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Array Tomography Workflow for the Targeted Acquisition of Volume Information using Scanning Electron Microscopy
Published on: July 15, 2021
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Large volume serial section tomography by Xe Plasma FIB dual beam microscopy.
T L Burnett1, R Kelley2, B Winiarski1
1School of Materials, University of Manchester, Manchester M13 9PL, UK; FEI Company, Achtseweg Noord 5, Bldg, 5651 GG, Eindhoven, The Netherlands.
Ultramicroscopy
|December 20, 2015
Summary
Xe(+) Plasma Focused Ion Beam-Scanning Electron Microscopy enables faster 3D microstructural analysis. This advanced technique allows for large-volume serial section tomography of materials like bainitic steel and WC-Co, overcoming limitations of older Ga(+) FIB systems.
Area of Science:
- Materials Science
- Microscopy
- Nanotechnology
Background:
- Focused Ion Beam-Scanning Electron Microscopes (FIB-SEM) with Gallium ions (Ga+) revolutionized 3D microstructural analysis via serial section tomography (SST).
- Ga+ FIB limitations include slow material removal rates, restricting probed volumes to tens of microns.
- Emerging Xenon ion (Xe+) Plasma Focused Ion Beam-Scanning Electron Microscope (PFIB-SEM) systems offer significantly faster material removal rates.
Purpose of the Study:
- To evaluate the potential of Xe+ PFIB-SEM for large-volume serial section tomography.
- To assess the feasibility of PFIB-SEM for analyzing complex microstructures in bainitic steel and WC-Co hard metals.
- To compare the performance and artifact generation of Xe+ PFIB-SEM against traditional Ga+ FIB-SEM.
Main Methods:
- Automated serial section tomography (SST) using Xe+ PFIB-SEM on bainitic steel and WC-Co samples.
- Optimization of milling parameters for precise sectioning and artifact minimization.
- Characterization of microstructural features and surface quality using SEM, EBSD, and TEM.
Main Results:
- Xe+ PFIB-SEM achieved material removal rates approximately 60x faster than Ga+ FIB, enabling large-volume (hundreds of microns) SST within 24 hours.
- Automated SST routines produced high-quality data with minimal artifacts, capturing microstructural features from nanometers to tens of microns.
- Electron backscattered diffraction (EBSD) maps showed high indexing rates, indicating low surface damage.
- Xe+ PFIB milling at high currents (60nA, 30kV) avoided amorphization and phase transformation issues observed with Ga+ FIB on WC-Co.
Conclusions:
- Xe+ PFIB-SEM significantly enhances capabilities for large-volume 3D materials characterization, including tomography, EDX, and EBSD.
- The method provides a feasible and efficient approach for analyzing complex microstructures at unprecedented scales.
- Xe+ PFIB-SEM overcomes critical limitations of Ga+ FIB, paving the way for advanced correlative and multi-modal 3D analyses.
