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Chapter 6. Molybdate Based Ceramic Electrode Materials 194 Finally, the conductivity of the tungstates was measured and was found to be <0.01 S/cm for both materials, SMW and SNW. In literature, the Fe-variant SFW, has been reported as an insulator [96, 97]. The insulating nature of W versus Mo can be explained by the relatively higher stability of Mo5+ versus W5+ [91]. This most likely relates to the narrow region of stability of W4+ as well, seen in the phase diagram earlier (Figure 6-2). Due to such a low conductivity, the tungstates could not be further studied as electrode materials. 6.3.3. Phase Stability and Microstructure The phases of all of the materials were examined by XRD before and after the conductivity tests. The microstructure of smooth polished surfaces was studied by SEM, as well. It was found that SNM exhibited the most remarkable changes, so SNM is the focus of this section. SCM exhibited similar behavior but was not studied in as much detail. The other materials, except for SM, were generally stable. Before testing, SNM was dense and its polished surface was smooth, with large 5-10 μm grains visible and sintered together. After all of the conductivity tests, as well as some additional heat treatments in reducing atmospheres, one surface of each sample was again polished and in the SEM the grain boundaries were clearly visible. However, it was not thermal etching – magnifying the areas revealed chains of nanoparticles lining the grain boundaries for the moderately-reduced sample SNM_2 (Figure 6-12 through Figure 6-15). The SEM micrograph taken with the backscatter detector (Figure 6-14) shows that the brightly-shaded nanoparticles are most likely metallic and electron-conductive, suggesting that they might be at least partly responsible for the enhanced electronic conductivity. On the polished surface of SNM_3, which has been exposed to a more reducing atmosphere for a longer time and exhibited higher conductivity, the apparent decomposition extended further into the grains (Figure 6-16). The polished surface of SNM_4, which had been reduced for several hundred hours, was almost completely decomposed – the grains were nearly gone and replaced with an remarkable topography with seemingly linear rows of the nanoparticles (Figure 6-17). We considered whether the nanoparticles might have aligned due to the electric field applied during conductivity testing, however similar features were observed on samples that were only reduced in a furnace without conductivity measurements and the orientation of the lines seem to be more related to the geometry of the grains that had been there than the direction of the electric field. In Figure 6-18, the polished surface of a sample that had been reduced by heat treatment without conductivity testing is shown. An apparent reaction front, from the upper left to the lower right, is visible. The edge of the sample was beyond the upper left of the image, and the center is beyond the lower right. It seems that, at least for this sample, the decomposition reactions took place at the surface and as the material was reduced at the grain boundaries, pathways were created for small amounts of the reducing gas to continue infiltrating the sample and continue the decomposition towards the bulk of the sample.PDF Image | Electrolysis of CO2 and H2O
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