Flow reactors are of increasing importance and have become crucial devices due to their wide application in chemical synthesis, electrochemical hydrogen evolution reaction (HER), or electrochemical waste water treatment. In many of these applications, catalyst materials such as transition-metal chalcogenides (TMCs) for the HER, provide the desired electrochemical reactivity for the HER. Generally, the flow electrolyzers' performance is evaluated as the overall output, but the decrease in activity of the electrolyzer is due to localized failure of the catalyst. Herein, we present a method for the spatially resolved (tens of micrometers) In Operando analysis of the catalytic activity under real operation conditions as well as the localized deposition of the catalyst in an operating model flow reactor. For these purposes, scanning electrochemical microscopy was applied for MoSx catalyst deposition and for localized tracking of the TMC activity with a resolution of 25 μm. This approach offers detailed information about the catalytic performance and should find broad application for the characterization and optimization of flow reactor catalysis under real operational conditions.

Department of Chemical and Biomolecular Engineering Yonsei University 50 Yonsei ro Seodaemun gu Seoul 03722 Korea

Department of Food Technology Mendel University in Brno Zemedelska 1 CZ 613 00 Brno Czech Republic

Department of Medical Research China Medical University Hospital China Medical University No 91 Hsueh Shih Road Taichung 40402 Taiwan

Future Energy and Innovation Laboratory Central European Institute of Technology Brno University of Technology Purkyňova 123 61200 Brno Czech Republic

Institute of Analytical Chemistry Chemo and Biosensors University of Regensburg 93053 Regensburg Germany

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