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Atom-probe tomography of surface oxides and oxidized grain boundaries in alloys from nuclear reactors

Published online by Cambridge University Press:  18 March 2013

Karen Kruska ,
David W Saxey ,
Takumi Terachi ,
Takuyo Yamada ,
Peter Chou ,
Olivier Calonne ,
Lionel Fournier ,
George D W Smith  and
Sergio Lozano-Perez
Karen Kruska
Affiliation:
University of Oxford, Department of Materials, Oxford, United Kingdom.
David W Saxey
Affiliation:
University of Oxford, Department of Materials, Oxford, United Kingdom. University of Western Australia, School of Physics, Perth, WA, Australia
Takumi Terachi
Affiliation:
Institute of Nuclear Safety Systems Inc., Tsuruga, Fukui, Japan.
Takuyo Yamada
Affiliation:
Institute of Nuclear Safety Systems Inc., Tsuruga, Fukui, Japan.
Peter Chou
Affiliation:
EPRI, Palo Alto, CA, United States.
Olivier Calonne
Affiliation:
Areva NP, Paris, France.
Lionel Fournier
Affiliation:
Areva NP, Paris, France.
George D W Smith
Affiliation:
University of Oxford, Department of Materials, Oxford, United Kingdom.
Sergio Lozano-Perez
Affiliation:
University of Oxford, Department of Materials, Oxford, United Kingdom.
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Abstract

The preparation of site-specific atom-probe tomography (APT) samples containing localized features has become possible with the use of focused ion beams (FIBs). This technique was used to achieve the analysis of surface oxides and oxidized grain boundaries in this paper. Transmission electron microscopy (TEM), providing microstructural and chemical characterization of the same features, has also been used, revealing crucial additional information.

The study of grain boundary oxidation in stainless steels and nickel-based alloys is required in order to understand the mechanisms controlling stress corrosion cracking in nuclear reactors. Samples oxidized under simulated pressurized water reactor primary water conditions were used, and FIB lift-out TEM and APT specimens containing the same oxidized grain boundary were prepared and fully characterized. The results from both techniques were found fully consistent and complementary.

Chromium-rich spinel oxides grew at the surface and into the bulk material, along grain boundaries. Nickel was rejected from the oxides and accumulated ahead of the oxidation front. Lithium, which was present in small quantities in the aqueous environment during oxidation, was incorporated in the oxide. All phases were accurately quantified and the effect of different experimental parameters were analysed.

Keywords

steelcorrosionelectron energy loss spectroscopy (EELS)
Type
Articles
Information
MRS Online Proceedings Library (OPL) , Volume 1514: Symposium HH – Advances in Materials for Nuclear Energy , 2013 , pp. 107 - 118
Copyright
Copyright © Materials Research Society 2013 

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