Production of 2-hydroxyethyl methacrylate-g-poly(ethylene terephthalate) nanofibers by electrospinning and evaluation of the properties of the obtained nanofibers

Nanofiber production was investigated from poly(ethylene terephthalate) (PET) polymers functionalized with hydroxyethyl methacrylate (HEMA) by grafting of HEMA monomers onto the PET fibers. HEMA grafted PET (PET-g-HEMA) copolymers were analyzed by scanning electron microscopy, Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy. PET and PET-g-HEMA were dissolved in trifluoroacetic acid and nanofibers were obtained by electrospinning. It was found that the PET and PET-g-HEMA polymers having grafting yield 20 and 55% could be converted to continuous, smooth, and beadles nanofibers. For characterization of the nanofiber membranes, thermogravimetric analysis, differential scanning calorimeter analysis, surface contact angle measurement, porosity analysis, and mechanical tests were applied. When compared with the original PET nanofibers, the thermal properties and degradation process of PET-g-HEMA nanofibers changed according to the amount of HEMA present in the structure of nanofibers. The contact angles of the nanofibers obtained from PET-g-HEMA polymers decreased whereas the water retention ability of the nanofibers increased compared to original PET nanofibers. The porosity of PET-g-HEMA nanofibers was found be high compared to PET nanofibers and whereas the mechanical properties of PET was higher than PET-g-HEMA nanofibers. The obtained nanofibers can be used in many fields such as biomaterial applications.     

The effects of processing variables on electrospun poly(ethylene glycol) fibrous hydrogels formed from the thiol-norbornene click reaction

Electrospinning has been used to create scaffolds with tunable micro/nano architecture, stiffness, and porosity to mimic native extracellular matrix. This study investigated the effects of electrospinning parameters and hydrogel formulation (solvent and crosslinker type) on the architecture and properties of fibrous poly(ethylene glycol) (PEG) hydrogels formed from a photoclick thiol-norbornene reaction. Fibrous hydrogels were prepared using hydrogel precursors (four-arm PEG norbornene and multi-thiol crosslinker), sacrificial poly(ethylene oxide) (PEO, 400 kDa), and photoinitiator (I2959) in either 2,2-triflouroethanol (TFE) or water. Three thiol crosslinkers- 2,2′-(ethylenedioxy)diethanethiol (EDT), pentaerythritol tetrakis(3mercaptopropionate) (PTMP), and PEG dithiol (PEGDT)- were investigated. Fibrous PEG networks with uniform fibers were produced at applied voltages of 10 or 12 kV for TFE and 16 kV for water. Fiber diameters of electrospun hydrogels were largely affected by the solvent when combined with PEO concentration and ranged from 0.5 to 3.5 mm in dry state. While the effect of crosslinker type on fiber diameter, morphology, and porosity of the fibrous hydrogel was minimal, it did modulate its shear modulus. To this end, this study provides the groundwork for selecting processing parameters to achieve desired properties of fibrous PEG thiol-norbornene hydrogels for intended tissue engineering applications ranging from neural, cardiovascular to musculoskeletal.     

Preparation and characterization of octadecane/polyurea nanocapsule‐embedded poly(ethylene oxide) nanofibers

This article describes the preparation and characterization of latent heat storage poly(ethylene oxide) nanofibers (LHS‐PEO nanofibers) with octadecane/polyurea (PCM/PU) nanocapsules. PCM/PU nanocapsules were prepared by interfacial polycondensation from toluene 2,4‐diisocyanate and ethylene diamine in a resin‐fortified emulsion system. LHS‐PEO nanofibers were prepared using an electrospinning procedure with varying PCM/PU nanocapsules content, i.e., from 0 to 8 wt %. The PCM/PU nanocapsules were polydisperse with an average diameter of 200 nm. The melting and freezing temperatures were determined as 23.7 and 28.2°C, respectively, and the corresponding latent heats were determined as 123.4 and 124.1 kJ kg^?1, respectively. The encapsulation efficiency of the PCM/PU nanocapsules was 78.1%. The latent heat capacity of the LHS‐PEO nanofibers increased as the PCM/PU nanocapsules content increased. Defects, such as holes and disconnection of the nanofibers, were observed, particularly inside the LHS‐PEO nanofibers. For packaging applications, mats were fabricated from the nanocapsules‐embedded nanofibers with varying nanocapsule content and the mats’ surface temperatures were monitored with a thermal imaging camera. The results proved the feasibility of using the LHS‐PEO nanofibers for thermal energy storage and functional packaging materials. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42539.     

Transformation of complex internal structures of poly(ethylene oxide)/chitosan oligosaccharide electrospun nanofibers

Electrospun nanofibers with a core–shell structure or an internal microphase‐separated structure were obtained from a homogeneous solution using a conventional single‐nozzle electrospinning setup. Because of the poor miscibility of poly(ethylene oxide) (PEO) and chitosan oligosaccharide (CS), the two polymers will separate into a core–shell structure (PEO as core, CS as shell) or an internal microphase‐separated structure (PEO as discrete phase, CS as continuous phase) depending on the fraction of each component in the solution. Moreover, the core–shell structure transforms to the internal microphase‐separated structure with a continuous decrease of the PEO fraction. The reason for the transition of these internal structures can be attributed to the different phase separation mechanisms. For the core–shell structure, phase separation proceeds in a mechanism of nucleation and growth; however, the internal microphase‐separated structure results from spinodal decomposition. Therefore, wide‐angle X‐ray diffraction and differential scanning calorimetry were employed to investigate PEO crystallization. Since both PEO and CS are biocompatible polymers, together with being able to control the fiber internal structure (core–shell or microphase separation), these electrospun nanofibers will have a great future in the biomedical field. Copyright © 2011 Society of Chemical Industry     

Morphologies of electrospun fibers of lignin in poly(ethylene oxide)/N,N‐dimethylformamide

The effects of polyethylene oxide (PEO) molecular weight (Mv), and volume fraction ( ) on the morphology of electrospun sulfur free softwood lignin nanofibers were investigated. Small amounts of PEO were used during preparations of the solutions to aid the electrospinning process. It was found that tripling the PEO volume fraction resulted in a transition from semi‐dilute un‐entangled to semi‐dilute entangled solutions. Conversely, the solution remained in the semi‐dilute un‐entangled regime as the molecular weight was increased by five times. The effects of molecular weight and volume fraction of PEO both on entanglement density and fiber morphology were unified by scaling PEO viscosities as a function of . We investigated and discussed conditions that would produce smooth fibers and conditions that would produce fibers with beads. In the case of beads‐on‐a‐string formation, bead widths remained constant regardless of the molecular weight and concentration of PEO, but the bead length changed. Additionally, we observed a decrease in the diameter of the fibers and the dimension of beads (length and width of beads) with an increase in the electric field used for electrospinning. The aspect ratio of beads increased with increases to both the electric field and the PEO molecular weight or concentration. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 44172.     

Mechanical properties of poly(ε-caprolactone) composites with electrospun cellulose nanofibers surface modified by 3-aminopropyltriethoxysilane

To enhance the reinforcement effects of regenerated cellulose nanofibers (RC-NF) in poly(ε-caprolactone) (PCL), we synthesized RC-NF-3-aminopropyltriethoxysilane (APS), the surface-modified RC-NF by APS. The RC-NF were fabricated by the saponification of electrospun cellulose–acetate nanofibers. The surface modification by APS was confirmed by the X-ray photoelectron spectroscopy (XPS). To enhance the mechanical property of PCL, the RC-NF and the RC-NF-APS were separately compounded into PCL by compression molding. It was found that, when the fiber concentration of RC-NF-APS was 17 wt %, the Young's modulus at room temperature increased from 698.0 to 744.7 MPa, whereas the storage modulus at 55 °C almost increased from 180 to 220 MPa. The micrographs of the fracture surface of the composites revealed that the surface modification prevented the pull-out of RC-NF from PCL. It was concluded that the mechanical properties of the composites were enhanced due to the improvement of the compatibility between RC-NF and PCL by the surface modification with APS. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48599.     

Fabrication of ceramic nanofibers using polydimethylsiloxane and polyacrylonitrile polymer blends

Nanofibers with several hundred of nanometers were successfully fabricated using electrospinning process and a mixture of two types of polymers which are: polydimethylsiloxane and polyacrylonitrile as precursors. After stabilization and carbonization at 1000 °C, three phases which are: silicon carbide (SiC), carbon, and oxy‐SiC were presented. Spectroscopic and microscopic techniques had confirmed the presence of nanocrystalline SiC and turbostratic carbons. These phases formed an intertwined network at the nanometric scale. In addition, the resulted fibers showed a core‐skin effect with skin richer in carbon and a core mainly dominated by silicon‐based phases in the form SiC or Si? O? C ceramics. A significant improvement was observed in both tensile strength and elastic modulus in these hybrid fibers. In term of crystallography, these nanofibers seem to exhibit similar microstructure that was observed in Nicalon fiber. However, it was difficult to determine the ratio of these phases and their influence on the physical properties of these hybrid fibers. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45967.     

Preparation and surface modification of electrospun aligned poly(butylene carbonate) nanofibers

In this study, aligned poly(butylene carbonate) nanofibers were fabricated by electrospinning with a high‐speed transfer roller as the receiving device. Cold plasma treatment technology was applied to improve its hydrophilicity and activity to expand its application in biological materials. The morphology of the fibers was investigated with scanning electron microscopy. X‐ray diffraction was used to research the impact of the rotation speed on the crystallization and orientation degree of the crystals. The tensile properties of the materials were evaluated by a universal tester. The surface properties of the fibers pretreated by Helium (He) and those grafted with gelatin were evaluated with water contact angle measurement and X‐ray photoelectron spectroscopy. The experimental results indicate that the order degree of fibers, crystallinity, and orientation of the crystalline region, including the mechanical properties, all increased correspondingly with the rotation speed. After plasma pretreatment, the hydrophilicity was improved significantly, and the grafting reaction was realized successfully. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Eudragit E100/poly(ethylene oxide) electrospun fibers for DNA removal from aqueous solution

The development of new strategies for production of low-cost deoxyribonucleic acid (DNA) adsorbents based on electrospun fibers of block copolymers [Eudragit E-100/poly(ethylene oxide) (PEO)] is a promising way for fast retrieval of free of degradation double-stranded DNA chains from aqueous solution. The adsorption takes place through electrostatic interaction between DNA and oppositely charged electrospun fibers that provide high surface area for DNA adsorption. The adsorption capacity observed for electrospun fibers of Eudragit E100/PEO (considering as target molecules the salmon sperm DNA) was in order of 44.31 mg g⁻¹, following the Langmuir model in a typical adsorption at solid/liquid interface (pseudo-second-order model), that characterizes the electrospun fibers as promising templates for removal of biologic components and further use in molecular biology techniques, as DNA amplification by polymerase chain reaction. The reuse and integrity of membranes after long period of adsorption were tested, confirming the potential of material as adsorbent. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47479.     

Effects of reversed arrangement of electrodes on electrospun nanofibers

The process of electrospinning can be affected by various parameters, leading to as‐prepared nanofibers with different morphology and properties. In order to explore the impact of DC(+) high‐voltage position on the resultant nanofibers, two setups with DC(+) high‐voltage individually tethered to the needle (S‐1) and the collecting plate (S‐2) were fabricated. Nanofibers produced by both setups under the same conditions were examined to distinguish their differences in morphology and electrostatic properties. It was found that the nanofibers with positive surface potential produced by the S‐1 setup have a larger surface coverage and porosity, smaller average diameter, and wider distribution of diameters. Furthermore, the differences between both setups in the trajectory of flying jets and the distribution of electric field intensity were studied. The results showed that the volume charge density (VCD) of the flying jets plays a crucial role in determining the morphology and electrostatic properties of the resultant nanofibers. The relationship between the position of DC(+) high‐voltage and the VCD of flying jets was then discussed, which could develop a better understanding of the process of electrospinning and deliver more accurate control over the production of various functional nanofibers. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44687.     

In situ synthesis of iron oxide nanoparticles on poly(ethylene oxide) nanofibers through an electrospinning process

Iron oxide nanoparticle coated poly(ethylene oxide) nanofibers as organic–inorganic hybrids with 200–400‐nm diameters were prepared by the in situ synthesis of iron oxide nanoparticles on poly(ethylene oxide) nanofibers through the electrospinning of a poly(ethylene oxide) solution having Fe²⁺ and Fe³⁺ ions in a gaseous ammonia atmosphere. Transmission electron microscopy analysis proved the presence of iron oxide nanoparticles on the polymer nanofibers. The thermal properties of the nanofiber mat were also studied with differential scanning calorimetry and thermogravimetric analysis techniques. X‐ray diffraction showed that the formed iron oxide nanoparticles were maghemite nanoparticles. The results were compared with those of the electrospinning of a poly(ethylene oxide) solution having Fe²⁺ and Fe³⁺ ions and a pure poly(ethylene oxide) solution in an air atmosphere. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Influence of processing conditions on polymorphic behavior,crystallinity, and morphology of electrospun poly(VInylidene fluoride) nanofibers

The polymorphism and crystallinity of poly(vinylidene fluoride) (PVDF) membranes, made from electrospinning of the PVDF in pure N,N‐dimethylformamide (DMF) and DMF/acetone mixture solutions are studied. Influence of the processing and solution parameters such as flow rate, applied voltage, solvent system, and mixture ratio, on nanofiber morphology, total crystallinity, and crystal phase content of the nanofibers are investigated using scanning electron microscopy, wide‐angle X‐ray scattering, differential scanning calorimetric, and Fourier transform infrared spectroscopy. The results show that solutions of 20% w/w PVDF in two solvent systems of DMF and DMF/acetone (with volume ratios of 3/1 and 1/1) are electrospinnable; however, using DMF/acetone volume ratio of 1/3 led to blockage of the needle and spinning process was stopped. Very high fraction of β‐phase (～79%–85%) was obtained for investigated nanofiber, while degree of crystallinity increased to 59% which is quite high due to the strong influence of electrospinning on ordering the microstructure. Interestingly, ultrafine fibers with the diameter of 12 and 15 nm were obtained in this work. Uniform and bead free nanofiber was formed when a certain amount of acetone was added in to the electrospinning solution. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42304.     

Composite chitosan/poly(ethylene oxide) electrospun nanofibrous mats as novel wound dressing matrixes for the controlled release of drugs

The aim of this study was to develop novel biomedical electrospun nanofiber mats for controlled drug release, in particular to release a drug directly to an injury site to accelerate wound healing. Here, nanofibers of chitosan (CS), poly(ethylene oxide) (PEO), and a 90 : 10 composite blend, loaded with a fluoroquinolone antibiotic, such as ciprofloxacin hydrochloride (CipHCl) or moxifloxacin hydrochloride (Moxi), were successfully prepared by an electrospinning technique. The morphology of the electrospun nanofibers was investigated by scanning electron microscopy. The functional groups of the electrospun nanofibers before and after crosslinking were characterized by Fourier transform infrared spectroscopy. X‐ray diffraction results indicated an amorphous distribution of the drug inside the nanofiber blend. In vitro drug‐release evaluations showed that the crosslinking could control the rate and period of drug release in wound‐healing applications. The inhibition of bacterial growth for both Escherichia coli and Staphylococcus aureus were achieved on the CipHCl‐ and Moxi‐loaded nanofibers. In addition, both types of CS/PEO and drug‐containing CS/PEO nanofibers showed excellent cytocompatibility in the cytotoxicity assays. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42060.     

Properties of electrospun poly(vinyl alcohol) hydrogel nanofibers crosslinked with 1,2,3,4‐butanetetracarboxylic acid

ABSTRACT: Electrospun nanofibrous hydrogel membranes have been gaining significant importance due to the combination of unique physical properties of nanofibers and biocompatibility of hydrogels. Thus, they are considered as potential candidates for medical textile applications. This study deals with electrospinning of poly(vinyl alcohol) (PVA) hydrogel nanofibrous membranes. The chemical crosslinking of PVA with proportionate quantities of 1,2,3,4 butanetetracarboxylic acid (BTCA) was undertaken to form hydrogel structures. Cross‐linked membranes were characterized by scanning electron microscopy, FT‐IR and thermogravimetric analysis, water swelling, and durability tests. FT‐IR analysis demonstrated the formation of ester linkages between PVA and BTCA and thermogravimetric analysis showed that crosslinking improved the thermal stability of the nanofibrous structure. Furthermore, the results indicated that crosslinking with BTCA improved water stability of PVA membranes and the nanofibrous structure was preserved after water treatment. It is envisaged that use of BTCA as a cross‐linker to form hydrogel nanofibers could be a practical and a promising method for medical textile applications, especially for wound dressings given its nontoxicity and immiscibility with polymer solutions. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

The morphology and mechanical properties of sodium alginate based electrospun poly(ethylene oxide) nanofibers

The electrospinning of sodium alginate, a natural biopolymer, was performed from aqueous solutions by blending with PEO, a biodegradable polymer. The conductivity and surface tension of solutions of sodium alginate and PEO were investigated by standard methods. The morphology, thermal, and mechanical properties of the electrospun nanofibers were studied using field emission scanning electron microscopy (FE‐SEM), fourier transform infrared spectroscopy (FT‐IR), energy dispersive X‐ray (EDX), differential scanning calorimetry (DSC) and tensile testing. Uniform, smooth, and ultra‐fine nanofibers with diameters of ～140–190 nm were obtained with solution concentrations of 6–7.2% and sodium alginate/PEO volume ratios of 30:70–50:50. The mechanical strength of the electrospun sodium alginate/PEO mats with good morphology was 21 MPa compared to PEO mats which had a strength of only 10 MPa. POLYM. ENG. SCI., 2009. © 2008 Society of Plastics Engineers     

Carbon nanofibers from renewable bioresources (lignin) and a recycled commodity polymer [poly(ethylene terephthalate)]

Utilizing inexpensive biorenewable and waste raw materials for the production of carbon nanofibers can pave the way for lowering their manufacturing cost. In this research, lignin is combined with recycled poly(ethylene terephthalate) (PET) to fabricate precursor fibers via electrospinning. The process is optimized using the Design of Experiments statistical methodology and fibers with minimum average diameter equal to 191 ± 60 nm are prepared. Investigation with Attenuated Total Reflection – Fourier Transform Infrared Spectroscopy reveals the lignin structural changes induced by the solvent (trifluoroacetic acid), which is used for the preparation of homogeneous solutions of lignin and PET in various concentrations, while it gives an indication of the blending of the two electrospun polymers. The good miscibility between lignin and PET is also confirmed with Differential Scanning Calorimetry. The subsequent carbonization of the precursor fibrous mats results in a fibrous carbon structure with average fiber diameters similar to those of the precursor fibers. The successful transformation into carbon nanofibers is affirmed by Energy Dispersive X‐ray Spectroscopy. The Carbon content of these nanofibers amounts to 94.3%. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43936.     

Crosslinked,electrospun chitosan–poly(ethylene oxide) nanofiber mats

Mechanical characterization of nanofiber mats is an underexplored area in biomaterial engineering. In this study, a chitosan–poly(ethylene oxide) copolymer blend was electrospun and crosslinked with glutaraldehyde (GA) for various time periods. The tensile and compressive mechanical integrity of the nanofibers was analyzed with increasing exposure to vapor crosslinking. Solubility, scanning electron microscopy characterization, Fourier transform infrared, uniaxial tensile tests, and nanoindentation analyses were used to identify these trends. The mechanical studies confirmed that the GA vapor crosslinking increased the stiffness and decreased the ductility of the electrospun mats. Increased exposure time to crosslinking led to changes in the mat surface color and resistance to dissolution. Scanning electron microscopy fiber counts verified that exposure to GA vapor crosslinking increased the average fiber diameter. By the use of vapor phase deposition, mechanical properties continued to change throughout the study. The crosslinking exposure time could be chosen to accommodate in vivo mechanical loading. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Structures and mechanical properties of electrospun cellulose nanofibers/poly(ε-caprolactone) composites

Poly(ε-caprolactone) (PCL) is one of the ecofriendly biodegradable polymers with excellent moldability but with rather low mechanical properties especially for the industrial and biomedical use. In this research, to overcome the problem, the two types of cellulose nanofibers, the cellulose acetate nanofibers (CA-NF) and the cellulose nanofibers (C-NF), were composited into PCL for the enhancement of the mechanical properties of PCL. CA-NF were prepared by electrospinning and converted into C-NF afterward by deacetylation. It was found that the Young's modulus of the CA-NF/PCL composite at the fiber concentration of 35 wt% significantly increased by ~3 times as compared with that of neat PCL, whereas C-NF/PCL of the same fiber concentration also increased by ~4.5 times. It was also found that the Young's moduli of CA-NF/PCL nearly reached the theoretical values calculated by the equation suggested by Tsai, but that the Young's moduli of C-NF/PCL could not reach the theoretical values. It indicates that CA-NF possessed better compatibility with PCL than C-NF, agreeing well with the fracture-surface analyses of the two composites by the scanning electron microscopy.     

Effects of the molecular structure from pitch fractions on the properties of pitch-based electrospun nanofibers

Mesophase pitch was separated into different pitch fractions to investigate the effect of pitch fractions on the properties of their nanofibers prepared by electrospinning. The evolution of different pitch fractions-derived nanofibers during stabilization and carbonization were explored, and the properties of the resultant carbon nanofibers (CNFs) as electrode materials for supercapacitor were compared. Results indicated that the hexane insoluble-toluene soluble (HI-TS) and toluene insoluble-tetrahydrofuran (THF) soluble (TI-THFS) fractions had good spinnability due to their narrow molecular weight distribution. Moreover, compared with HI-TS and THF insoluble (THFI), TI-THFS consisted of appropriate aromaticity and branched alkyl groups which promoted the stabilization and carbonization behaviors of its nanofibers, resulting in maintaining ideal fiber morphology of TI-THFS-derived nanofiber due to the mitigation of their exothermic reactions. Meanwhile, the TI-THFS-derived CNFs presented the highest surface area of 543 m² g⁻¹ and exhibited an excellent specific capacitance of 167 F g⁻¹ at 0.5 A g⁻¹ in 6 M KOH electrolyte.     

Preparation of superhydrophobic nanocomposite fiber membranes by electrospinning poly(vinylidene fluoride)/silane coupling agent modified SiO2 nanoparticles

Superhydrophobic nanocomposite fiber membranes were prepared by blend electrospinning of poly(vinylidene fluoride) (PVDF) mixed with silane coupling agent modified SiO₂ nanoparticles. The nanoparticles were prepared by the sol–gel method, and the average particle diameter was measured by dynamic light scattering (DLS) and transmission electron microscopy (TEM). The effects of the type of silane coupling agent, such as n‐octyltriethoxysilane, vinyltrimethoxysilane (A‐171), and vinyltriethoxysilane (A‐151), and the mass ratio of the modified silica particles and PVDF on the surface wettability of the composite fiber membrane were investigated. The results indicated that the incorporation of silane coupling agent modified silica particles into the PVDF membrane increased the roughness of the surface and formed micro/nano dual‐scale structure compared to the pristine PVDF membrane, which was responsible for the superhydrophobicity and self‐cleaning property of the nanocomposite fiber membranes. The value of water contact angle (CA) increased with the increase of the content of modified SiO₂ nanoparticles in the nanocomposite membrane, ranging from 149.8° to 160.1° as the mass ratio of modified 170 nm SiO₂ with PVDF matrix increased from 0.5:1 to 5:1, indicating the membrane possesses a superhydrophobic surface. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44501.