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.     

Comparison between artificial neural network and response surface methodology in the prediction of the production rate of polyacrylonitrile electrospun nanofibers

This paper focused on using response surface methodology (RSM) and artificial neural network (ANN) to analyze production rate of electrospun nanofibers. The three important electrospinning factors were studied including polymer concentration (wt %), applied voltage (kV) and the nozzle-collector distance (cm). The predicted production rates were in agreement with the experimental results in both ANN and RSM techniques. High regression coefficient between the variables and the response (R ²=0.975) indicates excellent evaluation of experimental data by second-order polynomial regression model. The regression coefficient was 0.988, which indicates that the ANN model was shows good fitting with experimental data. The obtained results indicate that the performance of ANN was better than RSM. It was concluded that applied voltage plays an important role (relative importance of 42.8 %) against production rate of electrospun nanofibers. The RSM model predicted the 2802.3 m/min value of the highest production rate at conditions of 15 wt % polymer concentration, 16 kV of the applied voltage, and 15 cm of nozzle-collector distance. The predicted value showed only 4.4 % difference with experimental results in which 2931.0 m/min at the same setting was observed.     

Evaluation of effective electrospinning parameters controlling gelatin nanofibers diameter via modelling artificial neural networks

The aim of this work was to evaluate the effective parameters for prediction of the electrospun gelatin nanofibers diameter using artificial neural network (ANN) technique. The various sets of electrospinning process including temperature, applied voltage and polymer and solvent concentrations were designed to produce pure gelatin nanofibers. The obtained results by analyzing Scanning Electron Microscopy (SEM) images indicated that the produced nanofibers diameter was in the range of 85 to 750 nm. Due to the volume of the data, k fold cross-validation method was used for data setting. Data were divided into the five categories and trained and tested using ANN technique. The results indicated that the network including 4 input variables, 3 hidden layers with 10, 18 and 9 nodes in each layers, respectively, and one output layer had the best performance in the testing sets. The mean squared error (MSE) and linear regression (R) between observed and predicted nanofibers diameter were 0.1531 and 0.9424, respectively. The obtained results demonstrated that the selected neural network model had acceptable performance for evaluating involved parameters and prediction of nanofibers diameter.     

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.     

Mapping the influence of electrospinning parameters on the morphology transition of short and continuous nanofibers

A theoretical model for the morphology transition of short and continuous nanofibers by electrospinning has been proposed. The influences of polymer concentration, applied voltage, and flow rate on the fabrication of short and continuous nanofibers were mapped for use as a reference in the design and construction of the theoretical model. The morphology transition of short and continuous nanofibers occurred mainly due to changes in the flow rate and voltage. According to the concentration of the polymer in the solution, the map of the short nanofiber region was narrowed as the polymer concentration increased. The theoretical model derived from the conservation of kinetic energy and potential energy experienced by the polymer solution resulted in an equation that could be used to calculate the voltage and flow rates under certain boundary conditions when cutting nanofibers. The boundary conditions for voltage were 4.7-4.9 kV, and the boundary conditions for flow rate were 0.1-1.1 µl/min.     

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.     

The effects of operating parameters on the fabrication of polyacrylonitrile nanofibers in electro-centrifuge spinning

Introduced recently, electro centrifuge is a new method for nanofiber production. In the electro-centrifuge method, fibers are produced by the simultaneous use of electrical and centrifugal forces. In this research, the effective parameters in the production of PAN nanofibers diameter and the influence of each of them have been discussed. These parameters are voltage, rotation speed, flow rate of exiting solution from nozzle and viscosity of solution. Also the capability of fiber production by this method is compared with the conventional electrospinning system. Results show that a significant enhancement can be achieved by proper adjustments of the polymer solution viscosity, applied voltage, and rotational velocity in fiber production rate. To exemplify, in a PAN polymer solution, the increased production rate of electro centrifuge varied from 193 to 1200 percent, as compared with a similar electrospinning method in which the polymer concentration and applied voltage varied in a range of 13 to 16 wt% and 15 to 10 kV, respectively.     

Preparation of poly(vinyl alcohol)/ZrO2 composite nanofibers via co-axial electrospinning with higher ZrO2 particle content

Poly(vinyl alcohol) (PVA)/zirconium oxide (ZrO₂) composite nanofibers with a skin-core structure were prepared and the effect of ZrO₂ particle content on uniform web formation was investigated. The optimized polymer concentration, tip to collector distance, and applied voltage for electrospinning were 11 wt%, 12 cm, and 20 kV, respectively. Skin-core PVA/ZrO₂ composite nanofibers containing up to 12 wt% ZrO₂ were successfully prepared, but it was difficult to obtain PVA/ZrO₂ composite nanofiber webs via conventional electrospinning. Increasing the amount of ZrO₂ caused the morphology of the PVA/ZrO₂ composite nanofibers to become a non-uniform nanoweb with irregular nanofiber diameters. While it was difficult to obtain a uniform nanofiber web containing a content of ZrO₂ over 6 wt% for conventional electrospinning, a more uniform nanofiber web could be obtained at up to 9 wt% ZrO₂ using a skin-core dual nozzle. More uniform webs could also be obtained when ZrO₂ was in the skin rather than the core.     

Effect of concentration on electrospun polyacrylonitrile (PAN) nanofibers

An allometrical scaling relationship between the diameter of electrospun nanofiber and solution concentration is established, the scaling exponent differs greatly between different polymers and the same polymer with different molecules or the same molecules with different properties. The diameter of electrospun polyacrylonitrile (PAN) nanofibers increases approximately linearly with solution concentration.     

Investigation of Parameters for Preparing Nanofiber Yarn via a Stepped Airflow-assisted Electrospinning

Electrospinning is a simple and cost-effective method to prepare fiber with nanometer scale. More importantly, 3D flexible nanofiber yarns that fabricated by electrospinning have shown excellent application prospects in smart textiles, wearable sensors, energy storage devices, tissue engineering, and so on. However, current methods for preparing electrospinning nanofiber yarns had some limitations, including low yarn yield and poor yarn structure. In this paper, a stepped airflow-assisted electrospinning method was designed to prepare continuously twisted nanofiber yarn through introducing stepped airflow into traditional electrospinning system. The stepped airflow could not only help to improve nanofiber yield, but also good for controlling the formed nanofibers to be deposited in a small area. In addition, the experimental methods of single factor variables were used to study the effects of stepped airflow pressure, applied voltage, spinning distance, solution flow rate, air pumping volume and friction roller speed on nanofiber yarn yield, nanofiber diameter, yarn twist and mechanical property. The results showed that prepared nanofiber yarns exhibited perfect morphologies and the yield of nanofiber yarn could reach to a maximum of 4.207 g/h. The breaking strength and elongation at break of the prepared yarn could reach to 23.52 MPa and 30.61 %, respectively.     

Antimicrobial and cellular activity of poly(L-lactide)/chitosan/Imipenem antibiotic composite nanofibers

Synthesis of biocompatible polymer nanofibers is valuable, due to their use as a cover for burns and as a replacement for bandage because of their antimicrobial properties. In this study, electrospinning of chitosan(Ch) and nanofibers synthesis with antibacterial properties was investigated. Nanofibers with antibacterial properties were synthesized by electrospun of Ch/poly(L-lactide)(PLA)/Imipenem(Imi) polymer solution. The results showed that the optimized ratio of Ch/PLA polymer solution was ratio of 50:50 and Ch 2 wt% and PLA 10 wt% polymer solution was the best weight percentage for nanofiber preparation. Also, the average diameter of Ch/PLA/Imi nanofibers was 143 nm and measured with ImageJ software. Afterwards, the antibacterial properties of Imi as additives (with different percentages) was studied in the polymer solution. The scanning electron microscopy (SEM) images and antibacterial tests were showed that the electrospun of Ch/PLA/Imi polymeric nanofibers were effective against Gram negative bacteria Escherichia coli (E. coli) and inhibited growth of E. coli. The growth and viability percentage of fibroblast cells with nanofibers in αMEM culture are at desirable levels after 6 days.     

A Novel Method to Fabricate High Strength Nanofiber Filaments: Morphology,Crystalline Structure,and Thermal and Mechanical Properties

Wet electrospinning is a simple and efficient method to manufacture continuous nanofiber filaments. However, polyacrylonitrile nanofiber filaments collected using a static water bath are limited for application in certain areas due to their low degree of alignment and breaking stress values. To improve these properties, a novel countercurrent flowing liquid bath collector was combined with a multi-needle electrospinning device. The morphologies, crystalline structures, thermal behaviors and mechanical properties of filaments fabricated under different countercurrent bath liquid motion conditions were investigated. In addition, the forces acting on the nanofibers in the bundling triangular zone under countercurrent liquid bath motion were analyzed. The results showed that the average nanofiber diameter of the filaments decreased with an increase in bath solution motion forces. The maximum alignment degree and breaking stress of the nanofibers were 85 % and 0.63 cN/dtex, respectively, achieved using a liquid flow rate of 80 ml/min and water inlet diameter of 6 mm. The alignment degree of the assembled nanofibers in the bundling triangular zone could be increased by 57 % when using a countercurrent flowing liquid compared with a static liquid bath.     

Scaling up the production rate of nanofibers by needleless electrospinning from multiple ring

Mass production of nanofibers is crucial in both laboratory research and industry application of nanofibers. In this study, multiple ring spinnerets have been used to generate needleless electrospinning. Multiple polymer jets were produced from the top of each ring in the spinning process, resulting in thin and uniform nanofibers. Production rate of nanofibers increased gradually with the increase of the number of rings in the spinneret. Spinning performance of multiple ring electrospinning, namely the quality and production rate of the as-spun nanofibers, was dependent on experimental parameters like applied voltage and polymer concentration. Electric field analysis of multiple ring showed that high concentrated electric field was formed on the surface of each ring. Fiber diameter together with production rate of needleless electrospinning was dependent on the strength and distribution of the electric field of the spinneret. Needleless electrospinning from multiple ring can be further applied in both laboratory research and industry where large amount of nanofibers must be employed simultaneously.     

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.     

An investigation on the effects of twist on geometry of the electrospinning triangle and polyamide 66 nanofiber yarn strength

The formation of a symmetric electrospinning triangle zone (E-triangle) via a technique based on using two oppositely charged nozzles is described for fabricating continuous twisted nanofiber yarn of polyamide (Nylon 66). This study shows how changing the dimensions and geometry of the E-triangle influences the distribution of nanofiber tension and diameter in this zone, and consequently how it affects the nanofiber yarn strength. The twist effect on the E-triangle geometry was investigated by changing the rotational speed of the twister plate of values of 96, 160, 224 and 288 rpm. The results showed that by increasing the twist rate, the apex angle of the E-triangle increased, whereas the height and width of the Etriangle decreased. An energy method was adopted to study the distribution of tension on nanofibers in the E-triangle. Considering a constant spinning tension, it was observed that the gradient of the nanofiber tension curve was steeper and the extreme values of tension on nanofibers were increased by increasing the twist rate. Furthermore, the mean diameter reduction of nanofibers confirmed these results. It is concluded that mechanical properties of nanofiber yarn have been considerably improved by increasing the twist rate and changing the shape of the E-triangle.     

Measuring tensile strength of nanofibers using conductive substrates and dynamic mechanical analyzer

Though the tensile strength of nanofibers is essential to determine their application fields, few studies have been conducted on this topic, due to the difficulties involved in the preparation of single nanofiber tensile specimens, the manipulation of the clamping device, and the sensing of the nano- force and strain. A bundle testing method was employed in this work to measure the tensile strength of nanofibers. For this purpose, a conductive substrate was designed to hold several thousand nanofibers extruded from a spinning nozzle and align them uniaxially during the electrospinning process. This substrate was designed for a dynamic mechanical analyzer (DMA), because most DMAs are equipped with fine sensors sensitive enough to measure a very small force and strain. Nylon 6 nanofibers were electrospun and collected on the substrate. Then, they were elongated simultaneously in the DMA until they were fractured, showing that the aligned nanofibers have superior tensile strength and modulus compared to their counterpart microfibers and thus suggesting that polymeric nanofibers have the potential to be used as reinforcement fibers for composite materials.     

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.     

Fabrication and characterization of nano Al<Subscript>2</Subscript>O<Subscript>3</Subscript> filled PVA:NH<Subscript>4</Subscript>SCN electrolyte nanofibers by electrospinning

Present paper reports a method of preparing polymer composite electrolyte nanofiber mat using polyvinyl alcohol (PVA), ammonium thiocynate (NH₄SCN) salt, and aluminium oxide (Al₂O₃) nano particles based on electrospinning technique. Two-stage process of preparation of nanofibers, namely, preparation of nano particles filled PVA electrolyte gel solution followed by its electrospinning has been used. The so obtained nanofibers have been characterized by XRD, DSC, SEM, and Conductivity measurements. XRD patterns affirm the formation of nanocomposite while SEM pictures reveal formation of fibers on a nano scale format (300–800 nm). Fibers of the electrolytes are seen to be thermally stable. Ionic conductivity of electrolyte fiber is seen to improve in the presence of nano filler at room temperature with a maximum at 5.31×10⁻³ Scm⁻¹ for 4 wt% filler concentration, which is comparable to that for corresponding dried gel electrolyte films.     

Core-sheath polyurethane-carbon nanotube nanofibers prepared by electrospinning

The core-sheath nanofibers consisting of polyurethane (PU) core and PU composites sheath with multi-walled carbon nanotubes (MWNTs) were prepared by electrospinning. At low MWNT concentration, MWNTs appeared highly aligned along the fiber axis with some curving in nanotubes, whereas in case of high concentration, some aggregation of MWNTs appeared due to difficulty in full dispersion of nanotubes. In comparison of the single component nanofiber webs, the core-sheath nanofiber webs showed much better mechanical properties of modulus and breaking stress, including an exceptional elongation-at-break. It indicates that the CNT-incorporated core-sheath structure is very effective for enhancing the mechanical properties of nanofiber webs. In addition, the core-sheath nanofibers demonstrated the fast shape recovery, compared with one component fibers of pure shape memory PU and PU/MWNTs, which provides the possibility of fabricating more sensitive intelligent 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.