Abstract
Atom probe tomography (APT) and (scanning) transmission electron microscopy ((S)TEM) are complementary techniques that provide spatially resolved chemical and structural information at the atomic scale. In this study, we employ two different STEM/APT correlative analysis methods to investigate Cr segregation at dislocation loops in ultra-high purity Fe–Cr alloys. APT needles for the correlative analysis were extracted either from bulk material or from thinned TEM lamellae. STEM analysis was used to determine the Burgers vectors of ion-irradiation-induced dislocation loops, while APT reconstruction of the same region revealed the Cr segregation to these loops. We extended the g•b = 0 invisibility criterion of dislocation loops from TEM mode in a lamella to STEM mode in a needle-shaped specimen. STEM and APT analysis on the same needle provide straightforward correlative analysis, although it is limited by a small observation volume. In contrast, iterative STEM analysis of TEM lamellae, followed by the selective extraction of specific regions of interest for APT analysis, expands the observation area by up to 100 times but requires additional time-consuming steps for APT needle extraction from the lamellae.
| Original language | English |
|---|---|
| Article number | ozaf039 |
| Journal | Microscopy and Microanalysis |
| Volume | 31 |
| Issue number | 3 |
| DOIs | |
| State | Published - Jun 1 2025 |
Funding
This research was sponsored by the Office of Fusion Energy Sciences, US Department of Energy under grant # DE-SC0023293 with the University of Tennessee. 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 acknowledge Institute for Advanced Materials and Manufacturing (IAMM) at University of Tennessee for assistance in using microscopes. APT research was supported by the Center for Nanophase Materials Sciences (CNMS), which is a US Department of Energy, Office of Science User Facility at Oak Ridge National Laboratory. The authors would like to thank James Burns for assistance in performing APT sample preparation and running the APT experiments. The authors are grateful to Dr. Jean Henry (CEA, France) for providing the high-purity Fe–Cr ingots. The authors acknowledge Institute for Advanced Materials and Manufacturing (IAMM) at University of Tennessee for assistance in using microscopes. APT research was supported by the Center for Nanophase Materials Sciences (CNMS), which is a US Department of Energy, Office of Science User Facility at Oak Ridge National Laboratory. The authors would like to thank James Burns for assistance in performing APT sample preparation and running the APT experiments. The authors are grateful to Dr. Jean Henry (CEA, France) for providing the high-purity Fe–Cr ingots. This research was sponsored by the Office of Fusion Energy Sciences, US Department of Energy under grant # DESC0023293 with the University of Tennessee. 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.
Keywords
- atom probe tomography
- chemical segregation
- correlative analysis
- dislocation loop
- scanning transmission electron microscopy
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