Characterization of thermally heat-treated polyacrylonitrile carbon fibers

Ginsparg, Aaron R.; Watts, Jeremy L.; Fahrenholtz, William G.; Dickerson, Matthew B.; Detwiler, Kaitlin N.; Brubaker, Zachary E.; Hilmas, Gregory E.

doi:10.1016/j.diamond.2025.112875

Characterization of thermally heat-treated polyacrylonitrile carbon fibers

Journal Article · Tue Sep 23 00:00:00 EDT 2025 · Diamond and Related Materials

DOI:https://doi.org/10.1016/j.diamond.2025.112875· OSTI ID:3002043

Ginsparg, Aaron R. ^[1]; Watts, Jeremy L. ^[1]; ^[1]; ^[2]; Detwiler, Kaitlin N. ^[2]; ^[3]; ^[1]

Missouri Univ. of Science and Technology, Rolla, MO (United States)
US Air Force Office of Scientific Research (AFOSR), Dayton, OH (United States)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

This study investigates the graphitization process of polyacrylonitrile (PAN) carbon fibers by subjecting commercial fibers to thermal heat treatment at temperatures ranging from 1400 to 2100 °C in 100 °C increments, using either argon or nitrogen gas atmospheres. Changes in crystallinity, surface morphology, and lattice parameters were analyzed for two commercial carbon fibers using X-ray diffraction, scanning electron microscopy, and Raman spectroscopy. Results indicated minimal changes in surface morphology with increasing heat-treatment temperature; however, crystallinity significantly increased. Crystallinity changes were more strongly dependent on temperature rather than gas atmosphere or fiber type. At intermediate heat-treatment temperatures (1600–1800 °C), fibers treated in argon showed a slight preference for graphitization. The highest level of graphitization was measured at 2100 °C. Crystallite size increased as the intensity ratio of the D1 to G Raman peaks increased, reaching a peak around ~1800 °C, after which the ratio started to decrease. This behavior aligns with Ferrari's three-stage model of carbon crystallization and is consistent with both the Marie-Mering degree of graphitization and Brubaker's Integrated Absolute Differential models, all of which describe the transformation from an amorphous to a more graphitic structure. At the higher heat-treatment temperatures, the changes between atmospheres and fiber types were measured to converge to similar levels of graphitization. In conclusion, this study evaluates the progressive change in commercial grade carbon fibers when heat-treated.

View Accepted Manuscript (DOE)

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC); US Air Force Office of Scientific Research (AFOSR)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 3002043

Journal Information:: Diamond and Related Materials, Journal Name: Diamond and Related Materials Journal Issue: B Vol. 159; ISSN 0925-9635

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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Characterization of thermally heat-treated polyacrylonitrile carbon fibers

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