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Fixture for applying three independent electrical contacts to electrochemical devices in traditional vacuum systems. (a) Probes are contacted against the patterned electrodes on the electrochemical device using springs. The device rests on a resistive heater. (b) Photograph showing the fixture operating a hot solid-oxide electrolyte device with Pt working, reference and counter electrodes. The cone collects photoelectrons into the differentially pumped energy analyzer of ALS beamline 11.02.
Electrical circuit used for electrochemical operation and characterization. The illustrated device on the -diameter heater has the working and counter electrodes on the top and bottom, respectively, of the electrolyte disk.
Bottom panel: resistance and temperature of a Ni film on a YSZ substrate as a function of time during heating. Top panel: the resistance change normalized by the resistance at , , as a function of temperature. The line is a linear fit to the data.
Using the fixture and APXPS to measure the local electrical potentials of a solid-oxide electrochemical device. (a) False-color image from the two-dimensional electron detector on ALS beamline 9.3.2. The y-axis gives the sample position of photoelectron emission. Dashed line is the boundary between the unbiased Pt film and the bare YSZ. Dashed black/white line is a guide-to-the-eyes of the peak position. (b) When the Pt is biased by , the Pt peaks shift to lower kinetic energy (higher apparent binding energy). (c) SEM micrograph showing Pt islands that are physically and, thus, electrically disconnected from the patterned Pt electrode near its edge.
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