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Synergy between transmission electron microscopy and powder diffraction: application to modulated structures.

Dmitry Batuk1, Maria Batuk1, Artem M Abakumov1

  • 1EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp, Belgium.

Acta Crystallographica Section B, Structural Science, Crystal Engineering and Materials
|April 2, 2015
PubMed
Summary
This summary is machine-generated.

Solving crystal structures of modulated compounds is difficult, especially with only powder samples. Combining transmission electron microscopy (TEM) with powder diffraction offers a powerful solution for detailed structural analysis.

Keywords:
anion-deficient perovskitesmodulated structurespowder diffractiontransmission electron microscopy

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Area of Science:

  • Materials Science
  • Crystallography
  • Solid-State Chemistry

Background:

  • Determining crystal structures of modulated compounds is challenging, particularly for polycrystalline materials.
  • Single-crystal X-ray crystallography is often insufficient for complex, non-single-crystal samples.

Purpose of the Study:

  • To demonstrate the efficacy of combining transmission electron microscopy (TEM) and powder diffraction for crystal structure solution.
  • To showcase how local structural information from TEM aids powder diffraction refinement.

Main Methods:

  • Utilized various transmission electron microscopy (TEM) techniques including electron diffraction (SAED, PED) and advanced imaging (HRTEM, HAADF-STEM, ABF-STEM).
  • Applied state-of-the-art spectroscopic methods like energy-dispersive X-ray analysis (EDX) and electron energy loss spectroscopy (EELS) for atomic resolution mapping.
  • Integrated TEM-derived local structural data with powder diffraction data for crystal structure refinement.

Main Results:

  • Successfully obtained detailed local structural information from anion-deficient perovskites using diverse TEM methods.
  • Demonstrated the successful refinement of crystal structures against powder diffraction data by incorporating TEM insights.
  • Showcased the complementary nature of TEM and powder diffraction for complex modulated materials.

Conclusions:

  • The combined approach of TEM and powder diffraction is a viable and powerful strategy for solving crystal structures of modulated compounds, especially those lacking single crystals.
  • TEM provides crucial local structural details that significantly enhance the accuracy and completeness of crystal structure determination from powder diffraction data.