Imaging of a Thin Oxide Film Formation from the Combination of Surface Reflectivity and Electrochemical Methods

Electrochemical methods (cyclic voltammetry (CV), potential steps, and electrochemical impedance spectroscopy) were successfully combined with in situ reflectometry measurements for a detailed analysis of the passive layer evolution as a function of the electrode potential. Interestingly, both EIS and surface reflectivity allowed a film thickness in the nanometer range to be readily determined. In addition, transient analyses of the reflectivity simultaneously recorded with CVs show the formation of both Fe₂O₃ and Fe₃O₄ oxides. The image analysis showed that the steel surface reactivity is heterogeneous and presents micrometric islands coated with a thicker oxide layer than the surrounding surface. The in situ combination of these techniques thus offers a powerful analytical description of the interface on a local scale and its transient response to a perturbation.