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Chapter 6. Molybdate Based Ceramic Electrode Materials 185 materials (SFM, SMM, SNM, and STM50), and 1 electrode was tested for the remaining materials. 6.3. Results and Discussion 6.3.1. Materials Synthesis The optimized synthesis parameters that were found are given for each material in Table 6-4. In some cases, Heating #1 was an initial heat treatment in air which was used to decompose the SrCO3 (otherwise it might remain as a carbonaceous material, since the pO2 is so low). For other materials Heating #1 was used to form an intermediate phase: for SM synthesis, the first heat treatment was 1000 °C for 8 h in air to form the oxidized phase, SrMoO4. The SrMoO4 was subsequently reduced in the listed Heating #2. According to literature [32, 35, 63-66] (and trials conducted in the present study), this is the most reliable way to obtain SrMoO3. Similarly, for LaMoO an initial heat treatment of 950 °C for 10 h in air was used to obtain La2Mo2O9. As in ref [24], the La2Mo2O9 was subsequently reduced to decompose it to an amorphous phase. The sintered densities were >90% theoretical for 1400 °C sintered samples and >66% for the 1300 °C sintered samples. Successful synthesis of the desired phase was often pO2 dependent – to obtain a reduced Mo valence, a reducing atmosphere was needed. Over-reduction can yield Mo metal, however, so careful control of the pO2 is necessary. Of the double perovskites, all that have 2+/6+ ordering when oxidized were possible to synthesize in air. In the literature, SMM produced by sol-gel synthesis is often sintered in reducing atmosphere [21], so a different sample, SMM_2, was sintered in reducing atmosphere – this will be further discussed in the following section 6.3.2. SFM had a narrower window of suitable pO2 required to form the phase and could not be synthesized in air – one or both of Fe2+/3+ and Mo6+ needed to be reduced. Synthesis in air yielded segregation of SrMoO4, and over-reduction yielded the Ruddleston-Popper phase Sr3FeMoO6.88 as has been reported in literature [67]. High phase purity was obtained for all materials except the reducing-sintered SMM_2, in which a few % MgO, SrMoO4, and Sr3MoO6 were present. These impurity phases were not present in the reducing-sintered SMM reported in literature [21], however in that study the powder was prepared by sol-gel synthesis, yielding a finer particle size, and the sintering temperature was only 1200 °C with a more strongly reducing atmosphere of dry 5% H2/Ar. In that study the intent was to sinter a porous electrode microstructure, not a dense sample. Here, on the other hand, solid state reaction was used and a dense sample was desired, so a higher sintering temperature was required. A stronger reducing atmosphere was found to result in thePDF Image | Electrolysis of CO2 and H2O
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