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TEM-EDS microanalysis: Comparison between different electron sources, accelerating voltages and detection systems.

Roberto Conconi1, María Del Mar Abad Ortega2, Fernando Nieto3

  • 1Department of Earth and Environmental Sciences, University of Milano-Bicocca, Piazza della Scienza 4, Milano 2016, Italy; Université de Lille, CNRS, INRAE, Centrale Lille, UMR 8207-UMET-Unité Matériaux et Transformations, Lille F-59000, France.

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Summary
This summary is machine-generated.

Transmission electron microscopy-energy dispersive spectroscopy (TEM-EDS) calibration is instrument-specific. Different TEMs and EDS systems yield unique k-factors, impacting elemental quantification accuracy.

Keywords:
Absorption correctionEnergy dispersive spectroscopyTransmission electron microscopyX-ray microanalysis

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Microscopy

Background:

  • Accurate elemental quantification using Transmission Electron Microscopy with Energy Dispersive Spectroscopy (TEM-EDS) is crucial for materials analysis.
  • Existing quantification methods, such as the Cliff and Lorimer approximation and absorption correction, rely on accurate calibration and k-factors.
  • Variations in Transmission Electron Microscopy (TEM) instruments and Energy Dispersive Spectroscopy (EDS) systems can affect quantification results.

Purpose of the Study:

  • To compare the performance of two TEM-EDS quantification methods: Cliff and Lorimer approximation and absorption correction.
  • To evaluate the influence of different TEM instruments (source type, accelerating voltage) and EDS systems (4-in-column vs. single SDD) on quantification results.
  • To determine the specificity of k-factors for different instrument and EDS system combinations.

Main Methods:

  • Employed two quantitative methods: Cliff and Lorimer approximation and absorption correction based on electroneutrality.
  • Conducted analyses using three distinct TEMs with varying source types (field emission vs. thermionic) and accelerating voltages (200 vs. 300 kV).
  • Utilized both 4-in-column silicon drift detector (SDD) and single SDD systems for EDS analysis.

Main Results:

  • EDS calibration is strictly instrument-specific; universally valid k-factors do not exist, necessitating system-specific k-factor sets.
  • 4-in-column SDD systems demonstrate higher efficiency and lower detection limits due to larger sensitive areas compared to single SDDs.
  • Field Emission Gun TEMs (FEG-TEMs) showed reduced radiation-induced migration of weakly bonded elements compared to conventional sources, attributed to smaller spot sizes and lower electron dose per atom.

Conclusions:

  • The absorption correction method is recommended for thick and/or dense samples, while the Cliff and Lorimer approximation is suitable for simpler, faster analyses in other cases.
  • The study highlights the necessity of determining distinct kO/Si factors for lighter and denser compounds.
  • Accurate elemental quantification in TEM-EDS requires careful consideration of instrument-specific parameters and appropriate method selection.