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Certification of Standard Reference Material 660c for powder diffraction

Published online by Cambridge University Press:  31 January 2020

David R. Black Open the ORCID record for David R. Black [Opens in a new window] ,
Marcus H. Mendenhall ,
Craig M. Brown ,
Albert Henins ,
James Filliben  and
James P. Cline
David R. Black*
Affiliation:
Materials Measurement Science Division of Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
Marcus H. Mendenhall
Affiliation:
Materials Measurement Science Division of Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
Craig M. Brown
Affiliation:
Center for Neutron Research, National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
Albert Henins
Affiliation:
Materials Measurement Science Division of Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
James Filliben
Affiliation:
Statistical Engineering Division, National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
James P. Cline
Affiliation:
Materials Measurement Science Division of Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
*
a)Author to whom correspondence should be addressed. Electronic mail: david.black@nist.gov
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Abstract

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to evaluate specific aspects of instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 660c, the fourth generation of this powder diffraction SRM, which is used primarily for calibrating powder diffractometers with respect to line position and line shape for the determination of the instrument profile function (IPF). It is certified with respect to lattice parameter and consists of approximately 6 g of lanthanum hexaboride (LaB6) powder. So that this SRM would be applicable for the neutron diffraction community, the powder was prepared from an isotopically enriched 11B precursor material. The microstructure of the LaB6 powder was engineered specifically to yield a crystallite size above that where size broadening is typically observed and to minimize the crystallographic defects that lead to strain broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the LaB6 powder. Both Type A, statistical, and Type B, systematic, uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.415 682 6 ± 0.000 008 nm (95% confidence).

Keywords

certificationdiffractometerlattice parameterStandard Reference MaterialX-ray diffraction
Type
Technical Article
Information
Powder Diffraction , Volume 35 , Issue 1 , March 2020 , pp. 17 - 22
Creative Commons
As a work owned by the United States Government, this Contribution is not subject to copyright within the United States. Outside of the United States, Cambridge is the exclusively licensed publisher of the Contribution. The United States Government retains a non-exclusive, irrevocable, worldwide license to publish or reproduce the published form of this Contribution far United States Government purposes.
Copyright
Copyright © The National Institute of Technology 2020 outside of the United States of America

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References

Bergmann, J., Kleeberg, R., Haase, A., and Breidenstein, B. (2000). “Advanced fundamental parameters model for improved profile analysis,” in Proceedings of the 5th European Conference on Residual Stresses, Vol. 347–349, edited by A. J. Böttger, R. Delhez, and E. J. Mittemeijer (Trans Tech Publications, Delft-Noordwijkerhout, The Netherlands), pp. 303–308.Google Scholar
BIPM (2006). “International System of Units (SI),” Bureau International des Poids et Mesures. Available at: https://www.bipm.org/utils/common/pdf/si_brochure_8_en.pdf (accessed August 2019).Google Scholar
Bruker (2017). TOPAS. Version 6 (Bruker AXS GmbH, Karlsruhe, Germany).Google Scholar
Cheary, R. W. and Coelho, A. A. (1992). “A fundamental parameters approach to X-ray line-profile fitting,” J. Appl. Crystallogr. 25, 109–121.CrossRefGoogle Scholar
Cheary, R. W. and Coelho, A. A. (1998a). “Axial divergence in a conventional X-ray powder diffractometer I. Theoretical foundations,” J. Appl. Crystallogr. 31, 851–861.CrossRefGoogle Scholar
Cheary, R. W. and Coelho, A. A. (1998b). “Axial divergence in a conventional X-ray powder diffractometer II. Implementation and comparison with experiment,” J. Appl. Crystallogr. 31, 862–868.CrossRefGoogle Scholar
Cline, J. P., Mendenhall, M. H., Black, D., Windover, D., and Henins, A. (2015). “The optics, alignment and calibration of laboratory X-ray powder diffraction equipment with the use of NIST standard reference materials,” J. Res. Natl. Inst. Stand. Technol. 120, 173–222.CrossRefGoogle Scholar
Cline, J. P., Mendenhall, M. H.Black, D., Windover, D., and Henins, A. (2019). “The optics and alignment of the divergent-beam laboratory X-ray powder diffractometer and its calibration using NIST Standard Reference Materials,” in International Tables for Crystallography, Volume H: Powder Diffraction, edited by Gilmore, C. J., Kaduk, J. A., and Schenk, H. (Wiley, Hoboken, NJ), pp. 224–251.CrossRefGoogle Scholar
Hölzer, G., Fritsch, M., Deutsch, M., Härtwig, J., and Förster, E. (1997). “Kα1,2 and Kβ1,3 X-ray emission lines of the 3d transition metals,” Phys. Rev. A 56(6), 4554–4568.CrossRefGoogle Scholar
JCGM 100 (2008). “Guide to the expression of uncertainty in measurement” (GUM 1995 with Minor Corrections), Joint Committee for Guides in Metrology (JCGM). Available at: https://www.bipm.org/utils/common/documents/jcgm/JCGM_100_2008_E.pdf (accessed August 2019).Google Scholar
Maskil, M. and Deutsch, M. (1988). “X-ray K alpha satellites of copper,” Phys. Rev. A 38, 3467–3472.CrossRefGoogle ScholarPubMed
Mendenhall, M. H., Mullen, K., and Cline, J. P. (2015). “An implementation of the fundamental parameters approach for analysis of X-ray powder diffraction line profiles,” J. Res. Natl. Inst. Stand. Technol. 120, 223–251.CrossRefGoogle ScholarPubMed
NCNR (2019). https://www.ncnr.nist.gov/resources/activation/ (accessed December 2019).Google Scholar
Pawley, G. S. (1981). “Unit-cell refinement from powder diffraction scans,” J. Appl. Cryst. 14, 357–361.CrossRefGoogle Scholar
Sirota, N. N., Novikov, V. V., Vinokrov, V. A., and Paderno, Y. B. (1998). “Temperature dependence of heat capacity and lattice constant of lanthanum and samarium hexaborides,” Phys. Solid State 40(11), 1856–1858.CrossRefGoogle Scholar
Taylor, B. N. and Kuyatt, C. E. (1994). “Guidelines for evaluating and expressing the uncertainty of NIST measurement results,” NIST Technical Note 1297; U.S. Government Printing Office (Washington, DC). Available at: https://www.nist.gov/pml/nist-technical-note-1297 (accessed August 2019).Google Scholar
Wang, J., Toby, B. H., Lee, P. L., Ribaud, L., Antao, S. M., Kurtz, C., Ramanathan, M., Von Dreele, R. B., and Beno, M. A. (2008). “A dedicated powder diffraction beamline at the Advanced Photon Source: commissioning and early operational results,” Rev. Sci. Instrum. 79, 085105.CrossRefGoogle ScholarPubMed