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

Journal Article · · Scientific Reports
 [1];  [2];  [1];  [3];  [4];  [4];  [5];  [2]; ORCiD logo [6]; ORCiD logo [6];  [1]
  1. Univ. of California, Los Angeles, CA (United States)
  2. Univ. of Wisconsin, Madison, WI (United States)
  3. Univ. of Michigan, Ann Arbor, MI (United States)
  4. Univ. of Colorado, Boulder, CO (United States)
  5. Northwestern Univ., Evanston, IL (United States)
  6. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

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.

Research Organization:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-05CH11231
OSTI ID:
1478362
Journal Information:
Scientific Reports, Vol. 8, Issue 1; ISSN 2045-2322
Publisher:
Nature Publishing GroupCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 4 works
Citation information provided by
Web of Science

References (42)

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
Exploring nanomaterials with 3D electron microscopy journal September 2015
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
Phase stability and structural defects in high-temperature Mo–Si–B alloys journal October 2008
Three-dimensional imaging of dislocations in a nanoparticle at atomic resolution journal March 2013
Oxidation of Molybdenum 550° to 1700°C journal January 1963
Structural and morphological studies of the growth of MoO3 scales during high-temperature oxidation of molybdenum journal April 1992
Deciphering chemical order/disorder and material properties at the single-atom level journal February 2017
Intermetallic Compounds for Strong High-Temperature Materials: Status and Potential journal August 1989
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
Coating Strategies for Oxidation Resistant High Temperature Mo-Si-B Alloys journal June 2006
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
Three-Dimensional Transmission Electron Microscopy:  A Novel Imaging and Characterization Technique with Nanometer Scale Resolution for Materials Science journal October 2000
Morphological and topological analysis of coarsened nanoporous gold by x-ray nanotomography journal January 2010
The development of columnar grain and single crystal high temperature materials through directional solidification journal October 1970
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
Mo-Si-B Alloys: Developing a Revolutionary Turbine-Engine Material journal September 2003
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
Three-Dimensional Electron Microscopy of Macromolecular Assemblies book January 2006
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
Equally sloped tomography with oversampling reconstruction journal August 2005
High Temperature Materials journal March 2006

Cited By (1)

Atomic electron tomography in three and four dimensions journal April 2020

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