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Chapter 6. Molybdate Based Ceramic Electrode Materials 186 Table 6-4. Optimized synthesis parameters for the molybdate materials. ―H‖ stands for dry 9% H2/Ar. ―w‖ stands for ―wet‖ (room-temperature humidified ~3% H2O); ―cw‖ stands for ―cold-wet‖ (~1.3% H2O). Composition SrMoO3 LaMoO Sr2CoMoO6 Sr2FeMoO6 Sr2MgMoO6 Sr2MgMoO6-δ Sr2MgWO6 Sr2NiMoO6 Sr2NiWO6 B site composition Heating #1 (powder) Acronym °C hr gas SM 1000 8 air LM 950 10 air SCM -- - Heating #2 (form Sinter dense phase, powder) sample °C hr gas °C hr gas SrTi0.5Mo0.5O3 SrTi0.5Ni0.25Mo0.25O3 Mo6+ Ni2+ SrV0.5Mo0.5O3 Mo6+ Mo5+/6+ Mo6+ Mo4+ Movarious+ Co2+ SFM 900 SMM_1 - SMM_2 850 SMW 900 SNM --- SNW --- STM 1200 12 w-H STNM502525 - - - SVM - - - 900 4 air 800 26H 900 10H 1300 12 air 1250 12 w-H 1300 12 air 1200 24H 1200 24H 1300 12 air 1300 12 air 1200 10 cw-H 1300 12 air 10 cw-H 1300 12 cw-H 1200 10 w-H 1400 12 air 1400 12 w-H 1400 12 air 1350 18 w-H 1350 18 w-H 1400 12 air 1400 12 air 1440 12 cw-H 1400 12 air 1300 12 cw-H Fe2+/3+ - - 12 air 12 air Mg2+ Mg2+ Mo5+/6+ W6+ Mg2+ Mo6+ Ni2+ W6+ Ni2+ Mo4+ Ti4+ Ti4+ Mo4+ V4+ formation of Mo metal, so the humidified 9% H2/Ar atmosphere was used. For the air-sintered samples, the compositions and synthesis conditions were optimized to eliminate SrMoO4 and SrWO4 impurities, which are commonly reported in literature to form during sintering in air (and found in the present study before optimization). Part of the optimization consisted of adding 2% excess NiO/MgO/etc. It did not seem to be a matter of there being insufficient NiO/MgO/etc in the precursors (for example, if some of the NiO had turned to carbonate over time, when measuring the weight of NiO to mix stoichiometric SNM, less Ni metal than expected would be present). It was found afterwards that another group recently reported needing to add 5 wt% excess NiO when preparing Sr2NiMoO6 by solid state reaction [68]. It is also worth noting that any remaining SrMoO4 will reduce to SrMoO3 in operating conditions – as mentioned above, this is in fact how SrMoO3 was prepared in the present study, and the SrMoO3 + 1⁄2 O2 SrMoO4 phase transition is reversible. Sr3MoO6 might also disappear during reduction. XRD data from a few of the compositions is shown in Figure 6-5. SrMoO3 and SrTiO3 appear to form a solid solution in SrTi0.5Mo0.5O3 – the peaks measured for SrTi0.5Mo0.5O3 fell directly between those of SrMoO3 and SrTiO3 (Figure 6-5a). A solid solution was also found for SrMo0.5V0.5O3. Based on the similar ionic radii, solid solutions are not unexpected and a literature search showed that they have been reported [69-71]. The double perovskites are all tetragonal at room temperature, evident by their peak splitting as shown for Sr2NiMoO6 (Figure 6-5b). They typically transition to cubic at 200-300 °C [68, 72-78]. The double-perovskite titanate hybrid, SrTi0.5Ni0.25Mo0.25O3, showed peaks between that of Sr2NiMoO6 and SrTiO3 (evident by the slight 2θ offset between Sr2NiMoO6 and SrTi0.5Ni0.25Mo0.25O3) – similar to SrTi0.5Mo0.5O3 in that both exhibited peaks in between their component oxides. Other XRD peaks that are indicative of double perovskites were present for SrTi0.5Ni0.25Mo0.25O3, but they were much smaller than those visible for Sr2NiMoO6.PDF Image | Electrolysis of CO2 and H2O
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