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Related Experiment Video

Updated: Dec 13, 2025

Atom Probe Tomography Analysis of Exsolved Mineral Phases
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Aggregated nanoparticles: Sample preparation and analysis by atom probe tomography.

Cédric Barroo1, Austin J Akey2, David C Bell3

  • 1Harvard John A. Paulson School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge MA 02138, USA; Department of Chemistry and Chemical Biology, Harvard University, 12 Oxford Street, Cambridge MA 02138, USA.

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|July 31, 2020
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Summary

Atom probe tomography (APT) successfully analyzed nanoparticle aggregates, overcoming sample porosity challenges. This method ensures accurate 3D material composition analysis for synthesized nanoparticles.

Keywords:
APTAggregated nanoparticlesAtom probe tomographyCu catalystFIB sample preparation

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Area of Science:

  • Materials Science
  • Nanotechnology
  • Analytical Chemistry

Background:

  • Atom probe tomography (APT) provides 3D material structure and composition but requires specialized sample preparation.
  • Porosity in nanoparticle aggregates complicates APT analysis, affecting sample stability and data accuracy.
  • Effective sample preparation is crucial for analyzing challenging nanostructured materials with APT.

Purpose of the Study:

  • To develop and validate a robust sample preparation method for analyzing nanoparticle aggregates using APT.
  • To accurately determine the 3D structure and composition of nanoparticle aggregates.
  • To assess the purity of synthesized nanoparticles for catalyst applications.

Main Methods:

  • Nanoparticle aggregates were mounted on a micromanipulator tip.
  • Electron-beam-assisted platinum deposition was used for embedding the aggregates.
  • Focused Ion Beam (FIB) milling and further Pt depositions were employed to create suitable APT tips.

Main Results:

  • Successful preparation of nanoparticle aggregate samples for APT analysis.
  • 3D reconstruction revealed the presence of 15-20 nm nanoparticles.
  • Mass spectral analysis confirmed the absence of trace elements, validating nanoparticle synthesis quality.

Conclusions:

  • The developed APT sample preparation technique is effective for analyzing porous nanoparticle aggregates.
  • This method enables precise 3D compositional analysis of nanomaterials.
  • APT serves as a critical quality control tool for synthesizing nanoparticles with desired compositions.