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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 113 surface. However, Ni wires prepared without the electropolishing step showed similar impedance once properly normalized (see section 5.3.2). Therefore, and since it would be difficult to similarly smoothen all the other metals by electropolishing (procedures for electropolishing some of the other metals are not well-known and in some cases not as straightforward as for Ni), all metals were simply heat-treated in a reducing atmosphere (9% H2 + 91 N2) at 600 °C after bending, to try to clean the surface of organic material. The bulb-tip wires were heat-treated in the same reducing atmosphere at 800 °C after melting the tip, which had caused some oxidation. The prepared wires were cleaned ultrasonically in ethanol and examined in SEM or optical microscope. (a) Bent-tip metal wire YSZ (b) Bulb-tip metal wire YSZ Porous Pt counter electrode Figure 5-1. Photographs and diagrams of the electrochemical cell set-ups used. (a) Bent metal wire electrode. Photograph: a Pd wire. (b) Melted bulb-tip metal wire electrode. Photographs: a Cu wire (top) and a Pt wire (bottom). All photographs were taken after testing. This Cu wire was stuck after testing and is roughened near the stem as a result of trying to pull it off of the YSZ surface. 5.2.2. Start-up of Electrochemistry Test The test rig was first cleaned of any stray particles by carefully applying compressed air. Four cells were assembled in the test rig in a laminar air flow chamber to try to avoid contamination. Each wire electrode was inserted into an alumina tube which held it in place and applied pressure downwards from a weight of 210 g attached above. The test set-up was similar to that used previously by Høgh and Schmidt [14, 15, 37, 39]. A Nernst probe (a cell formed on a closed-end tube of YSZ consisting of, internal chamber gasses/Pt/YSZ/Pt/air, where the Pt electrodes are porous and formed by sintering Pt paste) was located near the samples to measure the pO2. The test rig was heated to an initial temperature of 1000 °C or 850 °C (for the tests that included silver, to stay below the melting point of silver) in 9% H2 + 91% N2 and switched to 97% H2 + 3% H2O upon arriving at the initial temperature. For all gas compositions that included H2O, the H2O was supplied by flowing the proper amount of O2 to mix with the H2 stream which combusted to yield H2O, upstream of the cells and inside of the furnace. The H2, CO, and CO2 gasses were cleaned upstream of the rig. The gas flows during this time andPDF Image | Electrolysis of CO2 and H2O
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