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Chapter 5. Aspects of Metal-YSZ Electrode Kinetics 112 oxidation of H2 on Ni has been reported as many times faster than CO oxidation in some Ni electrode studies [32, 33], while in others they have been reported as nearly equal [34]. While different electrode geometries and test set-ups might be able to explain some cases, it has become clear that impurities accumulated at the TPB may be playing a large role in the inconsistencies, by complicating the interpretation of data and even by changing the reaction mechanism [1, 14, 27, 35-38]. Because of the known presence of impurities at the interface, the purity of the materials used in a study is noted when discussing the literature in the following sections. Specific points from electrode kinetics literature will be further addressed when relevant. 5.2. Experimental 5.2.1. Preparation of cells Cells with a metal wire electrode contacting a (Y2O3)0.08(ZrO2)0.92 (8 mol% YSZ , or 8YSZ) electrolyte pellet (approximately 8 mm diameter and 3 mm thick) with a porous Pt-paste counter electrode were assembled in a single-atmosphere custom test rig. The test set-up was similar to that used in [15]. A pseudo-three-electrode set-up was used, with the relatively large counter electrode expected to contribute negligible resistance and therefore serving as reference electrode. The YSZ pellets were fabricated from Tosoh TZ-8Y powder. The powder was used as- received and uniaxially pressed (187 MPa) followed by cold isostatic pressing (250 MPa) for 30 s each. The resulting pellets were sintered at 1550 °C for 2 h in air. One side of the pellets was then ground and polished in several steps, ending with 1 μm diamond paste. Finer polishing was also tried on 2 pellets and this showed no effect on the impedance data; the measurements were reproducible with or without the extra polishing. Scanning electron microscope (SEM) and atomic force microscope (AFM) scans of the surface showed a dense, smooth topography with a small concentration of tiny holes that did not extend far into the surface. The other side of each pellet was lightly ground. The pellets were cleaned in ethanol in an ultrasonic bath. The unpolished side was then painted with Pt paste which was subsequently sintered to form the porous Pt counter electrode. The metal wires had the following diameters and purity: Ni, 0.5 mm, 99.999% (Puratronic, Johnson Matthey); Cu, 0.5 mm, 99.999% (Puratronic, Johnson Matthey); Ag, 0.3 mm, purity unknown; Au, 0.3 mm, purity unknown; Pd, 0.5 mm, 99.95%; Pt, 0.5 mm, 99.95% (Ögussa). Some wires were cut and bent approximately 1 cm from the end, to form a ―J‖ shape (Figure 5-1) similar to references [35] [11, 14, 15, 36, 37, 39]. Other wires were melted at the end with a reducing torch flame, to form a bulbous tip (Figure 5-1) similar to ref. [6]. Some of the bent wires were annealed and electropolished as described in ref. [15]. These wires had a smoothPDF Image | Electrolysis of CO2 and H2O
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