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Updated: May 24, 2025

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

Kristiaan H Helfferich1, Johannes D Meeldijk2, Marijn A van Huis3

  • 1Materials Chemistry and Catalysis, Debye Institute for Nanomaterials Science, Utrecht University, Utrecht, The Netherlands.

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Summary

This study introduces a new method for analyzing elemental distribution in nanoscale materials, crucial for energy and catalysis. The technique uses resin embedding and advanced microscopy to overcome beam damage and accurately map elements in complex nanostructures.

Keywords:
Bimetallic catalystsColocation analysisEDX spectroscopyPd-Ni

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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.