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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 157 Figure 5-36. YSZ electrolyte pellets after tests in which strong cathodic polarizations were performed. (a) Photograph after a –2000 mV polarization. (b) Optical micrograph after a –1500 mV polarization. The metal electrode was strongly adhered to the YSZ and difficult to remove (the white in (b) is where fresh YSZ is exposed because the top layer was pulled off during removal of the electrode). The YSZ surface outside of the interface sometimes showed cracking as in (b). Blackening is believed to be the result of these trapped electrons in the YSZ subsurface, forming color centers. After the SCPs in the present tests, the electrolyte surface near the interface was visibly blackened (Figure 5-36). Reducing zirconia is known to increase the electronic conductivity [76, 77]. The decreasing RS in the impedance data indicates that electronic conductivity was induced in the YSZ during the SCPs. The increasing RS thereafter indicates loss of the electronic conductivity in the YSZ as it re-oxidizes. The RS seemed to increase more quickly in 50% H2O/H2 than in dry H2, which is consistent with re-oxidation because the pO2 is much greater in 50% H2O/H2. Re-oxidation of electrochemically reduced YSZ has been studied in the literature [78]. The blackened coloration seems to last much longer through oxidation than the electronic conductivity. —Lasting activation (decrease in LSRP). The activation could be the result of a few different mechanisms. The electrons that were trapped in the electrolyte surface might enhance the catalytic activity, proposed by ref. [67]. Impurities such as SiO2 that were blocking parts of the TPB might be reduced to metal and unblock parts of the TPB, proposed by ref. [14]. In the present study, polarization at between –500 and –1000 mV provided the first activation effects. The polarization was applied in dry H2 atmosphere (–1370 mV vs air at 850 °C). Therefore, this corresponds to an oxygen activity of –1870 to –2370 mV vs air (10-35 to 10-44 atm O2 at 850 °C). The maximum polarizations of –1500 and –2000 mV correspond to –2870 and –3370 mV vs air (10-53 to 10-62 atm O2 at 850 °C). According to thermodynamic data, silica is favored to reduce to Si at oxygen activities less than 10-33 atm at 850 °C [54]. ZrO2 is favored to reduce to Zr metal at 10-41 atm. The segregated impurities are known to be comprised of glassy Na-K-Ca-Mg-Al-Si phases which segregate as a ―rim ridge‖ at the perimeter of the interface [11, 14, 35-37, 39, 43, 79]. In the present study such phases were found as particles embedded in or attached to the metal wire in some locations, as well as on thePDF Image | Electrolysis of CO2 and H2O
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