Microstructural analysis of Sanicro 25 (42Fe22Cr25NiWCuNbN) after oxidation in steam for 25,000 h at 700 °C.

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Title: Microstructural analysis of Sanicro 25 (42Fe22Cr25NiWCuNbN) after oxidation in steam for 25,000 h at 700 °C.
Authors: Cempura, Grzegorz1 (AUTHOR) cempura@agh.edu.pl, Kruk, Adam1 (AUTHOR)
Source: Materials Characterization. Mar2025, Vol. 221, pN.PAG-N.PAG. 1p.
Subjects: Scanning transmission electron microscopy, Laves phases (Metallurgy), Electron microscope techniques, Three-dimensional imaging, Substrates (Materials science)
Abstract: The paper presents the results of structural studies on Sanicro 25 steel oxidation in a steam atmosphere at 700 °C over 25,000 h. Microstructural changes were analyzed in the oxide/steel interface region and at a greater distance, where microstructural changes were caused mainly by the high-temperature annealing. Microstructural analysis was performed using scanning and transmission electron microscopy techniques and FIB-SEM tomography techniques. The phase analysis of the substrate material was supported by thermodynamic simulations using the Thermo-Calc software package. The application of 3D volume imaging allowed visualization of the morphology of the oxide layer, pores, voids, and the substrate material (Cr 23 C 6 carbides, Laves phase, Z -phase, σ-phase, and Cu-rich phase). This enabled 3D spatial imaging of the distribution of voids and quantitative assessment of porosity at the oxide/metal boundary. Numerous large voids were observed in the substrate material below the metal/oxide boundary, with dimensions comparable to the grain size in the near-boundary area. Large voids with oxidized surfaces and others with clean inner surfaces were observed, which suggests the significant impact of steam on the formation of voids at the metal/oxide boundary. The structural studies did not reveal the presence of an internal oxidation zone. HRSTEM studies confirmed the presence of Cu-rich precipitates, coherent with the austenitic matrix and nucleating at dislocations and other structural elements. FIB-SEM tomography reconstruction and 3D visualization of microstructural elements with an 8 × 8 × 8.2 nm voxel size indirectly imaged dislocation networks by visualizing secondary precipitates, such as Cr 23 C 6 carbides and Laves phase precipitated at dislocations. In summary, the paper provides valuable insights into the mechanisms of high-temperature oxidation of Sanicro 25 steel in steam conditions and the effects of these processes on the material's microstructure. • FIB-SEM tomographic reconstruction of the microstructure elements in 3D using an 8 × 8 × 8.2 nm voxel allowed us to indirectly visualize dislocation systems by imaging secondary precipitates: carbides Cr 23 C 6 , Laves phase precipitates on dislocations. • The presence of steam during the high-temperature oxidation process of Sanicro 25 steel significantly affects the scale formation and void formation process in the scale/metal interface area. The formation of volatile oxide compounds leading to the formation of large voids in the material under the scale layer is possible. • Voids were found in the substrate material below the metal/oxides boundary, with dimensions of the material grain size in the border area, an oxidized inner surface, and a clean inner surface without a clear oxide layer. [ABSTRACT FROM AUTHOR]
Copyright of Materials Characterization is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Data: Microstructural analysis of Sanicro 25 (42Fe22Cr25NiWCuNbN) after oxidation in steam for 25,000 h at 700 °C.
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  Data: <searchLink fieldCode="DE" term="%22Scanning+transmission+electron+microscopy%22">Scanning transmission electron microscopy</searchLink><br /><searchLink fieldCode="DE" term="%22Laves+phases+%28Metallurgy%29%22">Laves phases (Metallurgy)</searchLink><br /><searchLink fieldCode="DE" term="%22Electron+microscope+techniques%22">Electron microscope techniques</searchLink><br /><searchLink fieldCode="DE" term="%22Three-dimensional+imaging%22">Three-dimensional imaging</searchLink><br /><searchLink fieldCode="DE" term="%22Substrates+%28Materials+science%29%22">Substrates (Materials science)</searchLink>
– Name: Abstract
  Label: Abstract
  Group: Ab
  Data: The paper presents the results of structural studies on Sanicro 25 steel oxidation in a steam atmosphere at 700 °C over 25,000 h. Microstructural changes were analyzed in the oxide/steel interface region and at a greater distance, where microstructural changes were caused mainly by the high-temperature annealing. Microstructural analysis was performed using scanning and transmission electron microscopy techniques and FIB-SEM tomography techniques. The phase analysis of the substrate material was supported by thermodynamic simulations using the Thermo-Calc software package. The application of 3D volume imaging allowed visualization of the morphology of the oxide layer, pores, voids, and the substrate material (Cr 23 C 6 carbides, Laves phase, Z -phase, σ-phase, and Cu-rich phase). This enabled 3D spatial imaging of the distribution of voids and quantitative assessment of porosity at the oxide/metal boundary. Numerous large voids were observed in the substrate material below the metal/oxide boundary, with dimensions comparable to the grain size in the near-boundary area. Large voids with oxidized surfaces and others with clean inner surfaces were observed, which suggests the significant impact of steam on the formation of voids at the metal/oxide boundary. The structural studies did not reveal the presence of an internal oxidation zone. HRSTEM studies confirmed the presence of Cu-rich precipitates, coherent with the austenitic matrix and nucleating at dislocations and other structural elements. FIB-SEM tomography reconstruction and 3D visualization of microstructural elements with an 8 × 8 × 8.2 nm voxel size indirectly imaged dislocation networks by visualizing secondary precipitates, such as Cr 23 C 6 carbides and Laves phase precipitated at dislocations. In summary, the paper provides valuable insights into the mechanisms of high-temperature oxidation of Sanicro 25 steel in steam conditions and the effects of these processes on the material's microstructure. • FIB-SEM tomographic reconstruction of the microstructure elements in 3D using an 8 × 8 × 8.2 nm voxel allowed us to indirectly visualize dislocation systems by imaging secondary precipitates: carbides Cr 23 C 6 , Laves phase precipitates on dislocations. • The presence of steam during the high-temperature oxidation process of Sanicro 25 steel significantly affects the scale formation and void formation process in the scale/metal interface area. The formation of volatile oxide compounds leading to the formation of large voids in the material under the scale layer is possible. • Voids were found in the substrate material below the metal/oxides boundary, with dimensions of the material grain size in the border area, an oxidized inner surface, and a clean inner surface without a clear oxide layer. [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Materials Characterization is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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RecordInfo BibRecord:
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      – Type: doi
        Value: 10.1016/j.matchar.2025.114751
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      – Code: eng
        Text: English
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        StartPage: N.PAG
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      – SubjectFull: Scanning transmission electron microscopy
        Type: general
      – SubjectFull: Laves phases (Metallurgy)
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      – SubjectFull: Electron microscope techniques
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      – SubjectFull: Three-dimensional imaging
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      – SubjectFull: Substrates (Materials science)
        Type: general
    Titles:
      – TitleFull: Microstructural analysis of Sanicro 25 (42Fe22Cr25NiWCuNbN) after oxidation in steam for 25,000 h at 700 °C.
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            NameFull: Kruk, Adam
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              M: 03
              Text: Mar2025
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              Y: 2025
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