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Reduction and nanoparticle nucleation of Cu2+ by decamethylferrocene was studied with cyclic and square‐wave voltammetry at a microscale liquid–liquid interface established at the tip of a micropipette. With square‐wave voltammetry, two reduction steps could be distinguished as two separate current waves. Comparing the experimental results of cyclic voltammetry with finite element method simulations, particle growth could be observed as an increasing limiting current. Furthermore, kinetic parameters could be estimated with square‐wave voltammetry simulations following Butler‐Volmer kinetics. [ABSTRACT FROM AUTHOR]