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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 114 during the gas variations were set such that the total was 6 L/h. Impedance spectra (IS) were then continuously measured at open-circuit voltage (OCV) for each of the 4 cells. The potentiostatic IS measurements typically used 9 to 13 points per decade, from 1 MHz to 3-100 mHz, with an AC RMS amplitude of 20-30 mV, using a Solartron 1255B+1287 or a Gamry Reference 600. The series resistance (RS; the high-frequency intercept with the real axis) was monitored during and after heat-up to the initial temperature, while the contact area expanded due to the metal creep. 5.2.3. Systematic Electrochemistry Characterization The following electrochemistry characterization procedures are the optimized result of an iterative process; it was found that the order of characterizations was important because changing some experimental parameters resulted in either permanent changes in the metal-YSZ interface or temporary changes that took more than a full day to return to steady-state, so these parameters were changed last. It was found that degradation during measurements was not significant, that the impedance was quite stable over days. This is in contrast to some other studies which used Ni pattern electrodes [22] and porous Ni electrodes [24], which may be due to morphological changes of the electrode-electrolyte interface in those tests, or their use of possibly contaminated gasses (here the gasses were cleaned before use). First, electrochemical impedance spectra were measured at OCV at a variety of conditions. The temperature was varied from 750-1000 °C for three ―base‖ gas compositions: 97% H2 + 3% H2O, 50% H2 + 50% H2O, and 50% CO + 50% CO2 (here after referred to as 3% H2O/H2, 50% H2O/H2, and 50% CO2/CO respectively). The temperature was varied non- consecutively (for example, 1000–850–750–800 °C rather than 1000–850–800–750 °C) to avoid including any time-varying effects in the trend, e.g. if the electrode performance is degrading with time, the temperature-dependent performance results would incorrectly include this degradation and not only represent temperature dependence. Then, at a fixed temperature (first 1000 °C and then 850 °C), the gas composition was varied systematically in H2/H2O/Ar and CO/CO2/Ar atmospheres. This variation included fixing the pH2O at 0.5 atm while lowering the pH2 in steps from 0.5 down to 0.01 atm with the balance supplied as argon. Similarly, the pH2 was kept constant and pH2O varied, and then in another variation the pO2 was kept constant by fixing the pH2/pH2O ratio, reducing both the pH2 and pH2O equally, together. Finally, the pCO2 was kept constant while changing the pCO. Time was allowed for the cells to nearly stabilize at each condition by measuring impedance spectra at OCV during the stabilization times. The stabilization times were usually several hours, significantly longer than the time it took for the gas composition to equilibrate according to the pO2. The ―base‖ conditions were returned to in between some variations to check that the performance had not appreciably changed. An example gas composition variation that included fixed pH2O, fixed pO2 and fixed pCO2 measurements performed at 1000 °C during a test is shown in Figure 5-2.PDF Image | Electrolysis of CO2 and H2O
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