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Atom Probe Tomography Analysis of Exsolved Mineral Phases
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Strategies for Preparing and Analyzing Thin Passive Films With Atom Probe Tomography.

Elizabeth J Kautz1,2, Kayla H Yano1, Josephine C Hartmann2

  • 1Energy and Environment Directorate, Pacific Northwest National Laboratory, Richland, WA 99352, USA.

Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
|July 24, 2025
PubMed
Summary

Atom probe tomography (APT) can now analyze thin passive films using a novel capping layer method. This technique improves elemental mapping of nanoscale surface films on alloys.

Keywords:
atom probe tomographycorrosionmultiprincipal element alloythin films

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Area of Science:

  • Materials Science
  • Surface Science
  • Analytical Chemistry

Background:

  • Atom probe tomography (APT) offers high-resolution 3D elemental and isotopic mapping, excelling at buried interfaces.
  • Analyzing thin nanoscale surface films, like passive films on alloys, presents significant challenges for APT due to sample preparation and data collection complexities.

Purpose of the Study:

  • To develop and validate sample preparation strategies for reliable APT characterization of thin passive films (∼2-5 nm thick) on alloys.
  • To overcome the limitations of applying APT to nanoscale surface films formed during alloy passivation.

Main Methods:

  • Investigated sample preparation involving deposition of a <100 nm capping layer prior to APT analysis.
  • Compared different capping layer materials (Pt, Ti, Ni/Cr bilayer) and deposition methods.
  • Utilized APT to analyze passive films on binary and multiprincipal element alloys.

Main Results:

  • A sputtered Ni/Cr bilayer capping layer enabled complete characterization of the entire passive film.
  • Concentration profiles clearly distinguished base alloy/passive film/capping layer interfaces.
  • Demonstrated reliable APT analysis of thin passive films previously difficult to study.

Conclusions:

  • A novel capping layer strategy significantly enhances APT's capability for analyzing thin passive films on alloys.
  • The sputtered Ni/Cr bilayer is identified as an effective capping material for detailed interface and composition analysis.
  • This approach opens new avenues for understanding alloy passivation mechanisms at the nanoscale.