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Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples
Published on: June 19, 2018
Automated three-dimensional X-ray analysis using a dual-beam FIB.
Miroslava Schaffer1, Julian Wagner, Bernhard Schaffer
1Research Institute for Electron Microscopy, Graz University of Technology, Steyrergasse 17, A-8010 Graz, Austria.
Ultramicroscopy
|February 3, 2007
Summary
We developed an automated 3D elemental analysis method for ceramics using focused ion beam microscopy and energy-dispersive X-ray spectrometry. This technique reconstructs 3D elemental maps, addressing automation challenges and data inaccuracies.
Area of Science:
- Materials Science
- Analytical Chemistry
- Microscopy
Background:
- Three-dimensional (3D) elemental analysis is crucial for understanding material microstructures.
- Automating serial sectioning and elemental analysis presents significant technical challenges.
- Insulating ceramic materials pose difficulties for ion beam microscopy and X-ray spectrometry.
Purpose of the Study:
- To present a fully automated method for 3D elemental analysis of a ceramic sample.
- To address challenges associated with large sample volumes, process automation, and insulating specimens.
- To develop and demonstrate post-acquisition data correction routines for improved accuracy.
Main Methods:
- Serial sectioning of a (Ca)MgTiO(x) ceramic sample using a focused ion beam (FIB) microscope.
- Energy-dispersive X-ray spectrometry (EDXS) for elemental analysis of each 2D cross-section.
- Reconstruction of a 3D elemental model from the stack of 2D EDXS data.
Main Results:
- A fully automated workflow for 3D elemental mapping was successfully demonstrated.
- A new routine for correcting drift effects during automated acquisition was implemented.
- The study identified and addressed potential errors in EDXS data caused by specimen voids, utilizing back-scattered electron images for correction.
Conclusions:
- The presented automated method enables robust 3D elemental analysis of complex ceramic materials.
- Post-acquisition correction routines are essential for accurate elemental mapping, especially for insulating samples with voids.
- This approach advances the capability for detailed microstructural and chemical characterization in three dimensions.
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