Nanoscale characterization of the heterogeneous interfacial oxidation layer of graphene/Cu based on a SEM electron beam induced reduction effect

Characterization of the interfacial oxidation layer of graphene/metal is a challenging task using conventional spectroscopy techniques because interfacial oxidation is heterogeneous at the nanoscale underneath the graphene. Here we developed a feasible method for nanoscale characterization of the interfacial oxidation layer of graphene/Cu (Gr/Cu) based on scanning electron microscopy (SEM) electron beam irradiation (EBI) induced reduction of interfacial oxides (SEM EBI-RIO method) at room temperature. The change in the thickness and coverage of the interfacial Cu oxide layer induced by EBI is responsible for the observed contrast reversal or change in SEM images of a targeted area with a width down to 200 nm in the EBI time scale of seconds to minutes. This method offers the capability of mapping heterogeneous interfacial oxidation of Gr/Cu with sub-100 nm spatial resolution and determining the range of thickness (1–5 nm) of the interfacial oxide layer. The SEM EBI-RIO method will be a powerful method to complement X-ray photoelectron spectroscopy (XPS), Raman microscopy, and high resolution transmission electron microscopy (HRTEM) for characterization of the interfacial oxidation layer of 2D materials and devices.