Characterization of zirconium carbide microspheres synthesized via internal gelation

Patrick C. Huston; Devon L. Drey; William F. Cureton; J. Matthew Kurley; Jake W. Mcmurray; S. Michelle Everett; Changyong Park; Maik Lang

doi:10.1016/j.jnucmat.2021.153218

Characterization of zirconium carbide microspheres synthesized via internal gelation

Patrick C. Huston, Devon L. Drey, William F. Cureton, J. Matthew Kurley, Jake W. Mcmurray, S. Michelle Everett, Changyong Park, Maik Lang

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

5 Scopus citations

Abstract

Microspheres of zirconium carbide with grain size 40-320 nm were synthesized using internal gelation techniques and characterized by scanning electron microscopy, synchrotron X-ray diffraction, and neutron total scattering. Compared with a polycrystalline benchmark ZrC sample prepared by plasma vapor phase deposition, the microspheres display lower variance in grain size and considerably lower microstrain, representative of a more homogenous internal microstructure. However, excess carbon was present in the microspheres, evident in both the X-ray and neutron diffraction data as well as a corresponding hypostoichiometric ZrC phase. The excess carbon phase is assumed to be pockets of carbon that remained unreacted through the combined internal gelation and subsequent carbothermic reduction synthesis process. Atomic-scale structural characterization with neutron PDF analysis confirmed the presence of localized nano-sized domains of graphite-like carbon material.

Original language	English
Article number	153218
Journal	Journal of Nuclear Materials
Volume	557
DOIs	https://doi.org/10.1016/j.jnucmat.2021.153218
State	Published - Dec 15 2021

Funding

This work was funded by the Department of Energy (DOE) Office of Nuclear Energy's Nuclear Energy University Program under US-DOE, contract DE-NE0008895. Synchrotron XRD measurements were performed at HPCAT (Sector 16), Advanced Photon Source (APS), Argonne National Laboratory. HPCAT operations are supported by DOE-NNSA's Office of Experimental Sciences. The Advanced Photon Source is a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357. HPCAT beam time was provided by the Chicago/DOE Alliance Center. This research used resources at the Spallation Neutron Source, a DOE Office of Science User Facility operated by the Oak Ridge National Laboratory. This material is based upon work supported under the Integrated University Program Graduate Fellowship (W. Cureton and D. Drey). The authors would like to express their thanks to A. Nelson (Oak Ridge National Laboratory) for insightful discussion, E. O'Quinn (University of Tennessee) for technical support, as well as K. Cooley and A. McAlister (both Oak Ridge National Laboratory) for support in sample synthesis.

Keywords

Microstructure
Neutron total scattering
Pair distribution function
Scanning electron microscopy
X-ray diffraction
Zirconium carbide

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10.1016/j.jnucmat.2021.153218

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title = "Characterization of zirconium carbide microspheres synthesized via internal gelation",

abstract = "Microspheres of zirconium carbide with grain size 40-320 nm were synthesized using internal gelation techniques and characterized by scanning electron microscopy, synchrotron X-ray diffraction, and neutron total scattering. Compared with a polycrystalline benchmark ZrC sample prepared by plasma vapor phase deposition, the microspheres display lower variance in grain size and considerably lower microstrain, representative of a more homogenous internal microstructure. However, excess carbon was present in the microspheres, evident in both the X-ray and neutron diffraction data as well as a corresponding hypostoichiometric ZrC phase. The excess carbon phase is assumed to be pockets of carbon that remained unreacted through the combined internal gelation and subsequent carbothermic reduction synthesis process. Atomic-scale structural characterization with neutron PDF analysis confirmed the presence of localized nano-sized domains of graphite-like carbon material.",

keywords = "Microstructure, Neutron total scattering, Pair distribution function, Scanning electron microscopy, X-ray diffraction, Zirconium carbide",

author = "Huston, {Patrick C.} and Drey, {Devon L.} and Cureton, {William F.} and Kurley, {J. Matthew} and Mcmurray, {Jake W.} and Everett, {S. Michelle} and Changyong Park and Maik Lang",

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T1 - Characterization of zirconium carbide microspheres synthesized via internal gelation

AU - Huston, Patrick C.

AU - Drey, Devon L.

AU - Cureton, William F.

AU - Kurley, J. Matthew

AU - Mcmurray, Jake W.

AU - Everett, S. Michelle

AU - Park, Changyong

AU - Lang, Maik

PY - 2021/12/15

Y1 - 2021/12/15

N2 - Microspheres of zirconium carbide with grain size 40-320 nm were synthesized using internal gelation techniques and characterized by scanning electron microscopy, synchrotron X-ray diffraction, and neutron total scattering. Compared with a polycrystalline benchmark ZrC sample prepared by plasma vapor phase deposition, the microspheres display lower variance in grain size and considerably lower microstrain, representative of a more homogenous internal microstructure. However, excess carbon was present in the microspheres, evident in both the X-ray and neutron diffraction data as well as a corresponding hypostoichiometric ZrC phase. The excess carbon phase is assumed to be pockets of carbon that remained unreacted through the combined internal gelation and subsequent carbothermic reduction synthesis process. Atomic-scale structural characterization with neutron PDF analysis confirmed the presence of localized nano-sized domains of graphite-like carbon material.

AB - Microspheres of zirconium carbide with grain size 40-320 nm were synthesized using internal gelation techniques and characterized by scanning electron microscopy, synchrotron X-ray diffraction, and neutron total scattering. Compared with a polycrystalline benchmark ZrC sample prepared by plasma vapor phase deposition, the microspheres display lower variance in grain size and considerably lower microstrain, representative of a more homogenous internal microstructure. However, excess carbon was present in the microspheres, evident in both the X-ray and neutron diffraction data as well as a corresponding hypostoichiometric ZrC phase. The excess carbon phase is assumed to be pockets of carbon that remained unreacted through the combined internal gelation and subsequent carbothermic reduction synthesis process. Atomic-scale structural characterization with neutron PDF analysis confirmed the presence of localized nano-sized domains of graphite-like carbon material.

KW - Microstructure

KW - Neutron total scattering

KW - Pair distribution function

KW - Scanning electron microscopy

KW - X-ray diffraction

KW - Zirconium carbide

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VL - 557

JO - Journal of Nuclear Materials

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Characterization of zirconium carbide microspheres synthesized via internal gelation

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