Bidimensional spectroelectrochemistry (Bidim-SEC) is an instrumental technique that provides operando UV/vis absorption information on electrochemical processes from two different points of view, using concomitantly a parallel and a normal optical configuration. The parallel configuration provides information about chemical species present in the diffusion layer, meanwhile the normal arrangement supplies information about changes occurring both in the diffusion layer and, mainly, on the electrode surface. The choice of a suitable cell to perform Bidim-SEC experiments is critical, especially while working under a thin-layer regime. So far, most of the proposed Bidim-SEC cells rely on the use of spacers to define the thin-layer thickness, which leads to working with constant thickness values. Herein, we propose a novel Bidim-SEC cell that enables easy-to-use micrometric control of the thin-layer thickness using a piezoelectric positioner. This device can be used for the study of complex interfacial systems and also to easily measure the key parameters of an electrochemical process. As a proof of concept, the study of the roughening of a gold electrode in KCl medium is performed, identifying key steps in the passivation and nanoparticle generation on the gold surface.
