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Quantitative Atomic-Site Analysis of Functional Dopants/Point Defects in Crystalline Materials by Electron-Channeling-Enhanced Microanalysis
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High sensitivity X-ray analysis for a low accelerating voltage scanning electron microscope using a transition edge

Keiichi Tanaka1, Akira Takano1, Atsushi Nagata1

  • 1Electron Beam Systems Design Dept., Hitachi High-Tech Corporation, Hitachinaka, 312-8504, Japan.

Microscopy (Oxford, England)
|May 27, 2020
PubMed
Summary

A new scanning electron microscope transition edge sensor offers high-energy resolution and improved detection limits for analyzing minor sample constituents. This advanced sensor enables precise elemental analysis even for trace elements, enhancing material science research.

Keywords:
X-ray analysiselectron microscopeenergy-dispersive spectrometrysuperconducting

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Physics

Background:

  • Traditional electron microscopy struggles with analyzing trace elements due to limited spatial resolution and sensitivity.
  • Low accelerating voltages in scanning electron microscopy (SEM) improve surface analysis resolution by limiting electron diffusion.
  • Transition edge sensors (TES) offer high energy resolution for X-ray spectroscopy.

Purpose of the Study:

  • To develop and characterize a novel scanning electron microscope transition edge sensor (SEM-TES) for analyzing minor and trace constituents in bulk samples and small particles.
  • To leverage low accelerating voltage SEM (<3 keV) for enhanced spatial resolution in elemental analysis.
  • To improve the sensitivity, energy resolution, and operational stability of X-ray detectors for trace element analysis.

Main Methods:

  • Utilized a scanning electron microscope equipped with a transition edge sensor (TES).
  • Operated the system at low accelerating voltages (<3 keV) to enhance spatial resolution.
  • Employed a cryogen-free dilution refrigerator for continuous operation.
  • Implemented thin X-ray film windows to improve transmission efficiency for specific elements (e.g., B-Kα).

Main Results:

  • Achieved high energy resolution of 7.2 eV at Al-Kα.
  • Demonstrated stable operation with peak shift stabilization within 1 eV for Nd-Mα over 27,000 seconds.
  • Improved transmission efficiency for B-Kα by approximately 30 times compared to previous systems.
  • Established detection limits for B-Kα as low as 0.038 wt% at 27,000 seconds.
  • Successfully separated Si-Kα and W-Mα lines, even with a peak intensity ratio of 0.01, demonstrating excellent peak separation ability.

Conclusions:

  • The developed SEM-TES system provides high-energy resolution and exceptional sensitivity for trace element analysis.
  • The system's stability and improved detection limits enable precise characterization of minor constituents in various samples.
  • The ability to resolve closely spaced X-ray lines, like Si-Kα and W-Mα, highlights the sensor's effectiveness in complex elemental analysis.