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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 150 was decreased) by a factor of 20-40 by the cathodic polarization. For the first part of the measurements, RS is rapidly increasing. By the end of the measurements, such drift appears to have mostly stopped, as it would otherwise be even more prominent in the low frequency data. Indeed, in subsequent OCV measurements in dry H2 the RS had returned to 180 Ω, close to that measured before the cathodic polarizations, and 6 hours later in 50% H2O/H2 the RS was back to normal at 195 Ω. The evolution of RS is summarized in Table 5-5. After the SCPs, the atmosphere was changed to 50% H2O/H2 and 50% CO2/CO. The IS measured in these conditions for each metal are shown in Figure 5-30 along with the IS measured at the same conditions before the SCPs. The SCP clearly activated all of the electrodes. In H2/H2O, the LSRP decreased by a factor of 5, 10, and 20 for Ni, Pt, and Cu respectively. In CO/CO2, the LSRP decreased by a factor of 50-60 for those same metals. For Pd, the decreases were somewhat less, about a factor of 5 in both atmospheres. However, but the measurements shown before the SCP were taken after some of the electrodes had been activated by the normal anodic/cathodic polarizations, e.g. the Pd electrode was still activated by more than an order of magnitude after H2 oxidation (see Figure 5-23e and section 5.3.4.3). In comparison with the first measurements at 850 °C in 50% H2O/H2 and 50% CO2/CO (see Figure 5-12), the electrodes were at this point activated by up to a factor of 150 depending on the metal and atmosphere (Figure 5-31). In general, it can be concluded that the SCP caused a decrease in LSRP by 1 to 2 orders of magnitude. In terms of the relative magnitudes of the LSRP, after the SCPs, Pd, Ni and Pt had the lowest values and were quite similar, with Pd slightly more active than Ni and Pt, and the LSRP for Cu was about a factor of 2-3 higher. The shapes of the IS consistently show, for all of the metals, 2 rate-limiting processes after the SCP. Assuming that the IS measured before the treatment in the same 50% H2O/H2 atmosphere also represent 2 processes (which overlap and are more difficult to distinguish visually), the high-frequency process has been activated the most. There is no shift in the summit frequency towards higher frequency as observed when other Ni electrodes were activated by oxidation (Figure 5-25 and section 5.3.5.1). The IS measured at OCV before and after the SCP for an Ni electrode, in 3% H2O/H2, is shown in Figure 5-32. In this gas composition, before the SCP, up to 3 impedance processes were identified (Figure 5-9a), whereas now the IS show a single semicircle, similar to impedance measured in 50% H2O/H2 (Figure 5-9b) and under anodic polarization in 3% H2O/H2 (Figure 5-18). The temperature dependence of LSRP in 50% H2O/H2 after the SCPs was measured from 850 to 750 °C. The activation energies were 1.1, 0.8, 1.1, and 1.1 eV for Cu, Ni, Pd, and Pt respectively, whereas earlier they were all in the range of 1.3-1.6 eV (section 5.3.3.3). The activation energy of Ni especially had decreased as a result of the SCP, halving from 1.6 to 0.8PDF Image | Electrolysis of CO2 and H2O
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