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Chapter 6. Molybdate Based Ceramic Electrode Materials 183 Conventional 4-point DC conductivity tests were performed on the sintered bars. First, #320 SiC grinding paper was used to remove a few microns from all surfaces of the bars. Pt wire and Pt paste were used to form the current leads at each end of a bar. Pt wire voltage probes with a fixed separation distance (built into the test set-up) were contacted to the surface. Electrochemistry tests were performed on most of the materials using a similar set-up as that described in Chapter 5. The cells consisted of pointed ceramic electrodes contacting a smooth polished YSZ pellet surface (prepared the same as in Chapter 5), with a much larger porous Pt counter electrode acting as a reference electrode (pseudo 3-electrode setup, see Figure 6-4), similar to the metal point electrode tests of Chapter 5. The pointed electrodes were prepared from the sintered pellets by grinding the pellets to a cone-like shape, as has been used in prior work [46-53]. In the present study, however, the pointed electrodes were made by hand-grinding on SiC paper affixed to a grinding wheel, with the grinding direction away from the tip so as to avoid getting SiC particles lodged in the electrode, which would contaminate the electrode with impurities (it was also verified by SEM on some electrodes that no SiC particles were present on the pointed tip nor anywhere on the electrode surface). This resulted in ―pyramid‖ rather than cone shaped electrodes. It was found that equivalent results could be obtained by machining the pellets into a cone versus the hand-grinding method. In fact, a number of electrode geometries using the same material were tested, as it was desired to find a standard platform to quickly test the electrochemical properties of different materials without going through the entire cell development process. The advantages and disadvantages of the different geometries will be reported in the future. The point-contact geometry is a very useful geometry, especially if the TPB can be measured after testing and used to apply correction factors to the Newman relation as done for the metal point electrode study of Chapter 5. For the materials studied here, given the sintering conditions used, it was possible to observe the TPB in the SEM after testing and measure its length. Pointed electrode Porous Pt counter electrode Figure 6-4. Photograph and diagram of ceramic cone-type point electrode used in the electrochemistry tests. Some donor-doped strontium titanate based materials known from literature were also included here for comparison, including Sr0.94Ti0.9Nb0.1O3 [10, 53, 54], La0.35Sr0.65TiO3 [55, 56], Y0.08Sr0.92TiO3 [57, 58], and Y0.08Sr0.88TiO3 [59-62]. These materials were also prepared by solidPDF Image | Electrolysis of CO2 and H2O
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