Systematic procedures for atom-probe field-ion microscopy studies of grain boundary segregation

B. W. Krakauer*, David N Seidman

*Corresponding author for this work

Research output: Contribution to journalArticle

71 Citations (Scopus)

Abstract

A procedure is presented for systematically and reproducibly preparing alloy specimens for the study of grain boundary (GB) segregation employing both transmission electron (TEM) and atom-probe field-ion microscopies (APFIM) to examine the same GB; the procedure is illustrated for an Fe(Si) alloy. A commercially available oxygen plasma source is incorporated in the sample preparation procedure to remove all traces of hydrocarbon build-up introduced during TEM GB analysis, thus allowing controlled backpolishing after a TEM analysis. Specifications for the optimum tip geometry, i.e., how a GB is positioned in a tip via backpolishing to maximize the probability of its observation and subsequent compositional analysis via APFIM, are empirically determined: 30-200 nm for the GB-to-tip separation, and 40-80 nm for the GB diam for shank angles less than 20°. It is demonstrated that accurate quantitative APFIM analyses of an Fe-3 at. % Si alloy are possible for pulse fractions ≥15% and specimen temperatures ≤55 K. Results are presented for a ∑≊3a GB that was first analyzed via TEM to determine its five macroscopic degrees of freedom, and then analyzed via APFIM to measure an average GB segregation enhancement factor for Si of 3.51±0.34 at 823 K.

Original languageEnglish (US)
Pages (from-to)4071-4079
Number of pages9
JournalReview of Scientific Instruments
Volume63
Issue number9
DOIs
StatePublished - Dec 1 1992

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Microscopic examination
Grain boundaries
grain boundaries
microscopy
Atoms
probes
Ions
atoms
ions
Transmission electron microscopy
transmission electron microscopy
joints (junctions)
Plasma sources
oxygen plasma
specifications
hydrocarbons
degrees of freedom
Hydrocarbons
Specifications
preparation

ASJC Scopus subject areas

  • Instrumentation
  • Physics and Astronomy (miscellaneous)

Cite this

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title = "Systematic procedures for atom-probe field-ion microscopy studies of grain boundary segregation",
abstract = "A procedure is presented for systematically and reproducibly preparing alloy specimens for the study of grain boundary (GB) segregation employing both transmission electron (TEM) and atom-probe field-ion microscopies (APFIM) to examine the same GB; the procedure is illustrated for an Fe(Si) alloy. A commercially available oxygen plasma source is incorporated in the sample preparation procedure to remove all traces of hydrocarbon build-up introduced during TEM GB analysis, thus allowing controlled backpolishing after a TEM analysis. Specifications for the optimum tip geometry, i.e., how a GB is positioned in a tip via backpolishing to maximize the probability of its observation and subsequent compositional analysis via APFIM, are empirically determined: 30-200 nm for the GB-to-tip separation, and 40-80 nm for the GB diam for shank angles less than 20°. It is demonstrated that accurate quantitative APFIM analyses of an Fe-3 at. {\%} Si alloy are possible for pulse fractions ≥15{\%} and specimen temperatures ≤55 K. Results are presented for a ∑≊3a GB that was first analyzed via TEM to determine its five macroscopic degrees of freedom, and then analyzed via APFIM to measure an average GB segregation enhancement factor for Si of 3.51±0.34 at 823 K.",
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Systematic procedures for atom-probe field-ion microscopy studies of grain boundary segregation. / Krakauer, B. W.; Seidman, David N.

In: Review of Scientific Instruments, Vol. 63, No. 9, 01.12.1992, p. 4071-4079.

Research output: Contribution to journalArticle

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