Electrospun SiO<Subscript>2</Subscript>/PMIA nanofiber membranes with higher ionic conductivity for high temperature resistance lithium-ion batteries

The nanofiber membrane prepared by electrospinning has been widely applied in lithium-ion batteries. A powerful strategy for designing, fabricating and evaluating Poly-m-phenylene isophthalamide (PMIA) nanofiber membrane with SiO₂ nanoparticles was developed by electrospinning in this paper. The morphology, crystallinity, thermal shrinkage, porosity and electrolyte uptake, and electrochemical performance of the SiO₂/PMIA nanofiber membranes were investigated. It was demonstrated that the nanofiber membrane with 6 wt% SiO₂ possessed notable properties, such as better thermal stability, higher porosity and electrolyte uptake, resulting in higher ionic conductivity (3.23×10^-3 S·cm^-1) when compared with pure PMIA nanofiber membrane. Significantly, the SiO2/PMIA nanofiber membrane based Li/LiCoO₂ cell exhibited more excellent cycling stability with capacity retention of 95 % after 50 cycles. The results indicated that the SiO₂-doped PMIA nanofiber membranes had a potential application as separator in high temperature resistance lithium-ion batteries.     

Electrospinning of <Emphasis Type="Italic">Bombyx mori</Emphasis> silk fibroin nanofiber mats reinforced by cellulose nanowhiskers

Cellulose nanowhisker (CNW) reinforced electrospun Bombyx mori silk fibroin (SF) nanofibers were fabricated. The morphology, structure, and mechanical properties of nanofibers were investigated by FE-SEM, TEM, FTIR, and tensile testing. It was found that the nanofiber size decreased obviously from 250 nm in the unreinforced mat to 77–160 nm in the CNW reinforced mats depending on the CNW content due to the increased conductivity of spinning dope. In the reinforced mats, the CNWs were embedded in the SF matrix separated from each other, and aligned along the fiber axis. There was a positive correlation between the CNW content and the tensile strength and Young’s modulus of reinforced mats. However the strain at break dropped gradually with the increase of CNW. When the CNW content was 2 w/w%, the tensile strength and Young’s modulus of reinforced SF nanofiber mats were about 2 times higher than those of unreinforced mat.     

Preparation and characterization of PVA/PU blend nanofiber mats by dual-jet electrospinning

A series of blend nanofiber mats comprising poly(vinyl alcohol) (PVA) and polyurethane (PU) were prepared by dual-jet electrospinning in various parameters. Orthogonal experimental design was used to investigate how those parameters affected on fiber diameters and fiber diameter distribution. Altogether three parameters having three levels each were chosen for this study. The chosen parameters were tip-to-collector distance (TCD), voltage and tip-to-tip distance (TTD). Fiber diameters, thermal properties, mechanical properties and hydrophilicity of the blend nanofiber mats were examined by scanning electron microscopy (SEM), thermogravimetric analysis (TGA), tensile test, contact angle and water absorption test, respectively. The results showed that the optimum conditions for PVA/PU blend nanofiber mats fabricated by dual-jet electrospinning were TCD of 20 cm, voltage of 18 kV and TTD of 4 cm. Besides, the thermal stability of PVA/PU blend nanofiber mats had been improved compared with pure nanofibers. Furthermore, the elongation and tensile strength of the blend nanofiber mats were significantly increased compared with pure PVA and pure PU, respectively. And the blend nanofiber mats exhibited well hydrophilicity.     

Comparison study on transparent composites with different patterns of nanofiber reinforcement

In this work, PA-6 core and PMMA shell composite nanofiber mats together with pure PMMA and PA-6 nanofibrous membranes were obtained through electrospinning. Two kinds of transparent composites were fabricated by hot pressing multilayers of the composite nanofiber mats and of the interlaced pure PA-6 with PMMA nanofibrous membranes, respectively, under the same processing condition and with the same amount of PA-6 nanofiber content. Tensile properties and visible light transmittances of the two transparent composites were characterized. It has been found that both the tensile behavior and the visible light transmittance of the composites obtained from the composite nanofiber mats were better than the counterparts from the interlaced pure PA-6 and PMMA nanofibrous membranes. With a minor loss of less than 10 % in the transparency, a maximal increase of around 20 % in the tensile modulus and tensile strength has been recognized for a transparent composite from the composite nanofibers. Although less efficient, the tensile strengths of the composites from the interlaced nanofibrous membranes were all higher than that of a transparent panel processed from the pure PMMA nanofibers.     

Metal ion adsorbability of electrospun wool keratose/silk fibroin blend nanofiber mats

In this study, electrospun wool keratose (WK)/silk fibroin (SF) blend nanofiber was prepared and evaluated as a heavy metal ion adsorbent which can be used in water purification field. The WK, which was a soluble fraction of oxidized wool keratin fiber, was blended with SF in formic acid. The electrospinnability was greatly improved with an increase of SF content. The structure and properties of WK/SF blend nanofibers were investigated by SEM, FTIR, DMTA and tensile test. Among various WK/SF blend ratios, 50/50 blend nanofiber showed an excellent mechanical property. It might be due to some physical interaction between SF and WK molecules although FTIR result did not show any evidence of molecular miscibility. As a result of metal ion adsorption test, WK/SF blend nanofiber mats exhibited high Cu²⁺ adsorption capacity compared with ordinary wool sliver at pH 8.5. It might be due to large specific surface area of nanofiber mat as well as numerous functional groups of WK. Consequently, the WK/SF blend nanofiber mats can be a promising candidate as metal ion adsorption filter.     

Preparation and characterization of bacterial cellulose/hydroxypropyl chitosan blend as-spun fibers

In the work, N-methylmorpholine-N-oxide monohydrate (NMMO·H₂O) was used as a solvent to solve bacterial cellulose (BC) and hydroxypropyl chitosan (HPCS) together, and regenerated bacterial cellulose (RBC)/HPCS blend as-spun fibers were prepared by blending BC with HPCS via wet-spinning in the Lyocell process. Structure and properties of the blend as-spun fibers were characterized by different techniques, together with the antibacterial activity of the blend as-spun fibers against Staphylococcus aureus. Results revealed that HPCS was mixed with BC very well. The blend as-spun fibers showed a rough and folded surface morphology and an interior pore structure on the cross-section. Compared with pure RBC as-spun fibers, the blend as-spun fibers had lower degree of crystallinity and thermal stability. Although extension at break of the blend as-spun fibers was lower than the pure RBC as-spun fibers, their tensile strength and modulus had been enhanced obviously. The blend as-spun fibers were also found to exhibit excellent antibacterial activities against S. aureus.     

Electrospun poly(ɛ-caprolactone)/nanoclay nanofibrous mats for tissue engineering

Nanofibrous mats of poly (?-caprolactone)/nanoclay nanocomposites were fabricated using electrospinning method. Effects of nanoclay content of the nanocomposite on final nanofiber structures were investigated and characterized by scanning electron microscope (SEM) and differential scanning calorimetry (DSC) analysis. The results showed that the presence of the nanoclay promoted the creation of fibrous structure in comparison with solely poly (?-caprolactone). Furthermore, increase in nanoclay content led to the formation of more uniform nanofiber structures and caused a decrease in the mean nanofiber diameter. DSC results showed that the addition of nanoclay reduced the crystallinity of the nanocomposite in compared with pristine PCL. Studies of the mechanical properties, wettability and degradability showed that the presence of nanoclay improved tensile modulus, tensile strength, wettability and biodegradability of the nanocomposites. To evaluate the effect of nanoclay on the cell adhesion and bioactivity of the poly (?-caprolactone)/nanoclay nanocomposites, fibroblasts cells were seeded on the mats. The results showed that the prepared nanocomposite could be a potential candidate for tissue engineering.     

Functional electrospun cellulosic nanofiber mats for antibacterial bandages

Functionalization of cellulosic nanofibers was established to develop antibacterial bandages. The functionalization was conducted through preparation of carboxymethyl cellulose (CMC) containing different metal nanoparticles (MNPs) such as copper nanoparticles (CuNPs), iron nanoparticles (FeNPs) and zinc nanoparticles (ZnNPs). Fourier Transform Infrared spectroscopy was used to characterize CMC containing MNPs and scanning electron microscopy coupled with high energy dispersive X-ray (SEM-EDX) to study the surface morphology of CMC with and without MNPs. Furthermore, back scattering electron detector was used to show the position of metal nanoparticles on the microcrystalline CMC. In addition, UV-visible spectroscopy was used to confirm MNPs formation. Nanofiber mats of CMC containing MNPs were synthesized using electrospinning technique. Surface morphology of electrospun CMC containing MNPs was characterized using SEM. The obtained data revealed that elctrospun CMC nanofibers containing MNPs were smooth and uniformly distributed without bead formation. The average fiber diameters were in the range of 150 to 200 nm and the presence of MNPs in the nanofiber did not affect the size of the electrospun nanofiber diameter. Transmission electron microscopy (TEM) images displayed that MNPs were existed inside and over the surface of the electrospun nanofibers without any agglomeration. The average particle diameters of MNPs were 29-39 nm for ZnNPs, 23-27 nm for CuNPs and 22-26 nm for FeNPs. Moreover, Water uptake of electrospun nanofiber mats and the release of MNPs from nanofibers were evaluated. Nevertheless, electrospun CMC nanofibers containing MNPs had an excellent antibacterial activity against Gram-negative bacteria Escherichia coli and Gram-positive bacteria Staphylococcus aureus.     

Effect of thermal annealing on mechanical properties of polyelectrolyte complex nanofiber membranes

Optimization of mechanical properties is required in the applications of tissue-engineered scaffolds. Thermal annealing strategy is proposed to improve the mechanical properties of polyelectrolyte complex nanofiber membranes. The effects of annealing on the structural and mechanical properties of electrospun chitosan-gelatin (CG) nanofiber membranes were investigated using tensile tests, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and differential scanning calorimetry (DSC). Tensile test results showed that annealing processing at 90 °C produced 1.3-fold and 1.1-fold increase on Young’s modulus and tensile strength, respectively. By scanning electron microscopy (SEM) observation, it was found there was a formation of partial interfiber bonding when annealing temperature was elevated over the glass transition temperature (T _g ) of CG nanofibers. FTIR results showed enhanced molecular interactions within fibers, suggesting that annealing treatment promoted the conjunction between chitosan and gelatin. In contrast, no detectable changes in crystallinity for CG nanofiber specimens were exhibited on XRD patterns following annealing treatment. In addition, thermal annealing induced the improvement in thermal stability, aqueous stability and swelling capacity. Therefore, annealing is proved to be an effective strategy for mechanical enhancement of polyelectrolyte complex nanofibrous scaffolds. The enhanced stiffness and strength is mainly attributed to the formation of interfiber bonding and strengthened molecular interactions between chitosan and gelatin.     

Solution Blowing of Polyacrylonitrile Nanofiber Mats Containing Fluoropolymer for Protective Applications

A new type of hydrophobic polyacrylonitrile (PAN) nanofiber is fabricated by solution blowing of a blend solution of fluorine-containing polyacrylate (FPA) and PAN. The nanofibers’ surface composition, hydrophobicity, and protection ability were evaluated to clarify the effects of FPA addition. Results revealed that FPA addition increased the nanofiber diameter, as well as enhanced the hydrophobicity and transport properties of the nanofiber mats. The mats had average water contact angles of 123.44°, 132.11°, and 137.11° for FPA contents of 0.66 wt%, 1.98 wt%, and 3.30 wt%, respectively. All these results suggested the potential of the solution blowing nanofiber mats as protection materials.     

EDC/NHS crosslinked electrospun regenerated tussah silk fibroin nanofiber mats

The tussah silk fibroin (TSF) nanofibers with 611 nm diameters were prepared by electrospinning with the solvent hexafluoroisopropanol (HFIP). And then, the TSF nanofibers were crosslinked by 1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide/N-Hydroxysuccinimide (EDC/NHS) crosslinking agent. The morphology and microstructure of the crosslinked TSF nanofibers were characterized by scanning electron microscopy (SEM), Fourier transforms infrared analysis (FTIR), X-ray diffraction, Instron electronic strength tester, and cell culture. After treatment with EDC/NHS crosslinking agent, the TSF nanofibers swelled and its average diameter increased from 611 to 841 nm. FTIR and X-ray diffraction results demonstrated that random coil, ??-helix, and ??-sheet co-existed in the TSF nanofiber mats, but the content of ??-sheet increased from 25.26 to 45.34 %, and the random coil content decreased from 32.47 to 24.94 %. Compared with the electrospun pure TSF nanofiber mats, the crosslinked TSF nanofiber mats exhibited a lower breaking tenacity and initial modulus, which were 5.51 MPa and 9.86 MPa, respectively. At the same time, the extension at break of the crosslinked TSF nanofiber achieved 109.38 %. In cell culture evaluation, the crosslinked TSF nanofibers were found to support cell adhesion and spreading fibroblast L373 and bone marrow mesenchymal stem cells (BMSCs), which had potential utility in a range of tissue engineering.     

Effect of degree of polymerization on the mechanical properties of regenerated cellulose fibers using synthesized 1-allyl-3-methylimidazolium chloride

1-Ally-3-methylimidazolium chloride ([AMIM]Cl) was successfully synthesized and was used as a green spinning solvent for cellulose. The celluloses of various degrees of polymerization (DP) were dissolved in the [AMIM]Cl to obtain 5 % (w/w) cellulose solutions, which were regenerated to cellulose fibers through wet spinning process. Of three different regenerated cellulose fibers with different DPs, a DP of 2,730 was gave the strongest regenerated fiber without drawing having a tensile strength of 177 MPa and an elongation at break of 9.6 % respectively, indicating that celluloses of higher molecular weight can be entangled and oriented more easily. Also maximum draw ratio of the as-spun fibers increased from 1.2 to 1.7 with increasing degree of polymerization leading to a tensile strength and modulus of 207 MPa and 48 GPa, respectively. Particularly the tensile modulus was substantially higher than those of lyocell and high performance viscose fibers of 20 GPa or less. The higher DP of pristine cellulose was critical in increasing the mechanical properties such as tensile strength and elongation at break of the as-spun fibers coupled with higher tensile modulus after drawing.     

Electrospun nanostructures based on polyurethane/MWCNTs for strain sensing applications

Electrically conductive nanofibers were fabricated from elastic polyurethane (PU) and PU/multiwalled carbon nanotubes (MWCNTs) nanocomposite by electrospinning method. The nanocomposites were electrospun at various MWCNTs loading. Electron microscopy was used to investigate nanofibers morphology and dispersion of MWCNTs in the electrospun nanofibers. The results showed that the presence of the MWCNTs promoted the creation of fibrous structures in comparison with the PU without MWCNTs. On the other hand, increasing the MWCNTs content resulted in a slight increase in the average fiber diameter. TEM micrographs and mechanical properties of the electrospun mats indicated that the homogeneous dispersion of MWCNTs throughout PU matrix is responsible for the considerable enhancement of mechanical properties of the nanofiber mats. Electrical behavior of the conductive mats was also studied, in view of possible sensor applications. Cyclic experiments were conducted to establish whether the electrical properties were reversible, which is an important requirement for sensor materials.     

Preparation and characterization of nylon-6/gelatin composite nanofibers via electrospinning for biomedical applications

Easy fabrication, porosity, good mechanical properties, and composition controllable of the electrospun nanofiber mat make this material a promising candidate for wound dressing applications. In the present study, nylon6/gelatin electrospun nanofiber mats are introduced as novel wound dressing materials. The introduced mats were synthesized by electrospinning of nylon6 and gelatin mixtures, three mats containing different gelatin content were prepared; 10, 20 and 30 wt%. Interestingly, addition of the gelatin did not affect the mechanical properties of the nylon 6, moreover the mat containing 10 wt% gelatin revealed higher mechanical properties due to formation of spider-net like structure from very thin nanofibers (～10 nm diameter) bonding the main nanofibers. Biologically study indicates that gelatin incorporation strongly enhances the bioactivity performance as increasing the gelatin content linearly increases the MC3T3-E1 cell attachment. Overall, the obtained results recommend exploiting the introduced mats as wound dressing material.     

Application of electrospun silk fibroin nanofibers as an immobilization support of enzyme

Silk fibroin (SF) nanofibers were prepared by electrospinning and their application as an enzyme immobilization support was attempted. By varying the concentration of SF dope solution the diameter of SF nanofiber was controlled. The SF nanofiber web had high capacity of enzyme loading, which reached to 5.6 wt%. The activity of immobilizedα-chymotrypsin (CT) on SF nanofiber was 8 times higher than that on silk fiber and it increased as the fiber diameter decreased. Sample SF8 (ca. 205 nm fiber diameter) has excellent stability at 25°C by retaining more than 90 % of initial activity after 24 hours, while sample SF11 (ca. 320 nm fiber diameter) shows higher stability in ethanol, retaining more than 45% of initial activity. The formation of multipoint attachment between enzyme and support might increase the stability of enzyme. From these results, it is expected that the electrospun SF nanofibers can be used as an excellent support for enzyme immobilization.     

Thermal degradation behaviors and fire retardant properties of poly(1,3,4-oxadiazole)s (POD) and poly(m-phenylene isophthalamide) (PMIA) fibers

Thermal degradation behaviors and fire retardant properties of poly(1,3,4-oxadiazole)s (POD) and poly(m-phenylene isophthalamide) (PMIA) fibers were investigated. The thermal gravimetric analysis (TGA) demonstrated that POD exhibited higher onset thermal degradation temperature (T_onset) than PMIA, exceeding nearly 80 °C. The thermal degradation kinetics, evaluated by the modified Coats-Redfern method, displayed that the apparent activation energy (E_a) of POD and PMIA fibers was similar when the conversion rate (α) ranges from 0.2 to 0.5, while with the α from 0.6 to 0.8, the E_a of POD was significantly lower than that of PMIA. The fire retardant performance of POD and PMIA fibers were evaluated by cone calorimeter under heat fluxes of 35, 50 and 75 kW/m², during which the temperature of the fibers were monitored by a thermocouple. Surprisingly, POD fibers showed inferior fire retardant performance in comparison with PMIA, with lower time to ignition (TTI) and higher peak heat release rate (PHRR). The origin of the different fire retardant properties of both fibers was revealed by analyzing the residual chars and gaseous products during thermal pyrolysis. The morphology confirmed that stable and compact chars can be formed in PMIA. In addition, the Fourier Transform Infrared Spectroscopy (FTIR) characterization of the residual char revealed that POD can form carbonaceous chars at the heat flux of 50 kW/m², while the heat flux of PMIA was 75 kW/m². The pyrolysis products characterized by pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) indicated that POD can be pyrolyzed completely at 600 °C, while the temperature of PMIA was 700 °C.     

Fabrication of silver nanoparticle/polyvinyl alcohol/polycaprolactone hybrid nanofibers nonwovens by two-nozzle electrospinning for wound dressing

In this study, two biodegradable polymers, polycaprolactone (PCL) and polyvinyl alcohol (PVA) were used to fabricate nanofiber nonwovens (NFNs). Also, the silver nanoparticles (AgNPs) successfully reduced by using tea polyphenols (TP) and incorporated in the NFNs via electrospinning. The morphologies of the NFNs and AgNPs were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), respectively. The PCL nanofibers and PVA nanofibers interweaved each other, and AgNPs with average diameter 1.53±0.15 nm were embedded in the PVA nanofibers. The properties of electrospun NFNs were characterized by pore property, swelling/weight loss, water contact angle, mechanical property, and antibacterial activity. The nanofibers cross-linked to each other forming the 3Dnetwork porous structure with diameter about 1-1.5 μm. Although the hydrophobic PCL was added in the hybrid NFNs, the NFNs still showed hydrophilic propriety, high swelling degree (i.e. swelling degree is 330 % for 48 h), and low weight loss (i.e. weight loss is 22.4 % for 48 h). Also, the hybrid PCL/PVA/AgNPs NFNs exhibited a suitable mechanical property for wound dressings (i.e. tensile strength is 4.27 MPa, and breaking elongation is 88 %). Moreover, the hybrid NFNs effectively inhibited growth of Escherichia coli and Staphylococcus aureus. In summary, this PCL/PVA/AgNPs NFNs may provide a promising candidate for accelerating wound healing.     

Solution blowing nylon 6 nanofiber mats for air filtration

Solution blowing process is a new nanofiber fabricating method with high productivity. In the present study, nylon 6 nanofiber mats were solution blown and the effects of spinning conditions on nanofibers morphology were investigated. The fiber diameter ranged from 150 to 750 nm which was affected by solution concentration, gas pressure and solution feeding rate. The solution blown fibers were three-dimensional curly which made loose construction in bulk. The filtration performance of solution blown mats was evaluated. The tested solution blown nanofiber mats showed high filtration efficiency of 83.10 % to 93.45 % for 0.3 µm particles filtration and extremely low pressure drop of 15.37 to 30.35 Pa. The results indicate the solution blown nanofiber mats will find potential application of high efficiency and low resistance filter.     

Facile fabrication of carbon nanotubes/polystyrene composite nanofibers for high-performance electromagnetic interference shielding

Polystyrene (PS) composites with nanofibrous structure consisting of multi-walled carbon nanotubes (MWCNTs) with 0-10 wt.% of nanofiller have been fabricated via electrospinning technique. The surface morphology and thermal properties of the composites were evaluated by scanning electron microscopy (SEM) and thermo-gravimetric analysis (TGA). The SEM analysis of the composite nanofibers samples revealed that the average diameter of the nanofibers increases with increasing MWCNTs content. The resultant MWCNTs/PS composite nanofibers diameters were in the range of 391±63 to 586±132 nm. The thermal stability of composites was increased after addition of MWCNTs to PS matrix. The electrical conductivity of the composites with different weight percentage of MWCNTs was investigated at room temperature. Electrical conductivity of MWCNTs/PS composite nanofiber followed percolation theory having a percolation threshold V _c= 0.45 vol% (~0.75 wt. %) and critical exponent q=1.21. The electrical conductivity and thermal properties confirmed the presence of good dispersion and alignment MWCNTs encapsulated within the electrospun nanofibers. The electromagnetic interference (EMI) shielding effectiveness of the MWCNTs/PS composites was examined in the measurement frequency range of 8.2-12.4 GHz (X-band). The total EMI shielding efficiency of MWCNTs/PS composite nanofibers increased up to 32 dB. The EMI shielding results for MWCNTs/PS composite nanofibers showed that absorption loss was the major shielding mechanism and reflection was the secondary mechanism. The present study has shown the possibility of utilizing MWCNTs/PS composite nanofibers as EMI shielding/absorption materials.     

Fabrication and properties of dope-dyed Poly(m-phenylene isophthalamide) fibers via wet spinning

Poly(m-phenylene isophthalamide) (PMIA) fibers play an irreplaceable role in the area of high-temperature resistance. It is usually difficult to dye PMIA fibers due to their rigid molecular structure and high crystallinity. In this study, the dope-dyed PMIA fibers with different amounts of pigment were fabricated by wet spinning. The properties of the pigment were analyzed, including size distribution and dispersive properties. The results showed that the pigment was easy to disperse in the fibers when the average diameter of the pigment was smaller than 500 nm. The color fastness of the colored PMIA fibers was tested, and their thermal properties and mechanical properties were also analyzed. The results of thermal gravity analysis (TGA) indicated that the colored PMIA fibers maintained good thermal performance. Compared to uncolored PMIA fibers, the colored PMIA fibers became lighter after exposing to simulated sunlight for 50 h. The breaking tenacity of fibers exceeded 2.0 cN/dtex, and the retentivity was above 80 % after being exposed to simulated sunlight for 50 h. These suggested the good mechanical performance of colored PMIA fibers. Dope-dyed PMIA fibers with good mechanical properties and thermal performance were successfully developed.