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Chapter 6. Molybdate Based Ceramic Electrode Materials 184 state reaction. It was found that the titanates with compositions that were not charge- compensated, Y0.08Sr0.92TiO3 and La0.35Sr0.65TiO3, needed to be sintered in a very reducing atmosphere (dry 9% H2/Ar) at high temperature (1450 °C) to eliminate impurity phases such as the pyrochlores Y2Ti2O7 and La2Ti2O7. All of the sintered titanates were generally harder than the molybdates. Since they were harder, the contact area did not develop into a well-defined interface and was more difficult to determine. An additional method to determine the contact area was developed. At the end of a test, a strong cathodic polarization was applied (as for the metal point electrodes, Chapter 5, but for a different purpose). This is known to blacken the YSZ at the interface within the contact area, which made an ―imprint‖ of the cone-tip contact area. The cells were cooled immediately afterwards and the YSZ surface was examined by optical microscope to estimate the contact area by the area that had been blackened. The tip of one Sr0.94Ti0.9Nb0.1O3 (STN) cone-shaped electrode was coated with Gd- doped ceria (Ce0.8Gd0.2O2; CGO) particles by vacuum infiltrating a single drop of an aqueous solution composed of precursor nitrates and ethanol. The preparation procedure for the infiltration solution followed that of a recent study that found CGO-infiltrated porous STN backbone electrodes to have remarkably high performance [10]. That concept was applied here to the cone-shaped electrode. In the present study, the CGO precursors loaded into the electrode tip were decomposed to form the CGO phase in situ in the reducing atmosphere, forming submicron-sized CGO particles. The electrochemistry tests were similar to those described in Chapter 5 but included a less extensive characterization. Simpler tests were used to more rapidly test the materials and get an idea of their relative performance, without attempting to understand their possible reaction mechanisms. After assembling the cells, they were heated up to 850 °C in dry 9% H2/Ar (or 9% H2/Ar that was humidified with 1% H2O for some of the samples). The gas atmosphere was switched to 3% H2O/H2 and impedance spectra (IS) were measured constantly at OCV while the interface stabilized, usually 12-24 h but in some cases up to 100 h to allow time to reduce the ceramic electrode material if it was not pre-reduced. The potentiostatic IS measurements typically used 6 to 9 points per decade, from 1 MHz to 3 mHz, with an AC RMS amplitude of 10 mV, using a Gamry Reference 600. OCV IS were measured at different temperatures from 850 to 700 °C, repeating a set-point more than once to check if the electrode performance had changed during the temperature variation. The gas atmosphere was changed to 50% H2O/H2 and to 50% CO2/CO and the temperature variation was repeated for each. In 50% H2O/H2 and 50% CO2/CO, cyclic potential sweeps were performed from OCV to +300 mV to –300 mV to OCV for at least 3 cycles. Finally, IS were measured under polarization in 100 mV increments, in the order OCV, +100 mV, +200 mV, +300 mV, –100 mV, –200 mV, –300 mV, with 5 minutes of fixed DC bias (chronoamperometry) at each given applied potential before the IS measurement. 2 or 3 electrodes of the same material were tested for 4 of thePDF Image | Electrolysis of CO2 and H2O
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