Optimization and investigation of the governing parameters in electrospinning the home‐made poly(l‐lactide‐co‐ε‐caprolactone‐diOH)

Poly(l ‐lactide‐co‐ε‐caprolactone‐diOH) (PCLA) with (ABA)_n type is synthesized using poly(lactic acid) (PLA) and poly(ε‐caprolactone) di‐OH (PCL‐diOH) via chain extending method. FT‐IR, ¹H‐NMR, and GPC data demonstrate that PLA and PCL‐diOH have reacted completely. The product is electrospun into ultrafine fibers subsequently. The optimum electrospinning parameters obtain from an orthogonal experiment are a solvent ratio (DMF/DCM) of 5/5, a polymer concentration of 28 wt %, a collector distance of 20 cm and a voltage of 18 kV. As a result, the average diameter of fibers is 0.77 µm and the uniformity is above 80%. Via range analysis, it is found that the order of the influence on diameter is solvent ratio, applied voltage, collector distance, and polymer concentration, successively. Single effect of the four governing factors on diameter and morphology is also experimentally investigated. This may provide clues for obtaining fibers with various structures by controlling the parameters. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 3600–3610, 2013     

Double‐nozzle air‐jet electrospinning for nanofiber fabrication

A novel double‐nozzle air‐jet electrospinning apparatus was developed to fabricate nanofibers on a large scale. The distribution of the electric field at different nozzle distances was simulated to analyze the jet path, productivity, and deposition area of nanofiber webs and the nanofiber morphology. Our experiments showed that the bubbles usually ruptured intermittently on the top surface of the two nozzles and the jets traveled in a straight path with a high initial velocity. A continuous and even thickness of the nanofiber webs were obtained when the nozzle distances was less than 55 mm. At nozzle distances of 55 mm, the received fibers were thin with the lowest standard deviation. Experimental parameters involving the applied voltage, collecting distance, and air flow rate were also investigated to analyze the nanofiber morphology at a nozzle distance of 55 mm. The results show that the nanofibers presented a finer and thinner diameter at an applied voltage of 36 kV, a collecting distance of 18 cm, and an air flow rate of 800 mL/min. The nanofiber production of this setup increased to nearly 70 times that with a single‐needle electrospinning setup. On the basis of the principle of this air‐jet electrospinning setup, various arrangements of multinozzle electrospinning setups could be designed for higher throughput of nanofibers. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2014 , 131, 40040.     

The effects of processing parameters on the morphology of PLA/PEG melt electrospun fibers

Electrospinning of a polymer melt is an ideal technique to produce highly porous nanofibrous or microfibrous scaffolds appropriate for biomedical applications. In recent decades, melt electrospinning has been known as an eco‐friendly procedure as it eliminates the cytotoxic effects of the solvents used in solution electrospinning. In this work, the effects of spinning conditions such as temperature, applied voltage, nozzle to collector distance and collector type as well as polyethylene glycol (PEG) concentration on the diameter of melt electrospun polylactic acid (PLA)/PEG fibers were studied. The thermal stability of PLA/PEG blends was monitored through TGA and rheometry. Morphological investigations were carried out via optical and scanning electron microscopy. Based on the results, blends were almost stable over the temperature range of melt electrospinning (170 ? 230 °C) and a short spinning time of 5 min. To obtain non‐woven meshes with uniform fiber morphologies, experimental parameters were optimized using ANOVA. While increasing the temperature, applied voltage and PEG content resulted in thinner fibers, PEG concentration was the most influential factor on the fiber diameter. In addition, a nozzle to collector distance of 10 cm was found to be the most suitable for preparing uniform non‐woven PLA/PEG meshes. At higher PEG concentrations, alterations in the collector distance did not affect the uniformity of fibers, although at lower distances vigorous bending instabilities due to polarity augmentation and viscosity reduction resulted in curly fibrous meshes. Finally, the finest and submicron scale fibers were obtained through melt electrospinning of PLA/PEG (70/30) blend collected on a metallic frame. © 2017 Society of Chemical Industry     

Effect of air blowing on the morphology and nanofiber properties of blowing‐assisted electrospun polycarbonates

Polycarbonate (PC) nanofibers are prepared using the air blowing‐assisted electrospinning process. The effects of air blowing pressure and PC solution concentration on the physical properties of fibers and the filtration performance of the nanofiber web are investigated. The air blowing‐assisted electrospinning process produces fewer beads and smaller nanofiber diameters compared with those obtained without air blowing. Uniform PC nanofibers with an average fiber diameter of about 0.170 μm are obtained using an applied voltage of 40 kV, an air blowing pressure of 0.3 MPa, a PC solution concentration of 16%, and a tip‐to‐collection‐screen distance (TCD) of 25 cm. The filtration efficiency improvement of the air blowing‐assisted electrospun web can be attributed to the narrow distribution of fiber diameter and small mean flow pore size of the electrospun web. Performance results show that the air blowing‐assisted electrospinning process can be applied to produce PC nanofiber mats with high‐quality filtration. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

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     

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     

Melt electrospinning of low‐density polyethylene having a low‐melt flow index

Melt electrospinning is a cheaper, more environmentally friendly, and safer alternative to solution electrospinning. We have designed a novel melt spinning device which incorporates a reverse of the normal polarity, with the capillary grounded and the collector grid at positive potential. The apparatus is much simpler and more economical than conventional equipment because no syringe pump is required. Low‐density polyethylene (LDPE) with a low‐melt flow index of 2 g/10 min, which is not suitable for spinning using current commercial methods, was chosen to highlight the advantages of melt electrospinning in general, and our device in particular. The effects of varying the electrospinning parameters such as temperature, electrostatic field, spinning distance, and capillary inner diameter, have been studied. Although it was found that temperatures higher than normal processing temperatures had to be employed in our electrospinning system to reduce the viscosity of the polymer melt sufficiently, good quality fibers with smooth and even surfaces, most of which had diameters smaller than 15 μm, were electrospun successfully. It was observed that there was an optimum point for the spinning distance (14–15 cm) and the capillary inner diameter (0.4–0.6 mm) to get fine fiber. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Morphology of ultrafine polysulfone fibers prepared by electrospinning

Ultrafine fibers of bisphenol‐A polysulfone (PSF) were prepared by electrospinning of PSF solutions in mixtures of N,N‐dimethylacetamide (DMAC) and acetone at high voltages. The morphology of the electrospun PSF fibers was investigated by scanning electron microscopy. Results showed that the concentration of polymer solutions and the acetone amount in the mixed solvents influenced the morphology and the diameter of the electrospun fibers. The processing parameters, including the applied voltage, the flow rate, and the distance between capillary and collection screen, were also important for control of the morphology of electrospun PSF fibers. It was suggested that uniform ultrafine PSF fibers with diameter of 300–400 nm could be obtained by electrospinning of a 20 % (wt/v) PSF/DMAC/acetone (DMAC:acetone = 9:1) solution at 10–20 kV voltages when the flow rate was 0.66 ml h^?1 and capillary–screen distance was 10 cm. Copyright © 2004 Society of Chemical Industry     

Preparation of poly(ether sulfone) nanofibers by gas‐jet/electrospinning

Poly(ether sulfone) (PES) nanofibers were prepared by the gas‐jet/electrospinning of its solutions in N,N‐dimethylformamide (DMF). The gas used in this gas‐jet/electrospinning process was nitrogen. The morphology of the PES nanofibers was investigated with scanning electron microscopy. The process parameters studied in this work included the concentration of the polymer solution, the applied voltage, the tip–collector distance (TCD), the inner diameter of the needle, and the gas flow rate. It was found from experimental results that the average diameter of the electrospun PES fibers depended strongly on these process parameters. A decrease in the polymer concentration in the spinning solutions resulted in the formation of nanofibers with a smaller diameter. The use of an 18 wt % polymer solution yielded PES nanofibers with an average diameter of about 80 nm. However, a morphology of mixed bead fibers was formed when the concentration of PES in DMF was below 20 wt % during gas‐jet/electrospinning. Uniform PES nanofibers with an average diameter of about 200 nm were prepared by this electrospinning with the following optimal process parameters: the concentration of PES in DMF was 25 wt %, the applied voltage was 28.8 kV, the gas flow was 10.0 L/min, the inner diameter of the needle was 0.24 mm, the TCD was 20 cm, and the flow rate was 6.0 mL/h. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Properties of aligned poly(L‐lactic acid) electrospun fibers

Poly(L‐lactic acid) (PLLA)‐aligned fibers with diameters in the nano‐ to micrometer size scale are successfully prepared using the electrospinning technique from two types of solutions, different material parameters and working conditions. The fiber quality is evaluated using scanning electron microscopy (SEM) to judge fiber diameter, diameter uniformity, orientation, and appearance of defects or beads. The smoothest fibers, most uniform in diameter and defect free, were found to be produced from 10% w/v chloroform/dimethylformamide solution using an accelerating voltage from 10–20 kV. Addition of 1.0% multiwalled carbon nanotubes (MWCNT) into the electrospinning solution decreases fiber diameter, improves diameter uniformity, and slightly increases molecular chain alignment. The fibers were cold crystallized at 120°C and compared with their as‐spun counterparts. The influences of the crystalline phase and/or MWCNT addition were examined using fiber shrinkage, temperature‐modulated calorimetry, X‐ray diffraction, and dynamic mechanical analysis. Crystallization increases the glass transition temperature, T_g, slightly, but decreases the overall fiber alignment through shrinkage‐induced buckling of the fibers when heated above T_g. MWCNT addition has little impact on T_g, but significantly increases the orientation of crystallites. MWCNT addition slightly reduces the dynamic modulus, whereas crystallization increases the modulus in both neat‐ and MWCNT‐containing fibers. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41779.     

Effect of ionic salts on the processing of poly(2‐acrylamido‐2‐methyl‐1‐propane sulfonic acid) nanofibers

We studied the effect of nanofiber uniformity on electrospinning due to the charging of added ionic salts, as compared to the droplet current nonadded ionic salts and the charge‐to‐mass ratio of a highly conducting liquid. Various ionic salt concentrations were investigated. For an ionic salt concentration of 0.01 mol %, an applied electric field of 15 kV, and a spinning distance of 15 cm, the experimental results show that uniform nanofibers that did not contain any beads were synthesized with an optimal ionic salt concentration, when the convective current was two orders of magnitude higher than the nonadded ionic salt droplet current. The obtained fibers were uniform, with diameters of around 70 nm. We were able to produce these uniform nanofibers by controlling the balance between two opposing factors during electrospinning, by increasing the number of charge carriers and decreasing the viscosity of the solution. The effect of the ionic salts on the morphology of the electrospun nanofibers was investigated with field‐emission scanning electron microscopy. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 1388–1393, 2005     

Optimization of the electrospinning processing‐window to fabricate nanostructured PE‐b‐PEO and hybrid PE‐b‐PEO/EBBA fibers

An electrospinning technique is used to obtain poly(ethylene‐b‐ethylene oxide) block copolymer (PE‐b‐PEO) fibers. Optimization of the electrospinning processing‐window is carried out by varying the concentration of the block copolymer solution and playing with three different electrospinning parameters, applied voltage, solvent and block copolymer solution flow rate. The influence of the concentration of the block copolymer solution over the length and diameter of the fibers is mainly studied and results indicate that the optimum conditions to fabricate PE‐b‐PEO block copolymer fibers are concentrations between 45 and 47 wt% of PE‐b‐PEO block copolymer and chloroform/DMF mixture ratio of 4:1 and 5:1. Moreover, low solvent and block copolymer solution flow rates led to the longest and widest fibers. Hybrid fibers are also fabricated modifying PE‐b‐PEO block copolymer fibers with low molecular weight N‐(4‐ethoxybenzylidene)?4‐butylaniline (EBBA) nematic liquid crystal using coaxial electrospinning technique. The morphology of the fabricated fibers is investigated from micro to nanoscale. Atomic force microscopy (AFM) results show self‐organization of investigated PE‐b‐PEO and hybrid PE‐b‐PEO/EBBA fibers on the nanometric scale, which make them interesting from the point of view of novel applications as template materials. POLYM. ENG. SCI., 57:1157–1167, 2017. © 2017 Society of Plastics Engineers     

Fabrication of large‐scale superhydrophobic composite films with enhanced tensile properties by multinozzle conveyor belt electrospinning

Large‐scale superhydrophobic composite films with enhanced tensile properties were prepared by multinozzle conveyor belt electrospinning. First, a strategy of conveyor belt electrospinning was introduced for large‐scale fabrication since the conveyor belt can expand the electrospinning area unlimitedly. During the electrospinning (or electrospraying) process, certain kinds of fibers are combined on the conveyor belt in one electrospinning (or electrospraying) step. The superhydrophobicity of electrospun film can be achieved by the presence of PS beads and bead‐on‐string PVDF fibers, while submicron PAN fibers are responsible for the improvement of mechanical properties. The result shows that CA value of the surface comprising of PS beads and bead‐on‐string PVDF fibers could reach up to 155.0°. As the submicron PAN fibers increased, the value of CA decreased, changing from 155.0° to 140.0°, meanwhile the tensile strength of composite film was enhanced from 1.14 to 4.12 MPa correspondingly which is beneficial to putting the films into practice. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39735.     

气流-静电纺丝法制备苯乙烯-丁二烯-苯乙烯嵌段共聚超细纤维

采用75%四氢呋喃(THF)和25%N,N-二甲基甲酰胺(DMF)的混合溶液作溶剂,通过气流-静电纺丝法制备了苯乙烯-丁二烯-苯乙烯嵌段共聚物(SBS)超细纤维。利用扫描电镜(SEM),研究了溶液浓度、电压、接收距离(喷丝孔到接收板的距离)、喷丝孔内径对静电纺纤维的直径和形貌的影响。研究发现:溶液浓度对电纺纤维的直径和形貌有非常重要的影响,当溶液浓度由10%增加到18%时,电纺纤维平均直径随之成线性增加;当电压由23.8kV增加到33.8kV时,纤维平均直径先减小后增加。最佳工艺条件为:溶液质量分数为14%,电压为28.8kV,接收距离为20cm,喷丝孔内径为0.27mm,所得SBS电纺超细纤维平均直径为429nm。     

A Comparison of Electric‐Field‐Driven and Pressure‐Driven Fiber Generation Methods for Drug Delivery

Polymeric fibers are prepared by using electric field driven fiber production technology—electrospinning and pressure driven fiber production technology—pressurized gyration. Fibers of four different polymers: polyvinylidene fluoride (PVDF), poly(methyl methacrylate (PMMA), poly(N‐isopropylacrylamide), and polyvinylpyridine (PVP), are spun by both techniques and differences are analyzed for their suitability as drug carriers. The diameters of electrospun fibers are larger in some cases (PVDF and PMMA), producing fibers with lower surface area. Pressurized gyration allows for a higher rate of fiber production. Additionally, drug‐loaded PVP fibers are prepared by using two poorly water‐soluble drugs (Amphotericin B and Itraconazole). In vitro dissolution studies show differences in release rate between the two types of fibers. Drug‐loaded gyrospun fibers release the drugs faster within 15 min compared to the drug‐loaded electrospun fibers. The findings suggest pressurized gyration is a promising and scalable approach to rapid fiber production for drug delivery when compared to electrospinning.     

Electrospun poly(L‐lactide)/poly(ε‐caprolactone) blend fibers and their cellular response to adipose‐derived stem cells

Polymer blending is one of the most effective methods for providing new, desirable biocomposites for tissue‐engineering applications. In this study, electrospun poly(L ‐lactide)/poly(ε‐caprolactone) (PLLA/PCL) blend fibrous membranes with defect‐free morphology and uniform diameter were optimally prepared by a 1 : 1 ratio of PLLA/PCL blend under a solution concentration of 10 wt %, an applied voltage of 20 kV, and a tip‐to‐collector distance of 15 cm. The fibrous membranes also showed a porous structure and high ductility. Because of the rapid solidification of polymer solution during electrospinning, the crystallinity of electrospun PLLA/PCL blend fibers was much lower than that of the PLLA/PCL blend cast film. To obtain an initial understanding of biocompatibility, adipose‐derived stem cells (ADSCs) were used as seed cells to assess the cellular response, including morphology, proliferation, viability, attachment, and multilineage differentiation on the PLLA/PCL blend fibrous scaffold. Because of the good biocompatibility and nontoxic effect on ADSCs, the PLLA/PCL blend electrospun fibrous membrane provided a high‐performance scaffold for feasible application in tissue engineering using ADSCs. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

气流-静电纺丝法制备聚对苯二甲酸乙二酯纳米纤维

采用50%苯酚和50%1,1,2,2-四氯乙烷的混合溶液为溶剂,通过气流-静电纺丝法制备了聚对苯二甲酸乙二酯(PET)纳米纤维。利用扫描电镜(SEM),研究了聚合物分子质量、溶液浓度、电压、接收距离(喷丝孔到接收板的距离)对电纺纤维形态结构的影响。结果表明:随着聚合物分子质量和溶液浓度增加,纤维平均直径也随之增加;纤维平均直径随电压的增加而减小;随接收距离的增加,纤维平均直径先减小后增加。最佳工艺条件为:聚合物特性黏度为0.818 dL/g,溶液质量分数为15%,电压为32 kV,接收距离为23 cm,所得PET电纺纳米纤维平均直径为85 nm。     

Electrospinning of hydroxypropyl cellulose fibers and their application in synthesis of nano and submicron tin oxide fibers

Synthesis of hydroxypropyl cellulose (HPC) fibers via electrospinning has been demonstrated, for the first time, in this investigation. The HPC solution in two different solvents, anhydrous ethanol and 2-propanol, has been utilized with two different tip-to-collector distance (10 and 15 cm) for synthesizing HPC fibers by varying applied voltage within the range of 10–30 kV. It has been shown that, nano (<100 nm) and submicron (>100 nm) HPC fibers can be obtained under the described electrospinning conditions. Average HPC fiber diameter and its bead formation tendency appear to be a function of nature of the solvent and the applied voltage. Characteristic features of electrospinning of HPC fibers appear to be in consonance with the established mechanism of polymer fiber formation via electrospinning. Use of electrospun HPC fibers in synthesizing and depositing highly porous network of nano and submicron tin oxide (SnO₂) fibers on microelectromechanical systems (MEMS) device has been demonstrated.     

Optimized statically non‐wetting hydrophobic electrospun surface of perfluorocyclobutyl aryl ether polymer

A statically non‐wetting highly hydrophobic fibrous surface was generated from biphenyl perfluorocyclobutyl aryl ether polymer (BP‐PFCB) by electrospinning. The optimization of solution parameters, which include concentration of the solution and number‐average molecular weight of the polymer, was followed by optimization of the instrumental parameters, which include flow rate, inter‐electrode voltage and inter‐electrode distance. Varying these parameters resulted in different degrees of hydrophobicity on the generated surfaces. The degree of hydrophobicity was determined by measuring static water contact angles. The effects of these variations in electrospinning parameters on the thickness of the fibers constituting the surface were also observed. It was found that the hydrophobic nature of the electrospun fibrous surface of BP‐PFCB depended on two factors: fluorine concentration and thickness of the fibers. During the optimization of the parameters, three different morphological regimes, namely beads, beaded fibers and fibers, were observed. The fine tuning of electrospinning parameters eventually produced a statically non‐wetting, highly hydrophobic surface which predominantly consisted of an intricate network of nanoscale fibers. © 2013 Society of Chemical Industry     

Nanofibrous nonwovens based on dendritic‐linear‐dendritic poly(ethylene glycol) hybrids

Dendritic‐linear‐dendritic (DLD) hybrids are highly functional materials combining the properties of linear and dendritic polymers. Attempts to electrospin DLD polymers composed of hyperbranched dendritic blocks of 2,2‐bis(hydroxymethyl) propionic acid on a linear poly(ethylene glycol) core proved unsuccessful. Nevertheless, when these DLD hybrids were blended with an array of different biodegradable polymers as entanglement enhancers, nanofibrous nonwovens were successfully prepared by electrospinning. The pseudogeneration degree of the DLDs, the nature of the co‐electrospun polymer and the solvent systems used for the preparation of the electrospinning solutions exerted a significant effect on the diameter and morphology of the electrospun fibers. It is worth‐noting that aqueous solutions of the DLD polymers and only 1% (w/v) poly(ethylene oxide) resulted in the production of smoother and thinner nanofibers. Such dendritic nanofibrous scaffolds can be promising materials for biomedical applications due to their biocompatibility, biodegradability, multifunctionality, and advanced structural architecture. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45949.