The phase stability and compatibility of intermediate temperature solid oxide fuel cell (IT-SOFC) composite cathodes of lanthanum nickelate, La 2 NiO 4+δ (LNO), and ceria-gadolinium oxide, Ce 0.9 Gd 0.1 O 2-δ (CGO10), have been investigated by high resolution synchrotron X-ray diffraction (XRD). No reaction was observed between LNO and CGO10 at temperatures of up to 900°C when the composite is open to an ambient air environment. However, in a sealed capillary environment the 50:50 wt% LNO:CGO10 composite undergoes a partially reversible reaction at temperatures of 750°C and above, whereby LNO decomposes to La 2 O 3 and Ni. Changes in the CGO10 Bragg peaks indicate that this component is actively involved in this process. This study shows that the phase stability of LNO:CGO10 composites is highly dependent on oxygen partial pressure. In addition, it is observed that ex-situ XRD is insufficient to determine the presence of reactivity in composite cathodes and that high resolution in-situ XRD measurements are required to obtain details of the complexity of phase stability in SOFC composite cathodes. Figure 1 oriented with the b axis in the long direction; a slight tilting of the nickel octahedra can be seen in the Bmab structure shown in Figure 1(a). From the studies discussed above 7, 18-21 it appears that LNO reacts with fluorite structured ceria based electrolytes and is apparently stable in contact with perovskite-type lanthanum gallate. However, all of these studies were performed using ex-situ XRD, that is, XRD was performed at room temperature after the composite had been annealed. With this method it is not possible to monitor any reactions as they develop, as either a function of temperature or time, nor is it possible to identify whether there is any degree of reversibility. This study differs from those previously undertaken through the use of in-situ synchrotron XRD, enabling a detailed probing of the reaction mechanisms as a function of temperature, time and environment. Whilst it is apparent from the ex-situ XRD studies, that there is ready formation of higher order Ruddlesden-Popper phases under certain conditions, it is likely that LNO phase stability is sensitive to oxygen partial pressure and temperature and there is a need to 5 investigate the reaction as it develops; for this reason, we have undertaken in-situ studies of LNO:CGO10 composites using high resolution synchrotron X-ray powder diffraction.
ExperimentalA 50:50 wt% composite of LNO:CGO10 was created from LNO powder (Cerpotech) and CGO10 powder (Praxair), which were calcined separately at 1400°C for 5 hours. The relative weight percentage of each powder was measured for the desired composition and the mixture was ballmilled with zirconia mixing balls for 24 hours in ethanol. The resultant composite powder was dried at 100°C for 16 hours. All synchrotron X-ray diffraction patterns were obtained on beamline I11 at the Diamond Light Source, UK. Technical descriptions of the I11 instrument can be found in the paper by Thompson et...