A Combination Method of Charge Density Measurement in Hard Materials Using Accurate, Quantitative Electron and X-ray Diffraction: The α-Al 2O3 Case

Victor A. Streltsov, Philip N.H. Nakashima, Andrew W.S. Johnson

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14 Citations (Scopus)

Abstract

Current X-ray diffraction techniques intended for "ideally imperfect" specimens provide structure factors only on a relative scale and ever-present multiple scattering in strong low-angle Bragg reflections is difficult to correct. Multiple scattering is implicit in the quantitative convergent beam electron diffraction (QCBED) method, which provides absolutely scaled structure factors. Conventional single crystal X-ray diffraction has proved adequate in softer materials where crystal perfection is limited. In hard materials, the highly perfect nature of the crystals is often a difficulty, due to the inadequacy of the conventional corrections for multiple scattering (extinction corrections). The present study on α-Al2O 3 exploits the complementarity of synchrotron X-ray measurements for weak and medium intensities and QCBED measurement of the strong low-angle reflections. Two-dimensional near zone axis QCBED data from different crystals at various accelerating voltages, thicknesses, and orientations have been matched using Bloch-wave and multislice methods. The reproducibility of QCBED data is better than 0.5%. The low-angle strong QCBED structure factors were combined with middle and high-angle extinction-free data from synchrotron X-ray diffraction measurements. Static deformation charge density maps for α-Al2O3 have been calculated from a multipole expansion model refined using the combined QCBED and X-ray data.

Original languageEnglish
Pages (from-to)419-427
Number of pages9
JournalMicroscopy and Microanalysis
Volume9
Issue number5
DOIs
Publication statusPublished - 1 Oct 2003
Externally publishedYes

Keywords

  • α-AlO
  • Corundum
  • Electron charge density
  • Quantitative convergent beam electron diffraction
  • synchrotron X-ray diffraction

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