Thermal pre-oxidation of polyacrylonitrile (PAN) fibers is a time-consuming and energy-consuming step in the production of PAN-based carbon fibers. In this paper, the effect of temperature on the structures and properties of PAN fibers cyclized in the supercritical carbon dioxide (Sc-CO2) medium was studied. The thermal behaviors of the PAN fibers were investigated by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). The cyclization reaction was sensitive to the heating temperature and gas atmosphere. The FT-IR results of the PAN fibers treated in the Sc-CO2 confirmed that the degree of cyclization increased with the increase of the cyclization temperature. Compared with the PAN fibers treated in the air, the PAN fibers treated in the Sc-CO2 showed a higher degree of cyclization even at the same temperature. These findings might be related to the osmotic action of Sc-CO2 causing the fibers to be further arranged in a regular manner, which was favorable for the cyclization reaction. Moreover, as one kind of high diffusion and high heat transfer media, the heat release during the cyclization of PAN fibers could be quickly removed by Sc-CO2, which achieved the progress of the rapid-entry cyclization reaction.
In order to obtain F-III fibers with high mechanical properties, pristine F-III fibers were hot drawn at the temperature of 250 °C, pressure of 14 MPa, tension of 6 g·d−1, and different times, which were 15 min, 30 min, 45 min, 60 min, 75 min, 90 min, and 105 min, respectively, in supercritical carbon dioxide (Sc-CO2) in this article. All the samples, including the pristine and treated F-III fibers, were characterized by a mechanical performance tester, wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), and thermogravimetric analysis (TGA). The results showed that the thermal stability of F-III fibers was enhanced to some extent, and the tensile strength and modulus of F-III fibers had great changes as the extension of treatment time during hot drawing in Sc-CO2, although the treatment temperature was lower than the glass transition temperature (Tg) of F-III fibers. Accordingly, the phase fraction, orientation factor fc of the (110) crystal plane, fibril length lf, and misorientation angle Bφ of all the samples were also investigated. Fortunately, the hot drawing in Sc-CO2 was successfully applied to the preparation of F-III fibers with high mechanical properties.
The hot-drawing process of polyacrylonitrile (PAN) fibers is an important step during the production of PAN-based carbon fibers. In this study, supercritical carbon dioxide (Sc-CO2) was used as one kind of media for thermal stretching of PAN fibers to study the effect of different pressures of Sc-CO2 on crystallinity, degree of orientation and mechanical property of PAN fibers during the hot-drawing process. The changes of microstructure and mechanical properties in the PAN fibers were investigated by wide-angle X-ray diffraction, small angle X-ray scattering and monofilament strength analysis. The results showed that as the pressure increased, the crystallinity and degree of orientation of PAN fibers increased. Furthermore, when the pressure was 10 MPa, the crystallinity increased from 69.78% to 79.99%, which was the maximum crystallinity among the different pressures. However, when the pressure was further increased, the crystallinity and degree of orientation of the fibers were reduced. The test results of the mechanical properties were consistent with the trends of crystallinity and degree of orientation, showing that when the pressure was 10 MPa, the tensile strength of the fibers increased from 4.59 cN·dtex−1 to 7.06 cN·dtex−1 and the modulus increased from 101.54 cN·dtex−1 to 129.55 cN·dtex−1.
The present paper provides a solution to enhance the reliability of bonding. The effect of the nonwoven carbon tissue (NWCT) composite adhesive layer on the bonding strength and reliability of aluminum alloy of single lap joints (SLJ) was investigated by embedding NWCT into the epoxy adhesive layer. The bonding strength, Weibull distribution, metallography of cross section, and fracture surface morphology of NWCT specimens were investigated. The results showed that the average bonding strength and Weibull characteristic strength (WCS) of NWCT-reinforced specimen were 16.78 and 17.17 MPa, which increased by 70.2 and 66.7%, respectively, compared with the neat specimen, and the Weibull modulus increased from 11.46 to 22.83, which indicated that NWCT specimens had higher bonding reliability. The mechanism of microcrack formation was obtained by analyzing the cross section of specimen loaded 95% WCS without macroscopic damage. The metallographic section showed that the microcrack of the neat specimen originated from the adhesive–aluminum interface, while the microcracks of the NWCT specimen originated from the interface between short carbon fibers (SCF) and adhesive. Typical failure modes were gained from visual observation and SEM. The failure mode of the neat specimen included more Al–adhesive interface failure, while the NWCT specimen included more internal failure of adhesive–SCFs with the fracture, pullout, peeling, and slippage of SCFs improving the toughness and bonding strength of the adhesive layer. The bridging effect of SCFs in the adhesive layer reinforced by NWCT can even the load and release the stress to improve the bonding reliability.
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