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Electron Beam-Induced Deposition for Atom Probe Tomography Specimen Capping Layers.

David R Diercks1, Brian P Gorman1, Johannes J L Mulders2

  • 11Department of Metallurgical and Materials Engineering,Colorado School of Mines,Golden,CO 80401,USA.

Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada
|October 18, 2016
PubMed
Summary

Dicobalt octacarbonyl and diiron nonacarbonyl are effective in situ capping layers for atom probe tomography silicon specimens. These precursors offer tunable evaporation fields, crucial for preserving near-surface features during analysis.

Keywords:
atom probe tomographydicobalt octacarbonyldiiron nonacarbonylelectron beam-induced depositionevaporation field

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Area of Science:

  • Materials Science
  • Nanotechnology
  • Surface Science

Background:

  • In situ electron beam-induced deposition (EBID) is vital for preparing atom probe tomography (APT) specimens.
  • Capping layers are essential for preserving near-surface features during APT analysis.
  • Evaluating precursor effectiveness for EBID capping is critical for optimizing specimen preparation.

Purpose of the Study:

  • To evaluate six precursors for in situ EBID capping layers in APT specimen preparation.
  • To assess the utility of these depositions, focusing on near-surface feature retention at the specimen apex.
  • To identify effective capping materials that minimize specimen damage and enhance APT analysis.

Main Methods:

  • Six precursors were deposited onto silicon posts using EBID.
  • Specimens were shaped into sub-70-nm radii needles using focused ion beam (FIB) milling.
  • Depositions were assessed based on composition, uniformity, evaporation behavior, evaporation fields, and Ga+ ion penetration depth.

Main Results:

  • Methyl cyclopentadienyl platinum trimethyl, palladium hexafluoroacetylacetonate, and dimethyl-gold-acetylacetonate [Me2Au(acac)] resulted in tip fracture above 3 kV.
  • Me2Au(acac) with O2 was inconclusive due to underlying silicon evaporation.
  • Dicobalt octacarbonyl [Co2(CO)8] and diiron nonacarbonyl [Fe2(CO)9] proved effective capping materials.
  • Co2(CO)8 and Fe2(CO)9 exhibit distinct evaporation fields (36 V/nm and 21 V/nm, respectively), offering flexibility in matching specimen material evaporation fields.

Conclusions:

  • Dicobalt octacarbonyl and diiron nonacarbonyl are suitable in situ capping materials for APT of silicon specimens.
  • The differing evaporation fields of Co2(CO)8 and Fe2(CO)9 provide valuable options for optimizing APT analysis.
  • Effective capping layers are crucial for high-resolution analysis of near-surface features in APT.