Orthogonal design preparation of phenolic fiber by melt electrospinning

Through orthogonal experimental methods, the melt electrospinning of pure phenolic fibers has been achieved. The preparation is based on an orthogonal experimental method, which was designed to investigate the optimal conditions for production through integrated effects of spinning temperature, gap between spinneret and collector, as well as applied voltage. We found that optimal spinning conditions at 160°C, a spinneret‐to‐collector gap of 8 cm, and applied voltage at 40 kV produce an average electrospun fiber diameter reaching 4.44 ± 0.76 μm, with narrow variance distribution. The fibers were cured in a solution with 18.5% formaldehyde and 12% hydrochloric acid, heated from room temperature to 80°C and maintained 1h. In this report, the morphology, structural changes, and heat resistance of the fibers are characterized. Obtained results reveal that curing the fiber reduces crystallization and improves heat resistance. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42574.     

Morphology of electrospun nylon‐6 nanofibers as a function of molecular weight and processing parameters

In the present study, the morphology and mechanical properties of nylon‐6 nanofibers were investigated as a function of molecular weight (30,000, 50,000, and 63,000 g/mol) and electrospinning process conditions (solution concentration, voltage, tip‐to‐collector distance, and flow rate). Scanning electron micrographs (SEM) of nylon‐6 nanofibers showed that the diameter of the electrospun fiber increased with increasing molecular weight and solution concentration. An increase in molecular weight increases the density of chain entanglements (in solution) at the same polymer concentration; hence, the minimum concentration to produce nanofibers was lower for the highest molecular weight nylon‐6. The morphology of electrospun fibers also depended on tip‐to‐collector distance and applied voltage concentration of polymer solution as observed from the SEM images. Trends in fiber diameter and diameter distribution are discussed for each processing variable. Mechanical properties of electrospun nonwoven mats showed an increase in tensile strength and modulus as a function of increasing molecular weight. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Enhanced mechanical properties of multilayer nano‐coated electrospun nylon 6 fibers via a layer‐by‐layer self‐assembly

We reported the mechanical properties of the polyelectrolyte multilayer nano‐coated electrospun fiber mats with different number of layers. Multilayer nano‐coatings composed of layers of PSS and PAH were successfully deposited onto electrospun nylon 6 fibers via layer‐by‐layer self‐assembly. Compared with pure nylon 6 fibers, the morphology of polyelectrolyte multilayer coated nylon 6 fibers was uniform and smooth. The mechanical properties of polyelectrolyte multilayer coated random and aligned nylon 6 fibers were remarkably enhanced. Moreover, it was found that the higher degree of alignment resulted in higher tensile strength, suggesting the combined effects of the alignment, the surface nanocoating and the formation of internal networks of polyelectrolytes on nylone 6 fibers. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

An investigation into the influence of electrospinning parameters on the diameter and alignment of poly(hydroxybutyrate‐co‐hydroxyvalerate) fibers

Electrospinning is an effective technology for the fabrication of ultrafine fibers, which can be the basic component of a tissue engineering scaffold. In tissue engineering, because cells seeded on fibrous scaffolds with varying fiber diameters and morphologies exhibit different responses, it is critical to control these characteristics of electrospun fibers. The diameter and morphology of electrospun fibers can be influenced by many processing parameters (e.g., electrospinning voltage, needle inner diameter, solution feeding rate, rotational speed of the fiber‐collecting cylinder, and working distance) and solution properties (polymer solution concentration and conductivity). In this study, a factorial design approach was used to systematically investigate the degree of influence of each of these parameters on fiber diameter, degree of fiber alignment, and their possible synergetic effects, using a natural biodegradable polymer, poly(hydroxybutyrate‐co‐hydroxyvalerate), for the electrospinning experiments. It was found that the solution concentration invoked the highest main effect on fiber diameter, whereas both rotational speed of the fiber‐collecting cylinder and addition of a conductivity‐enhancing salt could significantly affect the degree of fiber alignment. By carefully controlling the electrospinning parameters and solution properties, fibrous scaffolds of desired characteristics could be made to meet the requirements of different tissue engineering applications. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Shaping conjugated hollow fibers using a four‐segmented arc spinneret

This study discusses a light‐weight bicomponent hollow fiber that is formed from a low‐density material on the inside, such as polypropylene (PP), and a regularly dyeable material outside, such as polyterephthalate (PET) or nylon. Finite elements and the Optimesh‐3D remeshing approach are adopted to identify the main controlling factors of spinning the sheath‐core hollow fiber without the consideration of winding actions are performed, based on a four‐segmented arc spinneret design. The results indicate that the deflection of melt streams under the spinneret is a major factor that controls the gluing of the gap between arc segments. A greater mismatch between the viscosities of the sheath and the core causes a greater deflection and increases the likelihood of gluing events. Beyond deflection, die swelling under the spinneret is another issue of concern in the processing of bicomponent hollow fibers. Finally, the simulation results are compared with experimental data, and the most appropriate conditions for forming a PET/PP hollow fiber were obtained. POLYM. ENG. SCI., 2011. © 2010 Society of Plastics Engineers     

Rapid prototyping of a miniaturized Electrospinning setup for the production of polymer nanofibers

Fabrication of polymeric micro/nanofibers with controllable size, density, orientation, and composition is required for their translation into functional devices and materials. Electrospinning (ES) is a frequently used fiber fabrication technique, where ES parameters such as the applied electric field strength, architecture of the setup, and solution composition are manipulated to control the fiber properties. Here, we present a bench‐top method for fabricating miniaturized, integrated, and highly tunable ES setups based on shrinkable polymer substrates. We show that using a combination of numerical modeling and controlling different parameters in the ES setup, including the spinneret to collector distance, and spinneret and collector designs, it is possible to tune the density, alignment, and orientation of electrospun fibers. In this way, we have produced 300–600 nm wide poly(ethylene oxide) fibers arranged as nonwoven mats on planar electrodes, aligned fibers on electrode edges, and individual suspended fibers spanning gaps between collector electrodes. The ability to rapidly prototype ES setups should enable us to study the effects of spinneret–collector configurations on fiber morphology, distribution, and conformation and to aid in the development of miniaturized ES setups designed to serve specific applications. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40629.     

喷丝温度对PAN中空纤维成形与性能的影响

利用双弧狭缝孔形喷丝板,采用干喷湿法纺丝工艺,研究了PAN纺丝液在40～70℃喷丝温度范围内,对中空初生纤维成形与性能的影响。结果表明:喷丝温度对纤维截面的成形、外皮层厚度、异形度、中空度、声速取向等均会产生影响。随喷丝温度的增加,初生纤维外皮层厚度减小,纤维内外沿异形度逐渐降低且差距逐渐增加,中空度与声速取向在低温段降低幅度较大,而在高温段降幅减缓。     

Simulation of polyimide fibers with trilobal cross section produced by dry‐spinning technology

As one type of high performance fibers, polyimide fibers can be prepared from polyamic acid (PAA) solution by dry‐spinning technology. The transformation from the precursor of polyamic acid to polyimides via thermal cyclization reaction in the dry‐spinning process is a main distinguishing feature, which is very different from other fibers produced by dry‐spinning such as cellulose acetate fiber and polyurethane fiber. In this report, the dry‐spinning formation of polyimide fibers with trilobal cross section from PAA solution in N,N‐dimethylacetamide is simulated via a one‐dimensional model based on a viscoelastic constitutive equation, combined with profile degree equation of cross section and imidization kinetics equation. The glass transition temperature, imidization degree and profile degree of the filament along the spinline are predicted by the model, as well as relative parameters such as solvent mass fraction and temperature. As a simulated result, solidification of polyimide fibers take place about 150 cm from the spinneret which is farther than for cellulose acetate fiber (70 cm). Moreover, the final profile degree of fiber is affected by many spinning parameters, such as spinning temperature, surface tension, spinning solution concentration, major, and minor axis length of the spinneret hole. POLYM. ENG. SCI., 55:2148–2155, 2015. © 2015 Society of Plastics Engineers     

激光熔融静电纺丝PA6纤维的制备及表征

采用激光熔融静电纺丝法制备了聚已内酰胺(PA6)微纳米纤维和PA6/乙烯-乙烯醇共聚物(PA6/EVOH)复合纤维;研究了接收距离、应用电压和激光电流对PA6纤维直径的影响;并对PA6纤维的结构与性能进行了表征。结果表明:在接收距离13 cm,应用电压23 kV,激光电流35 mA,进料速度7.39 mm/min时,可得到PA6纤维的最小平均直径为1.62μm,与纯PA6纤维相比,PA6/EVOH复合纤维平均直径明显变小,达1.11μm;接收距离与PA6纤维直径之间没有明显的关系;应用电压在12～15 kV时,PA6纤维直径明显下降,在15～24 kV时,PA6纤维的平均直径变化不大;PA6纤维直径随激光电流的增加而减小;红外光谱分析及X射线衍射测试表明,激光熔融静电纺丝PA6纤维的分子链结构没有改变,PA6纤维中存在γ晶型,结晶度为48.7%、     

On the electrospinning of poly(vinyl alcohol) nanofiber mats: A revisit

Electrospinning was used to fabricate mats of poly(vinyl alcohol) (PVA; M_w = 72,000 Da, degree of hydrolysis ≈ 97.5–99.5) nanofibers from PVA solutions in reverse osmotic water. The effects of solution concentration, applied electrical potential, sonication, and collection distance on morphological appearance and diameters of the as‐spun fiber mats as well as those of the individual fibers were carefully investigated mainly by scanning electron microscopy. The effect of the distance from the center of the as‐spun fiber mat on morphological appearance and diameters of the as‐spun fibers was also investigated. The mechanical integrity of some as‐spun PVA fiber mats was also investigated. At all concentrations and applied electrical potentials investigated, the average diameters of the as‐spun PVA fibers ranged between 85 and 647 nm. The use of sonication to prepare a PVA solution caused the viscosity of the solution to decrease; hence, the observed decrease in the average diameters of the as‐spun fibers and the average diameters of the as‐spun fibers were practically the same throughout the as‐spun fiber mat. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Influence of grafting on structural and optical properties of nylon‐6 fibers

This study throws light on the change of the optical properties and some structural properties due to graft copolymerization of polydiallyldimethyl ammonium chloride (PDADMAC) and polyacrylamide (PAA) of nylon‐6 fibers. Multiple‐beam interferometric technique in transmission was used to study the change of the diameter, refractive indices, and birefringence of nylon‐6 fibers at different graft yields. The results were utilized to investigate the isotropic refractive index, the mean polarizabilities per unit volume, dielectric constant, dielectric susceptibility, and surface reflectivity for nylon‐6 and grafted nylon‐6 fiber. The effect of grafted PAA onto modified nylon‐6 fibers containing PDADMAC on the crystallinity was studied by X‐ray diffraction. These results reflect good effect of grafting on the optical and structural properties of nylon‐6 fibers. The opto‐thermal properties of grafted PAA with different graft yields have been studied. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

PA6静电纺纳米纤维

讨论了PA6静电纺丝工艺,利用扫描电镜(SEM)观察纤维的形态结构,研究了影响PA6静电纺丝 的因素及其对所形成纤维的形态、直径的影响。结果表明,在甲酸溶液中,PA6质量分数为8％、电压值为15 kV、喷丝头到收集板的垂直距离为20 cm是PA6静电纺丝的最佳工艺条件,可得到直径小于100 nm的PA6 纳米纤维。     

Needleless Electrospinning from a Tube with an Embedded Wire Loop

Enhancing the production rate while maintaining control in electrospinning has been a challenge for years. This work proposes a novel spinneret from a tube with a single wire loop embedded in its one end. With the feeding of solution precisely controlled and the spinning process stablized, multiple polymer jets can be continuously generated from the wire loop. The as‐spun fibers show nanofibrous structure and its fiber diameter is greatly affected by the applied voltage and polymer concentration. As compared to needle electrospinning, the wire loop spinneret generates a stronger electric field with a larger spinnable area due to its special geometrical structure and a higher applied voltage it is connected to. Slightly coarser nanofibers are fabricated as compared to the nanofibers from needle electrospinning and the production rate is as high as 0.48 g h^?1.     

Assessment of parameters influencing fiber characteristics of chitosan nanofiber membrane to optimize fiber mat production

Electrospun chitosan nanofiber mats have been obtained using chitosan solutions in a mixture of trifluoroacetic acid and dichloromethane. The relationship between processing parameters (solvent composition, polymer concentration in the solution, feeding rate, applied voltage, traveling distance between the needle, and the collector) and fiber morphology was studied. Taguchi's methodology was followed to determine which parameters have the strongest influence on mean fiber diameter and fiber homogeneity. Chitosan nanofibers obtained with this procedure were water soluble due to the protonation of amine side groups but were successfully neutralized by immersion in calcium carbonate solutions. It was established that fiber diameter is mainly determined by the solution concentration and the distance from the needle to the collector while other parameters have less influence. The set of parameters that produce the thinnest fibers were a concentration of 8 wt%, a TFA/DCM ratio of 80:20 (v/v%), a voltage of 30 kV, a flow rate of 6.0 mL/h, a gap distance of 10 cm, using a needle diameter of 0.5, allowing to produce randomly oriented mats with a mean fiber thickness of 66 nm. POLYM. ENG. SCI., 2012. © 2012 Society of Plastics Engineers     

Structure and property study of nylon‐6/clay nanocomposite fiber

The crystal structures of nylon‐6 and nylon‐6/clay fibers were investigated on annealing and drawing. Annealing increased the γ‐crystalline form of both fibers, as indicated by the DSC curves, and its effect was dominant in nylon‐6/clay fiber. On drawing, the γ‐crystalline form was easily converted into the α form in nylon‐6, whereas it was still observed at a relatively high spin‐draw ratio in nylon‐6/clay fiber. However, although the α‐crystal form was dominant in nylon‐6, the γ‐crystal form was dominant in nylon‐6/clay with annealing and drawing, on the basis of the XRD data. The fast crystallization rate of nylon‐6/clay compared with pure nylon‐6 was confirmed, on the basis of the Avrami exponent. The initial modulus of nylon‐6/clay fiber was 30 % higher than the neat nylon‐6 fiber. The reinforcing effect of clay on the dynamic storage modulus was observed. Copyright © 2004 Society of Chemical Industry     

Laser scanning confocal microscope characterization of dye diffusion in nylon 6 fibers treated with atmospheric pressure plasmas

The effect of atmospheric pressure plasma treatment on wettability and dyeability of nylon 6 fibers is investigated. The plasma treatments resulted in an average of 10°–20° decrease in the advancing contact angle and 20°–30° decrease in the receding contact angle. An increased dye diffusion rate of nylon 6 fibers was observed using laser scanning confocal microscope (LSCM). Scanning electron microscope confirmed that the fiber surfaces were roughened, and X‐ray photoelectron spectroscopy showed that the polar groups on the fiber surfaces increased after the plasma treatments. As the plasma treatment time increased, a greater degree of etching was achieved and more polar groups such as hydroxyl and carboxyl groups produced on the surfaces of the nylon 6 fibers, leading to a better wettability and thus a better dyeability of the fiber. This study proved that LSCM may be effectively used in detecting the change of dye diffusion rate in nylon fibers treated with plasmas and the mounting medium should have a close refractive index as the fiber to avoid distortion of the fiber cross section image. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Electrospinning of poly(hydroxybutyrate‐co‐hydroxyvalerate) fibrous tissue engineering scaffolds in two different electric fields

Poly(hydroxybutyrate‐co‐hydroxyvalerate) (PHBV) was electrospun into ultrafine fibrous nonwoven mats. Different from the conventional electrospinning process, which involves a positively charged conductive needle and a grounded fiber collector (i.e., positive voltage (PV) electrospinning), pseudo‐negative voltage (NV) electrospinning, which adopted a setup such that the needle was grounded and the fiber collector was positively charged, was investigated for making ultrafine PHBV fibers. For pseudo‐NV electrospinning, the effects of various electrospinning parameters on fiber morphology and diameter were assessed systematically. The average diameters of PHBV fibers electrospun via pseudo‐NVs were compared with those of PHBV fibers electrospun via PVs. With either PV electrospinning or pseudo‐NV electrospinning, the average diameters of electrospun fibers ranged between 500 nm and 4 μm, and they could be controlled by varying the electrospinning parameters. The scientific significance and technological implication of fiber formation by PV electrospinning and pseudo‐NV electrospinning in the field of tissue engineering were discussed. POLYM. ENG. SCI., 2011. © 2011 Society of Plastics Engineers     

聚醚砜的静电纺丝研究

采用聚醚砜(PES)的良溶剂二甲基甲酰胺(DMF)和非良溶剂丙酮(AC)为共溶剂体系,研究了溶剂组成、纺丝成形条件对静电纺丝PES纤维的形貌及纤维直径的影响。结果表明:DMF/AC的配比对于静电纺丝PES纤维形貌具有直接的调控作用,随着DMF/AC混合溶剂中AC用量的增加,纤维平均直径变大,纤维毡中串珠数目明显减少,纤维均一性变好;随着纺丝液浓度的升高,纺丝电压的增大,纤维的平均直径变大;接收距离的变化对纤维平均直径影响不大;PES最佳纺丝工艺条件为纺丝溶液质量分数13%,纺丝电压15 kV,接收距离10 cm,mDMF/mAC为8.5/1.5,在此条件下,可以获得纤维平均直径为96 nm的PES纤维毡。     

Electrospin of polysulfone in N,N’-dimethyl acetamide solutions

Nanofibers of polysulfone (PSU) were prepared by electro-spinning from 10∼20 wt.% PSU solutions in N,N’-dimethyl acetamide (DMAc) mixed with 0.0∼0.1 wt.% LiCl. With increasing PSU concentration, the morphology of fibers electrospun were bead, mixture of bead-fiber and fiber, and smooth fibers when PSU concentration was 10, 12–15, and 18–20 wt.%, respectively. The bead sizes decreased and fiber diameters increased as PSU concentration was increased. The fiber diameter decreased with increases of the LiCl concentration and the distance from spinneret to collection plate. The fiber diameter also decreased with decreasing solution feeding rate. The fiber diameter distribution electrospun from 20 wt.% PSU solutions was much broader than those electrospun from 18 wt.% PSU solution. For 18 wt.% PSU solution, the average fiber diameter (AFD) decreased when the applied voltage V was increased from 7 to 12 kV. However, for 20 wt.% PSU solutions, the AFD increased when V was increased from 7 to 12 kV. The different morphology of fibers electrospun from 18 and 20 wt.% PSU solutions was attributed to the much higher viscosity of 20 wt.% PSU solution than 18 wt.% PSU solution.     

The Online Measurement of Lyocell Fibers and Investigation of Elongational Viscosity of Cellulose N‐methylmorpholine‐N‐oxide Monohydrate Solutions

In this paper, the development of diameter and surface temperature of Lyocell fibers was measured online. The diameter and tensile force on the spin line in the coagulation bath were traced. The velocity, velocity gradient and the tensile stress profiles development of the fibers in the air gap were studied. The apparent elongational viscosity of cellulose N‐methylmorpholine‐N‐oxide monohydrate (NMMO‐MH) solutions was studied by steady‐state melt spinning theory. The decrease of the fiber diameter was mainly taking place near the spinneret, and the decrease of the diameter became more dramatic with increasing taking‐up speed. The surface temperature of the fibers was also dropping faster with increasing taking‐up speed for the heat transfer coefficient increased. The diameter of the Lyocell fibers almost did not change before and after it entered the coagulation bath. The tensile force on the spin line increases with increasing taking‐up speed and coagulation bath length. The velocity and the tensile stress increase slowly near the spinneret, and then accelerate. The apparent elongational viscosity of cellulose NMMO‐MH solutions decreases with increasing temperature at the same elongation rate and decreases with increasing elongation rate at the same temperature. The fiber of the Lyocell process was not really solidified in the air gap and a gel or rubbery state was formed.