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Catalysts 2021, 11, 482 13 of 19 our specific case, a higher pH on the electrode surface may be regarded as responsible for promoting the hydration of CO2 to carbonate and bicarbonate species, thus reducing CO2 concentration at the triple-phase boundary and negatively impacting its conversion to “more complex” multicarbon products. These findings demonstrate that pH can determine the course of reactions in different ways. Table 1. pH values of electrolytes (catholyte) at the surface of the electrode and after electrolysis (bulk). Electrolyte 1 M KHCO3 0.1 M KHCO3 Catalyst Material Cu-06 Cu-06 Cu-06 CuZ-06-03 CuZA-06-03-01 Cu-06 Cu-06 (15%wt Nafion) Cu-06 (30%wt Nafion) Cu-06 (45%wt Nafion) Real Applied Potential, V vs. Ag/AgCl −1.5 1.75 −2 −1.5 −1.5 −1.5 −1.5 −1.5 −1.5 Current Density, mA cm−2 15.6 26.3 34.6 11.5 13.5 4.7 3.5 2.25 2.1 Bulk pH, before/after the Co-Electrolysis 8.38/8.8 8.38/9.3 8.38/9.7 8.38/8.9 8.38/8.7 8.38/8.6 8.36/7.6 8.36/7.5 8.36/7.5 Calculated Surface pH (±0.05) 9.37 9.62 9.76 9.25 9.31 8.93 9.28 9.09 9.05 3. Materials and Methods 3.1. Materials Copper (II) nitrate trihydrate (CuN2O6·3H2O, 99–104%), zinc nitrate hexahydrate crys- tallised (Zn(NO3)2·6H2O, ≥99.0%) and aluminium nitrate nonahydrate (AlN3O9·9H2O, ≥98%), and sodium Carbonate (Na2CO3, ≥99%) were used in the preparation of the cata- lysts. Potassium bicarbonate (KHCO3, 99.7%) was used as electrolyte for the electrochemi- cal tests. Nafion perfluorinated resin solution Green Alternative (5 wt.% in lower aliphatic alcohols and water contains 15–20% water and Isopropanol for HPLC ((CH3)2CHOH, 99%) were employed in the preparation of the catalytic ink. All the materials were purchased from Sigma-Aldrich (Milan, Italy), and they were used as received unless otherwise specified. 3.2. Synthesis of CuZnAl-Oxide Based Catalysts The catalysts employed in our experimental work were CuZnAl-based catalysts obtained by the co-precipitation method. Briefly, the catalysts were prepared with a solution of hydrated metal nitrates (Cu(NO3)2, Zn(NO3)2, Al(NO3)3) as precursors and using a solution of Na2CO3 (1M) as precipitating agent. The CuZA-06-03-01 material constituted by CuO, ZnO, and Al2O3, was synthesised by using the metal nitrates in the following molar concentrations: Cu:Zn:Al = 0.6 M:0.3 M:0.1 M. Then, by using the same concentrations of precursors but deprived of Al (Cu:Zn = 0.6 M:0.3), the CuZ-06-03 catalyst was obtained to assess the contribution of Al. After that, also the Zn was also eliminated to study the role of this metal, resulting in the Cu-06 (0.6 M). More details about the catalyst preparation are given in the Supplementary Material (Section S3). At the end of the co-precipitation, the precipitate was filtered, left drying overnight at 60 ◦C in an oven and finally calcined at 350 ◦C for 3 h with a heating ramp of 2 ◦C min−1. Moreover, the oxidation state of copper species on the surface of the synthesised catalysts and the actual amount of each elements in the studied samples were investigated by means of X-ray Photoelectron Spectroscopy (XPS) and Inductively Coupled Plasma (ICP) techniques and are described in Section S4. However, identify the issues faced when operating a GDE-cell configuration is the main aim of this work. 3.3. Electrochemical Cell and Experimental Conditions A schematic view of the experimental set-up is shown in Figure 10 to provide an idea of the various involved components. The electrical supply to the Micro Flow elec-PDF Image | Gas Diffusion Electrode Systems for the Electro CO2 Conversion
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