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Chapter 6. Molybdate Based Ceramic Electrode Materials 206 only the LSRP in 3% H2O/H2 is given, because the material oxidized to SrMoO4 upon switching to 50% H2O/H2. From the rest of the results, one can see that SFM and the pre-reduced SNM materials have the highest electrocatalytic activity in the OCV measurements. The SMM electrode was made of the air-sintered material, so even though it was pre-reduced at 800 °C in dry 9% H2/Ar, its electrochemical performance was most likely lower than it would be for a reducing-sintered sample (see discussion about SMM in section 6.3.2). For all of the electrodes, LSRP in 3% H2O/H2 is lower than or equal to LSRP in 50% H2/H2. Most likely this can be attributed to the fact that 3% H2O/H2 is a more reducing atmosphere, which more strongly reduces the ceramic materials at least at the surfaces, leading to oxygen loss and a higher concentration of electrons and oxygen vacancies. Another noteworthy observation is that, whereas most of the materials have significantly lower performance in 50% CO2/CO than in 50% H2O/H2, SVM has almost the exact same performance, which suggests that V may be a good catalyst for the CO/CO2 reactions. At the other extreme, the much lower performance of SCM in CO/CO2 than in H2/H2O suggests that Co may not be a desirable catalyst for CO/CO2 reactions. Finally, also marked on the plot is the LSRP range obtained for the donor-doped strontium titanates. Although these titanates are known to provide poor performance as electrode materials, the fact that the new materials have 2 orders of magnitude lower LSRP values suggests that they are very promising electrocatalysts. SEM inspection of the electrode surfaces after testing showed the nanostructured surfaces described in the last section, for SNM and SCM. In fact, for the SNM electrode that was not pre-reduced, the decomposition was apparent in the sequence of impedance spectra measured during the electrochemistry test (Figure 6-29). At around hour 35 of the test, which was about 30 hours after having reached 850 °C and switched to 3% H2O/H2, the shape and magnitude of the impedance spectra suddenly changed. This change most likely indicates that the decomposition reached a threshold, at least at the surface. Perhaps the newly formed materials and nanostructured surface defined the interface region near the TPB at that point. Figure 6-29. Impedance spectra measured at OCV on the non-pre-reduced SNM electrode in 3% H2O/H2 at 850 °C. The numbers above each peak are the approximate summit frequency in Hz.PDF Image | Electrolysis of CO2 and H2O
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