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Related Experiment Video

Updated: Nov 12, 2025

In Situ Detection and Single Cell Quantification of Metal Oxide Nanoparticles Using Nuclear Microprobe Analysis
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Low-Voltage Electron-Probe Microanalysis of Uranium.

Mike B Matthews1,2, Stuart L Kearns2, Ben Buse2

  • 1AWE, Aldermaston, ReadingRG7 4PR, UK.

Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
|March 18, 2021
PubMed
Summary
This summary is machine-generated.

Electron-probe microanalysis of uranium (U) requires careful correction for surface oxidation and carbon coating. Addressing these issues significantly improves quantification accuracy, especially at lower accelerating voltages.

Keywords:
EPMAcarbonmass absorption coefficienturanium

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Nuclear Materials

Background:

  • Electron-probe microanalysis (EPMA) of uranium (U) and its alloys is challenging due to rapid oxidation and complex X-ray spectra.
  • Surface oxidation of U-metal can reach 15–20 nm within minutes, causing significant quantification errors (~30% at 5 kV).

Purpose of the Study:

  • To investigate and quantify the errors in EPMA of uranium due to surface oxidation and carbon coating.
  • To develop and validate correction strategies for accurate U analysis.

Main Methods:

  • Electron-probe microanalysis (EPMA) was employed to analyze uranium metal and UO2 reference materials.
  • Simulations and experimental measurements were used to assess the impact of oxide layers and carbon coatings on quantification.
  • Correction factors for oxide layers and carbon coatings were applied and evaluated.

Main Results:

  • U-metal oxidation forms a ~10 nm oxide layer in ~20 s, increasing to 15–20 nm, leading to ~30% quantification error at 5 kV.
  • A 15 nm carbon coating on UO2 reference material caused ~30% error for oxidized U samples at 5 kV.
  • Applying corrections for both oxide and coating improved accuracy to <±1% down to 7 kV and ~2% at 5 kV.
  • A previously unreported U N6–O4 line interference on the C Kα peak was identified, causing >1% error.

Conclusions:

  • Accurate EPMA of uranium necessitates corrections for both surface oxidation and carbon coatings.
  • The developed correction methods significantly enhance quantification accuracy, particularly at lower accelerating voltages.
  • Interference from uranium X-ray lines on light element peaks must be considered for precise analysis.