Local Hydrogen Concentration and Distribution in Pd Nanoparticles: An In Situ STEM‐EELS Approach

Local detection of hydrogen concentration in metals is of central importance for many areas of hydrogen technology, such as hydrogen storage, detection, catalysis, and hydrogen embrittlement. A novel approach to measure the hydrogen concentration in a model system consisting of cubic palladium nanoparticles (Pd NPs), with a lateral resolution down to 4 nm is demonstrated. By measuring the shift of the Pd bulk plasmon peak with scanning transmission electron microscopy (STEM) combined with energy electron loss spectroscopy (EELS) during in situ hydrogen gas loading and unloading, local detection of the hydrogen concentration is achieved in TEM. With this method, concentration changes inside the NPs at various stages of hydrogenation/dehydrogenation are observed with nanometer resolution. The versatility of in situ TEM allows to link together microstructure, hydrogen concentration, and local strain, opening up a new chapter in hydrogen research.