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Chapter 4. Co-electrolysis of CO2 and H2O in Solid Oxide Cells 96 apparently involves accumulation of impurities at the three-phase boundary (TPB) between the gas, Ni particles and YSZ particles where the reactions occur [17, 21, 27, 34, 38]. Several mechanisms for degradation have been proposed, and the mechanism might depend heavily on the gas atmosphere—impurities may originate from the test setup [17, 21], from the cell materials [38], and/or from the gasses [27, 34], or the gas atmosphere in combination with high temperature (e.g. 90% steam at 950 °C) may induce mobility of Ni leading to degradation of the electrode microstructure [21]. Characterizing cell durability is complicated by the fact that cell performance sometimes temporarily degrades (passivates) and then recovers (activates), and the real long-term degradation is occurring simultaneously [21, 34]. The magnitude of the cell operating voltage or resulting current density may also affect the durability. Cell durability at high current density (>0.5 A/cm2 electrolysis) has not been widely reported, although high current density operation may be necessary for an economical synthetic fuel production process (see Chapter 3, section 3.3.2). By analyzing the impedance spectra measured at systematically varied test conditions, the cell resistance can be broken down into contributions from the electrodes and electrolyte. Ideally, breaking down resistance can be aided by using a reference electrode that isolates the response of one of the two electrodes (three-electrode set-up). However, using a reference electrode with thin-electrolyte technological solid oxide cells is not possible – proper placement of a reference electrode is difficult and measurements are known to be distorted due to non- uniform current distribution [39-41]. Consequently, breaking down the resistance involves deconvolution of impedance spectra that have overlapping processes (similar characteristic frequencies). Prior methods of breaking down the cell resistance relied on performing a complex nonlinear least-squares regression to an equivalent circuit composed of an array of serially connected circuit elements (Voigt measurement model) – an inductor (L), a resistor (R), and five serial RQ (resistor in parallel with a constant phase element) subcircuits, or in common equivalent circuit notation, LR(RQ)(RQ)(RQ)(RQ)(RQ) [42, 43]. This equivalent circuit has 17 parameters (one for each L element, one for each R element, and two per Q element) that must be fitted to the impedance data, which requires careful and difficult analysis involving fixing some parameters while fitting others. Alternative methods of breaking down the resistance or at least for providing input data and constraints to the equivalent circuit would be useful. Recently, alternative methods to identify processes have been employed [44], including analysis of differences in impedance spectra (ADIS) [45] and transformation of the impedance data to the distribution of relaxation times (DRT) [46-48]. Both methods increase the resolution of the peaks of the specific processes at their characteristic frequencies, which is helpful for identifying the different processes. In the present study the DRT method is used to analyze the performance and degradation. See Chapter 1, section 1.2 for more information about the DRT and other impedance analysis techniques.PDF Image | Electrolysis of CO2 and H2O
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