Electrochemical CO₂ reduction is emerging as a compelling route for renewable energy storage and carbon neutrality. Focus on improving catalyst selectivity and energy efficiency resulted in a surge of catalysis-centered research. The advent of artificial intelligence and high-throughput screening enables parallelized catalyst characterization to accelerate discovery, but their implementation into application-relevant device configurations is challenging. We present a scalable, high-throughput platform based on infrared thermography that preserves realistic electrochemical environments from lab to industrially relevant scales. We demonstrate the spatial and electrochemical homogeneity of a 16-well parallel electrolyzer and validate a combinatorial testing approach using copper-based catalysts with varied loadings and precursor chemistries. The results highlight how activity trends can be rapidly mapped under controlled conditions, while also revealing the limitations of activity-only combinatorial testing, particularly for multiproduct electrochemical applications in complex environments like CO₂ electrolysis on Cu. This platform thus provides an efficient pre-screening tool to accelerate catalyst discovery when analyzed appropriately and paired with follow-up single catalyst testing. ... Read more

Electrolyte flooding in porous catalyst layers on gas diffusion electrodes (GDE) limits the stability and high-current performance of CO2 and CO electrolyzers. Here, we demonstrate the in situ electroreduction of graphene oxide (GO) to reduced graphene oxide (r-GO) within a silver catalyst layer on a carbon GDE. The r-GO introduces hydrophobicity regions in the catalyst layer that help mitigate electrolyte flooding during high current density CO2 electrolysis to CO. The flooding-resistant r-GO/Ag-coated GDE achieves a sustained Faradaic efficiency of CO at 94% for more than 8 h, compared to a rapid drop from 95% to 66% in an Ag-coated GDE without r-GO at 100 mA·cm–2. We found that GO enhances the electrochemically active surface area of the catalyst layer during CO2 electrolysis tests because the incorporation of GO increases the roughness of the catalyst layer. The in situ method of electrochemically reducing GO to r-GO provides a low-cost, practical approach that can be applied during standard spray-deposition procedures to develop flooding-resistant GDEs. ... Read more