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A Localized Multimicroscopy Approach for Studying Active Site Distribution During Electrodeposition

par Torres Morillo, Daniel ;Ustarroz Troyano, Jon
Référence Annual Meeting(76th: September, 2025: Mainz, Germany), Annual Meeting of the International Society of Electrochemistry
Publication Publié, 2025-09

Abstract de conférence

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Résumé :

Electrochemical nucleation and growth (EN&G) underpin advanced fabrication methods for coatings and nanostructured materials. Despite extensive studies, a comprehensive mechanistic understanding remains elusive due to spatial and temporal limitations: conventional techniques typically measure averaged electrochemical responses over macroscopic areas, missing critical microscale heterogeneities and local dynamics. Consequently, establishing precise correlations between local surface properties and nucleation events remains challenging.In our work, we address these limitations using a multimicroscopy approach combining high-throughput localized electrochemical characterization (Scanning Electrochemical Cell Microscopy, SECCM), correlative microscopy (FESEM), and advanced statistical and analytical modeling. By capturing spatially-resolved electrochemical descriptors and directly correlating these with microscale surface features, we reveal nucleation activity distributions that explicitly reflect surface heterogeneities, bridging the gap between macroscopic electrochemical responses and local nucleation dynamics [1].Our approach provides unprecedented insights into site-specific EN&G behaviors, uncovering information inaccessible via conventional macroscopic approach. Systematic studies across diverse electrodeposition systems (e.g., Cu, Au, Ag) and substrates (ITO, glassy carbon, Pt) established robust, generalized insights of intrinsic factors governing nucleation diversity [2,3]. Tailored statistical and analytical models applied to local current transients demonstrated direct, quantitative relationships between nucleation events and number of active sites [4]. This integrated methodology bridges the critical gap between the early stages of EN&G and the final properties of electrodeposits, enabling more accurate analyses of inherently heterogeneous electrochemical systems. Ultimately, our innovative approach provides the fundamental insights and control needed to rationally design tailored electrochemical interfaces, informing strategies toward advanced, sustainable coatings and functional nanostructures.1. D. Torres, M. Bernal, A. Demaude, S. Hussain, L. Bar, P. Losada-Pérez, F. Reniers, and J. Ustarroz, J. Electrochem. Soc., 169, 102513 (2022).2. D. Torres, J. Bailly, M. Bernal, L. B. Coelho, and J. Ustarroz, J. Solid State Electrochem., 28, 1719–1734 (2024).3. M. Bernal, D. Torres, S. S. Parapari, M. Čeh, K. Ž. Rožman, S. Šturm, and J. Ustarroz, Electrochim. Acta, 445 (2023).4. D. Torres, M. Bernal, and J. Ustarroz, Small Methods, 2401029, 1–13 (2024).