The Certification of Standard Reference Material 1979: Powder Diffraction Line Profile Standard for Crystallite Size Analysis
James P. Cline, Marcus H. Mendenhall, Joseph J. Ritter, David R. Black, Albert Henins, John E. Bonevich, Pamela S. Whitfield, James J. Filliben
This rather long-standing project has resulted in a National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) for the analysis of crystallite size from a consideration of powder diffraction line profile broadening. It consists of two zinc oxide powders, one with a crystallite size distribution centered at approximately 15 nm, and a second centered at about 60 nm. These materials display the effects of stacking faults that broaden specific hkl reflections and a slight amount of microstrain broadening. Certification data were collected on the high-resolution powder diffractometer located at beamline 11-BM of the Advanced Photon Source, and on a NIST-built laboratory diffractometer equipped with a Johansson incident beam monochromator and position sensitive detector. Fourier transforms were extracted from the raw data using a modified, two-step profile fitting procedure that addressed the issue of accurate background determination. The mean column lengths, (L)area and (L)vol, were then computed from the Fourier transforms of the specimen contribution for each reflection. Data were also analyzed with fundamental parameters approach refinements using broadening models to yield (L)area and (L)vol values. These values were consistent with the model-independent Fourier transform results; however, small discrepancies were noted for the (L)area values from both machines and both crystallite size ranges. The fundamental parameters approach fits to the laboratory data yielded the certified lattice parameters.