Skip to main content

Oxidation of Thin Nickel-Based Superalloy Specimens: Kinetics Study and Mechanical Integrity


The oxidation behavior of a nickel-based superalloy was investigated from 650 to 1,000 °C for up to 1,000 h in air. Samples with thicknesses ranging from 20 to 500 µm were used to document the evolutions of microstructure and oxide scale. Oxidation products and subsurface evolution of the metal microstructure were characterized by XRD and EDS analyses. Local breakaway was observed after 600 h at 800 °C and after 100 h at 900 °C due to the full consumption of Cr from the alloy. Room temperature tensile tests were performed on aged and pre-oxidized specimens with thicknesses ranging from 20 µm to 500 µm, at 800 °C. The results were compared to tensile tests performed on the as-received metallurgical state. Both size effects due to sample thickness reduction and to sample thickness/pre-oxidation width ratio were examined onto the mechanical behavior. Interestingly, the formation of TCP phases, the oxide layer and the subsequent Cr-depleted subsurface region from either aging or oxidation treatments impairs the mechanical integrity. Bulk and subsurface regions are impacted, especially for tens-of-micrometer thin samples.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5


  1. 1.

    S. Bose, High temperature coatings, (Elsevier, Butterworth-Heinemann, 2018).

    Google Scholar 

  2. 2.

    Young DJ. High Temperature Oxidation and Corrosion of Metals Second Edition. Elsevier; 2016.

  3. 3.

    J. Tong, S. Dalby, J. Byrne, M. B. Henderson, and M. C. Hardy, Creep, fatigue and oxidation in crack growth in advanced nickel base superalloys. International Journal of Fatigue. 23, 2001 (897–902).

    CAS  Article  Google Scholar 

  4. 4.

    A. Pineau and S. D. Antolovich, High temperature fatigue of nickel-base superalloys – A review with special emphasis on deformation modes and oxidation. Engineering Failure Analysis. 16, 2009 (2668–2697).

    CAS  Article  Google Scholar 

  5. 5.

    H. E. Evans, A. T. Donaldson, and T. C. Gilmour, Mechanisms of Breakaway Oxidation and Application to a Chromia-Forming Steel. Oxidation of Metals. 52, 1999 (379–402).

    CAS  Article  Google Scholar 

  6. 6.

    M. Zupan, M. J. Hayden, C. J. Boehlert, and K. J. Hemker, Development of high-temperature microsample testing. Experiment mechanics. 41, 2001 (242–247).

    CAS  Article  Google Scholar 

  7. 7.

    Texier D, Castro Moreno A, Monceau D, Hourcade D, Velay V, Andrieu E. Size effect on the plastic behaviour of polycrystalline materials: grain size, free surface and precipitation state. Submitted in Acta Materialia. .

  8. 8.

    Texier D, Ecochard M, Gheno T, Lours P. Screening breakaway in MCrAlY coatings for short-term oxidation at high temperature. Submitted in Corrosion Science. .

  9. 9.

    D. J. Young, A. Chyrkin, and W. J. Quadakkers, A Simple Expression for Predicting the Oxidation Limited Life of Thin Components Manufactured from FCC High Temperature Alloys. Oxid Met. 77, 2012 (253–264).

    CAS  Article  Google Scholar 

  10. 10.

    C. Keller, E. Hug, and X. Feaugas, Microstructural size effects on mechanical properties of high purity nickel. International Journal of Plasticity. 27, 2011 (635–654).

    CAS  Article  Google Scholar 

  11. 11.

    D. Texier, D. Monceau, J. C. Salabura, R. Mainguy, and E. Andrieu, Micromechanical testing of ultrathin layered material specimens at elevated temperature. Materials at High Temperatures. 33, 2016 (325–337).

    CAS  Article  Google Scholar 

  12. 12.

    Bradski G. The OpenCV library. Dr. Dobb’s Journal of Software Tools. 2000;

  13. 13.

    Sutton MA, Orteu JJ, Schreier H. Image Correlation for Shape, Motion and Deformation Measurements: Basic Concepts,Theory and Applications. Springer Science & Business Media; 2009.

  14. 14.

    C. Wagner, Beitrag zur Theorie des Anlaufvorgangs. Zeitschrift für Physikalische Chemie. 21B, 1933 (25–41).

    Article  Google Scholar 

  15. 15.

    R. Malacarne, L. Aranda, S. Mathieu, C. Desgranges, S. Knittel, M. Vilasi. Long-term isothermal oxidation behavior of two industrial polycrystalline nickel base alloys at 700°C – Evaluation of intergranular oxidation distribution and kinetic. submitted same Issue. 2020;

  16. 16.

    J. H. Chen, P. M. Rogers, and J. A. Little, Oxidation behavior of several chromia-forming commercial nickel-base superalloys. Oxid Met. 47, 1997 (381–410).

    CAS  Article  Google Scholar 

  17. 17.

    E. Chateau and L. Rémy, Oxidation-assisted creep damage in a wrought nickel-based superalloy: Experiments and modelling. Materials Science and Engineering: A. 527, 2010 (1655–1664).

    Article  Google Scholar 

  18. 18.

    Thébaud L. Etude des relations entre microstructure et propriétés mécaniques du nouveau superalliage base nickel AD730TM. PhD Thesis, ISAE-ENSMA; 2017.

  19. 19.

    A. A. N. Németh, D. J. Crudden, D. E. J. Armstrong, et al., Environmentally-assisted grain boundary attack as a mechanism of embrittlement in a nickel-based superalloy. Acta Materialia. 126, 2017 (361–371).

    Article  Google Scholar 

  20. 20.

    Wessman A, Laurence A, Cormier J, Villechaise P, Billot T, Franchet J-M. Thermal Stability of Cast and Wrought Alloy Rene 65. In: Superalloys 2016. Hoboken, NJ, USA: John Wiley & Sons, Inc.; 2016:793–800. doi:

  21. 21.

    Laurence A, Cormier J, Villechaise P, et al. Impact of the Solution Cooling Rate and of Thermal Aging on the Creep Properties of the New Cast & Wrought René 65 Ni-Based Superalloy. 8th International Symposium on Superalloy 718 and Derivatives. 2014;333–348. doi:10/ggf72s.

  22. 22.

    Laurence A. Impact du sur-vieillissement métallurgique sur le comportement et la durabilité du nouveau superalliage pour disque de turbine René 65. PhD Thesis, ISAE-ENSMA; 2015.

  23. 23.

    R. L. Amaro, S. D. Antolovich, R. W. Neu, and P. M. Singh, High temperature oxidation and γ depletion in the single-crystal superalloy PWA 1484. Materials at High Temperatures. 33, 2016 (476–488).

    CAS  Article  Google Scholar 

  24. 24.

    Wessman A. Physical Metallurgy of Rene 65, a Next-Generation Cast and Wrought Nickel Superalloy for use in Aero Engine Components. PhD Thesis, University of Cincinnati; 2016.

  25. 25.

    A. R. P. Singh, S. Nag, S. Chattopadhyay, et al., Mechanisms related to different generations of γ’ precipitation during continuous cooling of a nickel base superalloy. Acta Materialia. 61, 2013 (280–293).

    CAS  Article  Google Scholar 

  26. 26.

    E. Fedorova, D. Monceau, and D. Oquab, Quantification of growth kinetics and adherence of oxide scales formed on Ni-based superalloys at high temperature. Corrosion Science. 52, 2010 (3932–3942).

    CAS  Article  Google Scholar 

  27. 27.

    C. Keller, E. Hug, R. Retoux, and X. Feaugas, TEM study of dislocation patterns in near-surface and core regions of deformed nickel polycrystals with few grains across the cross section. Mechanics of Materials. 42, 2010 (44–54).

    Article  Google Scholar 

  28. 28.

    Mughrabi H. Some consequences of surface and size effects in plastically deformed copper single crystals. physica status solidi (b). 1971;44:391–402.

  29. 29.

    J. T. Fourie, Sub-surface dislocation structure of deformed copper. The Philosophical Magazine: A Journal of Theoretical Experimental and Applied Physics. 21, 1970 (977–985).

    CAS  Article  Google Scholar 

Download references


The authors would like to acknowledge Karim Choquet (ICA) and Remi Roumiguier (MIDIVAL) for technical help. This study was supported by SAFRAN Tech, SAFRAN Aircraft Engine and the Agence Nationale de la Recherche (ANR) [ANR-18-CE08-0003; ANR-JCJC-COMPAACT project funded from the AAPG2018].

Author information



Corresponding author

Correspondence to Charles Romain.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Romain, C., Texier, D., Desgranges, C. et al. Oxidation of Thin Nickel-Based Superalloy Specimens: Kinetics Study and Mechanical Integrity. Oxid Met 96, 169–182 (2021).

Download citation


  • Nickel-based superalloys
  • High-temperature oxidation
  • Breakaway
  • Gradient of microstructure and properties
  • Microtensile testing