Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method

G. W. Chinthaka Silva; Andrew A. Kercher; John D. Hunn; Rodger C. Martin; Gerald E. Jellison; Harry M. Meyer

doi:10.1016/j.jssc.2012.04.047

Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method

G. W. Chinthaka Silva, Andrew A. Kercher, John D. Hunn, Rodger C. Martin, Gerald E. Jellison, Harry M. Meyer

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

24 Scopus citations

Abstract

Samples with five different zirconium carbide compositions (C/Zr molar ratio=0.84, 0.89, 0.95, 1.05, and 1.17) have been fabricated and studied using a variety of experimental techniques. Each sample was zone refined to ensure that the end product was polycrystalline with a grain size of 10-100 μm. It was found that the lattice parameter was largest for the x=0.89 composition and smallest for the x=1.17 total C/Zr composition, but was not linear; this nonlinearity is possibly explained using electron densities calculated using charge flipping technique. Among the five samples, the unit cell of the ZrC _0.89 sample showed the highest electron density, corresponding to the highest carbon incorporation and the largest lattice parameter. The ZrC _0.84 sample showed the lowest carbon incorporation, resulting in a larger number of carbon vacancies and resultant strain. Samples with larger carbon ratios (x=0.95, 1.05, and 1.17) showed a slight decrease in lattice parameter, due to a decrease in electron density. Optical anisotropy measurements suggest that these three samples contained significant amounts of a graphitic carbon phase, not bonded to the Zr atoms.

Original language	English
Pages (from-to)	91-99
Number of pages	9
Journal	Journal of Solid State Chemistry
Volume	194
DOIs	https://doi.org/10.1016/j.jssc.2012.04.047
State	Published - Oct 2012

Funding

This work was carried out at Oak Ridge National Laboratory and was sponsored by the Office of Nuclear Energy, Science and Technology, US Department of Energy . We thank Bill Mackie at ATI Wah Chang in Albany, OR for the elemental analysis. Many thanks go to Dr. Gokul Vasudevamurthy at ORNL for supplying mounted samples for microscopic analysis. Special thanks go to Dr. Andrew Payzant for his valuable discussions to make this paper successful and for providing help in obtaining and analyzing the XRD powder patterns. Thanks also to Dr. Roberta Peascoe Meisner for XRD powder analysis and Dr. Ed Kenik for SEM support. Thanks to Dr. William A. Mackie at Applied Physics Technologies, Inc. for sample preparation and discussions. A portion of this research was conducted at the SHaRE User Facility, which is sponsored by the Division of Scientific User Facilities, Office of Basic Energy Sciences, US Department of Energy .

Funders	Funder number
Office of Nuclear Energy, Science and Technology
U.S. Department of Energy
Basic Energy Sciences

Keywords

Auger depth profile
Charge flipping
Optical anisotropy
SEM
Zirconium carbide

Access to Document

10.1016/j.jssc.2012.04.047

Cite this

Chinthaka Silva, G. W., Kercher, A. A., Hunn, J. D., Martin, R. C., Jellison, G. E., & Meyer, H. M. (2012). Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method. Journal of Solid State Chemistry, 194, 91-99. https://doi.org/10.1016/j.jssc.2012.04.047

@article{b665f9b1ddff436bb394feef5523d5f1,

title = "Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method",

abstract = "Samples with five different zirconium carbide compositions (C/Zr molar ratio=0.84, 0.89, 0.95, 1.05, and 1.17) have been fabricated and studied using a variety of experimental techniques. Each sample was zone refined to ensure that the end product was polycrystalline with a grain size of 10-100 μm. It was found that the lattice parameter was largest for the x=0.89 composition and smallest for the x=1.17 total C/Zr composition, but was not linear; this nonlinearity is possibly explained using electron densities calculated using charge flipping technique. Among the five samples, the unit cell of the ZrC 0.89 sample showed the highest electron density, corresponding to the highest carbon incorporation and the largest lattice parameter. The ZrC 0.84 sample showed the lowest carbon incorporation, resulting in a larger number of carbon vacancies and resultant strain. Samples with larger carbon ratios (x=0.95, 1.05, and 1.17) showed a slight decrease in lattice parameter, due to a decrease in electron density. Optical anisotropy measurements suggest that these three samples contained significant amounts of a graphitic carbon phase, not bonded to the Zr atoms.",

keywords = "Auger depth profile, Charge flipping, Optical anisotropy, SEM, Zirconium carbide",

author = "{Chinthaka Silva}, {G. W.} and Kercher, {Andrew A.} and Hunn, {John D.} and Martin, {Rodger C.} and Jellison, {Gerald E.} and Meyer, {Harry M.}",

year = "2012",

month = oct,

doi = "10.1016/j.jssc.2012.04.047",

language = "English",

volume = "194",

pages = "91--99",

journal = "Journal of Solid State Chemistry",

issn = "0022-4596",

publisher = "Elsevier",

}

Chinthaka Silva, GW, Kercher, AA, Hunn, JD, Martin, RC, Jellison, GE & Meyer, HM 2012, 'Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method', Journal of Solid State Chemistry, vol. 194, pp. 91-99. https://doi.org/10.1016/j.jssc.2012.04.047

Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method. / Chinthaka Silva, G. W.; Kercher, Andrew A.; Hunn, John D. et al.
In: Journal of Solid State Chemistry, Vol. 194, 10.2012, p. 91-99.

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

TY - JOUR

T1 - Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method

AU - Chinthaka Silva, G. W.

AU - Kercher, Andrew A.

AU - Hunn, John D.

AU - Martin, Rodger C.

AU - Jellison, Gerald E.

AU - Meyer, Harry M.

PY - 2012/10

Y1 - 2012/10

N2 - Samples with five different zirconium carbide compositions (C/Zr molar ratio=0.84, 0.89, 0.95, 1.05, and 1.17) have been fabricated and studied using a variety of experimental techniques. Each sample was zone refined to ensure that the end product was polycrystalline with a grain size of 10-100 μm. It was found that the lattice parameter was largest for the x=0.89 composition and smallest for the x=1.17 total C/Zr composition, but was not linear; this nonlinearity is possibly explained using electron densities calculated using charge flipping technique. Among the five samples, the unit cell of the ZrC 0.89 sample showed the highest electron density, corresponding to the highest carbon incorporation and the largest lattice parameter. The ZrC 0.84 sample showed the lowest carbon incorporation, resulting in a larger number of carbon vacancies and resultant strain. Samples with larger carbon ratios (x=0.95, 1.05, and 1.17) showed a slight decrease in lattice parameter, due to a decrease in electron density. Optical anisotropy measurements suggest that these three samples contained significant amounts of a graphitic carbon phase, not bonded to the Zr atoms.

AB - Samples with five different zirconium carbide compositions (C/Zr molar ratio=0.84, 0.89, 0.95, 1.05, and 1.17) have been fabricated and studied using a variety of experimental techniques. Each sample was zone refined to ensure that the end product was polycrystalline with a grain size of 10-100 μm. It was found that the lattice parameter was largest for the x=0.89 composition and smallest for the x=1.17 total C/Zr composition, but was not linear; this nonlinearity is possibly explained using electron densities calculated using charge flipping technique. Among the five samples, the unit cell of the ZrC 0.89 sample showed the highest electron density, corresponding to the highest carbon incorporation and the largest lattice parameter. The ZrC 0.84 sample showed the lowest carbon incorporation, resulting in a larger number of carbon vacancies and resultant strain. Samples with larger carbon ratios (x=0.95, 1.05, and 1.17) showed a slight decrease in lattice parameter, due to a decrease in electron density. Optical anisotropy measurements suggest that these three samples contained significant amounts of a graphitic carbon phase, not bonded to the Zr atoms.

KW - Auger depth profile

KW - Charge flipping

KW - Optical anisotropy

KW - SEM

KW - Zirconium carbide

UR - http://www.scopus.com/inward/record.url?scp=84866051895&partnerID=8YFLogxK

U2 - 10.1016/j.jssc.2012.04.047

DO - 10.1016/j.jssc.2012.04.047

M3 - Article

AN - SCOPUS:84866051895

SN - 0022-4596

VL - 194

SP - 91

EP - 99

JO - Journal of Solid State Chemistry

JF - Journal of Solid State Chemistry

ER -

Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method

Abstract

Funding

Keywords

Access to Document

Other files and links

Fingerprint

Cite this