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In Situ Observation of Reaction Fronts During the Initial Stages of Iron Surface Oxidation at 1150 °C

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Abstract

This study focuses on the initial stages of iron surface oxidation, studied by confocal scanning laser microscopy. Pure iron cubes were prepared and polished for in situ observation. Samples were oxidized for 2–60 s by dry air at 1150 °C. A dynamic oxidation process was observed, with two reaction fronts that moved from the sample edge to the center at around 20–30- and around 40–50-s oxidation, respectively. Scanning electron microscopy (SEM) was used to characterize the iron oxide surface morphology. Pyramidal features appeared first on the surface, and then the surface became flatter with time. X-ray diffraction was used to characterize the phases of the outermost oxide layer. Overall, the content of wüstite decreased and hematite content increased with oxidation time. SEM with a backscattered electron detector was used to measure the oxide layer thicknesses, and it was found that the oxide thickness increased parabolically with time. The different oxide layers within the scale were identified by an optical microscope with a polarized light source. Even after 2-s oxidation, an obvious magnetite layer was found on the wüstite layer, and after 10-s oxidation, an obvious hematite layer was observed on the magnetite layer. A thicker hematite layer was observed at the sample edge. The reasons for the morphology changes are discussed.

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Acknowledgements

The authors gratefully acknowledge support from the industrial members of the Center for Iron and Steelmaking Research at Carnegie Mellon University as well as the use of the Materials Characterization Facility at Carnegie Mellon University under Grant # MCF-677785.

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Authors and Affiliations

  1. Department of Materials Science and Engineering, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA, 15213, USA

    Ming Zhong, Yining He, Elyce A. Milligan, Petrus C. Pistorius & Bryan A. Webler

  2. Center for Iron and Steelmaking Research, Carnegie Mellon University, 5000 Forbes Avenue, Pittsburgh, PA, 15213, USA

    Ming Zhong, Petrus C. Pistorius & Bryan A. Webler

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  1. Ming Zhong
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  2. Yining He
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  3. Elyce A. Milligan
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Correspondence to Ming Zhong.

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Zhong, M., He, Y., Milligan, E.A. et al. In Situ Observation of Reaction Fronts During the Initial Stages of Iron Surface Oxidation at 1150 °C. Oxid Met 93, 449–463 (2020). https://doi.org/10.1007/s11085-020-09965-8

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