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PNNL-13501 - Pacific Northwest National Laboratory

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The testing setup consisted of a single alumina tube with<br />

the anode current and voltage leads down the center. The<br />

cathode electrical connections were made on the outside.<br />

The cell was cemented to the tube with Aremco cement to<br />

provide a gas seal. The fuel gas mixture of hydrogen with<br />

3% water flowed inside the tube while the cathode was<br />

exposed to ambient air. The arrangement was placed<br />

inside a Kanthol tube furnace and heated to 800°C where<br />

measurements were taken with a test rig from Arbin<br />

Instruments.<br />

Results and Accomplishments<br />

Development of Yttria-Stabilized Zirconia Electrolyte<br />

Sputtering Conditions<br />

The sputtering conditions required to produce dense,<br />

phase-stable yttria-stabilized zirconia electrolyte layers<br />

suitable for solid oxide fuel cell applications were<br />

established. Low temperature deposits in which the<br />

cermet substrate was not heated tended to produce an<br />

orthorhombic crystal structure in the yttria-stabilized<br />

zirconia deposit. This phase is unstable at temperatures<br />

required for subsequent processing of the electrodes and<br />

power output testing of the solid oxide fuel cell device (up<br />

to 1250°C). We found that at a 600°C deposit<br />

temperature, a tetragonal yttria-stabilized zirconia coating<br />

structure could be attained that was stable through<br />

——<br />

2 µm<br />

electrode processing and cell operation. Both the 7 and<br />

12 atom percent yttrium targets produced yttria-stabilized<br />

zirconia coatings with the tetragonal phase at 600°C.<br />

Microstructure of the yttria-stabilized zirconia electrolyte<br />

layer was also deemed a potentially important variable for<br />

solid oxide fuel cell operation. The microstructures of<br />

sputtered coatings are known to be related to a number of<br />

factors, including the substrate surface characteristics,<br />

deposition temperature, and sputtering gas pressure. An<br />

example of yttria-stabilized zirconia microstructure<br />

differences resulting from variations in substrate surface<br />

smoothness is shown in Figure 1. While the deposition<br />

temperature variable was restricted due to the phase<br />

considerations noted, experimental efforts were made to<br />

optimize gas pressure and substrate properties to achieve<br />

dense electrolyte coatings. Low sputtering pressures<br />

(≤ 2.5 m torr) were found to optimize production of dense<br />

coatings with minimal columnar structure. Similarly,<br />

during the course of this study, the processing parameters<br />

used to produce the cermet substrates were optimized to<br />

produce ceramic disks having a minimal surface texture.<br />

Optimization of these conditions allowed the production<br />

of highly dense yttria-stabilized zirconia microstructures.<br />

Figure 2 shows examples of high density ultrathin yttriastabilized<br />

zirconia electrode layers produced under<br />

optimal sputtering conditions.<br />

——<br />

2 µm<br />

Figure 1. Effect of substrate surface texture on the microstructure of sputtered yttria-stabilized zirconia coating. The coating on<br />

the left was produced on a porous cerment substrate having an irregular surface. The coating on the right was produced in the<br />

same coating run, but on a smooth glass substrate.<br />

Materials Science and Technology 331

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