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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 148 After the second oxidation, further characterization was performed. This high-resolution impedance data is included as Appendix 1. It contributes to the description of the original mechanisms (or close to the original mechanisms) of the Ni electrode before oxidation and may be useful for modeling purposes. 5.3.5.2. Strong Cathodic Polarization Strong cathodic polarization (SCP) was performed on the metal electrodes in dry H2. With very little H2O available, the cathodic current reduces other species. For example, it has been reported by a number of workers that zirconia can be electrochemically reduced at high cathodic overpotentials; SCP is also known to increase the electrocatalytic activity of metal/stabilized zirconia electrodes [14, 67-69]. Figure 5-27 shows strong cathodic polarization curves performed on one of the Ni electrodes. When each cathodic overpotential limit was reached (–500 mV, –1000 mV, and then –1500 mV), potentiostatic EIS was performed at that cathodic bias for a few minutes. The ―to – 1000 mV‖ curve exactly overlays the ―to –500 mV‖ curve, so the –500 mV polarization did not noticeably affect the interface, the electrode or electrolyte materials. After the application of – 1000 mV, however, the following curve ―to –1500 mV‖ follows a different current-voltage path, suggesting that –1000 mV has had some effect. The responses of the other metals are shown in Figure 5-28. Cu and Pt show a similar response. Pd, on the other hand, is already activated after the –500 mV sweep and has a different curvature with the current temporarily dropping from about –500 to –550 mV. This might have to do with hydrogen storage properties of Pd. Then the behavior in this range may indicate that in this overpotential range the small amount of steam present is being used up (more quickly than it is supplied) and other species begin to be reduced. The IS measured after each polarization curve, under each strong cathodic bias, are shown for the Ni electrode in Figure 5-29a. The other metals had very similar results. During the stronger polarizations (–1000 mV and –1500 mV), the RS decreased. The RS changed from 195 Ω at OCV to 35 Ω at –1500 mV, and appeared to be decreasing during the –1000 mV and – 1500 mV impedance scans based on the decreasing impedance at high frequencies. Indeed, the magnitude of the current measured during the –1500 mV potentiostatic IS (not shown) increased linearly by about 70% during the IS measurement. The spectra were not at all measured at steady-state and their shapes are significantly distorted, so they are used only to determine the approximate RS. The apparent low-frequency loop is also the result of the decreasing RS. The IS measured at OCV immediately before the polarizations and in between each are shown for the Ni electrode in Figure 5-29b. All of the metals appeared to be activated (LSRPPDF Image | Electrolysis of CO2 and H2O
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