Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples

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 co...

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Asıl Yazarlar: Christien, F, Downing, C, Moore, K, Grovenor, C
Materyal Türü: Journal article
Dil:English
Baskı/Yayın Bilgisi: 2012
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author Christien, F
Downing, C
Moore, K
Grovenor, C
author_facet Christien, F
Downing, C
Moore, K
Grovenor, C
author_sort Christien, F
collection OXFORD
description 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 10 13 to 4.8 10 14 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 5.0×10 14 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 4.5×10 12 atoms cm -2), i.e. ∼0.004 monolayer, with a counting time of only 10 min. © 2012 John Wiley and Sons, Ltd.
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spelling oxford-uuid:c2cf8989-0b16-41f4-8d92-c1b2bc8987872022-03-27T06:11:43ZQuantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samplesJournal articlehttp://purl.org/coar/resource_type/c_dcae04bcuuid:c2cf8989-0b16-41f4-8d92-c1b2bc898787EnglishSymplectic Elements at Oxford2012Christien, FDowning, CMoore, KGrovenor, CA 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 10 13 to 4.8 10 14 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 5.0×10 14 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 4.5×10 12 atoms cm -2), i.e. ∼0.004 monolayer, with a counting time of only 10 min. © 2012 John Wiley and Sons, Ltd.
spellingShingle Christien, F
Downing, C
Moore, K
Grovenor, C
Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
title Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
title_full Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
title_fullStr Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
title_full_unstemmed Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
title_short Quantification of grain boundary equilibrium segregation by NanoSIMS analysis of bulk samples
title_sort quantification of grain boundary equilibrium segregation by nanosims analysis of bulk samples
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AT downingc quantificationofgrainboundaryequilibriumsegregationbynanosimsanalysisofbulksamples
AT moorek quantificationofgrainboundaryequilibriumsegregationbynanosimsanalysisofbulksamples
AT grovenorc quantificationofgrainboundaryequilibriumsegregationbynanosimsanalysisofbulksamples