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

Area of Science:

• Materials Science
• Nanotechnology
• Analytical Chemistry

Background:

• Multicomponent nanostructured materials are vital for energy and catalysis.
• Understanding nanoscale elemental distribution is critical for material performance.
• Electron beam damage limits analysis of beam-sensitive materials using techniques like transmission electron microscopy.

Purpose of the Study:

• To develop a robust strategy for quantitatively assessing 3D elemental distributions in beam-sensitive nanostructured samples.
• To overcome limitations in studying nanoscale elemental proximity and achieving statistically relevant assessments.
• To provide practical guidelines for elemental co-localization analysis in multi-metallic samples.

Main Methods:

• Resin embedding of samples to enhance stability under electron beam irradiation.
• Combining electron tomography with energy-dispersive X-ray spectroscopy for elemental co-localization.
• Utilizing a methodology demonstrated on ~3 nm Palladium-Nickel (Pd-Ni) nanoparticles supported on mesoporous silica.

Main Results:

• Achieved sufficient sample stability for tomography-based quantification of elemental distributions at nano- and mesoscales.
• Obtained reliable co-localization results for elemental analysis in complex nanostructures.
• Demonstrated the effectiveness of the resin embedding and tomography-EDX approach for beam-sensitive materials.

Conclusions:

• The presented strategy offers a robust solution for quantitative 3D elemental distribution analysis in beam-sensitive nanostructured materials.
• The developed methodology enables accurate assessment of nanoscale elemental proximity, crucial for optimizing material performance.
• Practical guidelines are provided for elemental overlap analysis, advancing the study of multi-metallic systems.