EDX Array Tomography: 3D Imaging With Chemical Sensitivity and Submicron Resolution Through Ultramicrotomy and...

Area of Science:

• Materials Science
• Analytical Chemistry
• Nanotechnology

Background:

• Energy-dispersive X-ray spectroscopy (EDX) offers elemental contrast but lacks depth resolution for 3D imaging.
• Conventional EDX is limited to conductive samples, hindering analysis of multiphase materials with complex geometries.
• Existing methods struggle with depth limitations and charging artifacts in non-conductive samples.

Purpose of the Study:

• To develop a novel tomographic imaging method for multiphase samples using EDX.
• To overcome the limitations of conventional EDX in depth resolution and sample conductivity.
• To enable submicron resolution 3D analysis of polymer-containing multiphase materials for energy applications.

Main Methods:

• Adaptation of array tomography using an automated tape-collecting ultramicrotome (ATUMtome).
• Integration of scanning electron microscopy with EDX mapping for elemental analysis of serial sections.
• Surface coating of sections to mitigate charging artifacts during imaging.

Main Results:

• Achieved submicron resolution tomographic imaging of polymer-containing multiphase samples.
• Successfully imaged a multiphase microporous layer in a CO2 electrolyzer gas diffusion electrode.
• Overcame depth resolution limitations inherent in traditional EDX surface mapping.
• Mitigated charging artifacts on low-conductivity samples through surface coating.

Conclusions:

• EDX array tomography provides a powerful new approach for 3D elemental analysis of challenging materials.
• The technique is particularly valuable for analyzing complex multiphase samples in energy materials research.
• This method enables detailed digital modeling of components like CO2 electrolyzer electrodes, previously unachievable.