosheet coatings prepared by liquid-phase exfoliation. Optical absorption spectroscopy confirms the presence of mono- and few-layer MoS2 nanosheets in the dispersion, confirming the ultrathin nature of the deposited coating. Compared to standard 0° imaging, grazing-incidence SEM reveals clearer boundaries and discontinuities. Quantitative Sobel-based image analysis supports these observations, showing an increase in edge density from 5.9% to 7.6% and in average gradient magnitude from 0.151 to 0.172 a.u. under grazing incidence, indicating a higher amount of retrievable morphological information. The proposed approach relies only on standard stage tilting and provides a broadly applicable framework for the surface-sensitive morphological characterization of ultrathin 2D coatings and thin films.