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Chapter 6. Molybdate Based Ceramic Electrode Materials 196 but not decomposition to this extent to form a composite of multiple useful phases with an entirely nanostructured surface. The apparent reversibility of the conductivity measurements seen in Figure 6-9d when increasing and then decreasing the pO2 suggests interesting behavior – potentially reversible phase changes between SNM and the decomposed phases. To investigate this, an SNM sample that had been reduced at 800 °C in dry 9% H2/Ar for 10 h was re-oxidized in air at 800 °C for 10 h. One can clear see from the X-ray diffractograms (Figure 6-24) that the material completely decomposed into Sr3MoO6, SrMoO3, and Ni/MoNi4 particles upon reduction, and upon re-oxidation the double-perovskite phase was almost entirely recovered, accompanied by small fractions of SrMoO4 and NiO. The long-term SNM conductivity test described earlier (Figure 6-10a) was continued with pO2 variations including oxidation in air and re-reduction (Figure 6-25). After 24 h exposure to air at 800 °C, during which the conductivity dropped to about 0.1 S/cm, the high conductivity was mostly recovered within 24 h upon re-exposure to dry 9% H2/Ar. The quickness with which the high conductivity was recovered, in comparison with the 300 h that were needed for the initial reduction-decomposition, suggests that the ―extra‖ SrMoO4 and NiO phases observed in the XRD are quickly reduced back to SrMoO3 and Ni. As a layer in an electrode this could be quite advantageous, providing the ability to refresh or regenerate the nanostructured surface by oxidizing and then re-reducing it, which might restore the surface’s high electrocatalytic activity that might have been lost over time as the nanostructures coarsened or impurities accumulated. Adding Ti to the B-site, as SrTi0.5Ni0.25Mo0.25O3, prevented decomposition and reduced the total conductivity that could be attained, which shows that the extent of decomposition can be controlled by modifying the composition. In the next section, the electrocatalytic activity of this decomposed material and some of the other materials are investigated.PDF Image | Electrolysis of CO2 and H2O
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