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Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments
Published on: June 27, 2022
Optimized procedure for conventional TEM sample preparation using birefringence
Aleksander Brozyniak1, Karin Stadlmann1, Philipp Kürnsteiner1
1Christian Doppler Laboratory for Nanoscale Phase Transformations, Center for Surface and Nanoanalytics, Johannes Kepler University Linz, Altenberger Straße 69, 4040 Linz, Austria.
This study presents an optimized method for transmission electron microscopy (TEM) specimen preparation, using interference colors to accurately estimate thickness. This technique reduces ion-milling time and prevents sample damage during thinning.
Area of Science:
- Materials Science
- Analytical Chemistry
- Microscopy
Background:
- High-precision specimen preparation is crucial for quality transmission electron microscopy (TEM) analyses.
- Conventional methods for TEM specimen preparation can be time-consuming and prone to sample damage.
- Accurate thickness estimation is vital during mechanical thinning processes.
Purpose of the Study:
- To present an optimized procedure for conventional TEM specimen preparation.
- To utilize the thickness-dependence of interference colors in birefringent materials for accurate thickness estimation.
- To reduce ion-milling times and prevent damage during mechanical thinning.
Main Methods:
- Exploited thickness-dependence of interference colors in birefringent materials.
- Applied the method to sapphire and silicon carbide cross-section samples.
- Demonstrated suitability for dimpling and wedge-polishing techniques.
Main Results:
- Achieved accurate visual thickness estimation, especially for thicknesses below 20 µm.
- Reduced ion-milling times to below 30 minutes.
- Prevented specimen damage or breakage during mechanical thinning.
Conclusions:
- The presented method offers a precise and efficient approach for TEM specimen thickness estimation.
- This technique is particularly beneficial for thin specimens where mechanical methods lack accuracy.
- Optimized visual estimation can be further enhanced by RGB spectrum analysis of interference colors.
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The simplest type of preparation is the wet mount, in which the specimen is placed in a drop of liquid on the slide. A liquid specimen can be directly deposited on the slide using a dropper. Solid specimens, such as skin scraping, can be placed on the slide before adding a drop of liquid to prepare the wet mount. Sometimes the liquid is simply water, but stains are often added...

