Carbon dioxide (CO₂) electroreduction reaction (CO₂RR) offers a promising strategy for the conversion of CO₂ into valuable chemicals and fuels. CO₂RR in acidic electrolytes would have various advantages due to the suppression of carbonate formation. However, its reaction rate is severely limited by the slow CO₂ diffusion due to the absence of hydroxide that facilitates the CO₂ diffusion in an acidic environment. Here, we design an optimal architecture of a gas diffusion electrode (GDE) employing a copper-based ultrathin superhydrophobic macroporous layer, in which the CO₂ diffusion is highly enhanced. This GDE retains its applicability even under mechanical deformation conditions. The CO₂RR in acidic electrolytes exhibits a Faradaic efficiency of 87% with a partial current density $$( {j}_{{{{\rm{C}}}}_{2+}})$$( j C 2 + ) of −1.6 A cm⁻² for multicarbon products (C₂₊), and $$ {j}_{{{{{{\rm{C}}}}}}_{2+}}$$j C 2 + of −0.34 A cm⁻² when applying dilute 25% CO₂. In a highly acidic environment, C₂₊ formation occurs via a second order reaction which is controlled by both the catalyst and its hydroxide.

Amino acids were electrochemically synthesized from biomass-derivable α-keto acids and water with high faradaic efficiencies using safe and earth-abundant TiO ₂ .

The oxygen evolution reaction (OER) is a critical element for all sorts of reactions that use water as a hydrogen source, such as hydrogen evolution and electrochemical CO₂ reduction, and novel design principles that provide highly active sites on OER electrocatalysts push the limits of their practical applications. Herein, Au‐cluster loading on unilamellar exfoliated layered double hydroxide (ULDH) electrocatalysts for the OER is demonstrated to fabricate a heterointerface between Au clusters and ULDHs as an active site, which is accompanied by the oxidation state modulation of the active site and interfacial direct OO coupling (“interfacial DOOC”). The Au‐cluster‐loaded ULDHs exhibit excellent activities for the OER with an overpotential of 189 mV at 10 mA cm⁻². X‐ray absorption fine structure measurements reveal that charge transfer from the Au clusters to ULDHs modifies the oxidation states of trivalent metal ions, which can be active sites on the ULDHs. The present study, supported by highly sensitive spectroscopy combining reflection absorption infrared spectroscopy and modulation‐excitation spectroscopy and density functional theory calculations, indicates that active sites at the interface between the Au clusters and ULDHs promote a novel OER mechanism through interfacial DOOC, thereby achieving outstanding catalytic performance.