Quantifying elemental colocation in nanostructured materials using energy-dispersive X-ray spectroscopy

Multicomponent nanostructured materials are key amongst others for energy and catalysis applications. The nanoscale proximity of different metals critically determines the performance of these functional materials. However, it is difficult to study the spatial distribution of different elements at the nanoscale, especially achieving a statistically relevant assessment. Additionally, common support materials like metal oxides are sensitive to electron beam damage when using high resolution local techniques, such as transmission electron microscopy. We present a robust strategy to quantitatively assess elemental distributions in 3D nanostructured beam-sensitive samples. Key elements are resin embedding, and elemental co-localisation building on a combination of electron tomography and energy-dispersive X-ray spectroscopy. We showcase the methodology with ∼ 3 nm Pd-Ni nanoparticles supported on mesoporous silica. Epoxy resin-embedding ensured sufficient sample stability under the electron beam for tomography-based quantification of different mano- and mesoscale elemental distributions in these samples. Reliable co-location results were obtained and practical guidelines are provided for acquisition and post-processing, relevant for elemental overlap analysis in multi-metallic samples.