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Catalysts 2021, 11, 482 by the productivity of the gas products. At the same time, it should be observed that CO is the second product in terms of FEs, except the Cu-06 catalyst, for which a slightly higher FE towards formate than CO must be highlighted. Moreover, the FEs to all CO2 reduction products is below 10%. In this sense, Gutiérrez-Guerra et al. suggested that a low concen- tration of CO2 at the catalyst surface may be regarded as responsible for the high8koifn1e9tics of the hydrogen evolution reactions [29]. Therefore, the observed phenomenon can be considered a warning about the not proper diffusion of CO2 within the gas diffusion elec- trode, and hence of not proper functioning of the cell. higher FE towards formate than CO must be highlighted. Moreover, the FEs to all CO2 Figure 5d shows the high productivity of the Cu-06 and CuZ-06-03 catalysts towards reduction products is below 10%. In this sense, Gutiérrez-Guerra et al. suggested that a low CO2 reduction liquid products than of the CuZA-06-03-01 catalyst. When copper was syn- concentration of CO2 at the catalyst surface may be regarded as responsible for the high thesised in combination with ZnO (CuZ), higher selectivity and productivity towards 2- kinetics of the hydrogen evolution reactions [29]. Therefore, the observed phenomenon can propanol (C3+) can be highlighted than with the Cu-06. Instead, the Cu-06 material is more be considered a warning about the not proper diffusion of CO2 within the gas diffusion selective for ethanol. electrode, and hence of not proper functioning of the cell. Figure 5. Chronoamperometry responses (a), Faradaic efficiencies (FEs) (b), productivities of gas (c) Figure 5. Chronoamperometry responses (a), Faradaic efficiencies (FEs) (b), productivities of gas −2 a(ncd)alinqduildiq(udi)dp(rdo)dpurcotsdufocrtsCfuoZrAC-u0Z6-A03-0-061-0,3C-u01Z,-0C6u-0Z3-0a6n-d03Caun-d06Ccuat-a0l6ycstasta(~ly4smtsg(~c4mmg)cwmith)3w0i%th o3f0N%afioofnNtaefsitoendtienst1eMdiKnH1CMOKHaqCuOeo3uasqueleocutrsoleyletectarto−ly1t.e5aVt−v1s.5AVg/vAs.gACgl./AgCl. 3 Figure 5d shows the high productivity of the Cu-06 and CuZ-06-03 catalysts towards Ex-situ XRD characterisation was performed on the Cu-06 tested electrode to study CO2 reduction liquid products than of the CuZA-06-03-01 catalyst. When copper was the generated oxide-derived-Cu (e.g., Cu2O) under the here employed CO2 electroreduc- synthesised in combination with ZnO (CuZ), higher selectivity and productivity towards tion conditions. The analysis demonstrated that the crystalline phase composition has 2-propanol (C3+) can be highlighted than with the Cu-06. Instead, the Cu-06 material is changed during the test, as shown in Figure 6. The CuO (Cu2+) was entirely reduced to more selective for ethanol. Cu1+ [30]. The diffraction peaks in the XRD graph belong to Cu2O (JCPDS number: 00-050- Ex-situ XRD characterisation was performed on the Cu-06 tested electrode to study the 0667) and Graphite (JCPDS number: 00-041-1487) crystalline phases. There are some un- generated oxide-derived-Cu (e.g., Cu2O) under the here employed CO2 electroreduction known peaks at 22.65°, 28.02°, and 32.45°, which could be attributed to some carbonate conditions. The analysis demonstrated that the crystalline phase composition has changed species deposited on the catalyst surface since, a2f+ter testing, the electrode sur1+face pre- during the test, as shown in Figure 6. The CuO (Cu ) was entirely reduced to Cu [30]. The diffraction peaks in the XRD graph belong to Cu2O (JCPDS number: 00-050-0667) and Graphite (JCPDS number: 00-041-1487) crystalline phases. There are some unknown peaks at 22.65◦, 28.02◦, and 32.45◦, which could be attributed to some carbonate species deposited on the catalyst surface since, after testing, the electrode surface presented a greenish- white colour. It is plausible the CuO transformation to copper(II) hydroxy carbonates (malachite or azurite) during the electroreduction of CO2 in water, as reported in the literature [31]. Thus, the results demonstrated that the formation and in situ stabilisation of Cu1+ contributes to improving the selectivity to more reduced CO2 reduction products, like ethanol and 1-propanol, that were found with this oxide-derived copper [32]. By focusing on CuZA-06-03-01 and CuZ-06-03, a greater CO and formate production can be noted in the former case. Three possible reasons for this behaviour are here proposed. First, it might be associated with a significant role played by aluminium oxide in decreasing the binding energy for *CO. Thus the *CO could be easily desorbed as a CO molecule [33,34]. −2PDF Image | Gas Diffusion Electrode Systems for the Electro CO2 Conversion
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