Electrospinning preparation and characterization of cadmium oxide nanofibers

Using a facile synthesis route, cadmium oxide (CdO) nanofibers in the diameter range of 50–60 nm have been prepared employing the electrospinning technique followed by a single-step calcination from the aqueous solution of polyvinyl alcohol (PVA) and cadmium acetate dihydrate. Electron microscopy (EM) and the Brunauer–Emmett–Teller (BET) technique were employed to characterize the as-spun nanofibers as well as the calcined product. The specific surface area of the product was calculated to be 42.6711 m² g⁻¹. Infrared (IR) absorbance spectroscopy and X-ray powder diffractometery were conducted on the samples to study their chemical composition as well as their crystallographic structure. The study on the optical properties based on the photoluminescence (PL) spectrum demonstrated that the emission peaks of CdO nanofibers are centered at 493 and 528 nm. The direct bandgap of the CdO nanofibers was determined to be 2.51 eV.     

静电纺丝制备纳米纤维的研究进展

纳米纤维具有直径小、比表面积大和易于实现表面功能化等优点,受到了广泛的关注,而静电纺丝技术被认为是制备聚合物纳米纤维最简单有效的方法,因此国内外学者对静电纺丝技术进行了详细的研究。简单介绍了静电纺丝技术的工作原理,详细阐述了影响静电纺丝的主要工艺参数,包括溶剂、溶液的浓度及黏度、电导率、工作电压、纺丝速度和接收距离等,并叙述了静电纺丝纳米纤维在过滤材料、传感器和生物医学等方面的应用,也指出了该技术存在的一些问题及其应对措施。     

Electrospinning zwitterion-containing nanoscale acrylic fibers

Free radical copolymerization of n-butyl acrylate and a sulfobetaine methacrylamide derivative provided high molecular weight zwitterionic copolymers containing 6-13 mol% betaine functionality, and the electrospinning of low T_g zwitterionomers was explored for the first time. Copolymerizations were performed in dimethylsulfoxide (DMSO) rather than fluorinated solvents previously reported in the literature. Dynamic mechanical analysis of zwitterionomer films revealed biphasic morphology and featured a rubbery plateau and two distinct thermal transitions. Electrospinning from chloroform/ethanol (80/20 v/v) solutions at low concentrations between 2 and 7 wt% afforded nanoscale polymeric fibers with diameters near 100 nm. The presence of only 6 mol% zwitterion allowed the formation of low T_g, free-standing, non-woven mats, and we hypothesize that zwitterionic aggregation rather than chain entanglements facilitated electrospinning at these relatively low solution concentrations. To our knowledge, this is the first report of electrospun zwitterionic polymers and these non-woven membranes are expected to lead to new applications for sulfobetaine copolymers.     

Electrospinning of l-tyrosine polyurethanes for potential biomedical applications

Biodegradable segmented l-tyrosine polyurethanes (LTUs) have been developed using a tyrosine based chain extender desaminotyrosine-tyrosyl-hexyl ester (DTH). Two such biodegradable LTUs, polycaprolactone diol-hexamethylene diisocyanate-desaminotyrosine-tyrosyl-hexyl-ester (PCL-L-DTH) and polycaprolactone diol-4,4′-methylenebis(cyclohexyl isocyanate)-desaminotyrosine-tyrosyl-hexyl-ester (PCL-C-DTH), have been electrospun, and the effect of solution concentration on the membrane properties has been examined. Scanning electron microscopy (SEM) images show that fiber diameter and structural morphology of the electrospun LTU membranes are a function of the polymer solution concentration. It has been observed all concentrations of PCL-L-DTH lead to the formation of beaded nanofibers; whereas, PCL-C-DTH polyurethane leads to the formation of non-beaded fibers with diameters in the micrometer range. Furthermore, the average fiber diameter enlarges with an increase in the polymer solution concentration. Hydrolytic degradation studies show similar mass loss profiles for both PCL-L-DTH and PCL-C-DTH polyurethane membranes over a period of 28 days. However, the loss of structure and morphology is more readily observed in the case of PCL-L-DTH membranes. Based on the results obtained from this investigation, the electrospun non-woven LTU membranes show excellent potential for biomedical applications such as formulation of drug/gene delivery devices and tissue engineering scaffolds.     

Electrospinning preparation and microstructure characterization of homogeneous diphasic mullite ceramic nanofibers

In this work, diphasic mullite (3Al₂O₃·2SiO₂) nanofibers with good homogeneity were prepared by electrospinning method. Aluminum nitrate (AN) and aluminum isopropoxide (AIP) were used as alumina sources, commercial colloidal silica as silica source, and polyvinyl alcohol (PVA) as polymer additive. Precursor nanofibers with continuous and uniform structures were acquired at mass ratio of PVA to precursor sol from 0.06 to 0.09. γ-Al₂O₃ phase was obtained at 878 ^°C and mullite phase formed at 1322 ^°C upon heating of the precursor under air atmosphere. Calcined samples suggested mullite as dominant phase at 1300 ^°C and amorphous SiO₂ could even exist at 1400 ^°C. As-prepared nanofibers possessed continuous structures with subequal average diameters at 900–1200 °C. However, such morphological characteristics were lost at temperatures above 1300 ^°C due to rapid growth of crystal grains. Al and Si elements were uniformly distributed in fibers and mixed at nanoscale, confirming homogeneity and diphasic features of nanofibers.     

Continuous aligned polymer fibers produced by a modified electrospinning method

A novel and simple technique of manufacturing uniaxially aligned electrospun fibers with diameter of sub-micrometers is described. Compared with typical electrospinning setup, two oppositely placed metallic needles are used, and they are connected to positive and negative voltages, respectively. Fibers coming out of the two needles combine in a yarn, which is wound by a cylinder collector rotating at a high speed. Fibers manufactured by this method are continuous, well-aligned, and can be deposited over a large area. Poly(vinyl alcohol) (PVA) and poly(vinyl pyrrolidone) (PVP) are used to manufacture aligned fibers. An analysis of the possible mechanism of the fibers alignment is given. The influences of the concentration of the solution and the take-up velocity on the alignment of fibers were investigated.     

Multi-Phase Composite Nanofibers via Electrospinning of Latex Containing Nanocapsules with Core-Shell Morphology

Nanocapsules containing hexadecane (HD) as core material and polystyrene (PS) as shell, were electrospun with polyethylene oxide (PEO) as a matrix material into the fiber webs. The morphology and thermal properties of PEO fibers containing (1) both PS nanocapsules with core-shell morphology and solid PS particles, (2) only solid PS particles, and (3) without any PS particles, were compared and the effect of PEO concentration on morphology of the resultant fibers have been studied. The resultant fibers were characterized by means of Transmission Electron Microscopy (TEM), Differential Scanning Calorimetry (DSC), and Thermogravimetric Analysis (TGA). Both TEM observation and DSC analyses confirmed that the PS nanocapsules were encapsulated within the PEO nanofibers. The fibers had an average diameter of 950 nm for nanocapsules containing parts, 300 nm for solid particles containing parts, and 150 nm for usual parts. The phase change temperatures and phase transition heat of the produced fibers were determined by DSC analyses. TGA was also used to confirm the preparation of multi phase fibers and to determine the amount of HD within the fibers.     

Electrospinning and characterization of highly sulfonated polystyrene fibers

Nanofibers of highly sulfonated (IEC ∼4.5 meq/g) polystyrene (SPS) were successfully electrospun. To accomplish this, the process of electrospinning this difficult-to-spin material was studied in detail. Fiber quality was optimized by manipulating the process and solution variables to fabricate continuous bead-free fibers. Bead-free fibers (average diameter 260 nm) were electrospun from 25 wt% SPS (500 kDa) in DMF at an electrode separation of 10 cm, an applied voltage of 16.5 kV and a flow rate of 0.3 mL/h. With increasing solution concentration, and thereby the solution viscosity, the morphology changed from beads to bead-on-string fibers to continuous cylindrical fibers. Beaded fibers and continuous bead-free fibers of SPS (500 kDa) could be spun at ∼2 C_e and 3.5 C_e, respectively, where C_e is the entanglement concentration determined from solution-viscosity measurements. The onset of formation of beaded fibers coincided with a sharp transition in the scaling of the storage modulus-concentration relationship.     

Preparation of water-stable submicron fibers from aqueous latex dispersion of water-insoluble polymers by electrospinning

Submicron polystyrene (PS) fibers were prepared by electrospinning of an aqueous dispersion of PS latex and a small amount of poly(vinyl alcohol) (PVA) and subsequent extraction by water. Depending on particle size, surfactant, ratio of PS:PVA, and applied voltage fibers of different morphology and water stability were obtained. Analysis of latex fibers by TEM revealed hexagonal packaging of particles within the fibers.     

The morphology of electrospun polystyrene fibers

Electrospinning is a process of electrostatic fiber formation which uses electrical forces to produce polymer nanofibers from polymer solution. The electrospinning system consists of a syringe feeder system, a collector system, and a high power supplier. The important parameters in the morphology of electrospun polystyrene fibers are concentration, applied voltage, and solvent properties. Higher concentrations of the polymer solution form thicker fibers and fewer beads. When the concentration is 7 wt%, electrospun fibers have an average diameter of 340 nm, but as the concentration of PS increases to 17 wt%, the fiber diameter gradually thickens to 3,610 nm. The fiber morphology under different solvent mixture ratios and solvent mixtures has also been studied.     

Ultra-fine polyelectrolyte fibers from electrospinning of poly(acrylic acid)

Ultra-fine polyelectrolyte fibers have been generated from electrospinning of poly(acrylic acid) in aqueous and DMF solutions. The fiber diameters ranged from 80 to 500 nm and increased with increasing solution concentrations and electrospinning voltages. The fibers generated from the aqueous solutions were more homogeneous in sizes, especially when NaCl or NaOH was added. Higher voltages in electrospinning of the aqueous solutions also resulted in fibers with larger heat capacity in the glass transition region, and higher dehydration temperatures. These polyelectrolyte fibers could be rendered water-insoluble by incorporating β-cyclodextrin (at 20 wt% of PAA) in the aqueous solution, then heat-induced crosslinking was performed at 140 °C for 20 min. The resulting hydrogel fibers showed strongly pH-responsive swelling behaviors.     

Electrospinning of uniform polystyrene fibers: The effect of solvent conductivity

By means of the electrospinning technique, micron- and nanofibers can be obtained from polymer solutions under a very high electrical field. A special challenge is to produce bead-free uniform fibers since any minor changes in the electrospinning parameters such as slight variations in the polymer solutions and/or electrospinning experimental parameters may result in significant variations in the final nanofiber morphology. Furthermore, it is often not trivial at all to obtain reproducible uniform electrospun nanofibers for the optimized electrospinning conditions. Here we report that the conductivity of the solvent is the key factor for the reproducible electrospinning of uniform polystyrene (PS) fibers from dimethylformamide (DMF) solutions. It is shown that even slight changes in the conductivity of the DMF solutions can greatly affect the morphology of the resulting electrospun PS fibers. Here, we have carried out a thorough and systematic study on the effect of solution conductivity on the electrospinning of bead-free polystyrene (PS) fibers when dimethylformamide (DMF) was used as the solvent. Interestingly, we found out that different grades of solvent as-received (DMF) from various suppliers have slightly different solution conductivities. Consequently, the polymer solutions prepared with the same PS concentration have different conductivities, which are shown to have significant changes on the morphology of the PS fibers resulting in beaded or bead-free uniform fibers when electrospun under the identical electrospinning conditions. Such as, bead-free PS fibers were obtained from PS solutions in the range of 20% (w/v) through 30% (w/v) depending on the DMF grade used. In brief, it was observed that solutions with a higher conductivity yielded bead-free fibers from lower polymer concentrations, which confirms that the solution conductivity plays a very significant role in producing bead-free uniform PS fibers.     

Electrospinning fabrication of partially crystalline bisphenol A polycarbonate nanofibers: The effects of molecular motion and conformation in solutions

Partially crystalline bisphenol A polycarbonate (BPAPC) nanofibers were successfully fabricated using a combination of a centrifugal field (1800 rpm) and an electrostatic field (25 kV). The BPAPC solution properties are key factors for adequately electrospinning the partially crystalline BPAPC nanofibers. The correlation times (τ_c) of methyl (τ_c = 9.3 ns) and of benzene-ring (τ_c = 15.3 and 15.8 ns) motions in the 14 wt.% BPAPC/THF solution were longer than in CH₂Cl₂ and CHCl₃, as determined by NMR. The distribution-peak maximum of the hydrodynamic radius of BPAPC in the 14 wt.% THF solution (R_h = 15 Å) was higher than in CH₂Cl₂ (R_h = 9.2 Å) and CHCl₃ (R_h = 7.9 Å), as evidenced by DLS data. We conclude that the BPAPC assumed a denser, more worm-like chain conformation in THF solvation.     

Electrospinning synthesis of Na2MnPO4F/C nanofibers as a high voltage cathode material for Na-ion batteries

Three-dimensional carbon nanofibers embedded with Na₂MnPO₄F nanoparticles are fabricated via electrospinning method and investigated as cathode material for sodium ion batteries. The Na₂MnPO₄F nanoparticles with a size of about 10–30?nm are well-crystallized and the diameter of the carbon nanofibers are about 100?nm. Due to the ultrafine particle size of Na₂MnPO₄F together with high conductivity of the three-dimensional electron/ion hybrid network of carbon nanofibers, the material synthesized at 650?°C exhibit good electrochemical performance at room temperature. It is found that an obvious potential platform as high as 3.6?V during charge/discharge processes occurs and there is an initial specific capacity of 122.4?mAh?g^?1 at 0.05C rate, which is close to the theoretic capacity (one Na⁺ extracted) of Na₂MnPO₄F. This work suggests a new design strategy for high-performance Na₂MnPO₄F cathodes of sodium-ion batteries.     

Electrospinning preparation and characterization of alumina nanofibers with high aspect ratio

Alumina nanofibers were successfully prepared via an electrospinning technique combined with a sol–gel method. The electrospinning solution was prepared by dissolving aluminum isopropoxide (AIP) in distilled water and then mixing with a polyvinyl alcohol (PVA) aqueous solution. The as-spun fibers were calcined at different temperatures and characterized by TG–DTA, XRD, SEM–EDS, TEM–SAED, and BET analysis. Results showed that the average fiber diameter decreases with increasing calcination temperature. The as-spun nanofibers were amorphous. After calcination at 1000 °C, the nanofibers formed were composed of α-Al₂O₃ and γ-Al₂O₃, showing an average diameter of 30–90 nm and an aspect ratio of greater than 1000. The pore size of the obtained fibers was approximately 5 nm, which implies that these fibers are mesoporous materials.     

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.     

Nanoparticle filtration by electrospun polymer fibers

Polyacrylonitrile (PAN) fibers with mean diameters in 270-400 nm range were prepared by electrospinning for use as a filter media. Compared to commercial filters made of polyolefin and glass, the fibers of electrospun filters were more uniform in diameter. The performance of electrospun filters was evaluated by measuring the penetration of monodisperse NaCl nanoparticles (below 80 nm in size) through the filters. It was found that electrospun filters could be made which had nanoparticle penetration values comparable to commercial filters but with substantially less filter mass. The penetration of nanoparticles through the electrospun filter media could be reduced by increasing the filter thickness, which is controlled by the collection time during the electrospinning process. Nanoparticle collection by electrostatic forces was found to be negligible for electrospun filters. Filter quality factors and single fiber collection efficiencies were found to be independent of filter thickness for electrospun filters, and the penetration of nanoparticles through electrospun filters was in better agreement with theoretical predictions than was the measured penetration through a commercial filter. This study shows that electrospinning is a promising technology for the production of high performance nanoparticle filters.     

Electrospinning and structural characterization of ultrafine poly(butylene succinate) fibers

Biodegradable ultrafine poly(butylene succinate) (PBS) fibers were continuously electrospun for the first time from PBS solutions in chloroform (CF)/2-chloroethanol (CE) (7/3, w/w), CF/CE (6/4, w/w), dichloromethane (DM)/CE (7/3, w/w), DM/CE (6/4, w/w), and CF/3-chloro-1-propanol (9/1, w/w). These mixed solvents had an appropriate evaporation rate for the continuous electrospinning of PBS. The ultrafine PBS fibers had very high crystallinity and their average diameters were in the range of 125-315 nm. The annealed ultrafine PBS fibers exhibited a lamellar stack morphology containing crystalline and amorphous layers.     

Electrospinning of thermo-regulating ultrafine fibers based on polyethylene glycol/cellulose acetate composite

Ultrafine fibers of polyethylene glycol/cellulose acetate (PEG/CA) composite in which PEG acts as a model phase change material (PCM) and CA acts as a matrix, were successfully prepared as thermo-regulating fibers via electrospinning. The morphology observation from the electrospun PEG/CA composite fibers revealed that the fibers were cylindrical and had a smooth external surface. PEG was found to be both distributed on the surface and within the core of the fibers. Differential scanning calorimeter (DSC) was used to characterize the thermal properties of the composite fibers. The results indicated that the fibers imparted balanced thermal storage and release properties for their thermo-regulating function and the thermal properties were reproducible after 100 heating-cooling cycles.     

Magnesium Ferrite (MgFe2O4) Nanostructures Fabricated by Electrospinning

Magnesium ferrite (MgFe₂O₄) nanostructures were successfully fabricated by electrospinning method. X-ray diffraction, FT-IR, scanning electron microscopy, and transmission electron microscopy revealed that calcination of the as-spun MgFe₂O₄/poly(vinyl pyrrolidone) (PVP) composite nanofibers at 500–800 °C in air for 2 h resulted in well-developed spinel MgFe₂O₄ nanostuctures. The crystal structure and morphology of the nanofibers were influenced by the calcination temperature. Crystallite size of the nanoparticles contained in nanofibers increased from 15 ± 4 to 24 ± 3 nm when calcination temperature was increased from 500 to 800 °C. Room temperature magnetization results showed a ferromagnetic behavior of the calcined MgFe₂O₄/PVP composite nanofibers, having their specific saturation magnetization (M _s) values of 17.0, 20.7, 25.7, and 31.1 emu/g at 10 Oe for the samples calcined at 500, 600, 700, and 800 °C, respectively. It is found that the increase in the tendency of M _s is consistent with the enhancement of crystallinity, and the values of M _s for the MgFe₂O₄ samples were observed to increase with increasing crystallite size.