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Certification of SRM 640f line position and line shape standard for powder diffraction

Published online by Cambridge University Press:  02 July 2020

David R. Black Open the ORCID record for David R. Black [Opens in a new window] ,
Marcus H. Mendenhall Open the ORCID record for Marcus H. Mendenhall [Opens in a new window] ,
Albert Henins ,
James Filliben  and
James P. Cline
David R. Black*
Affiliation:
National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
Marcus H. Mendenhall
Affiliation:
National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
Albert Henins
Affiliation:
National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
James Filliben
Affiliation:
National Institute of Standards and Technology, Gaithersburg, Maryland20899, USA
James P. Cline
Affiliation:
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 be used to evaluate specific aspects of the instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 640f, the seventh generation of this powder diffraction SRM, which is designed to be used primarily for calibrating powder diffractometers with respect to line position; it also can be used for the determination of the instrument profile function. It is certified with respect to the lattice parameter and consists of approximately 7.5 g of silicon powder prepared to minimize line broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the Si powder. Both statistical and systematic uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.5431144 ± 0.000008 nm.

Keywords

certificationdiffractometerlattice parameterStandard Reference MaterialX-ray diffraction

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Type
Technical Article
Information
Powder Diffraction , Volume 35 , Issue 3 , September 2020 , pp. 156 - 159
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Copyright
Copyright © National Institute of Standards and Technology, 2020. This is a work of the US Government and is not subject to copyright protection within the United States. Published by Cambridge University Press on behalf of International Centre for Diffraction Data

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References

BIPM (2006). International System of Units (SI) (Bureau International des Poids et Mesures), https://www.bipm.org/utils/common/pdf/si_brochure_8_en.pdf (accessed August 2019).Google Scholar
Black, D., Mendenhall, M., Brown, C., Henins, A., Filliben, J., and Cline, J. (2020). “Certification of Standard Reference Material 660c for powder diffraction,” Powd. Diffr. 35(1), 17–22. doi:10.1017/S0885715620000068CrossRefGoogle Scholar
Bruker (2017). TOPAS. Version 6. Bruker AXS, Karlsruhe, Germany, 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. (2018). “The optics, alignment and calibration of laboratory X-ray powder diffraction equipment with the use of NIST Standard Reference Materials,” in International Tables for Crystallography Volume H: Powder Diffraction, edited by C. J. Gilmore, J. A. Kaduk, and H. Schenk (Wiley, Hoboken, NJ), Chapter: 3.1.Google Scholar
EerNisse, E. P. (1979). “Stress in thermal SiO2 during growth,” Appl. Phys. Lett. 35(1), 8–10.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) (2008); https://www.bipm.org/utils/common/documents/jcgm/JCGM_100_2008_E.pdf (accessed August 2019).Google Scholar
Kessler, E. G., Henins, A., Deslattes, R. D., Nielsen, L., and Arif, M. (1994). “Precision comparison of the lattice parameters of silicon monocrystals,” J. Res. Natl. Inst. Stand. Technol. 99, 1.CrossRefGoogle Scholar
Kessler, E. G., Szabo, C. I., Cline, J. P., Henins, A., Hudson, L. T., Mendenhall, M. H., and Vaudin, M. D. (2017). “The lattice spacing variability of intrinsic float-zone silicon,” J. Res. Natl. Inst. Stand. Technol. 122, 1.CrossRefGoogle Scholar
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
Mendenhall, M. H., Henins, A., Hudson, L. T., Szabo, C. I., Windover, D., and Cline, J. P. (2017). “High-precision measurement of the X-ray Cu Kα spectrum,”J. Phys. B: At. Mol. Opt. Phys. 50, 115004.CrossRefGoogle ScholarPubMed
Mendenhall, M. H., Black, D., and Cline, J. P. (2019). “The optics of focusing bent-crystal monochromators on X-ray powder diffractometers with application to lattice parameter determination and microstructure analysis,” J. Appl. Cryst. 52, 1087–1094.CrossRefGoogle ScholarPubMed
Pawley, G. S. (1981). “Lattice parameter refinement from powder diffraction scans,” J. Appl. Cryst. 14, 357–361.CrossRefGoogle Scholar
Schödel, R. and Bönsch, G. (2001). “Precise interferometric measurements at single-crystal silicon yielding thermal expansion coefficients from 12° to 28°C and compressibility,” in Recent Developments in Traceable Dimensional Measurements (SPIE), pp. 54–62. http://doi.org/10.1117/12.445624CrossRefGoogle 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
van Berkum, J. G. M., Sprong, G. J. M., de Keijser, T. H., Delhez, R., and Sonneveld, E. J. (1995). “The optimum standard specimen for X-ray diffraction line-profile analysis,” Powd. Diff. J. 10(2), 129–139.CrossRefGoogle Scholar
Vaughn, C. D. and Strouse, G. F. (2001). “The NIST Industrial Thermometer Calibration Laboratory,” in 8th Int'l Symp. Temperature and Thermal Measurements in Industry and Science, Berlin, June 2001. Available at: http://ws680.nist.gov/publication/get_pdf.cfm?pub_id=830734 (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