Novel dynamic method based on CV-SECM and SWV-SECM for the in situ chemical imaging of reactive metal surfaces undergoing corrosion and corrosion inhibition illustrated with the case of copper corrosion inhibition by benzotriazole

A novel dynamic method for the chemical imaging of actively corroding metal surfaces using scanning electrochemical microscopy (SECM) is proposed by using CV-SECM and SWV-SECM. This consists of an adequate coupling of a repetitive voltammetric operation at the SECM tip while conducting the rastering routine for scanning a reactive copper surface, as well as its inhibition by benzotriazole. In this method, gold microelectrodes are employed as SECM tips, and therefore their electrochemical behaviour towards collection and redissolution of Cu2+ ions from synthetic solutions containing Cu2+ ions. Next, the dynamic application of voltammetric methods for the collection and stripping of copper on the Au probes while mapping copper surfaces was investigated. The proof of concept first involved continuous cyclic voltammetry (CV-SECM) in an acidified NaCl solution, in terms of Cu2+ dissolution and surface redox activity (with SECM in the feedback mode). Then, square wave voltammetry (SWV-SECM) was used to detect small copper dissolution from corroding and inhibitor-protected metal surfaces. The results are consistent with a heterogeneous nature of copper degradation and the development of protective films and passive layers.