Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys

Parish, Chad M.; Field, Kevin G.; Certain, Alicia G.; Wharry, Janelle P.

doi:10.1557/jmr.2015.32

Title: Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys

Abstract

This paper provides a general overview of advanced scanning transmission electron microscopy (STEM) techniques used for characterization of irradiated BCC Fe-based alloys. Advanced STEM methods provide the high-resolution imaging and chemical analysis necessary to understand the irradiation response of BCC Fe-based alloys. The use of STEM with energy dispersive x-ray spectroscopy (EDX) for measurement of radiation-induced segregation (RIS) is described, with an illustrated example of RIS in proton- and self-ion irradiated T91. Aberration-corrected STEM-EDX for nanocluster/nanoparticle imaging and chemical analysis is also discussed, and examples are provided from ion-irradiated oxide dispersion strengthened (ODS) alloys. In conclusion, STEM techniques for void, cavity, and dislocation loop imaging are described, with examples from various BCC Fe-based alloys.

Authors:

Parish, Chad M. ^[1]; Field, Kevin G. ^[1]; Certain, Alicia G. ^[2]; Wharry, Janelle P. ^[3]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science and Technology Division
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Boise State Univ., ID (United States). Dept. of Materials Science and Engineering

Publication Date:: Mon Apr 20 00:00:00 EDT 2015

Research Org.:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Nuclear Energy (NE); USDOE Office of Science (SC), Biological and Environmental Research (BER)

OSTI Identifier:: 1185692

Grant/Contract Number:: AC05-00OR22725; 10-172; 10-678; 08-055; AC07-05ID14517

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Materials Research

Additional Journal Information:: Journal Volume: 30; Journal Issue: 9; Journal ID: ISSN 0884-2914

Publisher:: Materials Research Society

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; 47 OTHER INSTRUMENTATION; STEM; irradiation; Fe alloys; microscopy

Citation Formats


                    Parish, Chad M., Field, Kevin G., Certain, Alicia G., and Wharry, Janelle P. Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys.  United States: N. p., 2015. 
Web.  doi:10.1557/jmr.2015.32.

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                    Parish, Chad M., Field, Kevin G., Certain, Alicia G., & Wharry, Janelle P. Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys.  United States.  https://doi.org/10.1557/jmr.2015.32

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                    Parish, Chad M., Field, Kevin G., Certain, Alicia G., and Wharry, Janelle P. Mon .  
"Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys".  United States.  https://doi.org/10.1557/jmr.2015.32.  https://www.osti.gov/servlets/purl/1185692.

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@article{osti_1185692,

  title        = {Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys},

  author       = {Parish, Chad M. and Field, Kevin G. and Certain, Alicia G. and Wharry, Janelle P.},

  abstractNote = {This paper provides a general overview of advanced scanning transmission electron microscopy (STEM) techniques used for characterization of irradiated BCC Fe-based alloys. Advanced STEM methods provide the high-resolution imaging and chemical analysis necessary to understand the irradiation response of BCC Fe-based alloys. The use of STEM with energy dispersive x-ray spectroscopy (EDX) for measurement of radiation-induced segregation (RIS) is described, with an illustrated example of RIS in proton- and self-ion irradiated T91. Aberration-corrected STEM-EDX for nanocluster/nanoparticle imaging and chemical analysis is also discussed, and examples are provided from ion-irradiated oxide dispersion strengthened (ODS) alloys. In conclusion, STEM techniques for void, cavity, and dislocation loop imaging are described, with examples from various BCC Fe-based alloys.},

  doi          = {10.1557/jmr.2015.32},

  journal      = {Journal of Materials Research},

  number       = 9,

  volume       = 30,

  place        = {United States},

  year         = {Mon Apr 20 00:00:00 EDT 2015},

  month        = {Mon Apr 20 00:00:00 EDT 2015}

}

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This final technical report summarizes the research performed during October 2014 and December 2017, with a focus on investigating the radiation-induced microstructural and mechanical property modifications in optimized advanced alloys for sodium-cooled fast reactor (SFR) structural applications. To accomplish these objectives, the radiation responses of several different advanced alloys, including austenitic steel Alloy 709 (A709) and 316H, and ferritic/ martensitic Fe–9Cr steels T91 and G92, were investigated using a combination of microstructure characterizations and nanoindentation measurements. Different types of irradiation, including ex situ bulk ion irradiation and in situ transmission electron microscopy (TEM) ion irradiation, were employed in this study.more »« less
https://doi.org/10.2172/1434640

Full Text Available
Microstructure and Property Evolution in Advanced Cladding and Duct Materials Under Long-Term and Elevated Temperature Irradiation: Modeling and Experimental Investigation

Technical Report Wirth, Brian ; Morgan, Dane ; Kaoumi, Djamel ; ...

The in-service degradation of reactor core materials is related to underlying changes in the irradiated microstructure. During reactor operation, structural components and cladding experience displacement of atoms by collisions with neutrons at temperatures at which the radiation-induced defects are mobile, leading to microstructure evolution under irradiation that can degrade material properties. At the doses and temperatures relevant to fast reactor operation, the microstructure evolves by dislocation loop formation and growth, microchemistry changes due to radiation-induced segregation, radiation-induced precipitation, destabilization of the existing precipitate structure, and in some cases, void formation and growth. These processes do not occur independently; rather, theirmore »« less
https://doi.org/10.2172/1111139

Full Text Available
Friction stir welding and self-ion irradiation effects on microstructure and mechanical properties changes within oxide dispersion strengthened steel $$\mathrm{MA956}$$

Journal Article Getto, E. ; Johnson, M. ; Maughan, M. ; ... - Journal of Nuclear Materials

We report the joining process for oxide dispersion strengthened (ODS) alloys remains a key challenge facing the nuclear community. The microstructure and mechanical properties were characterized in the base material and friction stir welded ODS MA956 irradiated with 5 MeV Fe²⁺ ions from 400 to 500°C up to 25 dpa. Nanoindentation was performed to assess changes in hardness and yield stress, and the dispersed barrier hardening (DBH) model was applied to described results. A combination of scanning transmission electron microscopy (STEM) and atom probe tomography (APT) were used to assess evolution of the microstructure including dispersoids, network dislocations and dislocationmore »« less
https://doi.org/10.1016/j.jnucmat.2022.153795

Full Text Available
Recent Advances in Analytical Electron Microscopy for Irradiated Materials

Journal Article Parish, Chad M. ; Edmondson, Philip D. ; Field, Kevin G. ; ... - Transactions of the American Nuclear Society

Analytical electron microscopy (AEM) in the scanning transmission electron microscope (STEM) has long been a staple of post-irradiation examination (PIE) and materials development campaigns. Recently, new advances in both STEM hardware and post-processing data-analysis software, along with ancillary advances such as in focused ion beam (FIB) sample preparation, has led to exciting advances in the quantity and quality of data that can be obtained. This talk will summarize recent experiments performed at Oak Ridge National Laboratory (ORNL), especially work on neutron-irradiated materials and fuels taking advantage of a newly-installed latest-generation AEM tool in the ORNL irradiated materials laboratories. ORNL installedmore »« less
Effect of Irradiation on Strengthening of a Model Fe-9Cr Oxide Dispersion Strengthened Alloy

Journal Article Wharry, J. P. ; Swenson, M. J. ; Dolph, C. K. ; ... - Transactions of the American Nuclear Society

The growing energy demand will increasingly call upon advanced nuclear reactors to supply safe and reliable energy worldwide. However, structural and cladding materials in these reactors will be subject to extreme conditions of up to a few hundred displacements per atom (dpa) at temperatures as high as 600 deg. C. Oxide dispersion strengthened (ODS) alloys are leading candidates for these components because their dispersion of Y-Ti-O nanoclusters provides high strength at elevated temperatures and dimensional stability under irradiation. But recent work has suggested that the oxides are unstable under irradiation, which has serious implications on mechanical performance. Thus, the objectivemore »« less

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Title: Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys

Abstract

Citation Formats

Dependence on grain boundary structure of radiation induced segregation in a 9wt.% Cr model ferritic/martensitic steel journal, April 2013

Effect of grain boundary orientation on radiation-induced segregation in a Fe–15.2at.% Cr alloy journal, May 2013

Quantitative characterization of nanoprecipitates in irradiated low-alloy steels: advances in the application of FEG-STEM quantitative microanalysis to real materials journal, July 2006

High angle annular dark field imaging of stacking faults journal, April 1997

Dislocation loops and bubbles in oxide dispersion strengthened ferritic steel after helium implantation under stress journal, January 2008

Parallel simulation of electron-solid interactions for electron microscopy modeling journal, June 1992

Recent Developments in Irradiation-Resistant Steels journal, August 2008

A systematic approach for the study of radiation-induced segregation/depletion at grain boundaries in steels journal, June 2011

Relationship between lath boundary structure and radiation induced segregation in a neutron irradiated 9wt.% Cr model ferritic/martensitic steel journal, February 2014

Aberration-corrected scanning transmission electron microscopy: from atomic imaging and analysis to solving energy problems journal, September 2009

Direct observation of ion-irradiation-induced chemical mixing journal, November 2011

Fundamental concepts of stem imaging journal, January 1981

Morphology, structure, and chemistry of nanoclusters in a mechanically alloyed nanostructured ferritic steel journal, January 2012

Characterisation of radiation-damage microstructures by TEM journal, October 1994

A systematic study of radiation-induced segregation in ferritic–martensitic alloys journal, November 2013

Spectrum-image: The next step in EELS digital acquisition and processing journal, April 1989

Quantification of internal dislocation density using scanning transmission electron microscopy in ultrafine grained pure aluminium fabricated by severe plastic deformation journal, December 2010

The measurement and calculation of the X-ray spatial resolution obtained in the analytical electron microscope journal, October 1990

Electron Microscopical Techniques For The Observation Of Cavities journal, May 1979

Quantitative analysis of radiation-induced grain-boundary segregation measurements journal, July 1994

Effects of heavy-ion irradiation on the grain boundary chemistry of an oxide-dispersion strengthened Fe–12wt.% Cr alloy journal, October 2011

Radiation-induced segregation and phase stability in ferritic–martensitic alloy T 91 journal, October 2011

Phase-contrast imaging in aberration-corrected scanning transmission electron microscopy journal, June 2013

Chromium enrichment on the habit plane of dislocation loops in ion-irradiated high-purity Fe–Cr alloys journal, October 2014

Multislice simulation of transmission electron microscopy imaging of helium bubbles in Fe journal, October 2012

Helium solubility and bubble formation in a nanostructured ferritic alloy journal, February 2014

De-channelling contrast in annular dark-field STEM journal, February 1992

Statistical analysis of oxides particles in ODS ferritic steel using advanced electron microscopy journal, March 2012

Current and future aberration correctors for the improvement of resolution in electron microscopy journal, September 2009

Effect of processing parameters on the evolution of dislocation density and sub-grain size of a 12%Cr heat resistant steel during creep at 650°C journal, January 2011

Exploiting spatial-domain simplicity in spectral image analysis journal, February 2009

Automated Analysis of SEM X-Ray Spectral Images: A Powerful New Microanalysis Tool journal, January 2003

Microstructural evolution of proton irradiated T91 journal, June 2006

Aberration-Corrected X-Ray Spectrum Imaging and Fresnel Contrast to Differentiate Nanoclusters and Cavities in Helium-Irradiated Alloy 14YWT journal, March 2014

High-Resolution Scanning Transmission Electron Microscopy Study of Black Spot Defects in Ion Irradiated Silicon Carbide journal, August 2014

Response of nanostructured ferritic alloys to high-dose heavy ion irradiation journal, February 2014

Stability of the strengthening nanoprecipitates in reduced activation ferritic steels under Fe2+ ion irradiation journal, February 2014

Shape of prismatic dislocation loops in anisotropic α -Fe journal, September 2009

Effect of the α − γ Phase Transition on the Stability of Dislocation Loops in bcc Iron journal, April 2008

FIB and TEM Studies of Diamond Films Prepared by Laser-Assisted Combustion Flame Deposition in Open Atmosphere journal, July 2010

The formation and interpretation of defect images from crystalline materials in a scanning transmission electron microscope journal, January 1976

Background, status and future of the Transmission Electron Aberration-corrected Microscope project journal, August 2009

Quantitative X-Ray Spectrum Imaging of Lead Lanthanum Zirconate Titanate PLZT Thin-Films journal, November 2008

Electron-Excited Energy Dispersive X-Ray Spectrometry at High Speed and at High Resolution: Silicon Drift Detectors and Microcalorimeters journal, October 2006

Microstructural changes in a neutron-irradiated Fe–6 at.%Cr alloy journal, October 2014

TEM characterization of dislocation loops in irradiated bcc Fe-based steels journal, March 2013

Impact of He and Cr on defect accumulation in ion-irradiated ultrahigh-purity Fe(Cr) alloys journal, October 2013

Accounting for Poisson noise in the multivariate analysis of ToF-SIMS spectrum images journal, March 2004

Diffraction contrast STEM of dislocations: Imaging and simulations journal, August 2011

How dislocation substructures evolve during long-term creep of a 12% Cr tempered martensitic ferritic steel journal, March 2010

The microstructure and tensile properties of Fe–Cr alloys after neutron irradiation at 400°C to 5.5–7.1 dpa journal, August 1998

Imaging elastic strains in high-angle annular dark field scanning transmission electron microscopy journal, December 1993

Emergent Chemical Mapping at Atomic-Column Resolution by Energy-Dispersive X-Ray Spectroscopy in an Aberration-Corrected Electron Microscope journal, May 2010

Parallel simulation of electron-solid interactions: A rapid aid for electron microscope data interpretation journal, June 1993

Transmission electron microscopy of He-bubbles in aluminium journal, October 1976

Energy dispersive X-ray spectroscopy of bimetallic nanoparticles in an aberration corrected scanning transmission electron microscope journal, January 2008

Improvements in the X-Ray Analytical Capabilities of a Scanning Transmission Electron Microscope by Spherical-Aberration Correction journal, October 2006

Selectivity, local rank, three-way data analysis and ambiguity in multivariate curve resolution journal, January 1995

Fresnel fringes in electron microscope images journal, January 1974

On rotational ambiguity in model-free analyses of multivariate data journal, June 2006

Challenges to Quantitative Multivariate Statistical Analysis of Atomic-Resolution X-Ray Spectral journal, July 2012

The varimax criterion for analytic rotation in factor analysis journal, September 1958

The quantitative analysis of thin specimens journal, March 1975

Helium bubble distributions in a nanostructured ferritic alloy journal, March 2013

The density and pressure of helium in bubbles in implanted metals: A critical review journal, January 1985

Detecting density variations and nanovoids journal, May 2011

Response of nanoclusters in a 9Cr ODS steel to 1dpa, 525°C proton irradiation journal, December 2010

A comparison of multivariate statistical analysis protocols for ToF-SIMS spectral images journal, February 2009

Designing Radiation Resistance in Materials for Fusion Energy journal, July 2014

Fast algorithm for the solution of large-scale non-negativity-constrained least squares problems journal, October 2004

Nanometric crystal defects in transmission electron microscopy journal, January 2006

Microstructural changes in a neutron-irradiated Fe–15 at.%Cr alloy journal, November 2014

Operating temperature windows for fusion reactor structural materials journal, November 2000

The Effect of Probe Correctors on the Analytical Results of Non-ideal Samples journal, August 2014

High-Chromium Ferritic and Martensitic Steels for Nuclear Applications book, January 2001

Structural materials for fission & fusion energy journal, November 2009

Transmission Electron Microscopy book, January 2009

Dependence on grain boundary structure of radiation induced segregation in a 9wt.% Cr model ferritic/martensitic steel
journal, April 2013

Effect of grain boundary orientation on radiation-induced segregation in a Fe–15.2at.% Cr alloy
journal, May 2013

Quantitative characterization of nanoprecipitates in irradiated low-alloy steels: advances in the application of FEG-STEM quantitative microanalysis to real materials
journal, July 2006

High angle annular dark field imaging of stacking faults
journal, April 1997

Dislocation loops and bubbles in oxide dispersion strengthened ferritic steel after helium implantation under stress
journal, January 2008

Parallel simulation of electron-solid interactions for electron microscopy modeling
journal, June 1992

Recent Developments in Irradiation-Resistant Steels
journal, August 2008

A systematic approach for the study of radiation-induced segregation/depletion at grain boundaries in steels
journal, June 2011

Relationship between lath boundary structure and radiation induced segregation in a neutron irradiated 9wt.% Cr model ferritic/martensitic steel
journal, February 2014

Aberration-corrected scanning transmission electron microscopy: from atomic imaging and analysis to solving energy problems
journal, September 2009

Direct observation of ion-irradiation-induced chemical mixing
journal, November 2011

Fundamental concepts of stem imaging
journal, January 1981

Morphology, structure, and chemistry of nanoclusters in a mechanically alloyed nanostructured ferritic steel
journal, January 2012

Characterisation of radiation-damage microstructures by TEM
journal, October 1994

A systematic study of radiation-induced segregation in ferritic–martensitic alloys
journal, November 2013

Spectrum-image: The next step in EELS digital acquisition and processing
journal, April 1989

Quantification of internal dislocation density using scanning transmission electron microscopy in ultrafine grained pure aluminium fabricated by severe plastic deformation
journal, December 2010

The measurement and calculation of the X-ray spatial resolution obtained in the analytical electron microscope
journal, October 1990

Electron Microscopical Techniques For The Observation Of Cavities
journal, May 1979

Quantitative analysis of radiation-induced grain-boundary segregation measurements
journal, July 1994

Effects of heavy-ion irradiation on the grain boundary chemistry of an oxide-dispersion strengthened Fe–12wt.% Cr alloy
journal, October 2011

Radiation-induced segregation and phase stability in ferritic–martensitic alloy T 91
journal, October 2011

Phase-contrast imaging in aberration-corrected scanning transmission electron microscopy
journal, June 2013

Chromium enrichment on the habit plane of dislocation loops in ion-irradiated high-purity Fe–Cr alloys
journal, October 2014

Multislice simulation of transmission electron microscopy imaging of helium bubbles in Fe
journal, October 2012

Helium solubility and bubble formation in a nanostructured ferritic alloy
journal, February 2014

De-channelling contrast in annular dark-field STEM
journal, February 1992

Statistical analysis of oxides particles in ODS ferritic steel using advanced electron microscopy
journal, March 2012

Current and future aberration correctors for the improvement of resolution in electron microscopy
journal, September 2009

Effect of processing parameters on the evolution of dislocation density and sub-grain size of a 12%Cr heat resistant steel during creep at 650°C
journal, January 2011

Exploiting spatial-domain simplicity in spectral image analysis
journal, February 2009

Automated Analysis of SEM X-Ray Spectral Images: A Powerful New Microanalysis Tool
journal, January 2003

Microstructural evolution of proton irradiated T91
journal, June 2006

Aberration-Corrected X-Ray Spectrum Imaging and Fresnel Contrast to Differentiate Nanoclusters and Cavities in Helium-Irradiated Alloy 14YWT
journal, March 2014

High-Resolution Scanning Transmission Electron Microscopy Study of Black Spot Defects in Ion Irradiated Silicon Carbide
journal, August 2014

Response of nanostructured ferritic alloys to high-dose heavy ion irradiation
journal, February 2014

Stability of the strengthening nanoprecipitates in reduced activation ferritic steels under Fe2+ ion irradiation
journal, February 2014

Shape of prismatic dislocation loops in anisotropic α -Fe
journal, September 2009

Effect of the $α - γ$ Phase Transition on the Stability of Dislocation Loops in bcc Iron
journal, April 2008

FIB and TEM Studies of Diamond Films Prepared by Laser-Assisted Combustion Flame Deposition in Open Atmosphere
journal, July 2010

The formation and interpretation of defect images from crystalline materials in a scanning transmission electron microscope
journal, January 1976

Background, status and future of the Transmission Electron Aberration-corrected Microscope project
journal, August 2009

Quantitative X-Ray Spectrum Imaging of Lead Lanthanum Zirconate Titanate PLZT Thin-Films
journal, November 2008

Electron-Excited Energy Dispersive X-Ray Spectrometry at High Speed and at High Resolution: Silicon Drift Detectors and Microcalorimeters
journal, October 2006

Microstructural changes in a neutron-irradiated Fe–6 at.%Cr alloy
journal, October 2014

TEM characterization of dislocation loops in irradiated bcc Fe-based steels
journal, March 2013

Impact of He and Cr on defect accumulation in ion-irradiated ultrahigh-purity Fe(Cr) alloys
journal, October 2013

Accounting for Poisson noise in the multivariate analysis of ToF-SIMS spectrum images
journal, March 2004

Diffraction contrast STEM of dislocations: Imaging and simulations
journal, August 2011

How dislocation substructures evolve during long-term creep of a 12% Cr tempered martensitic ferritic steel
journal, March 2010

The microstructure and tensile properties of Fe–Cr alloys after neutron irradiation at 400°C to 5.5–7.1 dpa
journal, August 1998

Imaging elastic strains in high-angle annular dark field scanning transmission electron microscopy
journal, December 1993

Emergent Chemical Mapping at Atomic-Column Resolution by Energy-Dispersive X-Ray Spectroscopy in an Aberration-Corrected Electron Microscope
journal, May 2010

Parallel simulation of electron-solid interactions: A rapid aid for electron microscope data interpretation
journal, June 1993

Transmission electron microscopy of He-bubbles in aluminium
journal, October 1976

Energy dispersive X-ray spectroscopy of bimetallic nanoparticles in an aberration corrected scanning transmission electron microscope
journal, January 2008

Improvements in the X-Ray Analytical Capabilities of a Scanning Transmission Electron Microscope by Spherical-Aberration Correction
journal, October 2006

Selectivity, local rank, three-way data analysis and ambiguity in multivariate curve resolution
journal, January 1995

Fresnel fringes in electron microscope images
journal, January 1974

On rotational ambiguity in model-free analyses of multivariate data
journal, June 2006

Challenges to Quantitative Multivariate Statistical Analysis of Atomic-Resolution X-Ray Spectral
journal, July 2012

The varimax criterion for analytic rotation in factor analysis
journal, September 1958

The quantitative analysis of thin specimens
journal, March 1975

Helium bubble distributions in a nanostructured ferritic alloy
journal, March 2013

The density and pressure of helium in bubbles in implanted metals: A critical review
journal, January 1985

Detecting density variations and nanovoids
journal, May 2011

Response of nanoclusters in a 9Cr ODS steel to 1dpa, 525°C proton irradiation
journal, December 2010

A comparison of multivariate statistical analysis protocols for ToF-SIMS spectral images
journal, February 2009

Designing Radiation Resistance in Materials for Fusion Energy
journal, July 2014

Fast algorithm for the solution of large-scale non-negativity-constrained least squares problems
journal, October 2004

Nanometric crystal defects in transmission electron microscopy
journal, January 2006

Microstructural changes in a neutron-irradiated Fe–15 at.%Cr alloy
journal, November 2014

Operating temperature windows for fusion reactor structural materials
journal, November 2000

The Effect of Probe Correctors on the Analytical Results of Non-ideal Samples
journal, August 2014

High-Chromium Ferritic and Martensitic Steels for Nuclear Applications
book, January 2001

Structural materials for fission & fusion energy
journal, November 2009

Transmission Electron Microscopy
book, January 2009

Enhanced Detection Sensitivity with a New Windowless XEDS System for AEM Based on Silicon Drift Detector Technology
journal, July 2010

Chemical Mapping at the Atomic Level using Energy Dispersive X-ray Spectroscopy
journal, July 2011

Optimal scaling of TOF-SIMS spectrum-images prior to multivariate statistical analysis
journal, June 2004