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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Microscopy

Background:

  • Quantitative elemental composition mapping in transmission electron microscopy (TEM) traditionally relies on separate analytical techniques like EDX and EELS.
  • The choice of technique often depends on the elements present and available calibrations, limiting comprehensive analysis.
  • A unified framework for simultaneous EDX and EELS analysis to derive absolute concentrations without prior sample assumptions is lacking.

Purpose of the Study:

  • To develop a novel experimental approach and hardware configuration for the combined quantitative analysis of elemental compositions using EDX and EELS signals.
  • To reduce the reliance on estimated parameters such as densities, thicknesses, and ionization cross-sections for accurate elemental quantification.
  • To establish a method for deriving absolute volumetric concentrations of light and heavy elements in samples.

Main Methods:

  • Implementation of a combined hardware setup for simultaneous EDX and EELS data acquisition in TEM.
  • Development of an experimental approach utilizing calibrations on known specimens to measure inelastic mean free paths.
  • Leveraging EDX ζ-factor analysis to determine mass-thicknesses, which are then used to derive EELS cross-sections and elemental concentrations.

Main Results:

  • Successful integration of EDX and EELS signals for quantitative elemental mapping.
  • Reduced need for pre-existing knowledge of sample properties like density and thickness.
  • Accurate determination of elemental concentrations and partial energy-differential ionization cross-sections.
  • Enabling the conversion of EDX ζ-factors to EELS cross-sections and vice versa for a unified quantitative approach.

Conclusions:

  • The developed framework effectively combines EDX and EELS for accurate quantitative elemental analysis in TEM.
  • This approach overcomes limitations of individual techniques and reduces the need for extensive sample-specific parameter estimations.
  • The method provides a powerful tool for precise elemental mapping, particularly beneficial for light and heavy element analysis.