High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy

Bhattacharya, Arunodaya; Parish, Chad M.; Henry, Jean; Katoh, Yutai

doi:10.1016/j.ultramic.2019.03.015

Title: High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy

Abstract

Statistically significant crystal structure and composition identification of nanocrystalline features such as nanoparticles/nanoprecipitates in materials chemistry and alloy designing using electron microscopy remains a grand challenge. In this paper, we reveal that differing crystallographic phases of nanoprecipitates in alloys can be mapped with unprecedented statistics using transmission Kikuchi diffraction (TKD), on typical carbon-based electron-transparent samples. Using a case of multiphase, multicomponent nanoprecipitates extracted from an improved version of 9% chromium Eurofer-97 reduced-activation ferritic-martensitic steel we show that TKD successfully identified more than thousand M₂₃C₆, MX, M₇C₃, and M₂X (M=Fe, Cr, W, V, Ta; X = C, N) nanoprecipitates in a single scan, something that is currently unachievable using a transmission electron microscope (TEM) without incorporating a precision electron diffraction (PED) system. Precipitates as small as ~20–25 nm were successfully phase identified by TKD. We verified the TKD phase identification using high-resolution transmission electron microscopy (HRTEM) and convergent beam electron diffraction (CBED) pattern analysis of a few precipitates that were identified by TKD on same sample. TKD study was combined with state-of-art analytical scanning transmission electron microscopy (STEM)-energy dispersive X-ray (EDX) spectroscopy and multivariate statistical analysis (MVSA) which provided the complete crystal structure and distinct chemistries of the precipitates in themore »« less

Authors:

Bhattacharya, Arunodaya ^[1]; Parish, Chad M. ^[1]; Henry, Jean ^[2];

^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Univ. Paris-Saclay, Gif-sur-Yvette (France)

Publication Date:: Thu Mar 28 00:00:00 EDT 2019

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

Sponsoring Org.:: USDOE Office of Science (SC), Fusion Energy Sciences (FES)

OSTI Identifier:: 1505331

Alternate Identifier(s):: OSTI ID: 1636489

Grant/Contract Number:: AC05-00OR22725

Resource Type:: Accepted Manuscript

Journal Name:: Ultramicroscopy

Additional Journal Information:: Journal Volume: 202; Journal Issue: C; Journal ID: ISSN 0304-3991

Publisher:: Elsevier

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; Nanoprecipitates; Transmission Kikuchi diffraction; HRTEM; Analytical electron microscopy; Multi-variate statistical analysis (MVSA)

Citation Formats


                    Bhattacharya, Arunodaya, Parish, Chad M., Henry, Jean, and Katoh, Yutai. High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy.  United States: N. p., 2019. 
Web.  doi:10.1016/j.ultramic.2019.03.015.

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                    Bhattacharya, Arunodaya, Parish, Chad M., Henry, Jean, & Katoh, Yutai. High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy.  United States.  https://doi.org/10.1016/j.ultramic.2019.03.015

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                    Bhattacharya, Arunodaya, Parish, Chad M., Henry, Jean, and Katoh, Yutai. Thu .  
"High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy".  United States.  https://doi.org/10.1016/j.ultramic.2019.03.015.  https://www.osti.gov/servlets/purl/1505331.

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@article{osti_1505331,

  title        = {High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy},

  author       = {Bhattacharya, Arunodaya and Parish, Chad M. and Henry, Jean and Katoh, Yutai},

  abstractNote = {Statistically significant crystal structure and composition identification of nanocrystalline features such as nanoparticles/nanoprecipitates in materials chemistry and alloy designing using electron microscopy remains a grand challenge. In this paper, we reveal that differing crystallographic phases of nanoprecipitates in alloys can be mapped with unprecedented statistics using transmission Kikuchi diffraction (TKD), on typical carbon-based electron-transparent samples. Using a case of multiphase, multicomponent nanoprecipitates extracted from an improved version of 9% chromium Eurofer-97 reduced-activation ferritic-martensitic steel we show that TKD successfully identified more than thousand M23C6, MX, M7C3, and M2X (M=Fe, Cr, W, V, Ta; X = C, N) nanoprecipitates in a single scan, something that is currently unachievable using a transmission electron microscope (TEM) without incorporating a precision electron diffraction (PED) system. Precipitates as small as ~20–25 nm were successfully phase identified by TKD. We verified the TKD phase identification using high-resolution transmission electron microscopy (HRTEM) and convergent beam electron diffraction (CBED) pattern analysis of a few precipitates that were identified by TKD on same sample. TKD study was combined with state-of-art analytical scanning transmission electron microscopy (STEM)-energy dispersive X-ray (EDX) spectroscopy and multivariate statistical analysis (MVSA) which provided the complete crystal structure and distinct chemistries of the precipitates in the steel in a high throughput automated way. This technique should be applicable to characterizing any multiphase crystalline nanoparticles or nanomaterials. Furthermore the results highlight that combining phase identification by TKD with analytical STEM and modern data analytics may open new pathways in big data material characterization at nanoscale that may be highly beneficial for characterizing existing materials and in designing new materials.},

  doi          = {10.1016/j.ultramic.2019.03.015},

  journal      = {Ultramicroscopy},

  number       = C,

  volume       = 202,

  place        = {United States},

  year         = {Thu Mar 28 00:00:00 EDT 2019},

  month        = {Thu Mar 28 00:00:00 EDT 2019}

}

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Title: High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy

Abstract

Citation Formats

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Near-Unity Efficiency Energy Transfer from Colloidal Semiconductor Quantum Wells of CdSe/CdS Nanoplatelets to a Monolayer of MoS 2 journal, July 2018

Exploitation of Localized Surface Plasmon Resonance journal, October 2004

Phase-Pure Crystalline Zinc Phosphide Nanoparticles: Synthetic Approaches and Characterization journal, February 2014

Low-cost and nanoscale non-volatile memory concept for future silicon chips journal, March 2005

Tracking Metal Electrodeposition Dynamics from Nucleation and Growth of a Single Atom to a Crystalline Nanoparticle journal, June 2018

Nanostructured materials for advanced energy conversion and storage devices journal, May 2005

Chemical Synthesis and Characterization of γ-Co 2 NiGa Nanoparticles with a Very High Curie Temperature journal, October 2015

Effect of oriented γ′ precipitates on shape memory effect and superelasticity in Co–Ni–Ga single crystals journal, April 2014

Nanostructured high-strength molybdenum alloys with unprecedented tensile ductility journal, January 2013

Ultrastrong steel via minimal lattice misfit and high-density nanoprecipitation journal, April 2017

Development of next generation tempered and ODS reduced activation ferritic/martensitic steels for fusion energy applications journal, June 2017

Development of castable nanostructured alloys as a new generation RAFM steels journal, December 2018

General Synthetic Strategy for Libraries of Supported Multicomponent Metal Nanoparticles journal, April 2018

Processing and properties of magnesium containing a dense uniform dispersion of nanoparticles journal, December 2015

The development and stability of Y–Ti–O nanoclusters in mechanically alloyed Fe–Cr based ferritic alloys journal, August 2004

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

On the status and prospects for nanostructured ferritic alloys for nuclear fission and fusion application with emphasis on the underlying science journal, January 2018

Core-shell nanoparticle arrays double the strength of steel journal, February 2017

Some Reactions in the Iron–Carbon System: Application to the Tempering of Martensite journal, June 1951

Superior radiation-resistant nanoengineered austenitic 304L stainless steel for applications in extreme radiation environments journal, January 2015

Brittle intermetallic compound makes ultrastrong low-density steel with large ductility journal, February 2015

Nature of χ-Carbide and Its Possible Occurrence in Steels journal, October 1966

Creep-strengthening of steel at high temperatures using nano-sized carbonitride dispersions journal, July 2003

A New Nitride Precipitate in Iron-Silicon Alloys journal, October 1959

Recent status and improvement of reduced-activation ferritic-martensitic steels for high-temperature service journal, October 2016

Orientation and phase mapping in the transmission electron microscope using precession-assisted diffraction spot recognition: state-of-the-art results: REVIEW OF PACOM (ASTAR) APPLICATION journal, July 2013

Nanoscale Automated Phase and Orientation Mapping in the TEM journal, November 2012

High spatial resolution semi-automatic crystallite orientation and phase mapping of nanocrystals in transmission electron microscopes journal, April 2011

Metallurgical characterization of coupled carbon diffusion and precipitation in dissimilar steel welds journal, February 2016

Direct carbon replicas from metal surfaces journal, June 1956

Uses of Carbon Replicas in Electron Microscopy journal, December 1956

Quantitative assessment of extraction replicas for particle analysis journal, March 1968

Growth of Sulphide Films on Steel journal, August 1960

Replica Extraction Method on Nanostructured Gold Coatings and Orientation Determination Combining SEM and TEM Techniques journal, October 2014

Boron Autoradiography with the Electron Microscope journal, August 1969

Evolution of microstructure and mechanical properties during thermomechanical processing of a low-density multiphase steel for automotive application journal, August 2014

Coarsening behaviour of M23C6 carbides in creep-resistant steel exposed to high temperatures journal, July 2016

A Technique for Sampling Oxide Layers and Brittle Materials for Microdiffraction journal, April 1960

Freeze-fracture electron microscopy journal, March 2007

Transmission Kikuchi diffraction in a scanning electron microscope: A review journal, December 2016

Orientation mapping of nanostructured materials using transmission Kikuchi diffraction in the scanning electron microscope journal, September 2012

Transmission EBSD from 10 nm domains in a scanning electron microscope: TRANSMISSION EBSD IN THE SEM journal, November 2011

On the optimum resolution of transmission-electron backscattered diffraction (t-EBSD) journal, January 2016

Characterizing deformed ultrafine-grained and nanocrystalline materials using transmission Kikuchi diffraction in a scanning electron microscope journal, January 2014

Features of Transmission EBSD and its Application journal, July 2013

Grain boundary mediated hydriding phase transformations in individual polycrystalline metal nanoparticles journal, October 2017

Viewpoint: Nanoscale chemistry and crystallography are both the obstacle and pathway to advanced radiation-tolerant materials journal, January 2018

Grain orientations and grain boundaries in tungsten nonotendril fuzz grown under divertor-like conditions journal, January 2017

Nanostructure characterisation of flow-formed Cr–Mo–V steel using transmission Kikuchi diffraction technique journal, June 2015

Characterisation of nano-grains in MgB2 superconductors by transmission Kikuchi diffraction journal, May 2015

Grain size effect on deformation twinning propensity in ultrafine-grained hexagonal close-packed titanium journal, September 2013

The capability of Transmission Kikuchi Diffraction technique for characterizing nano-grained oxide scales formed on a FeCrAl stainless steel journal, May 2015

Eurofer Steel, Development to Full Code Qualification journal, January 2013

Development of new generation reduced activation ferritic-martensitic steels for advanced fusion reactors journal, September 2016

Electron densities in VN. I. High-precision x-ray-diffraction determination of the valence-electron density distribution and atomic displacement parameters journal, July 1987

Atom distributions in tau-carbide phases: Fe and Cr distributions in (Cr 23− x Fe x )C 6 with x = 0, 0·7 4 , 1·7 0 , 4·1 3 and 7·3 6 journal, June 1987

Formation of NaCl-type Cr carbide by carbon ion implantation journal, April 1993

Structure refinement for Cr2N journal, February 1990

Nucleation and growth of tungsten nanotendrils grown under divertor-like conditions journal, October 2018

Homeopathic ICA: A simple approach to expand the use of independent component analysis (ICA) journal, March 2015

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

TEM characterization on new 9% Cr advanced steels thermomechanical treated after tempering journal, March 2018

Niobium carbonitride precipitation and austenite recrystallization in hot-rolled microalloyed steels journal, March 1980

Laser melting and heat treatment of m2 tool steel: A microstructural characterization journal, July 1979

Precipitation in Interstitial Free High Strength Steels journal, January 2009

CASINO a Powerful Simulation Tool for Cathodoluminescence Applications journal, July 2006

Expansion of interatomic distances in platinum catalyst nanoparticles
journal, February 2010

Copper nanoparticle@graphene composite arrays and their enhanced catalytic performance
journal, February 2016

Near-Unity Efficiency Energy Transfer from Colloidal Semiconductor Quantum Wells of CdSe/CdS Nanoplatelets to a Monolayer of MoS ₂
journal, July 2018

Exploitation of Localized Surface Plasmon Resonance
journal, October 2004

Phase-Pure Crystalline Zinc Phosphide Nanoparticles: Synthetic Approaches and Characterization
journal, February 2014

Low-cost and nanoscale non-volatile memory concept for future silicon chips
journal, March 2005

Tracking Metal Electrodeposition Dynamics from Nucleation and Growth of a Single Atom to a Crystalline Nanoparticle
journal, June 2018

Nanostructured materials for advanced energy conversion and storage devices
journal, May 2005

Chemical Synthesis and Characterization of γ-Co ₂ NiGa Nanoparticles with a Very High Curie Temperature
journal, October 2015

Effect of oriented γ′ precipitates on shape memory effect and superelasticity in Co–Ni–Ga single crystals
journal, April 2014

Nanostructured high-strength molybdenum alloys with unprecedented tensile ductility
journal, January 2013

Ultrastrong steel via minimal lattice misfit and high-density nanoprecipitation
journal, April 2017

Development of next generation tempered and ODS reduced activation ferritic/martensitic steels for fusion energy applications
journal, June 2017

Development of castable nanostructured alloys as a new generation RAFM steels
journal, December 2018

General Synthetic Strategy for Libraries of Supported Multicomponent Metal Nanoparticles
journal, April 2018

Processing and properties of magnesium containing a dense uniform dispersion of nanoparticles
journal, December 2015

The development and stability of Y–Ti–O nanoclusters in mechanically alloyed Fe–Cr based ferritic alloys
journal, August 2004

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

On the status and prospects for nanostructured ferritic alloys for nuclear fission and fusion application with emphasis on the underlying science
journal, January 2018

Core-shell nanoparticle arrays double the strength of steel
journal, February 2017

Some Reactions in the Iron–Carbon System: Application to the Tempering of Martensite
journal, June 1951

Superior radiation-resistant nanoengineered austenitic 304L stainless steel for applications in extreme radiation environments
journal, January 2015

Brittle intermetallic compound makes ultrastrong low-density steel with large ductility
journal, February 2015

Nature of χ-Carbide and Its Possible Occurrence in Steels
journal, October 1966

Creep-strengthening of steel at high temperatures using nano-sized carbonitride dispersions
journal, July 2003

A New Nitride Precipitate in Iron-Silicon Alloys
journal, October 1959

Recent status and improvement of reduced-activation ferritic-martensitic steels for high-temperature service
journal, October 2016

Orientation and phase mapping in the transmission electron microscope using precession-assisted diffraction spot recognition: state-of-the-art results: REVIEW OF PACOM (ASTAR) APPLICATION
journal, July 2013

Nanoscale Automated Phase and Orientation Mapping in the TEM
journal, November 2012

High spatial resolution semi-automatic crystallite orientation and phase mapping of nanocrystals in transmission electron microscopes
journal, April 2011

Metallurgical characterization of coupled carbon diffusion and precipitation in dissimilar steel welds
journal, February 2016

Direct carbon replicas from metal surfaces
journal, June 1956

Uses of Carbon Replicas in Electron Microscopy
journal, December 1956

Quantitative assessment of extraction replicas for particle analysis
journal, March 1968

Growth of Sulphide Films on Steel
journal, August 1960

Replica Extraction Method on Nanostructured Gold Coatings and Orientation Determination Combining SEM and TEM Techniques
journal, October 2014

Boron Autoradiography with the Electron Microscope
journal, August 1969

Evolution of microstructure and mechanical properties during thermomechanical processing of a low-density multiphase steel for automotive application
journal, August 2014

Coarsening behaviour of M23C6 carbides in creep-resistant steel exposed to high temperatures
journal, July 2016

A Technique for Sampling Oxide Layers and Brittle Materials for Microdiffraction
journal, April 1960

Freeze-fracture electron microscopy
journal, March 2007

Transmission Kikuchi diffraction in a scanning electron microscope: A review
journal, December 2016

Orientation mapping of nanostructured materials using transmission Kikuchi diffraction in the scanning electron microscope
journal, September 2012

Transmission EBSD from 10 nm domains in a scanning electron microscope: TRANSMISSION EBSD IN THE SEM
journal, November 2011

On the optimum resolution of transmission-electron backscattered diffraction (t-EBSD)
journal, January 2016

Characterizing deformed ultrafine-grained and nanocrystalline materials using transmission Kikuchi diffraction in a scanning electron microscope
journal, January 2014

Features of Transmission EBSD and its Application
journal, July 2013

Grain boundary mediated hydriding phase transformations in individual polycrystalline metal nanoparticles
journal, October 2017

Viewpoint: Nanoscale chemistry and crystallography are both the obstacle and pathway to advanced radiation-tolerant materials
journal, January 2018

Grain orientations and grain boundaries in tungsten nonotendril fuzz grown under divertor-like conditions
journal, January 2017

Nanostructure characterisation of flow-formed Cr–Mo–V steel using transmission Kikuchi diffraction technique
journal, June 2015

Characterisation of nano-grains in MgB2 superconductors by transmission Kikuchi diffraction
journal, May 2015

Grain size effect on deformation twinning propensity in ultrafine-grained hexagonal close-packed titanium
journal, September 2013

The capability of Transmission Kikuchi Diffraction technique for characterizing nano-grained oxide scales formed on a FeCrAl stainless steel
journal, May 2015

Eurofer Steel, Development to Full Code Qualification
journal, January 2013

Development of new generation reduced activation ferritic-martensitic steels for advanced fusion reactors
journal, September 2016

Electron densities in VN. I. High-precision x-ray-diffraction determination of the valence-electron density distribution and atomic displacement parameters
journal, July 1987

Atom distributions in tau-carbide phases: Fe and Cr distributions in (Cr _{23− x} Fe _x )C ₆ with x = 0, 0·7 ₄ , 1·7 ₀ , 4·1 ₃ and 7·3 ₆
journal, June 1987

Formation of NaCl-type Cr carbide by carbon ion implantation
journal, April 1993

Structure refinement for Cr2N
journal, February 1990

Nucleation and growth of tungsten nanotendrils grown under divertor-like conditions
journal, October 2018

Homeopathic ICA: A simple approach to expand the use of independent component analysis (ICA)
journal, March 2015

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

TEM characterization on new 9% Cr advanced steels thermomechanical treated after tempering
journal, March 2018

Niobium carbonitride precipitation and austenite recrystallization in hot-rolled microalloyed steels
journal, March 1980

Laser melting and heat treatment of m2 tool steel: A microstructural characterization
journal, July 1979

Precipitation in Interstitial Free High Strength Steels
journal, January 2009

CASINO a Powerful Simulation Tool for Cathodoluminescence Applications
journal, July 2006