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X-Ray Microanalysis in the Variable Pressure (Environmental) Scanning Electron Microscope.

Dale E Newbury1

  • 1National Institute of Standards and Technology, Gaithersburg, MD 20899-8371.

Journal of Research of the National Institute of Standards and Technology
|July 23, 2016
PubMed
Summary
This summary is machine-generated.

Environmental scanning electron microscopy (ESEM) can introduce artifacts in electron-excited x-ray microanalysis due to gas scattering. These artifacts can lead to inaccurate elemental quantification, especially in fine microstructures.

Keywords:
energy dispersive x-ray spectrometryenvironmental scanning electron microscopy (ESEM)variable pressure scanning electron microscopy (VP-SEM)x-ray mappingx-ray microanalysisx-ray spectrometry

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Microscopy

Background:

  • Conventional scanning electron microscopy (SEM) is susceptible to artifacts in electron-excited x-ray microanalysis.
  • Variable pressure and environmental scanning electron microscopes (VP-ESEM) introduce additional complexities due to gas scattering.
  • Gas scattering can lead to direct spectral contributions from the environmental gas and remote x-ray generation.

Purpose of the Study:

  • To identify and characterize artifacts in electron-excited x-ray microanalysis within VP-ESEM.
  • To quantify the impact of gas scattering on elemental analysis accuracy.
  • To provide strategies for mitigating these artifacts.

Main Methods:

  • Utilized variable pressure and environmental scanning electron microscopes for x-ray microanalysis.
  • Investigated the effects of gas scattering on x-ray spectra.
  • Analyzed the influence of sample morphology (dispersed particles vs. fine microstructures) on artifact severity.
  • Developed and applied specimen preparation and spectral processing techniques.

Main Results:

  • Gas scattering causes spurious elemental signals, ranging from trace to major levels (< 0.01 to > 0.1 mass fraction).
  • Fine microstructures are more severely compromised by these artifacts than dispersed particle samples.
  • Artifacts manifest as both direct gas contributions and remote x-ray generation.
  • Optimized procedures can reduce the impact of spurious signals.

Conclusions:

  • Electron-excited x-ray microanalysis in VP-ESEM requires careful consideration of gas scattering artifacts.
  • Specimen preparation and spectral processing are crucial for accurate elemental quantification.
  • Understanding and controlling these artifacts are essential for reliable microanalysis, particularly in complex microstructures.