In-Situ Surface Analysis of SOFC Cathode Degradation Using High Temperature Environmental Scanning Electron Microscopy

Solid Oxide Fuel Cell (SOFC) cathode materials rely on the catalytic processes at their surfaces to reduce and incorporate oxygen. For many common cathode materials surface passivation occurs through 'A site' segregation at common operating temperatures [1]. These processes have a negative effect upon the oxygen reduction rates and therefore overall cell performance. Quantifying the true extent these segregation effects have on the exchange properties has not been fully explored but it is clear that the properties of the surface are essential.

Many techniques have been employed to study cell properties in-situ, however, surface studies are typically restricted to post mortem or ex-situ analysis due to the necessity of a high vacuum. In this study High Temperature Environmental Scanning Electron Microscopy (HT-ESEM) has been employed to analyse the morphology changes of common SOFC cathode materials in-situ. Samples of La_0.6Sr_0.4Co_0.2Fe_0.8O_3-x (LSCF) and La_0.6Sr_0.4CoO_3-x (LSC) were annealed from room temperature to 1000^oC at pressure ranges between 3 – 6mbar in atmospheres of Oxygen and Water. Using secondary electron imaging during the thermal annealing cycle morphological and compositional changes were able to be documented at temperature for the first time (Figure 1).

This technique has enabled detailed analysis of the surface degradation that occurs during SOFC fuel cell operation. Secondary phase precipitation rate and formation behaviour has been quantified over a range of temperatures and time scales furthering the understanding of SOFC cathode surfaces significantly.

[1] M. Kubicek, A. Limbeck, T. Fromling, H. Hutter, and J. Fleig, "Relationship between cation segregation and the electrochemical oxygen reduction kinetics of La_0.6Sr_0.4Co_0.2Fe0.8O₃ thin film electrodes" Journal of The Electrochemical Society, vol. 158, no. 6, pp. B727–B734, 2011.

Figure 1 - Showing in-situ growth of secondary phase particulates on a polished surface of LSCF