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Crystalline domain size and faulting in the new NIST SRM 1979 zinc oxide

Published online by Cambridge University Press:  14 November 2013

J. P. Cline ,
M. Leoni ,
D. Black ,
A. Henins ,
J. E. Bonevich ,
P. S. Whitfield  and
P. Scardi
J. P. Cline
Affiliation:
National Institute of Standards and Technology, Gaithersburg, MD
M. Leoni
Affiliation:
Dept. of Civil, Environmental and Mechanical Engineering, University of Trento, Trento, Italy
D. Black
Affiliation:
National Institute of Standards and Technology, Gaithersburg, MD
A. Henins
Affiliation:
National Institute of Standards and Technology, Gaithersburg, MD
J. E. Bonevich
Affiliation:
National Institute of Standards and Technology, Gaithersburg, MD
P. S. Whitfield
Affiliation:
National Research Council, Ottawa, Canada
P. Scardi
Affiliation:
Dept. of Civil, Environmental and Mechanical Engineering, University of Trento, Trento, Italy
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Abstract

A NIST SRM certified to address the issue of crystallite size measurement through a line profile analysis has been under development for several years. In order to prepare the feedstock for the SRM, nano-crystalline zinc oxide was produced from thermal decomposition of zinc oxalate. The thermal processing parameters were chosen to yield particles in two size ranges, one with a distribution centered at approximately 15 nm and another centered at 60 nm. Certification data were collected on a NIST-built diffractometer equipped with a Johansson incident beam monochromator and scintillation detector. Data were analyzed using whole powder pattern modeling to determine microstructural data. The analysis shows domains to be in the form of discs of a fairly small aspect ratio. While both materials exhibit the effects of stacking faults through broadening of specific hkl reflections, their presence in the 60 nm is more difficult to discern. Images of the crystallites obtained with transmission electron microscopy are consistent with the results from the X-ray diffraction analyses.

Keywords

NISTSRM 1979Line Profile Analysis

Information

Type
Technical Articles
Information
Powder Diffraction , Volume 28 , Supplement S2 , September 2013 , pp. S22 - S32
Copyright
Copyright © International Centre for Diffraction Data 2013 

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References

Auffrédic, J. P., Boultif, A., Langford, J. I. and Louër, D. (1995). “Early Stages of Crystallite Growth of ZnO Obtained from an Oxalate Precursor,” J. Am. Ceram. Soc. 78, 323–328.CrossRefGoogle Scholar
Caglioti, G., Paoletti, A. and Ricci, F. P. (1958). “Choice of Collimators for a Crystal Spectrometer for Neutron Diffraction,” Nucl. Instrum. 3(4), 223–228.CrossRefGoogle Scholar
Finger, L. W., Cox, D. E. and Jephcoat, A. P. (1994). “A Correction for Powder Diffraction Peak Asymmetry due to Axial Divergence,” J. Appl. Crystallogr. 27, pp. 892–900.Google Scholar
Guillou, N., Auffrédic, J. P. and Louër, D. (1995). “The early stages of crystallite growth of CeO2 obtained from a cerium oxide nitrate,” Powder Diffr. 10, 236–240.Google Scholar
Hölzer, G., Fritsch, M., Deutsch, M., Härtwig, J. and Förster, E. (1997). “Kα1,2 and Kα1,3 x-ray emission lines of the 3d transition metals,” Phys. Rev. A: At., Mol., Opt. Phys. 56, 4554–4568.Google Scholar
Langford, J. I., Boultif, A., Auffrédic, J. P. and Louër, D. (1993). “The use of pattern decomposition to study the combined X-ray diffraction effects of crystallite size and stacking faults in ex-oxalate zinc oxide,” J. Appl. Crystallogr. 26, 22–33.CrossRefGoogle Scholar
Langford, J. I. and Louër, D. (1982). “Diffraction line profiles and Scherrer constants for materials with cylindrical crystallites,” J. Appl. Crystallogr. 15 (1), 20–26.Google Scholar
Leoni, M., Confente, T. and Scardi, P. (2006). “PM2K: a flexible program implementing Whole Powder Pattern Modelling,” Z. Kristallogr. Suppl. 2006, Issue suppl 23, 249–254.CrossRefGoogle Scholar
Leoni, M. and Scardi, P. (2004). “Nanocrystalline domain size distributions from powder diffraction data,” J. Appl. Crystallogr. 37(4), 629–634.Google Scholar
Louër, D., Auffrédic, J. P., Langford, J. I., Ciosmak, D. and Niepce, J. C. (1983). “A precise determination of the shape, size and distribution of size of crystallites in zinc oxide by X-ray diffraction line-broadening analysis,” J. Appl. Crystallogr. 16, 183–191.CrossRefGoogle Scholar
NIST (2010). Lanthanum Hexaboride Powder Line Position and Line Shape Standard for Powder Diffraction (SRM 660b), Gaithersburg, MD; National Institute of Standards and Technology; U.S. Department of Commerce.Google Scholar
Scardi, P. and Leoni, M. (2001). “Diffraction line profiles from polydisperse crystalline systems,” Acta Crystallogr, Sect. A: Found. Crystallogr. 57 (5), 604–613.Google Scholar
Scardi, P. and Leoni, M. (2002). “Whole powder pattern modeling,” Acta Crystallogr ., Sect. A: Found. Crystallogr. 58, 190–200.CrossRefGoogle Scholar
Warren, B. E., (1969). X-ray Diffraction (Dover Publications, Inc., N.Y).Google Scholar