In situ and ex situ Raman analyses of porous Ni/CGO electrodes reveal differences in the amount, location and type of carbon formed during CO/CO2 electrolysis. The results demonstrate the limitations of optical in situ techniques applied to Solid Oxide Cells (SOCs) operated in electrolysis conditions. Increased carbon deposition close to the electrode-electrolyte interface is likely to be the result of high charge-transfer current in that area. The positive effect of a CGO interlayer on reducing carbon formation on the fuel electrode is demonstrated.
Raman spectroscopy is a powerful characterization tool for improving the understanding of solid oxide fuel cells (SOFCs), capable of providing direct, molecularly specific information regarding the physical and chemical processes occurring within functional SOFCs in real time. In this paper we give a summary of the technique itself and highlight ex situ and in situ studies that are particularly relevant for SOFCs. This is followed by a case study of carbon formation on SOFC Ni‐based anodes exposed to carbon monoxide (CO) using both ex situ and in situ Raman spectroscopy combined with computational simulations. In situ measurements clearly show that carbon formation is significantly reduced for polarized SOFCs compared to those held at open circuit potential (OCP). Ex situ Raman mapping of the surfaces showed clear variations in the rate of carbon formation across the surface of polarized anodes. Computational simulations describing the geometry of the cell showed that this is due to variations in gas access. These results demonstrate the ability of Raman spectroscopy in combination with traditional characterization tools, to provide detailed understanding of critical processes occurring within functional SOFCs.
A novel miniaturised heated stage for in operando optical measurements on solid oxide fuel cell electrode surfaces is described. The design combines the advantages of previously reported designs, namely, (i) fully controllable dual atmosphere operation enabling fuel cell pellets to be tested in operando with either electrode in any atmosphere being the focus of study, and (ii) combined electrochemical measurements with optical spectroscopy measurements with the potential for highly detailed study of electrochemical processes; with the following advances, (iii) integrated fitting for mounting on a mapping stage enabling 2-D spatial characterisation of the surface, (iv) a compact profile that is externally cooled, enabling operation on an existing microscope without the need for specialized lenses, (v) the ability to cool very rapidly, from 600 °C to 300 °C in less than 5 min without damaging the experimental apparatus, and (vi) the ability to accommodate a range of pellet sizes and thicknesses.
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