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

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

doi:10.1038/s41598-018-28348-3

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

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

^*Corresponding author for this work

Materials Science and Engineering

Research output: Contribution to journal › Article › peer-review

8 Scopus citations

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.

Original language	English (US)
Article number	10239
Journal	Scientific reports
Volume	8
Issue number	1
DOIs	https://doi.org/10.1038/s41598-018-28348-3
State	Published - Dec 1 2018

Funding

We acknowledge support from ONR MURI \u201CUnderstanding Atomic Scale Structure in Four Dimensions to Design and Control Corrosion Resistant Alloys\u201D on Grant Number N00014-14-1-0675. This work was also supported by STROBE: A National Science Foundation Science & Technology Center under Grant No. DMR 1548924, the Office of Basic Energy Sciences of the US DOE (DE-SC0010378), and the NSF DMREF program (DMR-1437263). J.M. thanks support through the University of Strasbourg Institute for Advanced Study (USIAS) Fellowship. The HAADF-STEM imaging and EDS spectra collecting were performed at the Molecular Foundry, LBNL, which is supported by the Office of Science, Office of Basic Energy Sciences of the U.S. DOE under Contract No. DE-AC02-05CH11231.

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Zhou, J., Taylor, M., Melinte, G. A., Shahani, A. J., Dharmawardhana, C. C., Heinz, H., Voorhees, P. W., Perepezko, J. H., Bustillo, K., Ercius, P., & Miao, J. (2018). Quantitative characterization of high temperature oxidation using electron tomography and energy-dispersive X-ray spectroscopy. Scientific reports, 8(1), Article 10239. https://doi.org/10.1038/s41598-018-28348-3

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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.",

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

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AU - Taylor, Matthew

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AU - Shahani, Ashwin J.

AU - Dharmawardhana, Chamila C.

AU - Heinz, Hendrik

AU - Voorhees, Peter W.

AU - Perepezko, John H.

AU - Bustillo, Karen

AU - Ercius, Peter

AU - Miao, Jianwei

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N2 - 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.

AB - 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.

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

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