The objective of this project was to perform post-test characterization of cathode samples that were subjected to electrolysis testing by Northwest Aluminum Technologies, Inc. (NAT), Seattle, WA. The electrolysis tests were performed in a novel low-temperature cell for smelting aluminum metal that is being developed by NAT with funding from the Office of Industrial Technologies, U.S. Department of Energy. Cathodes in this cell design were in the form of small, thin plates. After testing, the plates were sent to Pacific Northwest National Laboratory (PNNL), where they were mounted, cross sectioned, and polished. A combination of optical microscopy, scanning electron microscopy (SEM), and energy dispersive x-ray spectroscopy (EDS) analysis was then performed on them to determine the extent of degradation the samples had undergone, the characteristics of the Al metal layer that coated the cathodes, and the identity of reaction phases within and on the outside of the cathode material.