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Local Porosity Measurement From Scanning Electron Microscopy Images in the Backscattered Electrons Mode.

Loïc Sorbier1, Hedwige Poncet1, Vincent Lecocq1

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Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
|December 3, 2020
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This study introduces a new method using scanning electron microscopy to accurately measure local porosity in materials. The technique, validated against mercury intrusion porosimetry, reveals porosity fluctuations linked to material preparation.

Keywords:
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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Chemical Engineering

Background:

  • Accurate porosity measurement is crucial for understanding material properties.
  • Heterogeneous porous materials present challenges for traditional characterization methods.
  • Scanning electron microscopy (SEM) offers high-resolution imaging but requires robust quantification techniques for porosity.

Purpose of the Study:

  • To develop and validate a novel method for measuring local porosity in porous samples using SEM backscattered electron imaging.
  • To quantify porosity fluctuations in heterogeneous materials and correlate them with preparation parameters.
  • To provide a reliable alternative or complement to mercury intrusion porosimetry for porosity assessment.

Main Methods:

  • Porous samples were impregnated with polymer resin and analyzed using SEM in backscattered electron mode.
  • Image intensities were calibrated using pure resin and bulk phase signals.
  • A calibration model was validated using Monte Carlo simulations on virtual samples.
  • Uncertainties in porosity measurements were analyzed based on physical properties and signal variations.

Main Results:

  • The proposed SEM method accurately measures local porosity in heterogeneous alumina catalyst supports.
  • A good agreement was observed between averaged local porosity (SEM) and global porosity (mercury intrusion porosimetry).
  • Local porosity statistics successfully characterized porosity fluctuations, linking them to material preparation methods.

Conclusions:

  • The developed SEM-based method provides a quantitative and reliable approach for local porosity determination.
  • This technique is effective for characterizing heterogeneous porous materials like catalyst supports.
  • Understanding local porosity variations can inform material design and optimize preparation processes.