Hostname: page-component-77c89778f8-swr86 Total loading time: 0 Render date: 2024-07-17T16:05:23.007Z Has data issue: false hasContentIssue false
  • English
  • Français

The optimum standard specimen for X-ray diffraction line-profile analysis

Published online by Cambridge University Press:  10 January 2013

J. G. M. van Berkum ,
G. J. M. Sprong ,
Th. H. de Keijser ,
R. Delhez  and
E. J. Sonneveld
J. G. M. van Berkum
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
G. J. M. Sprong
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
Th. H. de Keijser
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
R. Delhez
Affiliation:
Delft University of Technology, Laboratory of Materials Science, Rotterdamseweg 137, 2628 AL Delft, The Netherlands
E. J. Sonneveld
Affiliation:
TNO Plastics and Rubber Research Institute, P.O. Box 6031, 2600 JA Delft, The Netherlands
Get access Rights & Permissions [Opens in a new window]

Abstract

A perfect general purpose standard specimen for high accuracy line-profile analysis is shown to be an illusion. Balancing the partly contradictory requirements, an optimum standard specimen for a parafocusing diffractometer is developed. To obtain the optimum standard specimen, a 5–10 μm particle size fraction is taken from the NIST certified Si powder SRM640a, about 1.5 mg/cm2 of this powder is uniformly deposited on a (510) oriented Si single-crystal wafer and the assembly is heat treated for 2 h at 1273 K to remove lattice imperfections. All procedures necessary are precisely given, easily applicable, and reproducing. For the present standard specimens, the random errors due to crystal statistics are quantified and shown to be acceptable for spinning specimens; the systematic errors due to residual size and transparency broadening are determined semi-empirically and can be eliminated, if desired. Thus the proposed optimum standard specimen allows the determination of instrumental line profiles free from systematic errors and with random errors in the line width of the order of 0.001 °2θ, allowing a full use of the capacities of modern diffractometers and data evaluation procedures.

Keywords

powder diffractioninstrumental broadeningstandard specimenline-profile accuracycrystal statistics
Type
Research Article
Information
Powder Diffraction , Volume 10 , Issue 2 , June 1995 , pp. 129 - 139
Copyright
Copyright © Cambridge University Press 1995

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Adler, T., and Houska, C.R. (1979). “Simplifications in the X-Ray Line-Shape Analysis,” J. Appl. Phys. 50, 3282–3287.CrossRefGoogle Scholar
Alexander, L., Klug., H.P., and Kummer, E. (1948). “Statistical Factors Affecting the Intensity of X-Rays Diffracted by Crystalline Powders,” J. Appl. Phys. 19, 742–753.CrossRefGoogle Scholar
Allen, T. (1990). Particle Size Measurement (Chapman and Hall, London), 4th ed., Chap. 7.CrossRefGoogle Scholar
Delhez, R., and Mittemeijer, E.J. (1975). “An Improved α 2 Elimination,” J. Appl. Cryst. 8, 609–611.CrossRefGoogle Scholar
Fawcett, T.G., Crowder, C.E., Brownell, S.J., Zhang, Y., Hubbard, C., Schreiner, W., Hamill, G.P., Huang, T.C., Sabino, E., Langford, J.I., Hamilton, R., and Louër, D. (1988). “Establishing an Instrumental Peak Profile Calibration Standard for Powder Diffraction Analyses: International Round Robin Conducted by the JCPDS-ICDD and the U.S. National Bureau of Standards,” Powder Diffr. 3, 209–218.CrossRefGoogle Scholar
Hubbard, C.R. (1983). “Certification of Si Powder Diffraction Standard Reference Material 640a,” J. Appl. Cryst. 16, 285–288.CrossRefGoogle Scholar
Klug, H.P., and Alexander, L.E. (1974). X-ray Diffraction Procedures (Wiley, New York), 2nd ed., p. 367.Google Scholar
Kogan, V.A., and Kupriyanov, M.F. (1992). “X-Ray Powder Diffraction Line Profiles by Fourier Synthesis,” J. Appl. Cryst. 25, 16–25.CrossRefGoogle Scholar
Kurita, M. (1981). “Simplified Equations for Peak Position and for Its Standard Deviation in X-Ray Stress Measurement,” J. Test. Eval. 9, 133–140.CrossRefGoogle Scholar
Parrish, W., and Huang, T.C. (1980). “Accuracy of the Profile Fitting Method for X-ray Polycrystalline Diffractometry,” in Accuracy in Powder Diffraction, NBS Special Publication 567, edited by Block, S. and Hubbard, C.R. (U.S. Government Printing Office, Washington), p. 98.Google Scholar
Sterling, T.D., and Pollack, S.V. (1968). Introduction to Statistical Data Processing (Prentice-Hall, Englewood Cliffs, New York), p. 355.Google Scholar
Stokes, A.R. (1948). “A Numerical Fourier-analysis Method for the Correction of Widths and Shapes of Lines on X-Ray Powder Photographs,” Proc. Phys. Soc. Lond. 61, 382–391.CrossRefGoogle Scholar
Timmers, J., Delhez, R., Tuinstra, F., and Peerdeman, F. (1992a). “X-ray Tracing, a Tool for Improved Accuracy in Powder Diffractometry,” in Accuracy in Powder Diffraction II, NIST Special Publication 846, edited by Prince, E. and Stalick, J.K. (U.S. Government Printing Office, Washington), p. 217.Google Scholar
Timmers, J., Pers, N.M. van der, Sprang, G.J.M., Keijser, Th.H. de, and Delhez, R. (1992b). “Notes on Slits and Monochromators in Accurate Powder Diffractometry,” Powder Diffr. 7, 83–88.CrossRefGoogle Scholar
Warren, B.E. (1969). X-ray Diffraction (Addison-Wesley, Reading, MA), p. 271.Google Scholar
Wilson, A.J.C. (1963). Mathematical Theory of Powder Diffractometry (Centrex, Eindhoven), p. 24.Google Scholar
Wilson, A.J.C. (1967). “Statistical Variance of Line-Profile Parameters. Measures of Intensity, Location and Dispersion,” Acta Cryst. 23, 888–898.CrossRefGoogle Scholar
Wolff, P.M. de (1958). “Particle Statistics in X-Ray Diffractometry,” Appl. Sci. Res. 7, 102–112.CrossRefGoogle Scholar
Wolff, P. M. de, Taylor, J. M., and Parrish, W. (1959). “Experimental Study of Effect of Crystallite Size Statistics on X-Ray Diffractometer Intensities,” J. Appl. Phys. 30, 63–69.CrossRefGoogle Scholar