Continuous and rapid stabilization of polyacrylonitrile fiber bundles assisted by atmospheric pressure plasma for fabricating large-tow carbon fibers

Kim, Soyoung; Lee, Sungho; Park, Sejoon; Jo, Seong Mu; Lee, Hunsu; Joh, Han‐Ik

doi:10.1016/j.carbon.2015.07.012

Cited by 45 publications

(32 citation statements)

References 17 publications

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“…The thermal stabilization process is a long and tedious heating process, which is the most energy- and time-consuming step. For these reasons, efforts have been made to reduce the energy and time consumption of the thermal stabilization process121314.…”

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confidence: 99%

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Comprehensive stabilization mechanism of electron-beam irradiated polyacrylonitrile fibers to shorten the conventional thermal treatment

Park

Yoo

Kang

et al. 2016

Sci Rep

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An electron beam was irradiated on polyacrylonitrile (PAN) fibers prior to thermal stabilization. The electron-beam irradiation effectively shortened the thermal stabilization process by one fourth compared with the conventional thermal stabilization process. A comprehensive mechanistic study was conducted regarding this shortening of the thermal stabilization by electron-beam irradiation. Various species of chain radicals were produced in PAN fibers by electron-beam irradiation and existed for a relatively long duration, as observed by electron spin resonance spectroscopy. Subsequently, these radicals were gradually oxidized to peroxy radicals in the presence of oxygen under storage or heating. We found that these peroxy radicals (CO) enabled such an effective shortcut of thermal stabilization by acting as intermolecular cross-linking and partial aromatization points in the low temperature range (100–130 °C) and as earlier initiation seeds of successive cyclization reactions in the next temperature range (>130–140 °C) of thermal stabilization. Finally, even at a low irradiation dose (200 kGy), followed by a short heat treatment (230 °C for 30 min), the PAN fibers were sufficiently stabilized to produce carbon fibers with tensile strength and modulus of 2.3 and 216 GPa, respectively, after carbonization.

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confidence: 99%

“…Recently, pioneering works have been performed by researchers to shorten the thermal stabilization time by ionizing radiation (gamma-ray or electron-beam) or plasma treatment prior to or during stabilization14151617. Among these technologies, electron-beam irradiation was found to be an especially powerful tool for treating polymer fibers.…”

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confidence: 99%

Comprehensive stabilization mechanism of electron-beam irradiated polyacrylonitrile fibers to shorten the conventional thermal treatment

Park

Yoo

Kang

et al. 2016

Sci Rep

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“…It is clear that the color of PAN fibers changed from white to yellow after e-beam irradiation. Previous studies indicate that the color change of PAN after irradiation was caused by the formation of conjugated double bonds (C=C) or color centers associated with radical species trapped within glassy polymer matrices [ 10 , 20 ]. During the course of stabilization, the PAN precursor fibers underwent a change in color from white to yellow, browns and black; this discoloration at elevated temperature is characteristic of acrylic fibers and is attributed to the conjugation bonds and aromatic structures generated by the oxygen-induced reaction of dehydrogenation [ 24 ].…”

Section: Resultsmentioning

confidence: 99%

“…This process consists of a series of sophisticated chemical reactions such as cyclization of the nitrile groups, dehydrogenation of the cross-linking chain molecules, as well as oxidation reaction [ 7 ]. The thermal stabilization reaction is exothermic, and the sudden evolution of heat can partially melt or even ignite the fiber [ 10 ]. Thus, the reaction rate of stabilization has to be restricted by lowering the reaction temperature.…”

Section: Introductionmentioning

confidence: 99%

Rapid and Continuous Preparation of Polyacrylonitrile-Based Carbon Fibers with Electron-Beam Irradiation Pretreatment

Yang

Liu

et al. 2018

Materials

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Thermal stabilization is a critical, yet time- and energy-consuming process during the preparation of PAN-based carbon fibers. In this work, automobile-grade carbon fibers with a 2.85 GPa tensile strength and a 203 GPa modulus are continuously produced with electron-beam (e-beam) irradiation pretreatment and 24 min thermal stabilization. Thermal and structural analyses reveal that e-beam irradiation can lower the onset temperature of the cyclization reaction and mitigate the heat release. Meanwhile, during the process of stabilization, e-beam irradiation can facilitate the evolution of both the chemical structure and the crystalline structure of polyacrylonitrile (PAN) fibers. Comparing to the industrial production of carbon fiber with a 40 min stabilization time, e-beam irradiated PAN fibers can achieve the same degree of stabilization with a 40% time savings.

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“…Various techniques, such as the application of magnetic field , and gamma irradiation have been used to improve the strength of CFs . Kim et al heated the PAN precursor fibers under an atmospheric pressure plasma for 30 min, followed by the carbonization process, thus slightly increased the strength. Naskar et al exposed the PAN fibers to ultraviolet (UV) radiation for a few seconds prior to pre‐oxidizing it at 320°C and resulted in better crosslinking and cyclization.…”

Section: Introductionmentioning

confidence: 99%

Microwave pre‐oxidation for polyacrylonitrile precursor coated with nano‐carbon black

Elagib

Hassan

Cheng

et al. 2018

Polymer Engineering & Sci

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A surface coating was successfully applied through dipping the polyacrylonitrile (PAN) precursor fibers in a carbon black (CB) bath containing a hydrolyzed binder. The coated fibers were pre-oxidized over the microwave furnace at temperatures ranging from 100 C to 170 C for different heating times. The changes in chemical structure were studied by Fourier transfer infrared spectroscopy combined with elemental analyzer. X-ray diffraction was employed to study the crystalline structure and its related parameters. Differential scanning calorimeter and thermogravimetry were used for thermal analysis. In addition, the fiber morphology and the mechanical properties were also evaluated. Scanning electron microscopy results confirmed the presence of CB on the surface of PAN precursor. The analysis in the chemical structure showed an apparent response of coated PAN fibers to the microwave heating, since the microwave field induced the cyclization and crosslinking reactions. The crystallinity and the crystallite height decreased. Furthermore, the tensile strength and elongation of pre-oxidized fibers decreased with the increase of heating time. The measured oxygen content revealed that the pre-oxidized fibers can withstand the high temperatures on the following stage (carbonization). POLYM. ENG. SCI., 59:457-464, 2019.

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Continuous and rapid stabilization of polyacrylonitrile fiber bundles assisted by atmospheric pressure plasma for fabricating large-tow carbon fibers

Cited by 45 publications

References 17 publications

Comprehensive stabilization mechanism of electron-beam irradiated polyacrylonitrile fibers to shorten the conventional thermal treatment

Comprehensive stabilization mechanism of electron-beam irradiated polyacrylonitrile fibers to shorten the conventional thermal treatment

Rapid and Continuous Preparation of Polyacrylonitrile-Based Carbon Fibers with Electron-Beam Irradiation Pretreatment

Microwave pre‐oxidation for polyacrylonitrile precursor coated with nano‐carbon black

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