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Abstract A simple and environmentally‐friendly approach was developed to synthesize 2D CuO nanosheets using electrochemical deposition. The formed 2D CuO nanosheets (NSs) exhibit numerous advantageous properties such as no toxicity, high electrical conductivity, large active surface area, and a p‐type semiconducting nature with a band gap of 1.2 eV. A sensitive electrochemical sensor was constructed for the amperometric detection of glucose to take advantage of these characteristics. The fabricated sensor displayed an excellent sensitivity of 2710 μA mM⁻¹ cm⁻²along with a wide linear range of 0.001–1.0 mM and a lower limit of detection of 0.8 μM (S/N=3). Additionally, the modified electrode possesses high selectivity and good stability. The outstanding electrocatalytic performance of the electrode is attributed to a large active surface area, unique structural morphology, and the high conductivity of the 2D CuO nanosheets. 

Precise control over catalyst composition and structure is essential for optimizing oxygen reduction reaction (ORR) performance in energy conversion devices. In this study, we design ORR catalysts using the layer-by-layer electrodeposition of Au and Ru on glassy carbon electrodes modified with self-assembled monolayers of metal complexes. Two surface modulation architectures are explored. In the first, we electrodeposit layers of metals using successively appended coordination complexes via multiple rounds of amide coupling. In the second, we utilize a templated method to regenerate thiol-metal coordination for successive layer-by-layer electrodeposition. Both methods offer tunable multi-metal and multi-layer architectures. Cyclic voltammetry and CN⁻poisoning studies confirm metal electrodeposition and catalytic function. Higher order layering of metals significantly enhances ORR performance, and rotating ring-disk electrode measurements show improved selectivity for water over H₂O₂with increasing metal layers. The most selective ORR catalyst for water is a five-layer Au electrode that reduces O₂by an average of 3.6 electrons in neutral media despite bulk Au favoring the two-electron pathway under analogous conditions. This work introduces a flexible and generalizable framework for constructing multi-metal catalysts with a high degree of compositional control, which could have applications in ORR cathodes and other electrocatalytic systems.