Current efforts focus on performance optimization of the catalyst layer in membrane electrode assemblies (MEAs), which in addition to detailed information on the as-synthesized and treated catalysts, also requires investigation of these materials when part of an electrode. Structure, composition, and morphology were determined with initial 2D characterization of the NWs and electrodes using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) via scanning transmission electron microscopy (STEM), and X-ray photoelectron spectroscopy (XPS), as well as synchrotron techniques including X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectroscopies. Beyond these methods, transmission X-ray microscopy (TXM) allowed for high resolution, non-destructive, element-specific analysis of the electrode structure with 2-D and 3-D visualization. Catalyst composition/structure and electrode fabrication conditions were varied to explore opportunities and limitations of in situ characterization of the electrodes with these low Pt loadings extended surface catalysts.
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