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Catalysts 2021, 11, 482 14 of 19 trochemical Cell (by ElectroCell, Tarm, Denmark) was ensured by a Biologic VSP-300 multichannel potentiostat (Bio-Logic SAS, Seyssinet-Pariset, France), which was operated in potentiostatic mode. The electrochemical tests were carried out at ambient conditions in a three-electrode cell configuration. The working electrode (WE) was a Cu-based GDE, while the counter electrode was an Ir-MMO plate, and the reference electrode was a 1 mm leak-free Ag/AgCl (3.4 M KCl). The cathodic and the anodic compartments were sepa- rated by a proton exchange membrane (Nafion 117 by Fuel Cell Store, College Station, TX, USA). The electrolyte supply was realised by two peristaltic pumps, with a flux rate of 26 mL min−1 for the catholyte compartment and 12 mL min−1 for the anolyte compartment. The external catholyte and anolyte flasks (0.1 M or 1 M of KHCO3 electrolyte solution) were filled with 30 mL and 35 mL of electrolyte, respectively, and were closed with rubber caps, which served both to isolate the system and to support the connection of the flexible tubes. The gas flow was kept constant via a mass flow controller (EL-Flow Select, PN64 by Bronkhorst High-Tech B.V., Ruurlo, The Netherlands) at 16.29 NmL min−1. The catholyte flow leaving the cell was sent to the external flask and recirculated, whereas, the gas outlet flow was directed to a gas/liquid separation flask, thus allowing the recovery of the liquid that crossed the GDE. re 10 Figure 10. A schematic view of the experimental set-up: (1) Gas chamber, (2) Catholyte chamber, (3) Ion exchange membrane, (4) Anolyte chamber. The manufacturing process of the different GDEs was based on the preparation of a catalytic ink and its deposition on porous carbon support (Toray carbon paper 060) by air-brushing. The catalytic ink was based on different components: (i) Cu NPs-based catalysts, in the powder form; (ii) Nafion (dispersion, 5%wt in water and 1-propanol) as a binder for the particles, which is necessary for their adhesion to the GDL; (iii) Vulcan XC 72R Carbon (VC) to improve dispersion and electrons conductivity of the electrocatalyst; (iv) isopropyl alcohol (isopropanol), as a carrier for the ink deposition because the ink must be fluid to be uniformly spread on the area of interest. Each Cu-based GDE was prepared with a geometric area of 10.2 cm2. The deposition process was performed by placing the carbon paper on a heating plate at 120 ◦C to ensure complete solvent evaporation. A pressure of 1.5 bar for the carrier gas in the airbrush inlet was chosen to have a regular ink uPDF Image | Gas Diffusion Electrode Systems for the Electro CO2 Conversion
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