Article révisé par les pairs
Résumé : Electrochemical nucleation and growth are traditionally described by classical atom‐by‐atom deposition models, yet the nanoscale dynamics governing phase formation at electrochemical interfaces remain poorly understood. Here, we directly visualize copper electrodeposition on glassy carbon by combining in situ electrochemical liquid‐cell transmission electron microscopy (EC‐TEM) with cyclic voltammetry, enabling direct correlation between global electrochemical signals and particle‐resolved structural dynamics. Real‐time imaging reveals that nanoparticle formation proceeds through a complex interplay of classical and non‐classical pathways. Beyond radial and dendritic growth, we observe a range of particle‐level processes, including mobility, coalescence, ripening‐like mass exchange, and discrete relocation events, reflecting coupled transport and morphological transformation at the nanoscale. Quantitative tracking of individual nanoparticles reveals localized mass‐transfer processes, including near one‐to‐one ripening dynamics and particle–particle interactions that redistribute material without producing a clear signature in the voltammetric response. These findings demonstrate that processes such as ripening, coalescence, and structural rearrangements can proceed without a discernible signature in the global electrochemical response. By bridging in situ nanoscale imaging with electrochemical analysis, this work provides direct mechanistic insight into early‐stage electrochemical phase formation and highlights the dynamic nature of metal growth at electrochemical interfaces.

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