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Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
Surface and interface analysis, 2012-03, Vol.44 (3), p.377-387
Christien, F.
Downing, C.
Moore, K. L.
Grovenor, C. R. M.
2012
Details
Autor(en) / Beteiligte
Christien, F.
Downing, C.
Moore, K. L.
Grovenor, C. R. M.
Titel
Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
Ist Teil von
Surface and interface analysis, 2012-03, Vol.44 (3), p.377-387
Ort / Verlag
Chichester, UK: John Wiley & Sons, Ltd
Erscheinungsjahr
2012
Link zum Volltext
Quelle
Wiley Online Library Journals Frontfile Complete
Beschreibungen/Notizen
A technique for the quantification of equilibrium grain boundary segregation by high resolution secondary ion mass spectroscopy (NanoSIMS) on simple metallographically polished surfaces has been demonstrated for the model system of sulphur segregation to nickel grain boundaries. Samples of nickel containing 5.4 wt ppm of sulphur were annealed at different temperatures to achieve different equilibrium sulphur grain boundary concentrations, ranging from less than 1% to about 50% of a monolayer. Quantification was carried out from sulphur concentration profiles acquired across about 20 grain boundaries in each sample. An internal standard (nickel containing a known concentration of sulphur in solid solution) was used for calibration. It is found that, depending on the annealing temperature, the average grain boundary sulphur concentration ranges from 0.9 to 25.8 ng cm–2 (or 1.7 1013 to 4.8 1014 atoms cm–2), i.e. ~0.015 to ~0.43 monolayer. Thermodynamic analysis gives a segregation free energy of −97.8 kJ mol–1 and a grain boundary sulphur concentration at saturation of 26.7 ng cm–2 (or 5.0×1014 atoms cm–2), i.e. ~0.44 monolayer, in good agreement with previous measurements on this system. The limit of detection of the technique is shown to be as low as 0.24 ng cm–2 (or 4.5×1012 atoms cm–2), i.e. ~0.004 monolayer, with a counting time of only 10 min. Copyright © 2012 John Wiley & Sons, Ltd.
Sprache
Englisch
Identifikatoren
ISSN: 0142-2421
eISSN: 1096-9918
DOI: 10.1002/sia.4806
Titel-ID: cdi_hal_primary_oai_HAL_hal_00866172v1
Format
–
Schlagworte
Atomic, molecular, and ion beam impact and interactions with surfaces
,
Auger electron spectroscopy (AES)
,
Condensed Matter
,
Condensed matter: electronic structure, electrical, magnetic, and optical properties
,
Condensed matter: structure, mechanical and thermal properties
,
Defects and impurities in crystals
,
microstructure
,
Electron and ion emission by liquids and solids
,
impact phenomena
,
Electron impact: auger emission
,
Exact sciences and technology
,
Grain and twin boundaries
,
Impact phenomena (including electron spectra and sputtering)
,
Materials Science
,
microbeam techniques
,
Physics
,
SIMS
,
Structure of solids and liquids
,
crystallography
,
surface analysis
,
traces
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