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5.3 Process A: Reductive Dimerization of CO2 to CO and CO32- 29 hexafluorophosphate (TBA-HFP) or ionic liquid solvent. Cells were assembled, evacuated to 0.01 psi pressure, and then back-filled with CO2 ("bone dry" grade) to the appropriate pressure. This evacuation/back-filling process was repeated for a total of five cycles. For Process B, the electrodes used were either carbon-based active material (free-standing film or coated onto Al foil), lithium titanium oxide (LTO) coated onto Al foil, or Pt/Teflonized carbon paper (all cells tested were symmetric). The electrolyte comprised a saturated solution of carbonate salt (Li, Na or Cs) in ionic liquid, in some cases containing 0.1 M trimethylneo-pentylammonium fluoride in an attempt to improve carbonate solubility. Cells were assembled, evacuated to 0.01 psi pressure, and then back-filled with Ar ("Ultra High Purity" grade) to the appropriate pressure, again for five evacuate/back-fill cycles. Cells were analyzed by DEMS before electrolysis, then connected to the BioLogic instrument for the prescribed experiments, and subsequently analyzed by DEMS following equilibration for at least one hour at room temperature after electrochemical testing. Figure 5.2: (a) Summary of CO2 reduction experiments showing working potential (left) and observed pressure change (right) as a function of electrolysis time and temperature, at 50 μA in MeCN. The bottom inset plot reveals Arrhenius behavior of the reaction from +25 to –20◦C. (b) Representative DEMS data for CO2 reduction in MeCN at 0◦C. Note that CO is a fragment ion of CO2 (hence, always observed regardless of CO concentration in a CO2 atmosphere); therefore, changes in gas-phase CO concentration are determined quantitatively by comparing the ratios of CO and CO2 peaks before and after electrolysis. 5.3 Process A: Reductive Dimerization of CO2 to CO and CO32- Literature investigations (Sampson & Kubiak, 2016) utilized an air-tight 3-electrode setup under 1 atm CO2 with glassy carbon working electrode, Ag/AgCl reference electrode, and Mg counter electrode (which behaves as a sacrificial electrode, providing Mg2+ to solution as MgCO3 precipitates during CO2 reduction); electrolysis was carried out at a constant potential of 2.1 VPDF Image | ISRU Challenge Production of O2 and Fuel from CO2
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