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Catalysts 2020, 10, x FOR PEER REVIEW 13 of 25 Catalysts 2020, 10, 1287 13 of 25 of bimetallic Cu85Ag15 foam was synthesized by an additive (citrate)-assisted electrodeposition approach [74]. Such a foam structure enables the phase-segregation of Cu and Ag, and the well-despersed nano-sized Ag in the Cu matrix. After activation by Cu oxidation/reduction, the Cu matrix. After activation by Cu oxidation/reduction, the Cu85Ag15 foam shows high selectivity Cu85Ag15 foam shows high selectivity towards ethanol with an FE of 33.7% at −1.0 V vs. RHE in 0.5 M towards ethanol with an FE of 33.7% at −1.0 V vs. RHE in 0.5 M KHCO3. Bimetallic CuPd catalyst KHCO3. Bimetallic CuPd catalyst with phase-separated atomic arrangements could achieve a FE of with phase-separated atomic arrangements could achieve a FE of 15% for ethanol formation at −0.75 V 15% for ethanol formation at −0.75 V vs. RHE in 1 M KOH [75]. While the ordered and disordered vs. RHE in 1 M KOH [75]. While the ordered and disordered Cu-Pd nanoparticles primarily produce Cu-Pd nanoparticles primarily produce CO. This demonstrates that geometric and structural effects CO. This demonstrates that geometric and structural effects may played a more improtant role than may played a more improtant role than electronic effects in determing catalytic performance for electronic effects in determing catalytic performance for various Cu-Pd bimetallic materials. Notably, various Cu-Pd bimetallic materials. Notably, the FE of CO2 electroreduction toward ethanol could be the FE of CO2 electroreduction toward ethanol could be tuned by introducing different amounts of Zn to tuned by introducing different amounts of Zn to generate an in situ source of mobile CO reactant, generate an in situ source of mobile CO reactant, and was maximized to 29.1% on Cu4Zn alloy electrode and was maximized to 29.1% on Cu4Zn alloy electrode at −1.05 V vs. RHE in 0.1 M KHCO3 (Figure 6) at −1.05 V vs. RHE in 0.1 M KHCO3 (Figure 6) [44]. Similarily, the bimetallic CuZn catalyst synthesized [44]. Similarily, the bimetallic CuZn catalyst synthesized by in situ electrochemical reduction in by in situ electrochemical reduction in ZnO-shell/CuO-core bimetal oxide also shows a preference ZnO-shell/CuO-core bimetal oxide also shows a preference toward−s2 ethanol production with a high towards ethanol production with a high FE of 41.4% at −200 mA·cm (−0.68 V vs. RHE) in a flow cell, FE of 41.4% at −200 mA·cm−2 (−0.68 V vs. RHE) in a flo−w2 cell, in comparison to 32% at −1.15 V vs. in comparison to 32% at −1.15 V vs. RHE (−31.8 mA·cm ) in a H-cell [76]. The in-situ-generated CO RHE (−31.8 mA·cm−2) in a H-cell [76]. The in-situ-generated CO on Zn sites is believed to combine the on Zn sites is believed to combine the adsorbed *CH3 on Cu sites and form a *COCH3 intermediate, adsorbed *CH3 on Cu sites and form a *COCH3 intermediate, which is exclusively reduced to which is exclusively reduced to ethanol. These results indicate that incorporating foreign metals into a ethanol. These results indicate that incorporating foreign metals into a Cu matrix can promote or Cu matrix can promote or alter the reaction routes of CO2 reduction and the FE of ethanol formation is alter the reaction routes of CO2 reduction and the FE of ethanol formation is greatly dependent on greatly dependent on the nanostructures and compositions of Cu-based alloys. the nanostructures and compositions of Cu-based alloys. Figure 6. (A) Scheme illustration of CO2 electroreduction process on CuxZn alloys. (B) The maximum Figure 6. (A) Scheme illustration of CO2 electroreduction process on CuxZn alloys. (B) The maximum faradaic efficiencies of ethanol and FEethanol/FEethylene ratios on different CuxZn alloy catalysts. faradaic efficiencies of ethanol and FEethanol/FEethylene ratios on different CuxZn alloy catalysts. Reproduced with permission [44]. Copyright 2016, American Chemical Society. Reproduced with permission [44]. Copyright 2016, American Chemical Society. 3.1.3. Cu/Carbon Composites 3.1.3. Cu/Carbon Composites Another viable strategy to stabilize the reaction intermediates and promote the ethanol formation Another viable strategy to stabilize the reaction intermediates and promote the ethanol is to incorporate porous carbons into Cu catalysts. The large surface area and pore volume of porous formation is to incorporate porous carbons into Cu catalysts. The large surface area and pore volume carbons will drive the thorough distribution of CO2 molecules on the surface of catalysts and create of porous carbons will drive the thorough distribution of CO2 molecules on the surface of catalysts abundant active sites for CO2 conversion. The Cu2O nanoparticles grown on a carbon support can be and create abundant active sites for CO2 conversion. The Cu2O nanoparticles grown on a carbon transformed into small fragmented nanoparticles during CO2 electroreduction, which were densely support can be transformed into small fragmented nanoparticles during CO2 electroreduction, connected to each other [77]. Such a unique morphology is proposed to promote C–C coupling and which were densely connected to each other [77]. Such a unique morphology is proposed to promote ethanol formation with FE of 12%. In a recent report, a nitrogen-doped carbon nanospike electrode C–C coupling and ethanol formation with FE of 12%. In a recent report, a nitrogen-doped carbon with electronucleated Cu nanoparticles is shown to acquire a fairly high FE of 63% at −1.2 V vs. RHE nanospike electrode with electronucleated Cu nanoparticles is shown to acquire a fairly high FE of in 0.1 M KHCO3 for the electroreduction of CO2 to ethanol [41]. Subsequently, an oxide-derived 63% at −1.2 V vs. RHE in 0.1 M KHCO3 for the electroreduction of CO2 to ethanol [41]. Subsequently, Cu/carbon catalyst prepared by a facile carbonization of Cu-based MOF (HKUST-1) at 1100 ◦C was an oxide-derived Cu/carbon catalyst prepared by a facile carbonization of Cu-based MOF reported to exhibit highly selective CO2 reduction to ethanol with a FE of 35% at −0.5 V vs. RHE in 0.1 (HKUST-1) at 1100 °C was reported to exhibit highly selective CO2 reduction to ethanol with a FE of M KHCO3 [78]. Such intriguing catalytic behaviors originate from the intrinsic activity of Cu and the 35% at −0.5 V vs. RHE in 0.1 M KHCO3 [78]. Such intriguing catalytic behaviors originate from the synergetic interaction between Cu and neighboring porous carbons. In a recent report of N-doped intrinsic activity of Cu and the synergetic interaction between Cu and neighboring porous carbons. porous carbon-supported Cu nanoparticles [79], the pyridinic N-decorated porous carbon could in In a recent report of N-doped porous carbon-supported Cu nanoparticles [79], the pyridinic situ produce the reactive CO intermediate, which will diffuse to neighboring Cu sites and combine N-decorated porous carbon could in situ produce the reactive CO intermediate, which will diffuse to with the C1 intermediates formed on Cu sites by C–C coupling to produce ethanol. By optimizing the neighboring Cu sites and combine with the C1 intermediates formed on Cu sites by C–C coupling to pyridinic N content up to 3.43%, the maximum ethanol FE of 64.6% was achieved at −1.05 V vs. RHE produce ethanol. By optimizing the pyridinic N content up to 3.43%, the maximum ethanol FE of in 0.2 M KHCO3. 64.6% was achieved at −1.05 V vs. RHE in 0.2 M KHCO3. 3.1.4. 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