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Chapter 6. Molybdate Based Ceramic Electrode Materials 180 One must also consider the thermodynamic stability of the valence states of the ions during synthesis and operation. Diagrams of phase stability versus temperature and pO2 for the Mo-O and W-O systems are shown in Figure 6-2. These are the constituent oxides of the perovskites, e.g. SrO + MoO2 SrMoO3. Knowledge of the preferred valence state based on the constituent oxides is useful as a guideline for synthesis parameters and as an indication of possible stability ranges during operation. Also marked on the diagram are typical operating conditions, 700-900 °C and 3%, 50%, and 90% H2O / H2. The 3% and 90% H2O conditions represent SOFC and SOEC starting conditions, and the 50% H2O condition represents the average gas compositions that would be seen across an operating cell (in either mode, fuel cell or electrolysis) run at high reactant utilization – as mentioned in section 5.1. As a simple test to briefly examine the Mo-O phase transitions, a bent Mo metal wire point electrode was used as with the other metal point electrodes described in Chapter 5. The Mo metal wire easily oxidized to MoO2 upon exposure to 50% H2O/H2, in agreement with the thermodynamic data. This was evident in the impedance measurements – MoO2 is still electron conductive but has lower electrochemical activity. Upon re-exposure to 3% H2O/H2, the electrode reduced back to metal. Figure 6-3 shows SEM micrographs of the surface of the wire that had been smooth before the experiment. After re-reduction the surface ―bloomed‖ into interesting nanostructures. The surface area increased, similar to the Ni electrode after oxidation (see section 5.3.5.1). One could say that the Mo metal wire was redox cycled between 3% H2O/H2 and 50% H2O/H2. 0 -6 -12 -18 -24 -300 300 600 900 1200 1500 0 300 600 900 1200 1500 90% H2O / H2 50% H2O / H2 3% H2O / H2 WO3(s) WO3(l ) WO3(s2) WO2(s) W(s) MoO3(l) MoO3(s) MoO2(s) Mo(s) MoxOy(g) T(oC) Figure 6-2. Phase stability for the Mo-O and W-O systems, according to thermodynamic data [40]. T(oC) log(pO2 (atm))PDF Image | Electrolysis of CO2 and H2O
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