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Chapter 6. Molybdate Based Ceramic Electrode Materials 195 An EDX map was performed on the particles in a grain boundary of sample SNM_2 (Figure 6-19). This clearly shows that the nanoparticles are Ni-rich, however they appear to not simply be Ni metal particles because the Mo signal does not drop within the scan area of the nanoparticles. Therefore they might be Ni-Mo alloy particles. XRD data of these surfaces completed the picture and revealed more phases besides the precipitated nanoparticles. According to the XRD data, within a few hours at 800 °C in dry 9% H2/Ar, SNM completely decomposes. First, Sr3MoO6 dominates and is accompanied by some SrMoO3 and Ni/MoNi4 nanoparticles. As reduction continues, the fraction of SrMoO3 and Ni/MoNi4 increases until there is nearly as much SrMoO3 as Sr3MoO6 after 300 h (for the 300-h conductivity tested sample, Figure 6-10a). A small fraction of Sr2MoO4 also sometimes accompanies the decomposed phases. We are therefore able to propose a decomposition mechanism, or two mechanisms that seem to be occurring and interplaying to different extents: 1. Sr2NiMoO6 1⁄2 SrMoO3 + 1⁄2 Sr3MoO6 + Ni + 3⁄4 O2 2. Sr2NiMoO6 1⁄4 Sr2MoO4 + 1⁄2 Sr3MoO6 + 1⁄4 MoNi4 + O2 From these reactions we can also surmise the source of the enhanced electronic conductivity based on the product phases. As shown earlier, SrMoO3 exhibits very high metallic conductivity. Sr2MoO4 has also been reported to have metallic conductivity [98] or perhaps even superconductivity [99]. The Sr3MoO6 strontium molybdate phase was found to be a mixed ionic-electronic conductor with oxygen ion transference numbers of 0.2–0.4 in the temperature range from 800 to 1050°C [100, 101]. The metallic nanoparticles may also enhance electronic conductivity, but since they appear to be largely disconnected they may not enhance it as much as would first appear. The observed decomposition can explain the increasing conductivity observed during measurement as well as the wide range of conductivity results in literature that were thought to be due only to the formation of oxygen vacancies and corresponding partial reduction of Mo6+ to Mo5+. It can also provide an alternative explanation for the high oxygen vacancy values that have been reported for SCM (δ = 0.14-0.17 in Sr2CoMoO6-δ) [42, 93], whereas a value of only 0.05 has been reported for SMM [87, 102, 103]. From an application standpoint this decomposition is not necessarily disadvantageous. The resulting composite material may provide excellent electrocatalytic activity. The nanostructures were observed all over the unpolished surfaces of the various samples (Figure 6-20 through Figure 6-23). Precipitation of Ni or Pd metal particles from titanate ceramics in a reducing atmosphere has been exploited in catalysis [104-107][108], and precipitation of Ni or Ru metal particles from chromite ceramic solid oxide cell anodes has been observed [109, 110],PDF Image | Electrolysis of CO2 and H2O
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