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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 120 (5.2) where is the measured area from the SEM micrograph and is the radius estimated from Newman equation (5.1) using the final RS and temperature measured at the end of the test (and the YSZ conductivity was estimated at this temperature based on literature [44]). Next, a roughness factor was applied, to account for the deviation in the perimeter length from a perfect circle: (5.3) where is the perimeter length measured from the SEM micrograph and is the perimeter length that corresponds to a perfect circle having the area of . Note that using these correction factors for times earlier in the test assumes that the overall shape of the contact area did not change by a lot during the slight creep and ―un-creep‖ that occurred after initial stabilization. A few example calculations of these correction factors are given in Table 5-2. One can see that the Newman relation consistently underestimated the contact area by about a factor of 2, and that all of the contact areas had a rough perimeter which was longer than that corresponding to a perfect circle. Electrode Ni-5 stands out from this group – it had a much higher roughness factor of 2.38. The flattened contact area of Ni-5 is shown in Figure 5-6 (labeled ―Ni‖). One can see that the perimeter boundary is very rough in comparison with most of the other wires, such as Cu and Pt (also shown in Figure 5-6). The other Ni electrodes listed in Table 5-2, Ni-1 to Ni-4, were the wires that included electropolishing as a final stage of preparation, so their surfaces were especially smooth and they formed an even smoother contact interface than that of the Pt wire shown in Figure 5-6. Without electropolishing, the bent Ni wire Ni-5 had a fractured surface going into the test. The Pd wire shown in Figure 5-6 shows a similar degree of fracture and resulting roughness. Using these correction factors, the impedance measurements can be normalized to either the contact area or the perimeter of the contact area by multiplying them by and respectively, where is the radius estimated by equation (5.1). Since the reaction sites have been linked to the TPB, the TPB length (TPBL), which is the perimeter for these point-contact electrodes, may be a useful metric to normalize resistances [4, 6, 19, 21, 24]. This is illustrated in Figure 5-8 – the TPBL-normalized impedance measurements are reproducible, whereas the area-normalized impedance measurements are not. The fact that the area-normalized impedance of the rough Ni-5 electrode is the farthest from the others whereas its TPBL-normalized impedance agrees well with that of the smooth, shorter-TPBL electrodes confirms that the TPB is the primary location of the reaction sites. The other metals showedPDF Image | Electrolysis of CO2 and H2O
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