Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy

Zhou, Jihan; Taylor, Matthew; Melinte, Georgian A.; Shahani, Ashwin J.; Dharmawardhana, Chamila C.; Heinz, Hendrik; Voorhees, Peter W.; Perepezko, John H.; Bustillo, Karen; Ercius, Peter; Miao, Jianwei

doi:10.1038/s41598-018-28348-3

Title: Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy

Abstract

We report quantitative characterization of the high temperature oxidation process by using electron tomography and energy-dispersive X-ray spectroscopy. As a proof of principle, we performed 3D imaging of the oxidation layer of a model system (Mo₃Si) at nanoscale resolution with elemental specificity and probed the oxidation kinetics as a function of the oxidation time and the elevated temperature. Our tomographic reconstructions provide detailed 3D structural information of the surface oxidation layer of the Mo₃Si system, revealing the evolution of oxidation behavior of Mo₃Si from early stage to mature stage. Based on the relative rate of oxidation of Mo₃Si, the volatilization rate of MoO₃ and reactive molecular dynamics simulations, we propose a model to explain the mechanism of the formation of the porous silica structure during the oxidation process of Mo₃Si. We expect that this 3D quantitative characterization method can be applied to other material systems to probe their structure-property relationships in different environments.

Authors:

Zhou, Jihan ^[1]; Taylor, Matthew ^[2]; Melinte, Georgian A. ^[1]; Shahani, Ashwin J. ^[3]; Dharmawardhana, Chamila C. ^[4]; Heinz, Hendrik ^[4]; Voorhees, Peter W. ^[5]; Perepezko, John H. ^[2];

^[6];

^[6]; Miao, Jianwei ^[1]

Univ. of California, Los Angeles, CA (United States)
Univ. of Wisconsin, Madison, WI (United States)
Univ. of Michigan, Ann Arbor, MI (United States)
Univ. of Colorado, Boulder, CO (United States)
Northwestern Univ., Evanston, IL (United States)
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

Publication Date:: 2018-07-06

Research Org.:: Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1478362

Grant/Contract Number:: AC02-05CH11231

Resource Type:: Accepted Manuscript

Journal Name:: Scientific Reports

Additional Journal Information:: Journal Volume: 8; Journal Issue: 1; Journal ID: ISSN 2045-2322

Publisher:: Nature Publishing Group

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE

Citation Formats


                    Zhou, Jihan, Taylor, Matthew, Melinte, Georgian A., Shahani, Ashwin J., Dharmawardhana, Chamila C., Heinz, Hendrik, Voorhees, Peter W., Perepezko, John H., Bustillo, Karen, Ercius, Peter, and Miao, Jianwei. Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy.  United States: N. p., 2018. 
Web.  doi:10.1038/s41598-018-28348-3.

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                    Zhou, Jihan, Taylor, Matthew, Melinte, Georgian A., Shahani, Ashwin J., Dharmawardhana, Chamila C., Heinz, Hendrik, Voorhees, Peter W., Perepezko, John H., Bustillo, Karen, Ercius, Peter, & Miao, Jianwei. Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy.  United States.  https://doi.org/10.1038/s41598-018-28348-3

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                    Zhou, Jihan, Taylor, Matthew, Melinte, Georgian A., Shahani, Ashwin J., Dharmawardhana, Chamila C., Heinz, Hendrik, Voorhees, Peter W., Perepezko, John H., Bustillo, Karen, Ercius, Peter, and Miao, Jianwei. Fri .  
"Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy".  United States.  https://doi.org/10.1038/s41598-018-28348-3.  https://www.osti.gov/servlets/purl/1478362.

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@article{osti_1478362,

  title        = {Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy},

  author       = {Zhou, Jihan and Taylor, Matthew and Melinte, Georgian A. and Shahani, Ashwin J. and Dharmawardhana, Chamila C. and Heinz, Hendrik and Voorhees, Peter W. and Perepezko, John H. and Bustillo, Karen and Ercius, Peter and Miao, Jianwei},

  abstractNote = {We report quantitative characterization of the high temperature oxidation process by using electron tomography and energy-dispersive X-ray spectroscopy. As a proof of principle, we performed 3D imaging of the oxidation layer of a model system (Mo3Si) at nanoscale resolution with elemental specificity and probed the oxidation kinetics as a function of the oxidation time and the elevated temperature. Our tomographic reconstructions provide detailed 3D structural information of the surface oxidation layer of the Mo3Si system, revealing the evolution of oxidation behavior of Mo3Si from early stage to mature stage. Based on the relative rate of oxidation of Mo3Si, the volatilization rate of MoO3 and reactive molecular dynamics simulations, we propose a model to explain the mechanism of the formation of the porous silica structure during the oxidation process of Mo3Si. We expect that this 3D quantitative characterization method can be applied to other material systems to probe their structure-property relationships in different environments.},

  doi          = {10.1038/s41598-018-28348-3},

  journal      = {Scientific Reports},

  number       = 1,

  volume       = 8,

  place        = {United States},

  year         = {2018},

  month        = {7}

}

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Title: Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy

Abstract

Citation Formats

Three-dimensional coordinates of individual atoms in materials revealed by electron tomography journal, September 2015

Electron tomography at 2.4-ångström resolution journal, March 2012

GENFIRE: A generalized Fourier iterative reconstruction algorithm for high-resolution 3D imaging journal, September 2017

A Model Based Iterative Reconstruction Algorithm For High Angle Annular Dark Field-Scanning Transmission Electron Microscope (HAADF-STEM) Tomography journal, November 2013

Towards three-dimensional structural determination of amorphous materials at atomic resolution journal, September 2013

Electron tomography and holography in materials science journal, April 2009

Simulations of inorganic–bioorganic interfaces to discover new materials: insights, comparisons to experiment, challenges, and opportunities journal, January 2016

Atomic-scale determination of surface facets in gold nanorods journal, October 2012

Three-dimensional study of cylindrical morphology in a styrene-butadiene-styrene block copolymer journal, March 1988

Vapor Pressure of Molybdenum Trioxide journal, January 1963

Oxidation of Molybdenum 550° to 1700°C journal, January 1963

Deciphering chemical order/disorder and material properties at the single-atom level journal, February 2017

Three-dimensional imaging of dislocations in a nanoparticle at atomic resolution journal, March 2013

Three-dimensional imaging of pore structures inside low-κ dielectrics journal, May 2010

Atomic electron tomography: 3D structures without crystals journal, September 2016

Three-Dimensional Elemental Mapping at the Atomic Scale in Bimetallic Nanocrystals journal, August 2013

Transmission electron microtomography without the “missing wedge” for quantitative structural analysis journal, January 2007

Embedded Nanostructures Revealed in Three Dimensions journal, September 2005

Topological complexity and the dynamics of coarsening journal, May 2004

Mo-Si-B Alloys for Ultrahigh-Temperature Structural Applications journal, June 2012

Development and Optimization of Regularized Tomographic Reconstruction Algorithms Utilizing Equally-Sloped Tomography journal, May 2010

3D electron microscopy in the physical sciences: the development of Z-contrast and EFTEM tomography journal, September 2003

Morphological and topological analysis of coarsened nanoporous gold by x-ray nanotomography journal, January 2010

Thermodynamic considerations in refractory metal‐silicon‐oxygen systems journal, July 1984

Radiation dose reduction and image enhancement in biological imaging through equally-sloped tomography journal, November 2008

Intermetallic Compounds for Strong High-Temperature Materials: Status and Potential journal, August 1989

Structural and morphological studies of the growth of MoO3 scales during high-temperature oxidation of molybdenum journal, April 1992

Mo-Si-B Alloys: Developing a Revolutionary Turbine-Engine Material journal, September 2003

Phase stability and structural defects in high-temperature Mo–Si–B alloys journal, October 2008

Oxide scale formation and isothermal oxidation behavior of Mo–Si–B intermetallics at 600–1000°C journal, February 1999

Formation of bimetallic clusters in superfluid helium nanodroplets analysed by atomic resolution electron tomography journal, October 2015

Nanomaterial datasets to advance tomography in scanning transmission electron microscopy journal, June 2016

Transient oxidation of Mo–Si–B alloys: Effect of the microstructure size scale journal, September 2009

The morphological evolution of dendritic microstructures during coarsening journal, April 2006

Coating Strategies for Oxidation Resistant High Temperature Mo-Si-B Alloys conference, January 2007

Exploring nanomaterials with 3D electron microscopy journal, September 2015

Three-Dimensional Transmission Electron Microscopy: A Novel Imaging and Characterization Technique with Nanometer Scale Resolution for Materials Science journal, October 2000

The development of columnar grain and single crystal high temperature materials through directional solidification journal, October 1970

Equally sloped tomography with oversampling reconstruction journal, August 2005

Coating Strategies for Oxidation Resistant High Temperature Mo-Si-B Alloys journal, June 2006

Atomic electron tomography in three and four dimensions journal, April 2020

Three-dimensional coordinates of individual atoms in materials revealed by electron tomography
journal, September 2015

Electron tomography at 2.4-ångström resolution
journal, March 2012

GENFIRE: A generalized Fourier iterative reconstruction algorithm for high-resolution 3D imaging
journal, September 2017

A Model Based Iterative Reconstruction Algorithm For High Angle Annular Dark Field-Scanning Transmission Electron Microscope (HAADF-STEM) Tomography
journal, November 2013

Towards three-dimensional structural determination of amorphous materials at atomic resolution
journal, September 2013

Electron tomography and holography in materials science
journal, April 2009

Simulations of inorganic–bioorganic interfaces to discover new materials: insights, comparisons to experiment, challenges, and opportunities
journal, January 2016

Atomic-scale determination of surface facets in gold nanorods
journal, October 2012

Three-dimensional study of cylindrical morphology in a styrene-butadiene-styrene block copolymer
journal, March 1988

Vapor Pressure of Molybdenum Trioxide
journal, January 1963

Oxidation of Molybdenum 550° to 1700°C
journal, January 1963

Deciphering chemical order/disorder and material properties at the single-atom level
journal, February 2017

Three-dimensional imaging of dislocations in a nanoparticle at atomic resolution
journal, March 2013

Three-dimensional imaging of pore structures inside low-κ dielectrics
journal, May 2010

Atomic electron tomography: 3D structures without crystals
journal, September 2016

Three-Dimensional Elemental Mapping at the Atomic Scale in Bimetallic Nanocrystals
journal, August 2013

Transmission electron microtomography without the “missing wedge” for quantitative structural analysis
journal, January 2007

Embedded Nanostructures Revealed in Three Dimensions
journal, September 2005

Topological complexity and the dynamics of coarsening
journal, May 2004

Mo-Si-B Alloys for Ultrahigh-Temperature Structural Applications
journal, June 2012

Development and Optimization of Regularized Tomographic Reconstruction Algorithms Utilizing Equally-Sloped Tomography
journal, May 2010

3D electron microscopy in the physical sciences: the development of Z-contrast and EFTEM tomography
journal, September 2003

Morphological and topological analysis of coarsened nanoporous gold by x-ray nanotomography
journal, January 2010

Thermodynamic considerations in refractory metal‐silicon‐oxygen systems
journal, July 1984

Radiation dose reduction and image enhancement in biological imaging through equally-sloped tomography
journal, November 2008

Intermetallic Compounds for Strong High-Temperature Materials: Status and Potential
journal, August 1989

Structural and morphological studies of the growth of MoO3 scales during high-temperature oxidation of molybdenum
journal, April 1992

Mo-Si-B Alloys: Developing a Revolutionary Turbine-Engine Material
journal, September 2003

Phase stability and structural defects in high-temperature Mo–Si–B alloys
journal, October 2008

Oxide scale formation and isothermal oxidation behavior of Mo–Si–B intermetallics at 600–1000°C
journal, February 1999

Formation of bimetallic clusters in superfluid helium nanodroplets analysed by atomic resolution electron tomography
journal, October 2015

Nanomaterial datasets to advance tomography in scanning transmission electron microscopy
journal, June 2016

Transient oxidation of Mo–Si–B alloys: Effect of the microstructure size scale
journal, September 2009

The morphological evolution of dendritic microstructures during coarsening
journal, April 2006

Coating Strategies for Oxidation Resistant High Temperature Mo-Si-B Alloys
conference, January 2007

Exploring nanomaterials with 3D electron microscopy
journal, September 2015

Three-Dimensional Transmission Electron Microscopy: A Novel Imaging and Characterization Technique with Nanometer Scale Resolution for Materials Science
journal, October 2000

The development of columnar grain and single crystal high temperature materials through directional solidification
journal, October 1970

Equally sloped tomography with oversampling reconstruction
journal, August 2005

Coating Strategies for Oxidation Resistant High Temperature Mo-Si-B Alloys
journal, June 2006

Atomic electron tomography in three and four dimensions
journal, April 2020