Skip to main content
U.S. Department of Energy
Office of Scientific and Technical Information

Application of Weak-Beam Dark-Field STEM for Dislocation Loop Analysis

Journal Article · · Microscopy and Microanalysis
DOI:https://doi.org/10.1093/mam/ozae067· OSTI ID:2406779
 [1];  [2];  [3];  [1];  [4]
  1. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
  2. Univ. of Tennessee, Knoxville, TN (United States); Los Alamos National Laboratory (LANL), Los Alamos, NM (United States)
  3. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)
  4. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States); Idaho National Laboratory (INL), Idaho Falls, ID (United States)

Nanoscale dislocation loops formed by irradiation can significantly contribute to both irradiation hardening and embrittlement of materials when subjected to extreme nuclear reactor environments. Here, this study explores the application of weak-beam dark-field (WBDF) scanning transmission electron microscopy (STEM) methods for quantitative irradiation-induced defect analysis in crystalline materials, with a specific focus on dislocation loop imaging and analysis. A high-purity Fe-5 wt% Cr model alloy was irradiated with 8 MeV Fe2+ ions at 450°C to a fluence of 8.8 × 1019 m-2, inducing dislocation loops for analysis. While transmission electron microscopy (TEM) has traditionally been the primary tool for dislocation imaging, recent advancements in STEM technology have reignited interest in using STEM for defect imaging. This study introduces and compares three WBDF STEM methods, demonstrating their effectiveness in suppressing background contrasts, isolating defect information for dislocation loop type classification, providing finer dislocation line images for small loop analysis, and presenting inside–outside contrast for identifying loop nature. Experimental findings indicate that WBDF STEM methods surpass traditional TEM approaches, yielding clearer and more detailed images of dislocation loops. The study concludes by discussing the potential applications of WBDF STEM techniques in defect analysis, emphasizing their adaptability across various material systems beyond nuclear materials.

Research Organization:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Sponsoring Organization:
USDOE Laboratory Directed Research and Development (LDRD) Program; USDOE Office of Science (SC), Fusion Energy Sciences (FES)
Grant/Contract Number:
AC05-00OR22725; SC0023293
OSTI ID:
2406779
Alternate ID(s):
OSTI ID: 2440195
Journal Information:
Microscopy and Microanalysis, Journal Name: Microscopy and Microanalysis Vol. 10; ISSN 1431-9276
Publisher:
Microscopy Society of America (MSA)Copyright Statement
Country of Publication:
United States
Language:
English

References (42)

The weak-beam method in electron microscopy journal September 1973
Influence of non-systematic reflexions on weak-beam and high-resolution bright-field images in high-voltage electron microscopy journal November 1974
A simple method for the analysis of dislocation loops by means of the inside-outside contrast on transmission electron micrographs journal October 1975
Transmission Electron Microscopy book January 2009
On the morphology of grain boundary discontinuous reactions and phase identification in an advanced Cr–Fe–Ni alloy journal April 2020
Characterisation of radiation-damage microstructures by TEM journal October 1994
The formation and interpretation of defect images from crystalline materials in a scanning transmission electron microscope journal January 1976
Fundamental concepts of stem imaging journal January 1981
Atomic site determination using the channeling effect in electron-induced x-ray emission journal January 1982
Z-contrast imaging of bulk crystal surfaces in scanning reflection electron microscopy journal August 1991
Radiation-Induced Effects on Microstructure book August 2020
Segregation of cascade induced interstitial loops at dislocations: possible effect on initiation of plastic deformation journal November 1997
High-temperature and low-stress creep anisotropy of single-crystal superalloys journal May 2013
Neutron irradiation effects in Fe and Fe-Cr at 300 °C journal June 2016
Dislocation loop evolution during in-situ ion irradiation of model FeCrAl alloys journal September 2017
Dynamic observation of dual-beam irradiated Fe and Fe-10Cr alloys at 435 °C journal May 2021
Embrittlement of irradiated ferritic/martensitic steels in the absence of irradiation hardening journal July 2008
TEM characterization of dislocation loops in irradiated bcc Fe-based steels journal March 2013
Transmission electron microscopy investigation of the microstructure of Fe–Cr alloys induced by neutron and ion irradiation at 300 °C journal June 2016
Microscopic origin of black spot defect swelling in single crystal 3C-SiC journal September 2018
STEM Characterization of Dislocation Loops in Irradiated FCC Alloys journal February 2021
Flash electropolishing of BCC Fe and Fe-based alloys journal December 2023
Defect-specific strength factors and superposition model for predicting strengthening of ion irradiated Fe18Cr alloy journal January 2024
Diffraction contrast STEM of dislocations: Imaging and simulations journal August 2011
Towards bend-contour-free dislocation imaging via diffraction contrast STEM journal October 2018
Dislocation Characterization using Weak Beam Dark Field STEM Imaging journal August 2018
Improved 4D-STEM Strain Mapping Precision Using Patterned Probes journal August 2019
Advances and Applications of Atomic-Resolution Scanning Transmission Electron Microscopy journal August 2021
Challenges in FIB TEM Sample Preparation: Damage Issues and Solutions journal August 2022
The role of stacking fault tetrahedra on void swelling in irradiated copper journal April 2024
Electron Microscope and Diffraction Study of Metal Crystal Textures by Means of Thin Sections journal October 1949
Atomic configuration of irradiation-induced planar defects in 3C-SiC journal March 2014
The Inorganic Crystal Structure Database (ICSD)—Present and Future journal January 2004
Resolving individual Shockley partials of a dissociated dislocation by STEM journal January 2017
Simplification of selective imaging of dislocation loops: diffraction-selected on-zone STEM journal February 2024
Dislocation decoration and raft formation in irradiated materials journal August 2005
The temperature dependence of heavy-ion damage in iron: A microstructural transition at elevated temperatures journal December 2010
Systematic row and zone axis STEM defect image simulations journal June 2011
Site-Specific Valence Determination by Electron Energy-Loss Spectroscopy journal February 1982
The principles and practice of the weak‐beam method of electron microscopy journal July 1973
Calculations and observations of the weak‐beam contrast of small lattice defects journal July 1973
Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys journal April 2015

Similar Records

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM
Conference · Mon Jul 01 00:00:00 EDT 2024 · OSTI ID:2428074

STEM Characterization of Dislocation Loops in Irradiated FCC Alloys
Journal Article · Tue Nov 10 23:00:00 EST 2020 · Journal of Nuclear Materials · OSTI ID:1872876