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Related Concept Videos

X-ray Diffraction of Biological Samples01:10

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X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
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The Certification of Standard Reference Material 1979: Powder Diffraction Line Profile Standard for Crystallite Size

James P Cline1, Marcus H Mendenhall1, Joseph J Ritter1,2

  • 1National Institute of Standards and Technology, Gaithersburg, MD 20899 USA.

Journal of Research of the National Institute of Standards and Technology
|July 31, 2024
PubMed
Summary
This summary is machine-generated.

A new National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) provides certified crystallite sizes for zinc oxide powders. This material aids in analyzing powder diffraction line profile broadening for accurate nanomaterial characterization.

Keywords:
Standard Reference Materialcrystallite sizeline profile analysis

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Area of Science:

  • Materials Science
  • Crystallography
  • Nanotechnology

Background:

  • Powder diffraction is crucial for determining crystallite size, but accurate analysis requires reliable standards.
  • Line profile broadening in diffraction patterns is influenced by factors like crystallite size, stacking faults, and microstrain.
  • Existing methods for crystallite size analysis can present challenges in background determination and model-dependent interpretations.

Purpose of the Study:

  • To develop and certify a Standard Reference Material (SRM) for accurate crystallite size analysis using powder diffraction.
  • To provide well-characterized zinc oxide (ZnO) powders with distinct crystallite sizes for method validation.
  • To compare crystallite size results obtained from model-independent Fourier transform methods and fundamental parameters approach.

Main Methods:

  • Development of two ZnO powders with mean crystallite sizes around 15 nm and 60 nm.
  • Data collection using a high-resolution powder diffractometer at the Advanced Photon Source and a laboratory diffractometer.
  • Application of a modified two-step profile fitting procedure for Fourier transform extraction and analysis of diffraction data.
  • Analysis using the fundamental parameters approach with various broadening models.

Main Results:

  • The NIST SRM consists of two ZnO powders exhibiting crystallite size distributions and characteristic diffraction line broadening.
  • Model-independent Fourier transform analysis yielded mean column lengths (〈L〉area and 〈L〉vol).
  • Results from the fundamental parameters approach were consistent with Fourier transform results, with minor discrepancies noted for 〈L〉area values.

Conclusions:

  • The developed SRM provides a reliable standard for crystallite size determination via powder diffraction.
  • Both Fourier transform and fundamental parameters approaches are effective for analyzing crystallite size, with the latter yielding certified lattice parameters.
  • The SRM facilitates improved accuracy and comparability in nanomaterial characterization.