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

Published online by Cambridge University Press:  17 October 2016

David R. Diercks ,
Brian P. Gorman  and
Johannes J. L. Mulders
David R. Diercks*
Affiliation:
Department of Metallurgical and Materials Engineering, Colorado School of Mines, Golden, CO 80401, USA
Brian P. Gorman
Affiliation:
Department of Metallurgical and Materials Engineering, Colorado School of Mines, Golden, CO 80401, USA
Johannes J. L. Mulders
Affiliation:
FEI Electron Optics, 5600 KA Eindhoven, The Netherlands
*
*Corresponding author.ddiercks@mines.edu
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Abstract

Six precursors were evaluated for use as in situ electron beam-induced deposition capping layers in the preparation of atom probe tomography specimens with a focus on near-surface features where some of the deposition is retained at the specimen apex. Specimens were prepared by deposition of each precursor onto silicon posts and shaped into sub-70-nm radii needles using a focused ion beam. The utility of the depositions was assessed using several criteria including composition and uniformity, evaporation behavior and evaporation fields, and depth of Ga+ ion penetration. Atom probe analyses through depositions of methyl cyclopentadienyl platinum trimethyl, palladium hexafluoroacetylacetonate, and dimethyl-gold-acetylacetonate [Me2Au(acac)] were all found to result in tip fracture at voltages exceeding 3 kV. Examination of the deposition using Me2Au(acac) plus flowing O2 was inconclusive due to evaporation of surface silicon from below the deposition under all analysis conditions. Dicobalt octacarbonyl [Co2(CO)8] and diiron nonacarbonyl [Fe2(CO)9] depositions were found to be effective as in situ capping materials for the silicon specimens. Their very different evaporation fields [36 V/nm for Co2(CO)8 and 21 V/nm for Fe2(CO)9] provide options for achieving reasonably close matching of the evaporation field between the capping material and many materials of interest.

Keywords

electron beam-induced depositionatom probe tomographyevaporation fielddicobalt octacarbonyldiiron nonacarbonyl
Type
New Approaches and Correlative Microscopy
Information
Microscopy and Microanalysis , Volume 23 , Special Issue 2: Atom Probe Tomography & Microscopy 2016 , April 2017 , pp. 321 - 328
Copyright
© Microscopy Society of America 2016 

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