The ability to perform compositional analysis, and visualize the resulting chemical maps in 3D, is essential to obtain the true elemental distribution or composition of a material, ultimately delivering new insights into the structure-function relationship of the sample.

Modern materials research is increasingly reliant on nanoscale analysis in three dimensions. Full 3D characterization includes chemical as well as imaging data, making 3D energy dispersive X-ray spectroscopy (EDS, also abbreviated EDX or XEDS) an indispensable technique. For the highest quality results, instrumentation with dynamic high-resolution imaging capabilities, as well as fast and quantitative data acquisition, is therefore required. The combination of flexibility in acquisition schemes (TEM, STEM, and EDS), the ability to easily and reproducibly optimize the experiment, and the fast and highly sensitive collection of the elemental distribution data are prerequisites for capturing the real 3D structure and composition of nanomaterials.

Electron tomography produces 3D reconstructions of materials by incrementally adjusting the angle at which the sample is observed. This produces a tilt series of images that can be digitally back projected to render the original sample volume. EDS spectra can be obtained alongside the the electron microscopy (EM) images, providing detailed elemental context. Below are just a few examples of EDS tomography use cases, covering a wide variety of scales, resolutions, and applications.

Thermo Fisher Scientific instruments offer a range of automation capabilities, allowing you to predetermine mapping conditions, drift compensation, and detector parameters, as well as autofocus and auto tilt conditions. This level of automation enables you to set up the EDS tomography experiment and then leave the system unattended for the complete data acquisition process. Visualization and reconstruction were performed with Thermo Scientific Inspect 3D and Avizo Software.


Resources

EDS tomography of P-Zn-In nanotubes, which are used as an electrode material for Na-ion and Li-ion batteries. The segregation of zinc has not been well known during synthesis; however, the elemental data clearly reveals the distribution of zinc relative to the other elements. It becomes evident that there is almost no concentration of zinc in the straight nanotubes. Sample courtesy of Dr. Reza Shahbazian Yassar, Michigan Tech University.

3D EDS TEM tomography of precipitates in an AlMgSi alloy. Sample courtesy of Thomas Kremmer and Stefan Pogatscher, University of Leoben, Austria.

EDS tomography data of organic nanoparticles in a polymer sheet.

EDS tomography data of a catalyst powder. Sample courtesy of Tampere University of Technology, Finland.

EDS tomography data of copper indium sulfide (CuInS2) nanostructures. Sample courtesy of Prof. Neerish Revaprasadu, University of Zululand, South Africa.

Example walkthrough of the EDS tomography workflow on the Talos S/TEM.
STEM and EDS tomography showing the distribution of the Palladium particles (red) relative to other elements of the vehicle aged catalyst material.
Digital slice of the reconstructed Ag-Pt core shell nanoparticle volume. Sample courtesy Prof. Yi Ding and Prof. Jun Luo, Center for Electron Microscopy, Tianjin University of Technology.
Segmented surface rendering of nanoparticles with elements present: Ag core, Platinum shell (to increase visibility, the Platinum shells have been colored semitransparent).

EDS tomography of P-Zn-In nanotubes, which are used as an electrode material for Na-ion and Li-ion batteries. The segregation of zinc has not been well known during synthesis; however, the elemental data clearly reveals the distribution of zinc relative to the other elements. It becomes evident that there is almost no concentration of zinc in the straight nanotubes. Sample courtesy of Dr. Reza Shahbazian Yassar, Michigan Tech University.

3D EDS TEM tomography of precipitates in an AlMgSi alloy. Sample courtesy of Thomas Kremmer and Stefan Pogatscher, University of Leoben, Austria.

EDS tomography data of organic nanoparticles in a polymer sheet.

EDS tomography data of a catalyst powder. Sample courtesy of Tampere University of Technology, Finland.

EDS tomography data of copper indium sulfide (CuInS2) nanostructures. Sample courtesy of Prof. Neerish Revaprasadu, University of Zululand, South Africa.

Example walkthrough of the EDS tomography workflow on the Talos S/TEM.
STEM and EDS tomography showing the distribution of the Palladium particles (red) relative to other elements of the vehicle aged catalyst material.
Digital slice of the reconstructed Ag-Pt core shell nanoparticle volume. Sample courtesy Prof. Yi Ding and Prof. Jun Luo, Center for Electron Microscopy, Tianjin University of Technology.
Segmented surface rendering of nanoparticles with elements present: Ag core, Platinum shell (to increase visibility, the Platinum shells have been colored semitransparent).

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