Determination of the oxide scale growth mechanism using 18O-tracer experiments in combination with Transmission Electron Microscopy and nanoscale Secondary Ion Mass Spectrometry
- Chalmers University of Technology, Department of Chemistry and Chemical Engineering, Division of Energy and Materials, Kemivägen 10, SE-41296 Gothenburg (Sweden)
- Chalmers University of Technology, Department of Chemistry and Chemical Engineering, Division of Analytical Chemistry, Kemivägen 10, SE-41296 Gothenburg (Sweden)
Highlights: • {sup 18}O-tracer experiments to determine oxide scale growth mechanism on a Fe-Cr alloy. • Cr{sub 2}O{sub 3} scale growth primarily by means of metal outwards diffusion in air at 850 °C • nanoSIMS mapping on TEM lamella more accurate than SIMS sputter depth profiling • nanoSIMS mapping on TEM lamella reveal information about local oxide growth. • Strong local variation of oxide scale growth - Abstract: Two-stage {sup 18}O{sub 2}/{sup 16}O{sub 2} exposures can be used to investigate the effect that alloying elements, secondary phases, or surface treatments have on the high temperature oxidation behaviour of certain materials. During subsequent exposures to {sup 16}O{sub 2}- and {sup 18}O{sub 2}-rich atmospheres, {sup 16}O- and {sup 18}O-rich layers are formed. Analysis of the layers using Secondary Ion Mass Spectrometry (SIMS) depth profiling allows for conclusions to be drawn about the oxide scale growth mechanism. The conclusions are, however, not entirely unambiguous due to the limited lateral resolution of the technology. Rough surface topography and the thickness variation of the oxide scale over the analysed volume add to the ambiguity of the findings. In this study, an Fe-20%Cr alloy was exposed to both {sup 18}O- and {sup 16}O-rich environments at 850 °C. Two methods were used to analyse the thermally grown Cr{sub 2}O{sub 3} scale: (1) traditional SIMS depth profiling and (2) preparation of a cross-sectional lamellae for Transmission Electron Microscopy (TEM), which, subsequently, was analysed in a NanoSIMS. The NanoSIMS {sup 16}O and {sup 18}O elemental maps were then superimposed on the TEM image. In comparison with traditional SIMS depth profiling, the nanoSIMS elemental maps reveal detailed information about local oxide growth in different parts of an oxide scale. Moreover, a clear {sup 16}O/{sup 18}O interface can be seen in the nanoSIMS maps, which is not the case in the sputter depth profiles. The findings of this study show that the aforementioned issues associated with sputter depth profiling can be eliminated by mapping a cross-section of an oxide scale using high resolution nanoSIMS.
- OSTI ID:
- 22804881
- Journal Information:
- Materials Characterization, Vol. 136; Other Information: Copyright (c) 2017 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); ISSN 1044-5803
- Country of Publication:
- United States
- Language:
- English
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