RT dataset T1 Dataset of the work “Bidimensional Spectroelectrochemistry with Tunable Thin-Layer Thickness” A1 Pérez Estébanez, Martín A1 Perales Rondon, Juan Víctor A1 Hernández Muñoz, Sheila A1 Heras Vidaurre, Aránzazu A1 Colina Santamaría, Álvaro K1 Química analítica K1 Chemistry, Analytic K1 Electroquímica K1 Electrochemistry AB 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 thinlayer 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. PB Universidad de Burgos YR 2025 FD 2025-05-20 LK https://hdl.handle.net/10259/10748 UL https://hdl.handle.net/10259/10748 LA eng NO Perez-Estebanez, M., Perales Rondón, J. V., Hernández Muñoz, S., Heras, A., & Colina, A. (2025). Dataset of the work “Bidimensional Spectroelectrochemistry with Tunable Thin-Layer Thickness” [Data set]. Universidad de Burgos. https://doi.org/10.71486/9G2C-3V84 NO Open Access funding provided thanks to the CRUE-CSIC agreement with American Chemical Society (ACS). This work was funded by the Ministerio de Ciencia e Innovacio?n and Agencia Estatal de Investigacion (MCIN/AEI/10.13039/501100011033 and PID2020-113154RBC21), Ministerio de Ciencia, Innovacion y Universidades (RED2022-134120-T), and Junta de Castilla y Leon and European Regional Development Fund (Grant number: BU036P23).M.P.-E. acknowledges Junta de Castilla y León and European Social Fund for his postdoctoral contract (BU036P23). J.V.P.-R. acknowledges Ministerio de Universidades and NextGenerationEU for his Maria Zambrano Fellowship. S.H. acknowledges Junta de Castilla y León and European Social Fund for her postdoctoral contract. DS Repositorio Institucional de la Universidad de Burgos RD 07-may-2026