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Correlative Atom Probe Tomography and Transmission Electron Microscopy Analysis of Grain Boundaries in Thermally Grown Alumina Scale

Published online by Cambridge University Press:  04 February 2019

Ivan Povstugar*
Central Institute for Engineering, Electronics and Analytics (ZEA-3) –– Analytics, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
Juliane Weber
Institute of Energy and Climate Research (IEK-6) –– Nuclear Waste Management and Reactor Safety, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany Chemical Science Division, Oak Ridge National Laboratory, 37831 Oak Ridge, TN, USA
Dmitry Naumenko
Institute of Energy and Climate Research (IEK-2) –– Microstructure and Properties of Materials, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
Taihong Huang
Institute of Energy and Climate Research (IEK-2) –– Microstructure and Properties of Materials, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany Faculty of Materials Science and Engineering, Kunming University of Science and Technology, 650093 Kunming, China
Martina Klinkenberg
Institute of Energy and Climate Research (IEK-6) –– Nuclear Waste Management and Reactor Safety, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
Willem J. Quadakkers
Institute of Energy and Climate Research (IEK-2) –– Microstructure and Properties of Materials, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
*Author for correspondence: Ivan Povstugar, E-mail:
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We employed correlative atom probe tomography (APT) and transmission electron microscopy (TEM) to analyze the alumina scale thermally grown on the oxide dispersion-strengthened alloy MA956. Segregation of Ti and Y and associated variation in metal/oxygen stoichiometry at the grain boundaries and triple junctions of alumina were quantified and discussed with respect to the oxidation behavior of the alloy, in particular, to the formation of cation vacancies. Correlative TEM analysis was helpful to avoid building pragmatically well-looking but substantially incorrect APT reconstructions, which can result in erroneous quantification of segregating species, and highlights the need to consider ionic volumes and detection efficiency in the reconstruction routine. We also demonstrate a cost-efficient, robust, and easy-handling setup for correlative analysis based solely on commercially available components, which can be used with all conventional TEM tools without the need to modify the specimen holder assembly.

Materials Science Applications
Copyright © Microscopy Society of America 2019 

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