Polymer electrolyte membrane water electrolyzers (PEMWEs) play a vital role in promoting the widespread adoption of renewable hydrogen. To successfully fabricate and integrate components, develop scalable manufacturing techniques, understand degradation mechanisms, and devise strategies to mitigate degradation, it is essential to thoroughly characterize materials and components in these devices. Due to the complexity of these systems and various interconnected problems, as well as the multitude of relevant scales, the use of multi-technique characterization and the development of novel characterization approaches and methods are crucial.This talk will highlight the complementary nature of electron and X-ray microscopy and spectroscopy methods for investigating surfaces, interfaces, and interactions with focus on catalyst layers (CLs) with an emphasis on analysis of as-prepared, tested and degraded samples. Micro X-ray computed tomography (XCT) provides both 2D and 3D analysis, but its resolution is not sufficient to identify catalyst layer features with enough detail, especially when Pt PTL coatings and low Ir-based catalyst loadings are used. On the other hand, Scanning Electron Microscopy (SEM) coupled with Energy Dispersive X-Ray Spectroscopy (EDS) provides superior resolution and enables the differentiation of PTL coatings and catalysts. Although SEM-EDS provides only 2D information, by employing a combination of top-down and cross-sectional analysis, a comprehensive understanding of catalyst distribution within the PTL can be attained, facilitating the initial assessment of PTLs and PTEs. The parameters extracted from SEM-EDS data can be used for a comprehensive quantitative assessment of the composition and distribution of catalysts, highlighting the differences between fabricated samples across a wide range of fabrication variables. Transmission Electron Microscopy (TEM) in tandem with EDS is also essential for nanoscale analysis of CLs, and PTEs. However, it is limited by its focus on small areas and necessitates complex sample preparation, especially for degraded samples. To complement these techniques, Time-of-Flight Secondary Mass Spectrometry (ToF-SIMS) has been developed as a promising complementary method to offer chemical insights, particularly valuable in analyzing protective coatings, catalyst layers, and interfaces between different layers. Furthermore, X-ray photoelectron spectroscopy (XPS) has high sensitivity in discerning catalyst evolution and subtle variations at the catalyst-ionomer interface, highlighting its complementary role in elemental and chemical composition analysis, especially in the context of tested and degraded samples.
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