Skip to main content
Log in

Insights into the thermal history of carbon fibers using Raman spectroscopy and a novel kinetic model

  • Composites & nanocomposites
  • Published:
Journal of Materials Science Aims and scope Submit manuscript

Abstract

Carbon fibers and carbon fiber composites are applied in high-performance applications, but a key consideration for application is their relative sensitivity to oxidative environments. To enable in-situ characterization of carbon fibers exposed to oxidative conditions, the Raman spectral response of T700 carbon fibers that have been exposed to a variety of dwell temperatures is reported herein with dwell times reaching up to 1 month. We evaluate the spectra holistically by using integrated absolute difference analysis. By combining this analysis with straightforward kinetic models, we connect the total Raman spectral response to the temperature-time curve that could yield such a shift in spectral parameters. Our work connects the Raman spectral response of carbon fibers to their thermal history and can easily be extended to other graphitic materials, such as nuclear graphite.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Figure 1
Figure 2
Figure 3

Similar content being viewed by others

Data availability

The data that support the findings of this study are available from the corresponding author upon reasonable request.

References

  1. Newcomb BA (2016) Processing, structure, and properties of carbon fibers. Compos A 91:262. https://doi.org/10.1016/j.compositesa.2016.10.018

    Article  CAS  Google Scholar 

  2. Böhm R, Thieme M, Wohlfahrt D, Wolz DS, Richter B, Jäger H (2018) Reinforcement systems for carbon concrete composites based on low-cost carbon fibers. Fibers 6:56. https://doi.org/10.3390/fib6030056

    Article  CAS  Google Scholar 

  3. Edie DD (1998) The effect of processing on the structure and properties of carbon fibers. Carbon 36(4):345–362. https://doi.org/10.1080/03602559408015290

    Article  CAS  Google Scholar 

  4. Matsumoto T (1985) Mesophase pitch and its carbon fibers. Pure Appl Chem 57(11):1553–1562. https://doi.org/10.1351/pac198557111553

    Article  CAS  Google Scholar 

  5. Ferrari AC, Robertson J (2000) Interpretation of Raman spectra of disordered and amorphous carbon. Phys Rev B 61:14095. https://doi.org/10.1103/PhysRevB.61.14095

    Article  CAS  Google Scholar 

  6. Ferrari AC, Robertson J (2001) Resonant Raman spectroscopy of disordered, amorphous, and diamondlike carbon. Phys Rev B 64:075414. https://doi.org/10.1103/PhysRevB.64.075414

    Article  CAS  Google Scholar 

  7. Brubaker ZE, Langford JJ, Kapsimalis RJ, Niedziela JL (2021) Quantitative analysis of Raman spectral parameters for carbon fibers: practical considerations and connection to mechanical properties. J Mater Sci. https://doi.org/10.1007/s10853-021-06225-1

    Article  Google Scholar 

  8. Brubaker ZE, Miskowiec A, Niedziela JL (2022) Raman spectroscopy of thermally perturbed carbon fibers: discriminating spectral responses of modulus classes and defect types. Phys Rev Mater 6:073603. https://doi.org/10.1103/PhysRevMaterials.6.073603

    Article  CAS  Google Scholar 

  9. Tong Y, Wang X, Su H, Xu L (2011) Oxidation kinetics of polyacrylonitrile-based carbon fibers in air and the effect on their tensile properties. Corros Sci 53(8):2484–2488. https://doi.org/10.1016/j.corsci.2011.04.004

    Article  CAS  Google Scholar 

  10. Cairo CAA, Florian M, Graça MLA, Bressiani JC (2003) Kinetic study by TGA of the effect of oxidation inhibitors for carbon-carbon composite. Mater Sci Eng A 358(1):298–303. https://doi.org/10.1016/S0921-5093(03)00302-2

    Article  CAS  Google Scholar 

  11. Bertran X, Labrugere C, Dourges MA, Rebillat F (2013) Oxidation behavior of pan-based carbon fibers and the effect on mechanical properties. Oxid Metals 80(3):299–309. https://doi.org/10.1007/s11085-013-9388-9

    Article  CAS  Google Scholar 

  12. Dhami TL, Manocha LM, Bahl OP (1991) Oxidation behaviour of pitch based carbon fibers. Carbon 29(1):51–60. https://doi.org/10.1016/0008-6223(91)90094-Y

    Article  CAS  Google Scholar 

  13. Kang PC, Chen GQ, Zhang B, Wu GH, Mula S, Koch CC (2011) Oxidation protection of carbon fibers by a reaction sintered nanostructured sic coating. Surf Coat Technol 206(2):305–311. https://doi.org/10.1016/j.surfcoat.2011.07.016

    Article  CAS  Google Scholar 

  14. Xiaowei L, Jean-Charles R, Suyuan Y (2004) Effect of temperature on graphite oxidation behavior. Nucl Eng Design 227(3):273–280. https://doi.org/10.1016/j.nucengdes.2003.11.004

    Article  CAS  Google Scholar 

  15. Irradiation Damage in Graphite Due to Fast Neutrons in Fission and Fusion Systems. TECDOC Series, vol. 1154. INTERNATIONAL ATOMIC ENERGY AGENCY, Vienna (2000). https://www.iaea.org/publications/5294/irradiation-damage-in-graphite-due-to-fast-neutrons-in-fission-and-fusion-systems

  16. Tuinstra F, Koenig JL (1970) Raman spectrum of graphite. J Chem Phys 53(3):1126–1130. https://doi.org/10.1063/1.1674108

    Article  CAS  Google Scholar 

  17. Zickler GA, Smarsly B, Gierlinger N, Peterlik H, Paris O (2006) A reconsideration of the relationship between the crystallite size La of carbons determined by X-ray diffraction and Raman spectroscopy. Carbon 44(15):3239–3246. https://doi.org/10.1016/j.carbon.2006.06.029

    Article  CAS  Google Scholar 

  18. Cançado LG, Takai K, Enoki T, Endo M, Kim YA, Mizusaki H, Jorio A, Coelho LN, Magalhães-Paniago R, Pimenta MA (2006) General equation for the determination of the crystallite size la of nanographite by Raman spectroscopy. Appl Phys Lett 88(16):1998–2001. https://doi.org/10.1063/1.2196057

    Article  CAS  Google Scholar 

  19. Matthews MJ, Pimenta MA, Dresselhaus G, Dresselhaus MS, Endo M (1999) Origin of dispersive effects of the Raman d band in carbon materials. Phys Rev B 59:6585. https://doi.org/10.1103/PhysRevB.59.R6585

    Article  Google Scholar 

  20. Okuda H, Young RJ, Wolverson D, Tanaka F, Yamamoto G, Okabe T (2018) Investigating nanostructures in carbon fibres using Raman spectroscopy. Carbon 130:178–184. https://doi.org/10.1016/j.carbon.2017.12.108

    Article  CAS  Google Scholar 

  21. Nikiel L, Jagodzinski PW (1993) Raman spectroscopic characterization of graphites: a re-evaluation of spectra/structure correlation. Carbon 31:1313–1317. https://doi.org/10.1016/0008-6223(93)90091-N

    Article  CAS  Google Scholar 

  22. Brubaker ZE, Miskowiec A, Cheng YQ, Daemen L, Niedziela JL (2022) Inelastic neutron spectra of polyacrylonitrile-based carbon fibers. Phys Rev Mater 6:013609. https://doi.org/10.1103/PhysRevMaterials.6.013609

    Article  CAS  Google Scholar 

Download references

Acknowledgements

This research was funded by the US Department of Energy. The authors thank S. Isbill and X. Zhou for critical review of the manuscript.

Author information

Authors and Affiliations

Authors

Contributions

ZEB was contributed to conceptualization, data curation, formal analysis, investigation, methodology, project administration, software, supervision, validation, visualization, writing—original draft, writing—review and editing. AM was contributed to funding acquisition, resources, writing—review and editing. JLN was contributed to funding acquisition, resources, supervision, writing—review and editing.

Corresponding author

Correspondence to Zach E. Brubaker.

Ethics declarations

Conflict of interest

The authors declare that they have no conflicts of interest to this work.

Ethical Approval

Not Applicable.

Additional information

Handling Editor: Gregory Rutledge.

Publisher's Note

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

Notice: This manuscript has been authored by UT-Battelle, LLC, under contract DE-AC05-00OR22725 with the US Department of Energy (DOE). The US government retains and the publisher, by accepting the article for publication, acknowledges that the US government retains a nonexclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so, for US government purposes. DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan (http://energy.gov/downloads/doe-public-access-plan).

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Brubaker, Z.E., Miskowiec, A. & Niedziela, J.L. Insights into the thermal history of carbon fibers using Raman spectroscopy and a novel kinetic model. J Mater Sci 58, 7613–7619 (2023). https://doi.org/10.1007/s10853-023-08512-5

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10853-023-08512-5

Navigation