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Atomic Absorption Spectroscopy: Atomization Methods01:25

Atomic Absorption Spectroscopy: Atomization Methods

Atomic Absorption Spectroscopy (AAS) atomizes samples through flame atomization or electrothermal atomization. Flame atomization typically involves a nebulizer and spray chamber assembly to combine the sample with a fuel–oxidant mixture, creating a fine aerosol mist that enters a burner. Typically, the fuel and oxidant are combined in an approximately stoichiometric ratio. However, for atoms that are easily oxidized, a fuel-rich mixture may be more advantageous. Only about 5% of the aerosol...

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Significant Oxygen Underestimation When Quantifying Barium-Doped SrTiO Layers by Atom Probe Tomography.

Richard J H Morris1, Jhao-Rong Lin1,2, Jeroen E Scheerder1

  • 1imec, Kapeldreef 75, Leuven 3001, Belgium.

Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
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PubMed
Summary

Atom probe measurements underestimated oxygen in barium-doped strontium titanate (Ba-SrTiO) layers. This occurred because oxygen and titanium ions evaporated together, skewing composition quantification.

Keywords:
atom probe tomographybarium-doped strontium titanatecomposition quantificationenergy elastic recoil diffractionoxygen underestimationperovskitesrutherford backscattering spectroscopy

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Area of Science:

  • Materials Science
  • Surface Science
  • Analytical Chemistry

Background:

  • Accurate compositional analysis of advanced materials like barium-doped strontium titanate (Ba-SrTiO) is crucial for understanding their properties.
  • Atom probe tomography (APT) is a powerful technique for nanoscale compositional mapping, but its accuracy can be affected by complex evaporation behaviors.
  • Previous studies have highlighted potential challenges in quantifying oxygen content in oxide materials using APT.

Purpose of the Study:

  • To investigate the accuracy of atom probe tomography (APT) for quantifying the composition of Ba-doped SrTiO layers.
  • To identify the reasons for discrepancies between APT measurements and benchmark compositional analyses.
  • To explore the underlying physical mechanisms responsible for potential measurement errors.

Main Methods:

  • Quantitative compositional analysis using Rutherford backscattering spectrometry (RBS) and time-of-flight/energy elastic recoil detection (ToF/E-ERD) as benchmark techniques.
  • Atom probe tomography (APT) measurements on Ba-doped SrTiO samples with varying titanium content.
  • Analysis of ion species, evaporation fields, and charge states to understand measurement artifacts.

Main Results:

  • APT measurements showed a significant underestimation of oxygen content (over 14 at.%) compared to benchmark analyses.
  • The ratio of oxygen to titanium in the samples was significantly higher (2.6–12.7) than measured by APT (1.4–1.7).
  • This discrepancy was attributed to the co-evaporation of oxygen and titanium as molecular ions, and potentially a field emission and neutral oxygen desorption process.

Conclusions:

  • Standard APT quantification methods are insufficient for accurately determining oxygen content in Ba-doped SrTiO due to complex evaporation phenomena.
  • The co-evaporation of molecular ions and potential neutral desorption significantly impacts the measured oxygen-to-titanium ratio.
  • Further investigation incorporating ion species, evaporation physics, and theoretical modeling is necessary to refine APT analysis for such materials.