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Related Concept Videos

X-ray Crystallography02:18

X-ray Crystallography

The size of the unit cell and the arrangement of atoms in a crystal may be determined from measurements of the diffraction of X-rays by the crystal, termed X-ray crystallography.
Diffraction
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In the late 1800s, the revelation that light extended beyond visible wavelengths led to the discovery of X-rays by Wilhelm Roentgen. Recognized as high-energy electromagnetic radiation with short wavelengths, X-rays prompted exploration into their interaction with crystals. Max von Laue proposed in 1912 that the periodic arrangement of atoms, ions, or molecules in crystals would cause them to diffract X-rays, a hypothesis confirmed through experiments with copper sulfate and zinc sulfide...
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A scanning electron microscope (SEM) is used to study the surface features of a sample by using an electron beam that scans the sample surface in a two-dimensional manner. Typically, areas between ~1 centimeter to 5 micrometers in width can be imaged. SEM can be used to image bacteria, viruses, tissues as well as larger samples like insects. Conventional SEM gives a magnification ranging from 20X to 30,000X and spatial resolution of 50 to 100 nanometers.
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Quantitative Atomic-Site Analysis of Functional Dopants/Point Defects in Crystalline Materials by Electron-Channeling-Enhanced Microanalysis
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A quantitative analysis of the cone-angle dependence in precession electron diffraction.

J Ciston1, B Deng, L D Marks

  • 1Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208, USA. j-ciston@northwestern.edu

Ultramicroscopy
|September 15, 2007
PubMed
Summary

Precession electron diffraction (PED) optimizes charge density measurements in andalusite. Increasing the precession angle reduces unwanted reflections but can obscure subtle charge density effects.

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Area of Science:

  • Crystallography
  • Materials Science
  • Electron Microscopy

Background:

  • Precession electron diffraction (PED) is a valuable technique for simplifying electron diffraction analysis.
  • It offers a way to mitigate dynamical scattering issues inherent in traditional methods.
  • Understanding optimal parameters is crucial for maximizing PED's utility.

Purpose of the Study:

  • To systematically investigate the impact of precession angle on PED patterns.
  • To determine optimal conditions for observing kinematically forbidden reflections.
  • To assess the best settings for measuring valence charge density in andalusite.

Main Methods:

  • Performed a systematic study varying the precession semiangle from 6.5 to 32 mrad in five steps.
  • Analyzed andalusite samples using precession electron diffraction.
  • Quantified the decay of kinematically forbidden reflections with increasing precession angle.

Main Results:

  • Intensities of kinematically forbidden reflections exhibit exponential decay as precession semiangle increases.
  • Charge density effects are most clearly observed at moderate precession angles (6.5-13 mrad).
  • Higher precession angles lead to more kinematical diffraction patterns.

Conclusions:

  • Optimal precession angles balance the reduction of dynamical scattering with the visibility of charge density information.
  • Moderate precession angles are recommended for accurate valence charge density measurements using PED.
  • PED is a powerful tool for crystallographic studies, with careful parameter selection enhancing its capabilities.