Correlative atom probe tomography and transmission electron microscopy analysis of grain boundaries in thermally grown alumina scale

Ivan Povstugar, Juliane Weber, Dmitry Naumenko, Taihong Huang, Martina Klinkenberg, Willem J. Quadakkers

Research output: Contribution to journalArticlepeer-review

15 Scopus citations

Abstract

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.

Original languageEnglish
Pages (from-to)11-20
Number of pages10
JournalMicroscopy and Microanalysis
Volume25
Issue number1
DOIs
StatePublished - Feb 1 2019

Funding

We are grateful to Dr. Egbert Wessel (IEK-2, Forschungszentrum Jülich, Germany) for the assistance with electron microscopy measurements. The help of Maximilian Kruth (Ernst Ruska Centre for Microscopy and Spectroscopy with Electrons, Forschungszentrum Jülich, Germany) in testing the correlative setup is acknowledged. One of the authors (T. Huang) would like to acknowledge the China Scholarship Council for funding his work.

Keywords

  • alumina
  • atom probe tomography
  • correlative microscopy
  • thermally grown oxide
  • transmission electron microscopy

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