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

Polymers ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 63 ◽  
Author(s):  
Wei Dang ◽  
Jie Liu ◽  
Xiaoxu Wang ◽  
Kaiqi Yan ◽  
Aolin Zhang ◽  
...  

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.

2017 ◽  
Vol 30 (6) ◽  
pp. 720-730 ◽  
Author(s):  
Zuoqiang Wu ◽  
Shijie Wang ◽  
Lishuai Zong ◽  
Nan Li ◽  
Jinyan Wang ◽  
...  

Phthalonitrile resins exhibit excellent thermostability and mechanical strength after curing. However, poor processability made them difficult to fabricate fiber-reinforced composites with desirable integrated performance. In this article, a novel mixed phthalonitrile resin was developed to be used as the matrix for glass fiber–reinforced laminates. Poly (aryl ether nitrile phthalazinone) oligomer end-capped by phthalonitrile units (PPEN-PN) was firstly designed and blended with bisphenol-based phthalonitrile monomers (BP-PN) (Figure 1), which were obtained according to the literature procedure. A novel mixed curing agent (zinc chloride and 4,4-diamine-diphenylsulfone) was also exploited to accelerate curing rate of the resins. Solubility tests, differential scanning calorimetry and rheological studies revealed that the mixed resins exhibited good processability with low processing viscosity. Thermal gravimetric analysis indicated that the cured resins were stable below 530 to approximately 570 °C in nitrogen atmosphere after low-cost curing procedure. In air, char yields of the resins were between 30 to approximately 40% when heated to 800 °C. The laminates reinforced by E-glass fiber cloth possessed a bending strength of 668 MPa with interlaminar shear strength of 84.6 MPa at room temperature. 50% of the strength and modulus was maintained when heated to 400 °C. Consequently, this type of laminates may be potential candidates for aerospace applications.


Materials ◽  
2018 ◽  
Vol 11 (8) ◽  
pp. 1270 ◽  
Author(s):  
Jia Yang ◽  
Yuchen Liu ◽  
Jie Liu ◽  
Zhigang Shen ◽  
Jieying Liang ◽  
...  

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.


2021 ◽  
Vol 2 (4) ◽  
pp. 454-465
Author(s):  
Ehsan Samimi-Sohrforozani ◽  
Sara Azimi ◽  
Alireza Abolhasani ◽  
Samira Malekian ◽  
Shahram Arbab ◽  
...  

Polyacrylonitrile (PAN) fibers with unique properties are becoming increasingly important as precursors for the fabrication of carbon fibers. Here, we suggest the preparation of porous PAN composite fibers to increase the homogeneity and thermal stability of the fibers. Based on the thermodynamics of polymer solutions, the ternary phase diagram of the PAN/H2O/Dimethylformamide (DMF) system has been modeled to introduce porosity in the fibers. Adding a conscious amount of water (4.1 wt.%) as a non-solvent to the PAN solution containing 1 wt.% of graphene oxide (GO), followed by wet spinning, has led to the preparation of porous composite fibers with high thermal stability and unique physicochemical properties. Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) results elucidate that PAN/GO/H2O porous composite fibers have a higher thermal decomposition temperature, increased residual weight, reduced heat release rate, and higher crystallinity in comparison with the pristine PAN fibers, being a promising precursor for the development of high-performance carbon fibers. The results show a promising application window of the synthesized PAN fibers in electronic and electrochemical devices.


Holzforschung ◽  
2018 ◽  
Vol 72 (9) ◽  
pp. 727-734 ◽  
Author(s):  
Xuefeng Jiang ◽  
Qin Ouyang ◽  
Dapeng Liu ◽  
Jing Huang ◽  
Hongbo Ma ◽  
...  

AbstractLow-cost precursor fibers (PFs) were prepared from blends of a wheat straw lignin (WSL) and a commercial textile-grade polyacrylonitrile (PAN) by wet spinning, and then the precursors were converted into carbon fibers (CFs) by thermal stabilization and carbonization. The PFs were characterized by scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). The lignin content in the blends was found to play an important role in the PF structure, which was closely related to the change of intermolecular forces in the spinning solution. The lignin, acting as the carboxylic acid comonomer, had significantly promoted the thermal stabilization of the lignin/PAN blend PFs, which helped to further decrease the production cost of CFs. With increasing lignin contents, the carbon content of CFs remained at about 95%. The carbon of lignin could be utilized for the preparation of CFs.


2017 ◽  
Vol 68 (8) ◽  
pp. 1895-1902
Author(s):  
Ioana Cristina Tita ◽  
Eleonora Marian ◽  
Bogdan Tita ◽  
Claudia Crina Toma ◽  
Laura Vicas

Thermal analysis is one of the most frequently used instrumental techniques in the pharmaceutical research, for the thermal characterization of different materials from solids to semi-solids, which are of pharmaceutical relevance. In this paper, simultaneous thermogravimetry/derivative thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC) were used for characterization of the thermal behaviour of candesartan cilexetil � active substance (C-AS) under dynamic nitrogen atmosphere and nonisothermal conditions, in comparison with pharmaceutical product containing the corresponding active substance. It was observed that the commercial samples showed a different thermal profile than the standard sample, caused by the presence of excipients in the pharmaceutical product and to possible interaction of these with the active substance. The Fourier transformed infrared spectroscopy (FT-IR) and X-ray powder diffraction (XRPD) were used as complementary techniques adequately implement and assist in interpretation of the thermal results. The main conclusion of this comparative study was that the TG/DTG and DSC curves, together with the FT-IR spectra, respectively X-ray difractograms constitute believe data for the discrimination between the pure substance and pharmaceutical forms.


2016 ◽  
Vol 9 (1) ◽  
pp. 126-136 ◽  
Author(s):  
Dionisio H. Malagón-Romero ◽  
Alexander Ladino ◽  
Nataly Ortiz ◽  
Liliana P. Green

Hydrogen is expected to play an important role as a clean, reliable and renewable energy source. A key challenge is the production of hydrogen in an economically and environmentally sustainable way on an industrial scale. One promising method of hydrogen production is via biological processes using agricultural resources, where the hydrogen is found to be mixed with other gases, such as carbon dioxide. Thus, to separate hydrogen from the mixture, it is challenging to implement and evaluate a simple, low cost, reliable and efficient separation process. So, the aim of this work was to develop a polymeric membrane for hydrogen separation. The developed membranes were made of polysulfone via phase inversion by a controlled evaporation method with 5 wt % and 10 wt % of polysulfone resulting in thicknesses of 132 and 239 micrometers, respectively. Membrane characterization was performed using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), atomic force microscopy (AFM), and ASTM D882 tensile test. Performance was characterized using a 23 factorial experiment using the time lag method, comparing the results with those from gas chromatography (GC). As a result, developed membranes exhibited dense microstructures, low values of RMS roughness, and glass transition temperatures of approximately 191.75 °C and 190.43 °C for the 5 wt % and 10 wt % membranes, respectively. Performance results for the given membranes showed a hydrogen selectivity of 8.20 for an evaluated gas mixture 54% hydrogen and 46% carbon dioxide. According to selectivity achieved, H2 separation from carbon dioxide is feasible with possibilities of scalability. These results are important for consolidating hydrogen production from biological processes.


2021 ◽  
Vol 2 (1) ◽  
Author(s):  
Fausta Loffredo ◽  
Loredana Tammaro ◽  
Tiziana Di Luccio ◽  
Carmela Borriello ◽  
Fulvia Villani ◽  
...  

AbstractTungsten disulfide (WS2) nanotubes (NTs) are examined here as a filler for polylactide (PLA) for their ability to accelerate PLA crystallization and for their promising biocompatibility in relevant to biomedical applications of PLA-WS2 nanocomposites. In this work, we have studied the structural and thermal properties of PLA-WS2 nanocomposite films varying the concentration of WS2 NTs from 0 (neat PLA) to 0.6 wt%. The films were uniaxially drawn at 90 °C and annealed at the same temperature for 3 and 10 min. Using wide angle x-ray scattering, Raman spectroscopy and differential scanning calorimetry, we probed the effects of WS2 NT addition on the structure of the PLA films at various stages of processing (unstretched, stretching, annealing). We found that 0.6 wt% of WS2 induces the same level of crystallinity in as stretched PLA-WS2 as annealing in neat PLA for 10 min. These data provide useful insights into the role of WS2 NTs on the structural evolution of PLA-WS2 composites under uniaxial deformation, and extend their applicability to situations where fine tuning of PLA crystallinity is desirable.


2019 ◽  
Vol 3 (2) ◽  
pp. 35 ◽  
Author(s):  
Miguel Reis Silva ◽  
António M. Pereira ◽  
Nuno Alves ◽  
Gonçalo Mateus ◽  
Artur Mateus ◽  
...  

This work presents an innovative system that allows the oriented deposition of continuous fibers or long fibers, pre-impregnated or not, in a thermoplastic matrix. This system is used in an integrated way with the filamentary fusion additive manufacturing technology and allows a localized and oriented reinforcement of polymer components for advanced engineering applications at a low cost. To demonstrate the capabilities of the developed system, composite components of thermoplastic matrix (polyamide) reinforced with pre-impregnated long carbon fiber (carbon + polyamide), 1 K and 3 K, were processed and their tensile and flexural strength evaluated. It was demonstrated that the tensile strength value depends on the density of carbon fibers present in the composite, and that with the passage of 2 to 4 layers of fibers, an increase in breaking strength was obtained of about 366% and 325% for the 3 K and 1 K yarns, respectively. The increase of the fiber yarn diameter leads to higher values of tensile strength of the composite. The obtained standard deviation reveals that the deposition process gives rise to components with anisotropic mechanical properties and the need to optimize the processing parameters, especially those that lead to an increase in adhesion between deposited layers.


2021 ◽  
Vol 21 (10) ◽  
pp. 5235-5240
Author(s):  
Hua-Hui Chen ◽  
Jing-Jing Cao ◽  
Hai-Ping Hong ◽  
Nan Zheng ◽  
Jie Ren ◽  
...  

In Situ transformed carbon fibers/Al2O3 ceramic matrix nanocomposites with Cao–MgO–SiO2 sintering agent were prepared by hot-pressed sintering technology in vacuum. In the sintering process, pre-oxidized polyacrylonitrile fibers (below named as pre-oxidized PAN fibers) were used as the precursors of In Situ transformed carbon fibers. The micro/nanostructure of composites and interface between In Situ transformed carbon fibers and matrix were investigated, as well as the properties of composites. The results showed that the composites could be sintered well at a relatively low temperature of 1650 °C. During the sintering, the precursors, pre-oxidized PAN fibers, were In Situ transformed into carbon fibers, and the In Situ transformed carbon fibers had the graphitelike structure along the fiber axial direction. The carbon atoms arrangement in the surface layer of the fiber was more orderly than the core. A typical diffraction peak of carbon fiber at 26°, which corresponded to the (002) crystal plane, was observed, and the inter-planar spacing was approximately 0.34 nm. The CaO–MgO–SiO2 sintering agent formed MgAl2O4 and CaAl2Si2O8 phases in the interface between In Situ transformed carbon fibers and matrix, therefore improving the interface bonding, and thereby modifying the mechanical properties of the composites.


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