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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 116 followed by re-reduction in an H2-rich atmosphere. In some tests, a strong cathodic polarization was applied to some of the electrodes, based on ref. [14]. The gas atmosphere was set to dry H2, reaching a pO2 sensor value of –1370 mV vs air at 850 °C (pO2 < 10-24 atm). Then, the following potential sweeps were performed at 20 mV/s: 0 to –500 mV, 0 to –1000 mV, and –1500 mV. Upon reaching each cathodic voltage, IS were also measured under that voltage. After both extreme conditions, OCV-IS temperature variations and/or polarization characterizations were performed. Table 5-1 summarizes the parameters that were changed during the tests. After the test, the cells were disassembled and the electrode was lifted off the electrolyte surface. Both surfaces were examined in the SEM. The final contact area and perimeter (TPB length) were measured from the SEM micrographs using Adobe Photoshop CS4 Extended. Table 5-1. Summary of the parameters changed during the electrochemical testing. Metal Ni Cu Pd Pt Ag Au Gas composition H2/H2O with ranges 0.01 < pH2 < 1.0 and 0 < pH2O < 0.62 Fixed pH2 Fixed pH2O Fixed pO2 (via dilution by Argon) CO/CO2 with ranges 0.03 < pCO < 0.86 and 0.05 < pCO2 < 0.5 Fixed pCO2 Extreme condition: oxidation by air Temperature 750 °C to 1000 °C Polarization +300 mV to –500 mV potential sweeps and EIS at 50-100 mV increments of DC bias Extreme condition: –1500 mV Time At the start, time for stabilization of interface After changing parameters, waited for steady-state Tests ran up to 800 hours 5.3. Results and Discussion In the following sections, the results are presented and specific results are accompanied by discussion. A broader discussion of all the observed phenomena in terms of reaction mechanisms follows in section 5.4. 5.3.1. Initial Stabilization of the Interface Upon arriving at the initial temperature (850-1000 °C), RS decreased logarithmically for each cell and nearly stabilized within 10-50 h depending on the metal and the temperature (Figure 5-3). This was observed for each metal, as has been observed for Ni wire electrodes in thePDF Image | Electrolysis of CO2 and H2O
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