Abstract
The preparation of transmission electron microscopy (TEM) samples is a critical step in the characterization of materials, and the focused ion beam (FIB) technique is a commonly used method. However, a significant limitation of this technique is the FIB-induced damages on the foil surfaces, which can obscure the real features of interest, particularly in radiation effects studies. To overcome this limitation, this study presents a detailed description of the flash electropolishing technique, which can be used to remove the FIB damage from samples. The flash electropolishing technique has been successfully applied to a range of materials, including Fe, Fe-based model alloys, commercial Fe-Cr alloys, and advanced Fe-Cr alloys, both in their as-received and ion-irradiated states. Furthermore, the parameters used for Fe-Cr model alloys can be adjusted for commercial and advanced alloys with minimal modifications. The study also examined the effects of electropolishing variables, such as perchloric acid concentration, electropolishing temperature, Cr concentration, and voltage. Qualitatively, a general trend and scoping test strategy is explored in our experiments. Overall, the flash electropolishing technique offers a promising solution to the challenges posed by FIB-induced damages in the preparation of TEM samples.
| Original language | English |
|---|---|
| Article number | 154672 |
| Journal | Journal of Nuclear Materials |
| Volume | 586 |
| DOIs | |
| State | Published - Dec 1 2023 |
Funding
The authors thank Dr. Xing Wang and Dr. Siwei Chen for the helpful discussion and Dr. Arunodaya Bhattacharya and Dr. Ling Wang for introducing the flash electropolishing method. This research was sponsored by the Office of Fusion Energy Sciences, U.S. Department of Energy under grant # DE- SC0023293 with the University of Tennessee and The Low Activation Materials Development and Analysis at Oak Ridge National Laboratory. The fabrication of the Fe-Cr binary alloys has been carried out within the framework of the EUROfusion Consortium and has received funding from the Euratom research and training program 2019–2020 under Grant Agreement No. 633053 . The authors would also like to acknowledge funding from the State of Tennessee and Tennessee Higher Education Commission (THEC) through their support of the Center for Materials Processing. Note: This manuscript has been co-authored by UT-Battelle, LLC under Contract No. DE-AC05–00OR22725 with the U.S. Department of Energy. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so. The Department of Energy will provide public access to these results with full access to the published paper of federally sponsored research in accordance with the DOE Public Access Plan ( http://energy.gov/downloads/doe-public-access-plan ).
Keywords
- Electrochemistry
- FIB induced damages
- Flash electropolishing
- Flash polishing
- Ion irradiation
- TEM