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.     

Effect of hot-stretching on morphology and mechanical properties of electrospun PMIA nanofibers

Well-aligned PMIA nanofiber mats were fabricated by electrospinning and then hot-stretching along the fiber axis was used to improve the mechanical properties of nanofibers in this paper. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Differential scanning calorimetry (DSC) were used to characterize the morphology and properties of nanofibers. The results showed that the nanofibers became thinner and better alignment than the as-spun nanofibers after hotstretching, and the average diameter of the nanofibers decreased with the increasing of the tensile force. In the same time, hotstretching improved the crystallinity and T _g of the as-spun PMIA nanofibers. The tensile strength and modulus of the hotstretched nanofiber mats peaked at ca.50 % and ca.196 % respectively at the tensile force of 12 N compared with the as-spun nanofiber mats.     

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.     

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.     

Fabrication of silk fibroin based three dimensional scaffolds for tissue engineering

Herein we report successful synthesis of silk fibroin (SF) three dimensional scaffolds (SF 3D-scaffold) from SF sponge and SF nanofibers. Both the nanofibers and sponge were prepared from Bombyx mori fibroin. The SF 3D-scaffold was prepared by electrospinning the fibroin nanofibers over the sponge. Surface morphology was determined by scanning electron microscopy (SEM), while nanofiber diameter and pore size were measured using imageJ software. Effect of spinning time on the pore size and cell adhesion was determined. Average diameter of the SF nanofibers was measured to be 320 nm and pore size was found to reduce with increasing spinning time, such that, for 1 h spinning time pore size was 231 µm and the same for 3.5 h was 4.1 µm. However, the number of pores increased with spinning time. The results confirmed adhesion of MC3T3-E1 cells on the SF sponge, SF nanofibers and SF three dimensional scaffolds. Higher cell adhesion was found on the three dimensional scaffold in comparison to the nanofibers and sponge, possibly due to highly porous structure with very small and numerous pores in the resultant composite; hence more cell adhesion sites. The cell adhesion result confirmed biocompatibility of the SF 3D-scaffold and hence its suitability for applications in tissue engineering.     

Study on the stability and reusability of Glutamate Dehydrogenase immobilized on bacterial cellulose nanofiber

In this study, a simple method with improved properties for Glutamate Dehydrogenase immobilization is proposed by using bacterial cellulosic nanofiberas as a novel and inexpensive biomatrix. Acetobacter xylinum ATCC 10245 has been chosen and cultivated for synthesis of this nanofiber with the diameter of 30-70 nm. Thereafter, Glutamate Dehydrogenase was immobilized into the nanofiber pores in two steps: 1) enzyme adsorption and 2) crosslinking by glutaraldehyde. Optimum pH for the activity of immobilized enzyme and optimum temperature was reported in this work. Also the relative activity of immobilized enzyme was about 38 % in comparison to the enzyme activity of the first day after about two months. Moreover after reusing of the enzyme for 9 cycles, the immobilized enzyme retained over 83 % of its initial activity. Glutamate Dehydrogenase is immobilized on bacterial cellulosic nanofiber for the first time which can affect on facilitation of Glutamate production. Also can be a good method for having a stable and robust immobilized Glutamate Dehydrogenase that can withstand harsh operating conditions in processes which are common in these kind of reactions.     

Preparation of amidoxime-modified polyacrylonitrile nanofibers immobilized with laccase for dye degradation

A novel approach to preparing multifunctional composite nanofibrous membrane was developed. Polyacrylonitrile (PAN) nanofibrous membrane was fabricated by electrospinning and then the nitrile groups in PAN copolymer was chemically modified to obtain amidoxime modified PAN (AOPAN) nanofiber membrane which was further used as a functional support for laccase immobilization. During the process of reactive dye degradation catalyzed by the AOPAN nanofiber membrane immobilized with laccase, metal ion adsorption occurred at the same time. The chemical modification was confirmed by Fourier transform spectroscopy (FTIR). Scanning electron microscope (SEM) was employed to investigate the surface morphologies of the electrospun nanofibers before and after laccase immobilization. The effects of environmental factors on laccase activity were studied in detail. It was found that the optimum pH and temperature for the activity of immobilized laccase was 3.5 and 50 °C. The relative activity retention of the immobilized laccase decreased dramatically during the initial four repeated uses. After 20 days’ storage, the activity retention of immobilized laccase was still high above 60 %. It has also proved that laccase immobilized on AOPAN nanofiber membrane performed well in dye degradation and metal ion adsorption.     

Fabrication of silk fibroin/eggshell nanofiber membranes for facemasks

We report our study on fabrication of soluble eggshell membrane (SESM) and silk fibroin (SF) nanofibers composite (SF/SESM) for facemasks by electrospinning. Biocompatibility of the SF and SESM, determined from hydrophilicity results, is exploited in SF/SESM nanocomposite for facemask application. The SF/SESM nanocomposites were prepared in different ratios of SF and SESM. The samples were characterized by scanning electron microscopy (SEM), FTIR and water droplet adsorption tests conducted via water contact angle (WCA) and water droplet diffusion. The results revealed that addition of SESM has insignificant effect on the electrospinnability of SF nanofibers in the studied ratios. The SEM results depicted regular morphology of the nanofibers except increase in nanofiber diameter with addition of SESM. The FTIR results confirmed respective peaks of SF and SESM in SF/SESM nanocomposite. WCA of the nanofibers decreased with addition of SESM such that for SF/SESM30, 30 % SESM, it reduced to 0 ° from 101 ° for pure SF nanofibers. The research results demonstrate SF/SESM30 nanocomposite as optimum ratio of SF and SESM for facemasks and other biomedical applications.     

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.     

RSM and ANN approaches for modeling and optimizing of electrospun polyurethane nanofibers morphology

This paper focused on using response surface methodology (RSM) and artificial neural network (ANN) to analyze polyurethane (PU) nanofibers morphology synthesized by electrospinning. The process was characterized in detail by using experimental design to determine the parameters that may affect the nanofibers morphology such as polymer concentration, a tip to collector distance and applied voltage. It was concluded that solution concentration plays an important role (relative importance of 79.85 %) against nanofibers diameter and its standard deviation. Based on the results, applied voltage has a different effect on the nanofiber diameter at low and high solution concentrations. Moreover, the tip to collector distance parameter has no significant impact on the average nanofiber diameter. The finest PU nanofiber (201 nm) was obtained from experimental under conditions of: 9 w/v% polymer concentrations, 12 cm tip to collector distance and 16 kV applied voltage. The results show a very good agreement between the experimental and modeled data. It was demonstrated that both models (specially, in case of neural network) are excellent for predicting diameter of PU nanofibers. Furthermore, numerical optimization has been performed by considering desirability function to access the region in design space that introduces minimum average diameter.     

Meltblown nanofiber media for enhanced quality factor

Nanofibers definitely hold great advantage and promise in filtration as they have very high specific surface area, which ensures greater probability of capturing the particles and hence, the filtration efficiency of the nanofiber filter media is high. Electrospun nanofibers are prohibitively expensive due to extremely low production rate. With recent advances in melt blowing technology, nanofibers could be produced at production rate few orders of magnitude higher than that of conventional single syringe electrospinning and hence, quite cost effective. Influence of air pressure and die to collector distance (DCD) were studied on the number average fiber diameter for the nanofibers as well as the performance properties of the nonwoven webs, each factor at three discrete levels. The nanofibers were as fine as 260 nm. A very encouraging observation of the study is very high values of quality factor observed for nanofiber nonwoven filter media. In order to compare the filtration efficiency of different nanofiber nonwoven media samples with different basis weight, a novel term of specific filtration efficiency is proposed and was found that the specific filtration efficiency with the increase in DCD or air pressure.     

Antibacterial effect of carbon nanofibers containing Ag nanoparticles

Silver nanoparticles imbedded in polyacrylonitrile (PAN) nanofibers and converted into carbon nanofibers by calcination was obtained in a simple three-step process. The first step involves conversion of silver ions to metallic silver nanoparticles, through reduction of silver nitrate with dilute solution of PAN. The second step involves electrospinning of viscous PAN solution containing silver nanoparticles, thus obtaining PAN nanofibers containing silver nanoparticles. The third step was converting PAN/Ag composites into carbon nanofibers containing silver nanoparticles. Scanning electron microscopy (SEM) revealed that the diameter of the nanofibers ranged between 200 and 800 nm. Transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) showed silver nanoparticles dispersed on the surface of the carbon nanofibers. The obtained fiber was fully characterized by measuring and comparing the FTIR spectra and thermogravimetric analysis (TGA) diagrams of PAN nanofiber with and without imbedded silver nanoparticles, in order to show the effect of silver nanoparticles on the electrospun fiber properties. The obtained carbon/Ag composites were tested as gram-class-independent antibacterial agent. The electrosorption of different salt solutions with the fabricated carbon/Ag composite film electrodes was studied.     

Fabrication and characterization of nanofibers based on poly(lactic acid)/chitosan blends by electrospinning and their functionalization with phospholipase A1

In this work, electrospinning of poly(lactic acid) (PLA), chitosan and their blends has been investigated, and nanofibers with a diameter ranging from 90 nm to 1.9 microns were produced and used as carriers for immobilization of the phospholipase A1. A strong influence of chitosan (CS) and the solvent trifluoroacetic acid (TFA) on the morphology, distribution of the nanofibers diameter and on their hydrophobicity was observed. The yield of phospholipase A1 (PLA1) on non-woven fibers was evaluated using the method of Bradford. Their activities and their reutilisability were assessed titrimetrically using soybean lecithin as substrate. The results showed that the degree of immobilization on the non-woven fibers of pure PLA and mixtures PLA/CS4 and PLA/SC6 are 73, 54, 45 % respectively and can be reused up to 4 cycles without significant loss of enzyme activity. Moreover, a remarkable improvement of the activity of phospholipase A1 on non-woven based on pure PLA fibers was observed, indicating that most of the enzymes were probably in their active form.     

Enhanced mechanical properties of silk fibroin-based composite plates for fractured bone healing

We successfully fabricated bacterial cellulose/silk fibroin (BC/SF) composite plates having similar strength to that of human cortical bone (12.8–17.7 GPa). The mechanical properties of the BC/SF composite plates were investigated at various BC nanofiber contents. The BC nanofibers acted as good reinforcements for the stress transfer produced by the interactions between the BC nanofibers and the SF matrix, as confirmed by the molecular deformation of the BC nanofibers. The BC/SF composite plates have a promising potential as a replacement material for existing metal bone plate.     

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.     

Sericin-fixed filk fiber as an immobilization support of enzyme

In this study, we attempted to evaluate a novel use of sericin-fixed silk fiber (SFx) as an immobilization support of enzyme. Sericin was fixed on the silk fiber using glutaraldehyde as a fixation reagent. After 6 hours of fixation, the degree of fixation increases linearly with linear decrease of the amount of bound α-chymotrypsin (CT). This suggests that the increase of the degree of fixation is due to the further crosslinking of free aldehyde groups on the surface of sericin-fixed silk fiber (SFx). Even though perfect fixation was not achieved, sericin did not dissolve seriously and could be removed by further washing. The specific activity did not differ significantly after 6 hours of fixation. The activity of immobilized CT on SFx decreased to its half after 6 hours of incubation at 50°C. However, it retained 78% of initial activity even after 1 hour of treatment with 100% ethanol. As a result, the SFx could be used as an immobilization support of enzyme in non-aqueous media at ambient temperature.     

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.     

The study on the air volume fraction of electrospun nanofiber nonwoven mats

Electrospinning is an efficient method to produce polymer fibers with a diameter range from nanometers to a few microns using an electrically driven jet. Electrospun nanofiber nonwoven fabrics can be applied into different areas with higher air volume fraction, especially applied into textile materials with good warmth retention property. In this article, the air volume fraction in nonwoven mats made of electrospun nanofibers was verified by studying fiber volume fraction in the mats. Then the relationship between fiber volume fraction and fiber diameter was derived, and the fiber volume fraction is in direct ratio to the square of fiber radius. By experimental verification, to get electrospun PAN nanofiber nonwoven mats with high air volume fraction about 99 %, it can fix the polymer concentration on 8 %. The voltage fixed on 20 kV, the tip-to-collector distance on 15 cm. The experiment is in accordance with the theory excellently.     

Preparation and characterization of (polyurethane/nylon-6) nanofiber/ (silicone) film composites <Emphasis Type="Italic">via</Emphasis> electrospinning and dip-coating

This paper reports on the preparation and characterization of nanofibers and nanofiber/film composites fabricated by electrospinning and dip-coating. The polymers in this study consist of polyurethane, nylon-6, and silicone. Scanning electron microscopy (SEM), fiber distribution, X-ray diffraction (XRD) analysis, Fourier transform infrared spectroscopy (FTIR) and tensile tests were conducted. The electrospun nylon-6 nanofiber/dip-coated silicone film (dried for 5 min) showed the optimum tensile strength and strain results, showing an increase in tensile strength of 63 % compared to pure nylon-6 nanofiber alone. XRD and FTIR verified the presence of individual polymers in the composite matrix. The electrospun PU nanofiber produced the biggest fiber diameter, while electrospun nylon-6, and PU/nylon-6 produced uniform fiber diameters, with PU/nylon-6 obtaining very random and curved fiber morphology.     

Antimicrobial gelatin nanofibers containing silver nanoparticles

Gelatin is one of the most promising biomaterials due to its excellent biocompatibility and biodegradability. In order to improve the antimicrobial activity of gelatin, gelatin nanofibers containing silver nanoparticles were prepared by electrospinning gelatin/AgNO₃/formic acid system, followed by UV irradiation. They were characterized by UV-visible spectroscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction analysis. It was observed that the silver nanoparticles, which presented quasi-sphere shaped and 9–20 nm average diameters, were generated on the surface of the gelatin nanofibers. The size of the silver particles can be adjusted by changing the content of AgNO₃. With increasing the amount of AgNO₃, the average diameters of fibers decreased. The gelatin-Ag nanocomposites were found effective against Staphylococcus aureus and Pseudomonas aeruginosa. From these results, it is expected that the electrospun antimicrobial gelatin nanofiber mat can be used as an excellent wound dressing.