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

ABSTRACT: 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.

PROVIDER: S-EPMC6117685 | BioStudies | 2018-01-01T00:00:00Z

REPOSITORIES: biostudies

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

Project description: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.

| S-EPMC4923868 | BioStudies

Effects of γ-Ray Irradiation on the Radial Structure Heterogeneity in Polyacrylonitrile Fibers during Thermal Stabilization.

Project description:The radial structural heterogeneity of thermally-stabilized polyacrylonitrile (PAN) fiber is considered to be a limiting factor affecting the mechanical properties of the resulting carbon fibers. In this study, we demonstrate that a low-dose (60 kGy) γ-ray irradiation pretreatment can effectively mitigate the radial structural heterogeneity of PAN fibers after thermal stabilization. The characterization results indicate that low-dose γ-ray irradiation only affects the physical structure of PAN through decreasing its crystalline size and crystallinity, rather than inducing chemical cross-linking and/or intramolecular cyclization. It is proposed that an increased amorphous region in PAN fibers prompted by low-dose γ-ray irradiation can facilitate oxygen diffusion from skin to core during stabilization, which results in the increased structural homogeneity of stabilized PAN fibers.

2018-01-01 | S-EPMC6403893 | BioStudies

Structural Transformation of Polyacrylonitrile (PAN) Fibers during Rapid Thermal Pretreatment in Nitrogen Atmosphere.

Project description:The modification before the stabilization process could tune the exothermic behavior and the structural evolution of PAN fibers during stabilization. In this study, we demonstrate that a rapid thermal pretreatment in nitrogen can effectively mitigate the exothermic behavior of PAN fibers, such as decreasing the initial temperature, broadening the exothermal peak, and decreasing the nominal heat release during heating the fibers in air. The color of fibers has shown gradual changes from white to light yellow, yellow and brown during thermal pretreatment in nitrogen with the increase of pretreating temperature and time. The differential scanning calorimetry (DSC), Fourier Transform Infrared Spectrometer (FTIR), X-ray diffraction (XRD), and Thermogravimetric Analysis (TG) characterization have been applied to analyze the thermal properties, chemical and physical structural difference between PAN, and thermally pretreated PAN fibers. The thermal pretreatment of PAN fibers in nitrogen could induce cyclization, dehydrogenation, and cross-linking reactions, in which the cyclization play an important role on improving the cyclization index of stabilized PAN fibers. Meanwhile, the pretreatment can result in noticeable changes of the aggregation structure of PAN fibers, as indicated by the increase of crystallinity and crystalline size. These structural modifications can benefit the main cyclization reaction during stabilization and enhance the carbon yield in resultant carbon fibers. The rapid thermal pretreatment in nitrogen could increase efficiency of modification on PAN fibers, and that could save much time and energy. It is beneficial to manufacture low-cost carbon fibers and to spread the applications of carbon fibers.

| S-EPMC7023665 | BioStudies

Dry-Jet Wet Spinning of Thermally Stable Lignin-Textile Grade Polyacrylonitrile Fibers Regenerated from Chloride-Based Ionic Liquids Compounds.

Project description:In this paper, we report on the use of amorphous lignin, a waste by-product of the paper industry, for the production of high performance carbon fibers (CF) as precursor with improved thermal stability and thermo-mechanical properties. The precursor was prepared by blending of lignin with polyacrylonitrile (PAN), which was previously dissolved in an ionic liquid. The fibers thus produced offered very high thermal stability as compared with the fiber consisting of pure PAN. The molecular compatibility, miscibility, and thermal stability of the system were studied by means of shear rheological measurements. The achieved mechanical properties were found to be related to the temperature-dependent relaxation time (consistence parameter) of the spinning dope and the diffusion kinetics of the ionic liquids from the fibers into the coagulation bath. Furthermore, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and dynamic mechanical tests (DMA) were utilized to understand in-depth the thermal and the stabilization kinetics of the developed fibers and the impact of lignin on the stabilization process of the fibers. Low molecular weight lignin increased the thermally induced physical shrinkage, suggesting disturbing effects on the semi-crystalline domains of the PAN matrix, and suppressed the chemically induced shrinkage of the fibers. The knowledge gained throughout the present paper allows summarizing a novel avenue to develop lignin-based CF designed with adjusted thermal stability.

| S-EPMC7504658 | BioStudies

Metallic Supports Accelerate Carbonization and Improve Morphological Stability of Polyacrylonitrile Nanofibers during Heat Treatment.

Project description:Electrospun poly(acrylonitrile) (PAN) nanofibers are typical precursors of carbon nanofibers. During stabilization and carbonization, however, the morphology of pristine PAN nanofibers is not retained if the as-spun nanofiber mats are treated without an external mechanical force, since internal stress tends to relax, causing the whole mats to shrink significantly, while the individual fibers thicken and curl. Stretching the nanofiber mats during thermal treatment, in contrast, can result in fractures due to inhomogeneous stress. Previous studies have shown that stabilization and carbonization of PAN nanofibers electrospun on an aluminum substrate are efficient methods to retain the fiber mat dimensions without macroscopic cracks during heat treatment. In this work, we studied different procedures of mechanical fixation via metallic substrates during thermal treatment. The influence of the metallic substrate material as well as different methods of double-sided covering of the fibers, i.e., sandwiching, were investigated. The results revealed that sandwich configurations with double-sided metallic supports not only facilitate optimal preservation of the original fiber morphology but also significantly accelerate the carbonization process. It was found that unlike regularly carbonized nanofibers, the metal supports allow complete deoxygenation at low treatment temperature and that the obtained carbon nanofibers exhibit increased crystallinity.

| S-EPMC8401406 | BioStudies

Thermal, Electrical and Surface Hydrophobic Properties of Electrospun Polyacrylonitrile Nanofibers for Structural Health Monitoring.

Project description:This paper presents an idea of using carbonized electrospun Polyacrylonitrile (PAN) fibers as a sensor material in a structural health monitoring (SHM) system. The electrospun PAN fibers are lightweight, less costly and do not interfere with the functioning of infrastructure. This study deals with the fabrication of PAN-based nanofibers via electrospinning followed by stabilization and carbonization in order to remove all non-carbonaceous material and ensure pure carbon fibers as the resulting material. Electrochemical impedance spectroscopy was used to determine the ionic conductivity of PAN fibers. The X-ray diffraction study showed that the repeated peaks near 42° on the activated nanofiber film were α and β phases, respectively, with crystalline forms. Contact angle, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR) were also employed to examine the surface, thermal and chemical properties of the carbonized electrospun PAN fibers. The test results indicated that the carbonized PAN nanofibers have superior physical properties, which may be useful for structural health monitoring (SHM) applications in different industries.

2015-01-01 | S-EPMC5455402 | BioStudies

Carbonization of single polyacrylonitrile chains in coordination nanospaces.

Project description:It has been over half a century since polyacrylonitrile (PAN)-based carbon fibers were first developed. However, the mechanism of the carbonization reaction remains largely unknown. Structural evolution of PAN during the preoxidation reaction, a stabilization reaction, is one of the most complicated stages because many chemical reactions, including cyclization, dehydration, and cross-linking reactions, simultaneously take place. Here, we report the stabilization reaction of single PAN chains within the one-dimensional nanochannels of metal-organic frameworks (MOFs) to study an effect of interchain interactions on the stabilization process as well as the structure of the resulting ladder polymer (LP). The stabilization reaction of PAN within the MOFs could suppress the rapid generation of heat that initiates the self-catalyzed reaction and inevitably provokes many side-reactions and scission of PAN chains in the bulk state. Consequently, LP prepared within the MOFs had a more extended conjugated backbone than the bulk condition.

| S-EPMC8162375 | BioStudies

High Throughput Centrifugal Electrospinning of Polyacrylonitrile Nanofibers for Carbon Fiber Nonwovens.

Project description:Carbon nanofiber nonwovens are promising materials for electrode or filtration applications; however, their utilization is obviated by a lack of high throughput production methods. In this study, we utilize a highly effective high-throughput method for the fabrication of polyacrylonitrile (PAN) nanofibers as a nonwoven on a dedicated substrate. The method employs rotational-, air pressure- and electrostatic forces to produce fibers from the inner edge of a rotating bell towards a flat collector. We investigate the impact of all above-mentioned forces on the fiber diameter, morphology, and bundling of the carbon-precursor PAN fibers. The interplay of radial forces with collector-facing forces has an influence on the uniformity of fiber deposition. Finally, the obtained PAN nanofibers are converted to carbon nonwovens by thermal treatment.

| S-EPMC8072871 | BioStudies

Tailoring the Stabilization and Pyrolysis Processes of Carbon Molecular Sieve Membrane Derived from Polyacrylonitrile for Ethylene/Ethane Separation.

Project description:For ethylene/ethane separation, a CMS (carbon molecular sieve) membrane was developed with a PAN (polyacrylonitrile) polymer precursor on an alumina support. To provide an excellent thermal property to PAN precursor prior to the pyrolysis, the stabilization as a pre-treatment process was carried out. Tuning the stabilization condition was very important to successfully preparing the CMS membrane derived from the PAN precursor. The stabilization and pyrolysis processes for the PAN precursor were finely tuned, and optimized in terms of stabilization temperature and time, as well as pyrolysis temperature, heating rate, and soaking time. The PAN stabilized at >250 °C showed improved thermal stability and carbon yield. The CMS membrane derived from stabilized PAN showed reasonable separation performance for ethylene permeance (0.71 GPU) and ethylene/ethane selectivity (7.62), respectively. Increasing the pyrolysis temperature and soaking time gave rise to an increase in the gas permeance, and a reduction in the membrane selectivity. This trend was opposite to that for the CMS membranes derived from other polymer precursors. The optimized separation performance (ethylene permeance of 2.97 GPU and ethylene/ethane selectivity of 7.25) could be achieved at the pyrolysis temperature of 650 °C with a soaking time of 1 h. The separation performance of the CMS membrane derived from the PAN precursor was comparable to that of other polymer precursors, and surpassed them regarding the upper bound trade off.

| S-EPMC8781130 | BioStudies

Synthesis of electrospun polyacrylonitrile- derived carbon fibers and comparison of properties with bulk form.

Project description:This study deals with the fabrication of polyacrylonitrile (PAN) nanofibers via an electrospinning process followed by stabilizing and carbonization in order to remove all non-carboneous matter and ensure a pure carboneous material. The as-spun PAN fibers were stabilized in air at 270°C for one hour and then carbonized at 750, 850, and 950°C in an inert atmosphere (argon) for another one hour. Differential scanning calorimetry and Raman spectroscopy were employed to determine the thermal and chemical properties of PAN. Surface features and morphologies of PAN-derived carbon nanofibers were investigated by means of scanning electron microscopy (SEM). SEM micrograms showed that fiber diameters were reduced after carbonization due to evolution of toxic gases and dehydrogenation. The Raman spectra of carbonized fibers manifested D/G peaks. The Raman spectroscopy peaks of 1100 and 500 cm-1 manifested the formation of ? phase and another peak at 900 cm-1 manifested the formation of ?-phase. The water contact angle measurement of carbonized PAN fibers indicated that the nanofibers were superhydrophobic (? > 150o) due to the formation of bumpy and pitted surface after carbonization. In DSC experiment, the stabilized fibers showed a broad exothermic peak at 308°C due to cyclization process. The mechanical andThermal analysis was used to ascertain mechanical properties of carbonized PAN fibers. PAN-derived carbon nanofibers possess excellent physica and mechanical properties and therefore, they may be suitable for many industrial applications such as energy, biomedical, and aerospace.

| S-EPMC6084898 | BioStudies

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