Spatial distribution of sp3 defects in carbon fibers via time-of-flight secondary ion mass spectrometry

Derek B. Dwyer; Zachary E. Brubaker; Anton V. Ievlev; Sara Isbill; Jennifer Neu; Andrew Miskowiec

doi:10.1016/j.carbon.2025.120735

Spatial distribution of sp³ defects in carbon fibers via time-of-flight secondary ion mass spectrometry

Research output: Contribution to journal › Article › peer-review

Abstract

Defects play a significant role in the material properties of carbon fibers (CF). Several defects result in the formation of sp³ bonds in an otherwise sp²-dominant graphitic structure. Understanding the distribution of these defects within CF provides insight into their properties and the effect of manufacturing conditions. Reports showed time-of-flight secondary ion mass spectrometry (ToF-SIMS) is capable of characterizing the spatial distribution of sp² and sp³ content in carbon materials. Here, ToF-SIMS was utilized to investigate the spatial distribution of sp³ defects in T700, T1000, and M46 CF. M46 had the lowest sp³ content. Center-to-edge analysis revealed that T700 CF had a gradient of sp³ defects starting from the center and increasing to the edge, whereas M46 CF had a sudden increase in sp³ defects roughly 1 μm from the edge. Comparatively, T1000 CF had a relatively uniform radial distribution of sp³ defects, except for a newly identified sp² rich region at 0.8 μm from the center. This is hypothesized to originate from a skin–core structure that forms during CF manufacturing. This work demonstrates the utility of ToF-SIMS for characterizing the spatial distribution of sp³ defects within CF, establishing new ways to understand CF formation.

Original language	English
Article number	120735
Journal	Carbon
Volume	245
DOIs	https://doi.org/10.1016/j.carbon.2025.120735
State	Published - Oct 2025

Funding

This work was sponsored by the National Nuclear Security Administration. ToF-SIMS characterization was conducted at the Center for Nanophase Materials Sciences, which is a US Department of Energy Office of Science user facility, and using instrumentation within Oak Ridge National Laboratory's Materials Characterization Core, provided by UT-Battelle, LLC, under Contract No. DE-AC05-00OR22725 with the US Department of Energy. 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 ).

Keywords

Carbon fibers
Hydrogen defects
Oxygen defects
Time-of-flight secondary ion mass spectrometry (ToF-SIMS)
sp hybridization

Access to Document

10.1016/j.carbon.2025.120735

Cite this

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title = "Spatial distribution of sp3 defects in carbon fibers via time-of-flight secondary ion mass spectrometry",

abstract = "Defects play a significant role in the material properties of carbon fibers (CF). Several defects result in the formation of sp3 bonds in an otherwise sp2-dominant graphitic structure. Understanding the distribution of these defects within CF provides insight into their properties and the effect of manufacturing conditions. Reports showed time-of-flight secondary ion mass spectrometry (ToF-SIMS) is capable of characterizing the spatial distribution of sp2 and sp3 content in carbon materials. Here, ToF-SIMS was utilized to investigate the spatial distribution of sp3 defects in T700, T1000, and M46 CF. M46 had the lowest sp3 content. Center-to-edge analysis revealed that T700 CF had a gradient of sp3 defects starting from the center and increasing to the edge, whereas M46 CF had a sudden increase in sp3 defects roughly 1 μm from the edge. Comparatively, T1000 CF had a relatively uniform radial distribution of sp3 defects, except for a newly identified sp2 rich region at 0.8 μm from the center. This is hypothesized to originate from a skin–core structure that forms during CF manufacturing. This work demonstrates the utility of ToF-SIMS for characterizing the spatial distribution of sp3 defects within CF, establishing new ways to understand CF formation.",

keywords = "Carbon fibers, Hydrogen defects, Oxygen defects, Time-of-flight secondary ion mass spectrometry (ToF-SIMS), sp hybridization",

author = "Dwyer, \{Derek B.\} and Brubaker, \{Zachary E.\} and Ievlev, \{Anton V.\} and Sara Isbill and Jennifer Neu and Andrew Miskowiec",

note = "Publisher Copyright: {\textcopyright} 2025",

year = "2025",

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doi = "10.1016/j.carbon.2025.120735",

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T1 - Spatial distribution of sp3 defects in carbon fibers via time-of-flight secondary ion mass spectrometry

AU - Dwyer, Derek B.

AU - Brubaker, Zachary E.

AU - Ievlev, Anton V.

AU - Isbill, Sara

AU - Neu, Jennifer

AU - Miskowiec, Andrew

PY - 2025/10

Y1 - 2025/10

N2 - Defects play a significant role in the material properties of carbon fibers (CF). Several defects result in the formation of sp3 bonds in an otherwise sp2-dominant graphitic structure. Understanding the distribution of these defects within CF provides insight into their properties and the effect of manufacturing conditions. Reports showed time-of-flight secondary ion mass spectrometry (ToF-SIMS) is capable of characterizing the spatial distribution of sp2 and sp3 content in carbon materials. Here, ToF-SIMS was utilized to investigate the spatial distribution of sp3 defects in T700, T1000, and M46 CF. M46 had the lowest sp3 content. Center-to-edge analysis revealed that T700 CF had a gradient of sp3 defects starting from the center and increasing to the edge, whereas M46 CF had a sudden increase in sp3 defects roughly 1 μm from the edge. Comparatively, T1000 CF had a relatively uniform radial distribution of sp3 defects, except for a newly identified sp2 rich region at 0.8 μm from the center. This is hypothesized to originate from a skin–core structure that forms during CF manufacturing. This work demonstrates the utility of ToF-SIMS for characterizing the spatial distribution of sp3 defects within CF, establishing new ways to understand CF formation.

AB - Defects play a significant role in the material properties of carbon fibers (CF). Several defects result in the formation of sp3 bonds in an otherwise sp2-dominant graphitic structure. Understanding the distribution of these defects within CF provides insight into their properties and the effect of manufacturing conditions. Reports showed time-of-flight secondary ion mass spectrometry (ToF-SIMS) is capable of characterizing the spatial distribution of sp2 and sp3 content in carbon materials. Here, ToF-SIMS was utilized to investigate the spatial distribution of sp3 defects in T700, T1000, and M46 CF. M46 had the lowest sp3 content. Center-to-edge analysis revealed that T700 CF had a gradient of sp3 defects starting from the center and increasing to the edge, whereas M46 CF had a sudden increase in sp3 defects roughly 1 μm from the edge. Comparatively, T1000 CF had a relatively uniform radial distribution of sp3 defects, except for a newly identified sp2 rich region at 0.8 μm from the center. This is hypothesized to originate from a skin–core structure that forms during CF manufacturing. This work demonstrates the utility of ToF-SIMS for characterizing the spatial distribution of sp3 defects within CF, establishing new ways to understand CF formation.

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KW - Oxygen defects

KW - Time-of-flight secondary ion mass spectrometry (ToF-SIMS)

KW - sp hybridization

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