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Article

A Guide for Industrial Needleless Electrospinning of Synthetic and Hybrid Nanofibers

by
Baturalp Yalcinkaya
* and
Matej Buzgo
Respilon Membranes s.r.o., Nové sady 988/2, Staré Brno, 602 00 Brno, Czech Republic
*
Author to whom correspondence should be addressed.
Polymers 2025, 17(22), 3019; https://doi.org/10.3390/polym17223019
Submission received: 14 September 2025 / Revised: 28 October 2025 / Accepted: 11 November 2025 / Published: 13 November 2025
(This article belongs to the Special Issue Fiber Spinning Technologies and Functional Polymer Fiber Development)
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Abstract

This study presents a comprehensive investigation into the large-scale production of synthetic and hybrid (nanoparticle-loaded) nanofibers using needleless electrospinning. A diverse range of polymers, including polyamide 6 (PA6) and its other polymer combinations, recycled PA6, polyamide 11 (PA11), polyamide 12 (PA12), polyvinyl butyral (PVB), polycaprolactone (PCL), polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyurethane (PU), polyvinyl alcohol (PVA), and cellulose acetate (CA), were utilized to fabricate nanofibers with tailored properties such as polymer solution concentrations and various solvent systems. Furthermore, an extensive variety of nano- and micro-particles, including TiO2, ZnO, MgO, CuO, Ag, graphene oxide, CeO2, Er2O3, WO3, MnO2, and hyperbranched polymers, were incorporated into the polymeric systems to engineer multifunctional nanofibers with enhanced structural characteristics. The study examines the impact of polymer–nano/micro-particle interactions, fiber morphology, and the feasibility of large-scale production via needleless electrospinning. The resulting nanofibers exhibited diameters starting from 80 nm, depending on the polymer and processing conditions. The incorporation of TiO2, CeO2, WO3, Ag, and ZnO nanoparticles into 15% PA6 solutions yielded well-dispersed hybrid nanofibers. By providing insights into polymer selection, nano- and micro-particle integration, and large-scale production techniques, this work establishes a versatile platform for scalable hybrid nanofiber fabrication, paving the way for innovative applications in nanotechnology and materials science.

1. Introduction

Electrospinning has undergone a significant transformation, advancing from laboratory-scale production to industrial pilot and large-scale manufacturing within a quarter of the 21st century [1,2,3,4,5]. One of the first studies on electrospinning was conducted in the United States by Formhals [6], who demonstrated the first laboratory-scale electrospinning prototypes. Later, in the USSR, Petryanov [7] advanced the process to semi-industrial fiber production. One of the most pivotal innovations in this progress was the development of the needleless electrospinning method, pioneered by Oldřich Jirsák [8]. Instead of using a needle apparatus, this technique utilizes a conductive cylinder partially immersed in a polymer solution. As the cylinder rotates around its axis, it carries the polymer solution, forming a thin film layer on its surface. When a high-voltage electric field is applied, the surface tension of the polymer solution on the cylinder is overcome, leading to the formation of multiple Taylor cones and spinning jets [9]. Thanks to this breakthrough, electrospinning technology has reached a new era in nanofiber production.
This advancement paved the way for high-efficiency needleless electrospinning systems, leading to the establishment of commercial enterprises, with Elmarco s.r.o [10,11,12] (Czech Republic) being one of the pioneers in the field. The contributions of these innovative companies have significantly impacted nanotechnology, enabling the development of various high-performance functional products across different industries [13,14,15,16]. Among the most beneficial applications of nanofibers are air filtration systems [17,18]. The extremely fine structure of nanofibers results in a large specific surface area, high porosity, and small pore sizes. This unique morphology enables nanofiber-based filters to perform surface filtration efficiently, achieving a removal rate of up to 99.97% for PM0.3 without clogging, thereby ensuring easy cleaning and maintaining high air permeability, such as 85 L/m [19,20,21]. Another significant market shift occurred with the decision to ban the use of polytetrafluoroethylene (PTFE) polymers in various industries. As a result, thermoplastic polyurethane (TPU) nanofibers, known for their high air permeability (62 mm/s) and water repellency with a water contact angle of 151.2°, have gained substantial demand, particularly in the functional apparel industry [22,23,24,25]. Due to their elastic and durable structure, PU nanofibers have demonstrated twice the water vapor permeability compared to PTFE-based membranes while maintaining the same level of water resistance [26].
With each advancement in electrospinning technology, polymers commonly used in the plastics and textile industries have been gradually processed into a nanofiber form [27]. Regardless of the production method or system, both synthetic and hybrid polymers have found their place at the nanoscale [28]. Among the most frequently electrospun and widely utilized nanofibers are synthetic polymers such as polyamide [29], polyurethane [24], and polyacrylonitrile [30]. In addition to the high-volume production of synthetic polymers, various other polymers have been extensively studied and fabricated in laboratory settings [31,32]. These include polyvinyl alcohol (PVA) [33], polyvinylpyrrolidone (PVP) [34], polycaprolactone (PCL) [35], polylactic acid (PLA) [36], polyglycolic acid (PGA) [37], polyethylene oxide (PEO) [38], polyethylene terephthalate (PET) [39], polybenzimidazole (PBI) [40], poly (amide-imide) (PAI) [41], polycarbonate (PC) [42], polyvinylidene fluoride (PVDF) [43], polyaniline (PANI) [44], and polypyrrole (PPy) [45]. These polymers continue to be widely explored for their potential applications in electrospinning.
Natural polymers that have been electrospun into nanofiber form include collagen [46], gelatin [47], chitosan [48], cellulose and its derivatives [49], alginate [50], silk fibroin [51], hyaluronic acid [52], dextran [53], and keratin and fibrinogen [54]. Although these materials are primarily utilized in laboratory settings or small-scale applications, polymers such as polyamide 6 [55], polyurethane [56,57], polyacrylonitrile [58], and collagen [59] have found extensive use in the various industry, leading to large-scale production and commercialization.
Upon realizing the evidence that natural and synthetic nanofibers alone could not achieve the desired high functionality, researchers began developing composite, blend, and hybrid nanofibers. By combining different materials, nanofibers with enhanced properties, including antibacterial, antiviral, waterproof, conductive, heat-resistant, photocatalytic, and piezoelectric functionalities, were successfully created. Notable examples include PLA/PCL [60,61,62], PCL/chitosan [63,64,65], PVA/gelatin [66,67], PAN/PANI [68,69], PVP/TiO2 [70,71], PVA/GO [72], and PVDF/carbon nanotubes [73], each offering specific advanced characteristics tailored for diverse applications.
Only a limited number of polymers are suitable for the free-surface nanofiber electrospinning system. Achieving optimal fiber production characterized by fine fiber morphology, bead-free structure, and the absence of non-fibrous areas requires extensive research and development. The optimization process is primarily influenced by factors such as polymer solution concentration, additives, and process parameters, including the distance between electrodes and the applied voltage.
In this study, we hypothesize that each polymer possesses a specific concentration range that enables the formation of uniform, bead-free nanofibers under optimized large-scale production conditions using the needleless electrospinning method. Therefore, the primary purpose of this work is to systematically investigate and optimize a wide range of polymer and their nanoparticle-loaded solution suitable for industrial-scale electrospinning. By evaluating the influence of polymer, solvent, and nanoparticle type and concentration on fiber morphology and spinnability, the study aims to establish a comprehensive guideline for optimal parameters in large-scale nanofiber fabrication. The findings are expected to serve as a practical reference for both academic researchers and industrial manufacturers in developing high-performance and functional electrospun nanofiber products, such as water-air separation membranes, biomedical and healthcare applications, and antibacterial and breathable waterproof membranes.

2. Materials and Methods

2.1. Materials

Polyamide 6 (PA6), regenerated PA6 (r-PA6), polyamide 11 (PA11), polyamide 12 (PA12), polyvinyl butyral (PVB), polycaprolactone (PCL), polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyurethane (PU), polyvinyl alcohol (PVA), cellulose acetate (CA) and chitosan (CS) were chosen as polymeric source for electrospinning. Nanoparticles, including titanium dioxide (TiO2), zinc oxide (ZnO), magnesium oxide (MgO), copper oxide (CuO), silver (Ag), cerium oxide (CeO2), erbium oxide (Er2O3), tungsten trioxide (WO3), manganese dioxide (MnO2), graphene oxide (GO), and hyperbranched polymers were used as additive. The complete list of polymers, including their commercial names, characteristics, and suppliers, is presented in Table 1. The types of nano- and micro-particles, their sizes, and origins are presented in Table 2. Table 3 presents the list of solvents along with their sources.

2.2. Solution Preparation

Two distinct steps have been employed to prepare solutions of synthetic polymers and their hybrid formations. The initial portion of the synthetic polymer powder/granule is introduced to solvents while gently stirring to prevent the formation of aggregates. The solutions are stirred overnight to guarantee total dissolution and uniformity. Hybrid solution preparation involves the gradual incorporation of metal oxide particles into the solvent system, followed by thorough mixing with an IKA T-25 ULTRA-TURRAX homogenizer from IKA Werke GmbH, Staufen im Breisgau, Germany, for 30 min. Once an optimal dispersion of micro/nano particles is achieved within the solvent system, the micro/nano particles are introduced into the polymer solution at the concentration specified in the provided concentration table (refer to the respective polymer solution concentration table in the relevant polymer section) and further mixed mechanically. Each polymer solution was prepared in 50 mL bottles.

2.3. Electrospinning of Synthetic and Hybrid Nanofibers

Nanofibers were produced using a free-surface needleless electrospinning technique, in which the polymer solution was supplied onto a thin, fixed conductive metal spinneret Figure 1.
The electrospinning system utilized in this study is an industrial-scale machine with a width of 80 cm and a length of 2 m. Before nanofiber production, it is essential to maintain the electrospinning chamber at specific humidity and temperature levels. These environmental conditions are regulated by an integrated air-drying system, which controls relative humidity and temperature to ensure stable fiber formation. The industrial-scale needleless electrospinning setup operates with a roll-to-roll nanofiber deposition system Figure 2.
A 45 gsm polypropylene nonwoven substrate is loaded into the unwinder unit and fed into the spinning chamber, where nanofibers are deposited onto the backing material. The rewinder unit then collects the coated nonwoven. All other process parameters, including polymer solution properties and electrospinning conditions, are optimized for each polymer type and detailed in the respective nanofiber sections.

2.4. Characterization of Nanofibers

The morphology and average diameter of the produced synthetic and hybrid nanofibers were analyzed using scanning electron microscopy (SEM, Phenom ProX, Thermo Fisher Scientific, Waltham, MA, USA). To prepare the samples, nanofiber specimens with their nonwoven substrate were cut into appropriate dimensions (0.75 cm2) to ensure compatibility with the SEM sample holder. Since nanofibers on a nonwoven substrate are typically non-conductive, a conductive coating is necessary to minimize charging effects and enhance imaging quality. Therefore, a 5 nm gold layer was deposited onto the samples using a LUXOR_AU sputter coater (Aptco Technologies, Frankfurt am Main, Germany), ensuring optimal conductivity for high-resolution SEM imaging.

3. Results and Discussion

3.1. Electrospinning of CA Nanofibers

The process of cellulose acetate is essential due to its unique properties and prospective uses in various industries [74]. The most significant aspects are its hydrophilicity, biodegradability, and sustainability. However, the process of electrospinning cellulose acetate polymer into nanofibers is a complex process. There are several types of cellulose acetate (CA), including cellulose acetate butyrate (CAB) and cellulose acetate propionate (CAP). Moreover, cellulose acetate from Eastman is produced by the esterification of cellulose with differing degrees of substitution. The classification of these compounds as diacetate or triacetate is contingent upon their level of acetylation. Cellulose acetates, such as CA-320S, possess a high hydroxyl content, indicating that not all hydroxyl groups on the cellulose backbone are subjected to acetylation. This signifies that certain goods are not completely acetylated (not triacetate) but fall within the diacetate category. CAB and CAP products are mixed esters, including acetate and other ester groups (such as butyrate or propionate). Hence, they are not distinctly categorized as diacetate or triacetate [75,76,77]. An important fact is that not all cellulose acetate polymers can be spun. After conducting an extensive analysis of several types of cellulose acetate and grades (product name indicates the solution viscosity, which correlates with molecular weight 0.2–0.5–1–3–5–10–30) [78], CA 398-10 type CA was utilized for the manufacturing of nanofibers. The process parameters of CA nanofiber are given in Table 4. The polymer concentration, mixture of the solvents, solvent ratios, fiber diameter, and SEM images are given in Table 5.
The solution feed rates are typically expressed in mbar/h in industrial-size electrospinning devices; however, a direct calculation of the flow rate in mL/h is also possible. Each polymer solution was prepared in 50 mL, and each production was set at 30 min.
Flow Rate = Total Volume/Time = 50 mL/0.5 h =100 mL/h
Cellulose acetate can be easily transformed into nanofibers using a DMAC/Acetone [79] solvent system due to the excellent balance of solubility, viscosity control, and evaporation behavior provided by this mixture. DMAC acts as a suitable solvent for CA, ensuring sufficient polymer chain entanglement and enhancing solution conductivity, which is essential for stable electrospinning [80]. Meanwhile, acetone’s high volatility enables rapid solvent evaporation and fiber solidification during the spinning process. Multiple concentrations, grades, and solvent systems were examined, and it was found that just one concentration and solvent ratio (15%, 5:5) successfully enabled the electrospinning of cellulose acetate polymer solutions. Nevertheless, the nanofibers created are not sufficiently strong or stable on the surface of the substrate. It is advisable to combine the CA polymer with another polymer for improved results.

3.2. Electrospinning of PCL Nanofibers

Polycaprolactone (PCL) is a biodegradable polymer, a type of polyester that the human body can readily absorb [81]. It is commonly employed in various medical fields, including drug administration, tissue engineering, and wound healing [82]. PCL is renowned for its excellent biocompatibility, low toxicity, and effortless processing [83]. The process parameters for PCL nanofibers are listed in Table 6. The polymer concentration, solvent mixture, solvent ratios, fiber diameter, and SEM images are presented in Table 7.
Polycaprolactone is a hydrophobic, semi-crystalline polymer that requires an appropriate solvent system for effective electrospinning [84]. A solvent mixture of acetic acid, formic acid, and chloroform works well [85]. On the other hand, chloroform provides good solubility for the hydrophobic PCL chains, enabling fast solvent evaporation and facilitating fiber solidification. Similarly, a well, while ethanol adjusts the solution’s polarity and conductivity, leading to better fiber formation and reducing defects such as beads [86]. These mixed solvent systems strike a balance between solubility, viscosity, conductivity, and evaporation rate, all of which are critical factors for producing uniform and smooth PCL nanofibers.
The electrospinning of PCL using chloroform as a solvent yielded non-uniform nanofibers, rather than uniform nanofibers. Alternative solvent systems and polymer blending strategies were explored to address this issue. The use of acidic solvent solutions significantly improved the quality and morphology of PCL nanofibers while also enhancing production efficiency. Furthermore, incorporating natural polymers such as cellulose acetate and chitosan, as well as synthetic polymers like polyethylene oxide, in the blending process further increased fiber uniformity and productivity. Although microfibers lack the high surface area and nanoscale features of nanofibers, they can still be advantageous for tissue engineering and medical applications. Their larger diameters provide increased mechanical strength and structural integrity, which support cell adhesion, proliferation, and extracellular matrix deposition, making them suitable for use as scaffolds in regenerative medicine.

3.3. Electrospinning of PA6 Nanofibers

Polyamide 6 is a widely used polymer in the production of nanofibers, particularly in the filtration and apparel industries [87]. It is a market leader in these segments due to its excellent mechanical properties and versatility. Coating corrugated 80/20 cellulose/synthetic paper with PA6 nanofibers enhances filtration efficiency, enabling it to meet F-class or HEPA (High-Efficiency Particulate Air) standards [88]. Additionally, PA6 nanofibers are utilized in high-performance sportswear [23,89] and personal protective clothing [90] due to their breathability, durability, and lightweight nature. Therefore, the development and characterization of PA6 nanofibers using an industrial-scale electrospinning device are essential for optimizing their performance in these applications. The process parameters of PA6 nanofiber are given in Table 8. Various concentrations and diverse solvent systems have been investigated, and the results are presented in Table 9.
Polyamide 6 (PA6) nanofibers can be effectively fabricated by electrospinning using solvent systems such as acetic acid (AA) and formic acid (FA) with chloroform or dichloromethane (DCM) [91]. The combination of AA and FA provides good solubility for PA6 due to their polar protic nature, where formic acid enhances solubility and acetic acid helps control viscosity and fiber smoothness [92]. The addition of chloroform, a volatile, non-polar solvent, can improve fiber formation by reducing surface tension and promoting faster solvent evaporation, resulting in smoother fibers with potential surface porosity if used in excess. Alternatively, replacing chloroform with dichloromethane (DCM), a more volatile solvent, further increases the evaporation rate during spinning. Various solvent and co-solvent systems combinations, along with two different PA6 sources, were investigated to generate a dataset for evaluating the morphology of PA6 nanofibrous membranes. All polymer solutions produced high-quality nanofibers free from beads and non-fibrous regions, except those with low polymer concentrations. Blending solvent and co-solvent systems proved highly efficient in facilitating uniform nanofiber deposition. Characterization of morphology revealed exceptionally low fiber diameter values, which are highly beneficial for filtration applications. The measured fiber diameters ranged between 100 and 250 nm, falling within the optimal range for high-performance filtration. Evaluation tests confirmed that PA6 is one of the most suitable polymers for industrial-scale nanofiber production using needleless electrospinning technology. Low-diameter nanofibers are ideal for air and water filtration due to their high surface area and superior filtering capacity. In contrast, larger-diameter fibers provide enhanced mechanical strength, making them well-suited for apparel membranes.

3.4. Electrospinning of PA11 and PA12 Nanofibers

Polyamide 11 and Polyamide 12 are polymers that exhibit exceptional resistance to chemicals, heat, and mechanical stress, surpassing even the performance of Polyamide 6 [93]. PA11 and PA12 have not been previously subjected to electrospinning in industrial-scale equipment. Preparing their polymer solution is as challenging as compared to PA6 [94]. In this research, we attempted to prepare nanofibers on a large scale using PA11 and PA12 for the first time. The process parameters of PA11 and PA12 nanofibers are given in Table 10. Various concentrations and diverse solvent systems have been studied, and the results are illustrated in Table 11.
The process of producing nanofibers from Polyamide 11 and Polyamide 12 is challenging. Although the fibers, ranging in size from nano to a few microns, were successfully deposited, their characteristics, production rates, and surface structures did not meet the intended standards. This approach has demonstrated the potential for further enhancement. The combination of polyamide 11 and polyamide 12 with polyvinyl butyral resulted in the formation of dense nanofibers, simultaneously enhancing both production and quality.

3.5. Electrospinning of PAN Nanofibers

Polyacrylonitrile is a synthetic polymer that is widely used in various industrial applications [95]. It is a thermoplastic polymer that is made from acrylonitrile monomers through polymerization [96]. The polymer has a linear structure, consisting of repeating units of acrylonitrile. PAN polymer electrospinning is particularly useful for creating nanofibers with diameters ranging from 50 to 300 nanometers [97]. These fibers have a high surface area, high porosity, and high mechanical strength, making them ideal for various applications, such as filtration. The process parameters of the PAN nanofiber are given in Table 12. Different concentrations and solvent systems have been studied, and the results are illustrated in Table 13.
Polyacrylonitrile nanofibers are widely fabricated by electrospinning using solvents like N, N-dimethylformamide and N, N-dimethylacetamide, both of which offer good solubility for PAN due to their strong polar aprotic nature [98]. DMF is the most preferred solvent because of its balanced volatility, high dielectric constant, and ability to produce uniform, smooth, and fine nanofibers due to stable jet formation and controlled solvent evaporation [99]. In contrast, DMAC has a slightly higher boiling point and slower evaporation rate, which can result in thicker fibers, wet deposition, or fused structures if spinning conditions are not optimized. The slower evaporation of DMAC may require higher applied voltage, longer collector distance, or lower flow rates to ensure complete solvent removal [100]. Polyacrylonitrile polymers have exceptional thermal and chemical resilience, making them very suitable for nanofiber applications [101].
Additionally, they offer versatile nanofiber production capabilities when used in electrospinning technology. PAN exhibits solubility in several aromatic polymers, with DMAC and DMF being particularly favorable choices due to their ability to produce high-quality and productive nanofibers. In this set of samples, PAN was successfully electrospun using an industrial-scale electrospinning apparatus. Increasing concentration resulted in the formation of high-quality surface morphologies without the presence of beads. PAN dissolved in DMF solvent has a higher nanofiber deposition efficiency due to the lower boiling point. However, DMAC solvent can also serve as a viable alternative for polyacrylonitrile polymers.

3.6. Electrospinning of PVDF Nanofibers

Polyvinylidene fluoride (PVDF) is a widely utilized polymer in large-scale industrial production for creating nanofibers [102]. This is primarily due to its ability to be electrospun, as well as its chemical and mechanical stability, piezoelectric characteristics, and ease of processing [103]. Exceptional features suggest that the electrospinning of PVDF polymer holds excellent promise as a viable method. The process parameters of PVDF nanofiber are given in Table 14. Various solution concentrations have been studied, and the results are illustrated in Table 15.
The use of industrial-scale needleless electrospinning for polyvinylidene fluoride has demonstrated the feasibility of producing nanofibers. Nevertheless, there is still potential for enhancing the quality of PVDF nanofibers. Nanofibers with minimal bead formation and a low non-fibrous region were successfully produced utilizing a concentration of only 20% w/v. Hence, to enhance the quality of PVDF nanofibers, it is necessary to adjust both environmental and process parameters. This is because PVDF is a highly sensitive polymer to humidity in electrospinning technology [104,105]. Therefore, precise calibration is crucial for achieving an improved nanofiber morphology.

3.7. Electrospinning of PU Nanofibers

The unique features and numerous applications of electrospun polyurethane nanofibers have made them highly important in various sectors [106]. The most essential characteristics of polyurethane nanofibers are their customizable mechanical strength and their ability to act as barriers against unwanted liquids and particles [107,108]. The process parameters for the production of PU nanofibers are listed in Table 16. Various concentration systems have been studied, and the results are illustrated in Table 17.
The electrospinning of polyurethane polymers is in great demand for the production of nanofibers because of their exceptional mechanical strength, impact resistance, and flexibility. PU nanofiber is an ideal choice for textile garments or coveralls. Due to their simplicity in lamination, polyurethane nanofibers can be effortlessly combined with other textile surfaces, such as knitted or woven fabrics made of polyester or cotton. The nanofibers become thicker and bead-free as the concentration of PU increases.

3.8. Electrospinning of PVB Nanofibers

PVB is a synthetic polymer classified as a member of the polyvinyl acetal resin group [109]. Nevertheless, the electrospinning process enables the fabrication of nanofibers possessing distinctive properties and promising applications [110]. Primarily, it exhibits solubility in nearly all solvents commonly employed in electrospinning, particularly those that are non-toxic. Consequently, this attribute results in PVB nanofibers being highly environmentally friendly [111]. It can also be mixed with other polymers because it is soluble in different solvents. The process parameters of the PVB nanofiber are given in Table 18. Various concentrations and diverse solvent systems have been studied, and the results are illustrated in Table 19.
The utilization of a solvent and co-solvent combination including ethanol and chloroform for dissolving PVB is crucial due to the inherent high flammability of ethanol. Additionally, the electrospinning process occasionally generates sparks between the lower and top electrodes. In order to address safety concerns and enhance the efficiency of PVB nanofiber production, solvent solutions are employed. Among these, chloroforms have been found to yield high-quality fibers, but with a thicker consistency. The quality of nanofibers obtained from ethanol with ethylene acetate and acid systems was not superior to that of nanofibers obtained from chloroform systems. The microscope images reveal the production of significantly thick fibers using needleless electrospinning, indicating the potential for further enhancement.

3.9. Electrospinning of PVA Nanofibers

The electrospinning process is commonly employed to fabricate nanofibers with diameters ranging from a few nanometers to micrometers using polyvinyl alcohol (PVA) [107]. PVA and PVB are synthetic polymers classified under the polyvinyl ester group, each possessing unique characteristics and uses. PVA is a water-soluble polymer that is generated by partially or completely hydrolyzing polyvinyl acetate. Hence, it is necessary to use a crosslinking treatment or agent either prior to or following the electrospinning process of PVA [108]. The process parameters of the PVA nanofiber are given in Table 20. Various concentrations and diverse solvent systems have been studied, and the results are illustrated in Table 21.
The large-scale fabrication of polyvinyl alcohol nanofibers can be simply accomplished by utilizing industrial-sized needleless electrospinning. PVA polymer was spun into nano or microfibers using various concentrations and solvent solutions.

3.10. Electrospinning of PA6 Nanofibers Containing Nanoparticles

Polyamide 6 polymer is an excellent candidate for filtering applications and textile manufacturing. Consequently, the incorporation of nanoparticles holds significant potential to enhance PA6 nanofibers by enabling functionalities such as self-cleaning, photocatalysis, chemical absorption, and antibacterial and antiviral properties.
This comprehensive investigation involved 15 wt% PA6 dissolved in the AA/FA/CH solution system, which was mixed with various nanoparticles at concentrations of 5, 15, and 30 wt%. The tables below display the SEM pictures of the utilized nanoparticles and their concentrations in relation to Polyamide 6 nanofibers. The process parameters of PA6 hybrid nanofibers are given in Table 22. Various concentrations and diverse nanoparticle systems have been studied, and the results are illustrated in Table 23.
Polyamide 6 solutions blended with nanoparticles (as shown in the Table above) were successfully spun into hybrid nanofibers using an industrial-size needleless electrospinning method. Through the implementation of large-scale production, we have successfully manufactured a quantity of hybrid nanofiber fabric measuring 3–4 m2 from each polymer solution.
The SEM images indicate that the nanofibers possess well-defined morphologies, with little to no presence of beads. Nanofiber mats have no non-fibrous area and an extremely small fiber diameter. The distribution of fiber sizes ranges from 80 nm to 300 nm. The polyamide 6 nanofibers possess a thin structure, resulting in nanoparticles that appear to be primarily situated on the surface of the fibers. Elevating the concentration of nanoparticles in polymer solutions undoubtedly enhances nanoparticle loading on the surface of the nanofibers.
In this study, a new method for achieving uniform dispersion using the IKA T-25 ULTRA-TURRAX, IKA-Werke, Staufen, Germany, a high-shear disperser (or homogenizer), was attempted. Its main advantage lies in generating extremely high shear forces (up to 24,000 rpm), which can break apart aggregates by applying intense mechanical shear. This method worked well for some metal oxides, even at higher concentrations; however, certain metal oxides still exhibited aggregation. This may be attributed to free-surface electrospinning, as the amount of polymer solution used in industrial-scale electrospinning is always large. The surface of the fibers is well scattered with metal oxide nanoparticles, specifically TiO2, ZnO, CeO2, WO3, silver, and combinations of TiO2 and ZnO particles. MgO, CuO, and Er2O3 tend to agglomerate and form clusters of nanoparticles on the surface of nanofibers. Graphene nanoparticles are not visible when observed under a scanning electron microscope. However, the nanofibrous fabric exhibits a black coloration on its surface due to the presence of graphene (Figure 3).

3.11. Electrospinning of PAN Nanofibers Containing Nanoparticles

Polyacrylonitrile is a highly promising polymer for the large-scale production of nanofibers. In this section, a hybrid nanofiber utilizing polyacrylonitrile polymers and nanoparticles has been developed due to its adaptable manufacturing and effortless spinnability. The process parameters of PAN hybrid nanofibers are given in Table 24. Various concentrations and diverse nanoparticle systems have been studied, and the results are illustrated in Table 25.

3.12. Electrospinning of PU Nanofibers Containing Nanoparticles

The polyurethane polymer has been selected as the third most promising type of polymer for creating hybrid nanofibers. These nanofibers are generated by adding nanoparticles to the polyurethane nanofiber matrices, which enhances the material’s capabilities. The process of hybridization enables the combination of distinct characteristics from both nanofibers and nanoparticles, resulting in customized materials that exhibit improved performance. The strong mechanical strength and flexible structure of polyurethane hybrid nanofibers make them highly promising for applications in apparel and garment textiles. Consequently, a selection of nanoparticles was mixed with polyurethane nanofibers in this series of experiments. The process parameters of PU hybrid nanofibers are given in Table 26. Various concentrations and diverse nanoparticle systems have been studied, and the results are illustrated in Table 27.
The interaction of polyurethane hybrid nanofibers with metal oxide nanoparticles has been successfully achieved on a large scale using industrial-scale needleless electrospinning. Each 50 mL polymer solution yielded approximately 5–6 square meters of hybrid nanofibers, with a thickness range of 8 to 20 microns. The morphology and quality of the nanofibers were excellent, with their thickness ranging from 350 nm to 550 nm. Consequently, specific nanoparticles were found both on the surface and within the nanofiber matrices. These behaviors are observable using TiO2, WO3, and ZnO nanoparticles. Graphene nanoparticles were not visible when observed under a scanning electron microscope. However, the nanofibrous fabric exhibited a black coloration on its surface due to the presence of graphene. Elevating the concentration of nanoparticles in polymer solutions undoubtedly enhances nanoparticle loading on the surface of the nanofibers. The phenomenon can be readily analyzed using scanning electron microscopy images.
The development of pristine and nanoparticle-loaded nanofibers produced via industrial-scale electrospinning represents a significant advancement in materials science and nanotechnology. In Table 28, the exploration of pristine and nanoparticled nanofibers in industrial electrospinning processes was summarized and described.

4. Conclusions

In the present study, a diverse range of widely utilized polymers and nanoparticles were successfully processed into pristine and hybrid (nanoparticle-loaded) nanofibers using needleless electrospinning. Critical processing parameters and polymer solution preparation strategies were systematically investigated and reported. Optimal nanofiber morphologies of PA6, PA11, PA12, PVB, PCL, PAN, PVDF, PVA, PU, and CA were identified based on scanning electron microscopy analysis, and indicated with a star symbol (★) to assist future studies. The resulting nanofibers exhibited diameters starting from 80 nm. Additionally, potential application areas for the produced nanofibers were outlined.
CA (430 nm), PA11 (4590 nm), and PA12 (790 nm) generally formed nano- and micro-structured fibers, resulting in mechanically weak, cotton-like fibers. PVA (245 nm), PVB (720 nm), and PVDF (495 nm) fibers, on the other hand, produced durable and fine nanofibers with very high production efficiency. PCL fibers formed strong nano- and micro-fibers (700–3000 nm), which can be used in applications such as biodegradable materials for wound dressings, providing robust and reliable fiber structures. Specifically, optimal electrospinning parameters were determined for the commonly studied PA6, PAN, and PU nanofibers. Highly uniform and stable PA6 nanofibers with an average diameter of approximately 250 nm were obtained from 12.5% and 15% PA6 solutions using AA/FA/DCM and AA/FA/CH solvent systems. The incorporation of TiO2, CeO2, WO3, Ag, and ZnO nanoparticles into 15% PA6 solutions yielded well-dispersed hybrid nanofibers. Furthermore, PAN and PU nanofibers produced from 15% polymer solutions in DMF exhibited relatively larger diameters, enhancing both surface attachment and encapsulation of nanoparticles. The introduced microparticles predominantly resided on the nanofiber surfaces, maintaining their functional activity.
The central hypothesis of this work was that a unified process–structure relationship can be established for a broad spectrum of polymers and hybrid nanofibers through needleless electrospinning, enabling reproducible large-scale production without the need for material-specific redesign. The present results confirm this hypothesis and provide the first experimentally validated guideline integrating polymer type, solvent system, and operational parameters for scalable electrospinning. In conclusion, the findings of this study provide a comprehensive guideline for the production and optimization of pristine and hybrid nanofibers using needleless electrospinning. The presented results are expected to serve as a valuable resource for researchers, facilitating future developments in nanofiber fabrication and broadening their potential applications across various industrial sectors.
Moving forward, future research is anticipated to focus on expanding the library of processable polymers and functional nanoparticles compatible with needleless electrospinning. The integration of machine learning and artificial intelligence-assisted optimization techniques could significantly accelerate the parameter screening process, reducing experimental workload and improving reproducibility. Moreover, the development of environmentally friendly solvent systems and bio-based polymers will be crucial to align nanofiber production with sustainability goals. The exploration of multifunctional nanofibers tailored for emerging fields, such as smart textiles, energy harvesting, environmental remediation, and biomedical applications, is expected to further enhance the industrial relevance and societal impact of nanofiber technologies.

Author Contributions

Conceptualization, B.Y.; methodology, B.Y.; software, B.Y.; validation, M.B.; formal analysis, M.B.; investigation, B.Y.; resources, M.B.; data curation, B.Y.; writing—original draft preparation, B.Y.; writing—review and editing, B.Y.; visualization, B.Y.; supervision, M.B.; project administration, M.B.; funding acquisition, M.B. All authors have read and agreed to the published version of the manuscript.

Funding

This paper is funded by the European Union European Defence Fund EDF-2021-OPEN-R-2 under grant agreement 101110262, project Nano-SHIELD. The views and opinions expressed are, however, those of the authors only and do not necessarily reflect those of the European Union. Neither the European Union nor the granting authority can be held responsible for them.

Institutional Review Board Statement

Not applicable.

Data Availability Statement

Data are contained within the article.

Conflicts of Interest

Authors Baturalp Yalcinkaya and Matej Buzgo were employed by the company Respilon Membranes s.r.o. The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

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Polymers 17 03019 g001
Figure 1. Needleless electrospinning spinneret body and spinning process.
Figure 1. Needleless electrospinning spinneret body and spinning process.
Polymers 17 03019 g001
Polymers 17 03019 g002
Figure 2. Industrial-size needleless electrospinning devices.
Figure 2. Industrial-size needleless electrospinning devices.
Polymers 17 03019 g002
Polymers 17 03019 g003
Figure 3. PA6 nanofibers with GO nanoparticles.
Figure 3. PA6 nanofibers with GO nanoparticles.
Polymers 17 03019 g003
Table 1. The list of polymers.
Table 1. The list of polymers.
Polymer NameCommercial NameType and Key
Properties		Supplier NameOrigin Country
CACellulose acetate (CA-398-10)Semi-synthetic polymer derived from cellulose; 39.8% acetyl content; Tg ≈ 190 °C;EastmanKingsport, TN, USA
PCLPolycaprolactone
(Mn) 80,000		Aliphatic biodegradable polyester; low Tg (−60 °C), Tm ≈ 60 °C; high flexibility.Sigma AldrichBurlington, MA, USA
PA6Ultramid® B24Synthetic polyamide with high crystallinity, Tg ≈ 50 °C, Tm ≈ 220 °C; good spinnability and mechanical strengthBASFLudwigshafen, Germany
PA6Econyl 27Chemically regenerated nylon 6 from waste; same structure as PA6 but higher purity; sustainable alternativeEconylTrento, Italy
PA11Rilsan®Long-chain aliphatic bio-polyamide from castor oil; Tm ≈ 190 °C; low moisture uptake, high flexibilityArkemaFrance, Colombes
PA12VESTAMID® LLong-chain polyamide; Tm ≈ 178 °C; very low water absorption, high chemical resistance.EvonikGermany, Essen
PVBMowital B 60 HAmorphous thermoplastic with hydroxyl groups (~18–22%); Tg ≈ 70 °C.KurarayGermany, Hattersheim
PANPolyacrylonitrileSemi-crystalline polymer; Tg ≈ 95 °C; precursor for carbon fibers; highly polar nitrile groups aid jet stabilityGoodfellowHuntingdon, UK
PVDFKynar 761ASemi-crystalline fluoropolymer; Tm ≈ 170 °C; piezoelectric and hydrophobic; excellent chemical resistanceArkemaColombes, France
PULarithane AL 286Thermoplastic elastomer; Shore A ≈ 85; soft segment polyester-based; high elasticity, durableNovotexGaggiano, Italy
PVAPoval™ 5-88Water-soluble synthetic polymer; 88 mol% hydrolyzed; Mw ≈ 89,000–98,000.KurarayHattersheim, Germany
CSChitosan—Medium molecular weightNatural cationic polysaccharide; deacetylation ~75–85%; Mw ≈ 190–310 kDa.Sigma AldrichBurlington, MA, USA
Table 2. List of additives.
Table 2. List of additives.
AdditiveParticle SizeSupplier Name
TiO2200 nmNanografi (Düsseldorf, Germany)
ZnO NP30–50 nmNanografi
MgO NP55 nmNanografi
MgO NP500–1500 nmNanografi
CuO NP38 nmNanografi
CuO NP78 nmNanografi
CuO NP20 µmArgaman (Jerusalem, Israel)
Ag100 nmNanografi
Graphene Oxide<2 µmGraphene-XT (Bologna, Italy)
CeO28–28 nmNanografi
Er2O38–90 nmNanografi
WO355 nmNanografi
MnO2<200 mesh size (micron powder)Nanografi
Hyperbranched PolymerPFLDHB-G4-PEG10K-OHPolymer Factory (Stockholm, Sweden)
Hyperbranched PolymerPFLDHB-G4-PEG10K-NH3+Polymer Factory
Table 3. List of the solvents.
Table 3. List of the solvents.
SolventAcronymSupplier Name
DichloromethaneDCMVWR International s.r.o (Stříbrná Skalice, Czech)
Formic acidFAVWR International s.r.o
Acetic acidAAVWR International s.r.o
ChloroformCHVWR International s.r.o
MethanolMethaVWR International s.r.o
EthanolEthVWR International s.r.o
AcetonitrileAceVWR International s.r.o
DimethylacetamideDMACVWR International s.r.o
DimethylformamideDMFVWR International s.r.o
Ethyl acetateEAVWR International s.r.o
Demineralized waterDW-
Table 4. Process parameters of CA nanofibers electrospinning.
Table 4. Process parameters of CA nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−20/+70kV
Distance between electrodes315mm
Solution feeding rates125mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature25/22Rh%/°C
Table 5. Solution parameters, SEM images, and fiber diameters of CA nanofibers.
Table 5. Solution parameters, SEM images, and fiber diameters of CA nanofibers.
Polymer: Cellulose Acetate 398-10
Main Solvents: DMAC/Ace
Ratio of solvents5/55/55/55/5
Solution concentration w/v (%)1012.51517.5
SEM Image
Magnifications
10k×–15k×–10k×		Polymers 17 03019 i001Polymers 17 03019 i002Polymers 17 03019 i003High viscosity
no spinning
Fiber diameters (nm)
★ Best conditions		340 ± 35410 ± 32430 ± 42 ★-
Ratio of solvents9/17/33/71/9
Solution concentrations w/v (%)15151515
SEM Image
Magnifications
0–10k×–10k×		No fiber
only solution spray—wet surface		Polymers 17 03019 i004Polymers 17 03019 i005High viscosity
No spinning
Fiber diameters (nm)--1375 ± 126-
Table 6. Process parameters of PCL nanofibers electrospinning.
Table 6. Process parameters of PCL nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−30/+70kV
Distance between electrodes350mm
Solution feeding rates100–250mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature38/25Rh%/°C
Table 7. Solution parameters, SEM images, and fiber diameters of PCL nanofibers.
Table 7. Solution parameters, SEM images, and fiber diameters of PCL nanofibers.
Polymer: Polycaprolactone
Main Solvents: Chloroform
Solution concentration w/v (%)1012.515
Ratio of solvents---
SEM Image
Magnifications
5k×–1k×–1k×		Polymers 17 03019 i006Polymers 17 03019 i007Polymers 17 03019 i008
Fiber diameters (nm)765 ± 1521210 ± 1341450 ± 164
Solution concentrations w/v (%)1012.515
Ratio of solvents5/5 CH/Eth5/5 CH/Eth5/5 CH/Eth
SEM Image
Magnifications
5k×–5k×–5k×		Polymers 17 03019 i009Polymers 17 03019 i010Polymers 17 03019 i011
Fiber diameters (nm)
★ Best conditions 		2430 ± 2302870 ± 2753055 ± 351 ★
Solution concentration w/v (%)1012.515
Ratio of solvents5/5 CH/Metha5/5 CH/Metha5/5 CH/Metha
SEM Image
Magnifications
5k×–5k×–5k×		Polymers 17 03019 i012Polymers 17 03019 i013Polymers 17 03019 i014
Fiber diameters (nm)3240 ± 4204330 ± 4414680 ± 530
Solution concentrations w/v (%)1012.515
Ratio of solvents5/5 CH/(AA:FA 1:1))5/5 CH/(AA:FA 1:1)5/5 CH/(AA:FA 1:1)
SEM Image
Magnifications
500×–500×–1k×		Polymers 17 03019 i015Polymers 17 03019 i016Polymers 17 03019 i017
Fiber diameters (nm)5430 ± 5395670 ± 6106055 ± 647
Solution concentration w/v (%)1012.515
Ratio of solvents5/5 CH/Ace5/5 CH/Ace5/5 CH/Ace
SEM Image
Magnifications
5k×–500×–5k×		Polymers 17 03019 i018Polymers 17 03019 i019Polymers 17 03019 i020
Fiber diameters (nm)1890 ± 2801975 ± 3152055 ± 421
Solution concentration w/v (%)1012.515
Ratio of solvents7/3 (AA:FA 1:1)/CH7/3 (AA:FA 1:1)/CH7/3 (AA:FA 1:1)/CH
SEM Image
Magnifications
5k×–5k×–5k×		Polymers 17 03019 i021Polymers 17 03019 i022Polymers 17 03019 i023
Fiber diameters (nm)
★ Best conditions		525 ± 95 ★640 ± 110670 ± 153
Solution concentration w/v (%)15% (2/1)
PCL/CA 398-3		15% (2/1)
PCL/CAB CA 381-2		15% (2/1)
PCL/CAP CA 482-0.5
Ratio of solvents5/5 (AA:FA 1:1)/CH 5/5 (AA:FA1:1)/CH5/5 (AA:FA 1:1)/CH
SEM Image
Magnifications
5k×–5k×–5k×		Polymers 17 03019 i024Polymers 17 03019 i025Polymers 17 03019 i026
Fiber diameters (nm)825 ± 168840 ± 175725 ± 158 ★
Solution concentration w/v (%)15% (9/1)
PCL/CS		15% (6/4)
PCL/PEO
Ratio of solvents5/5 (AA:FA 1:1)/(CH:FA 1:1)5/5 (AA:FA 1:1)/CH
SEM Image
Magnifications
10k×–5k×–0		Polymers 17 03019 i027Polymers 17 03019 i028
Fiber diameters (nm)
★ Best conditions		775 ± 163 ★670 ± 145 ★
Table 8. Process parameters of PA6 nanofibers electrospinning.
Table 8. Process parameters of PA6 nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−27/+70kV
Distance between electrodes320mm
Solution feeding rates80–100mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature35/22Rh%/°C
Table 9. Solution parameters, SEM images, and fiber diameters of PA6 nanofibers.
Table 9. Solution parameters, SEM images, and fiber diameters of PA6 nanofibers.
Polymer: Polyamide 6 (Econyl 27)
Main Solvents: AA/FA
Solution concentration w/v (%)1012.515
Ratio of solvents2/12/12/1
SEM Image
Magnifications
30k×–20k×–20k×		Polymers 17 03019 i029Polymers 17 03019 i030Polymers 17 03019 i031
Fiber diameters (nm)
★ Best conditions		65 ± 29 ★150 ± 53200 ± 68
Solution concentration w/v (%)1012.515
Ratio of solvents3/23/23/2
SEM Image
Magnifications
10k×–20k×–10k×		Polymers 17 03019 i032Polymers 17 03019 i033Polymers 17 03019 i034
Fiber diameters (nm)90 ± 35135 ± 59290 ± 83
Solution concentration w/v (%)1012.515
Ratio of solvents1/1/1 AA/FA/DCM1/1/1 AA/FA/DCM1/1/1 AA/FA/DCM
SEM Image
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i035Polymers 17 03019 i036Polymers 17 03019 i037
Fiber diameters (nm)
★ Best conditions		185 ± 63440 ± 84 ★620 ± 126
Solution concentration w/v (%)1012.515
Ratio of solvents1/1/1 AA/FA/CH1/1/1 AA/FA/CH1/1/1 AA/FA/CH
SEM Image
Magnifications
10k×–10k×–5k×		Polymers 17 03019 i038Polymers 17 03019 i039Polymers 17 03019 i040
Fiber diameters (nm)
★ Best conditions		130 ± 75230 ± 80 ★520 ± 113 ★
Polymer: Polyamide 6 (BASF 24)
Main solvents: AA/FA
Solution concentration w/v (%)1012.515
Ratio of solvents1/1/1 AA/FA/DCM1/1/1 AA/FA/DCM1/1/1 AA/FA/DCM
SEM Image
Magnifications
20k×–20k×–20k×		Polymers 17 03019 i041Polymers 17 03019 i042Polymers 17 03019 i043
Fiber diameters (nm)
★ Best conditions		220 ± 135310 ± 142 ★400 ± 168
Solution concentration w/v (%)1012.515
Ratio of solvents1/1/1 AA/FA/CH1/1/1 AA/FA/CH1/1/1 AA/FA/CH
SEM Image
Magnifications
10k×–20k×–10k×		Polymers 17 03019 i044Polymers 17 03019 i045Polymers 17 03019 i046
Fiber diameters (nm)
★ Best conditions		250 ± 95400 ± 148 ★650 ± 163 ★
Table 10. Process parameters of PA11 and PA12 nanofibers electrospinning.
Table 10. Process parameters of PA11 and PA12 nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−30/+70kV
Distance between electrodes315mm
Solution feeding rates80–100mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature30/28Rh%/°C
Table 11. Solution parameters, SEM images, and fiber diameters of PA11, PA12 nanofibers.
Table 11. Solution parameters, SEM images, and fiber diameters of PA11, PA12 nanofibers.
Polymer: Polyamide 11, 12, and Polyvinyl Butyral
Main Solvents: FA/DCM
Polymer: Polyamide 11
Solution concen. w/v (%)1012.515
Ratio of solvents1/1 FA/DCM1/1 FA/DCM1/1 FA/DCM
SEM Image
Magnifications
10k×–20k×–10k×		Polymers 17 03019 i047Polymers 17 03019 i048Polymers 17 03019 i049
Fiber diameters (nm)4590 ± 4636455 ± 5196745 ± 736
Polymer: Polyamide 12
Main solvents: FA/DCM
Solution concen. w/v (%)1012.510
Ratio of solvents1/1 FA/DCM1/1 FA/DCMFA
SEM Image
Magnifications
5k×–1k×–1k×		Polymers 17 03019 i050Polymers 17 03019 i051Polymers 17 03019 i052
Fiber diameters (nm)
★ Best conditions		620 ± 4751465 ± 498790 ± 517 ★
Solution concen. w/v (%)12.515 (2/1)
PA11/ PVB		15 (2/1)
PA12/ PVB
Ratio of solventsFA1/1 FA/DCM1/1 FA/DCM
SEM Image
Magnifications
1k×–2.5k×–5k×		Polymers 17 03019 i053Polymers 17 03019 i054Polymers 17 03019 i055
Fiber diameters (nm)
★ Best conditions		1510 ± 2642395 ± 454870 ± 224 ★
Table 12. Process parameters of PAN nanofibers electrospinning.
Table 12. Process parameters of PAN nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−30/+70kV
Distance between electrodes350mm
Solution feeding rates100–150mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature21/23Rh%/°C
Table 13. Solution parameters, SEM images and fiber diameters of PAN nanofibers.
Table 13. Solution parameters, SEM images and fiber diameters of PAN nanofibers.
Polymer: Polyacrylonitrile
Main Solvents: DMAC and DMF
Solution concen. w/v (%)91012.5
Ratio of solventsDMACDMACDMAC
SEM Image
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i056Polymers 17 03019 i057Polymers 17 03019 i058
Fiber diameters (nm)335 ± 132350 ± 146410 ± 155
Solution concen. w/v (%)1012.515
Ratio of solventsDMFDMFDMF
SEM Image
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i059Polymers 17 03019 i060Polymers 17 03019 i061
Fiber diameters (nm)
★ Best conditions		165 ± 94210 ± 106 ★545 ± 210 ★
Solution concen. w/v (%)17.520
Ratio of solventsDMFDMF
SEM Image
Magnifications
10k×–5k×		Polymers 17 03019 i062Polymers 17 03019 i063
Fiber diameters (nm)720 ± 2582670 ± 410
Table 14. Process parameters of PVDF nanofibers electrospinning.
Table 14. Process parameters of PVDF nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−30/+70kV
Distance between electrodes320mm
Solution feeding rates50–150mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature24/20Rh%/°C
Table 15. Solution parameters, SEM images, and fiber diameters of PVDF nanofibers.
Table 15. Solution parameters, SEM images, and fiber diameters of PVDF nanofibers.
Polymer: Polyvinylidene Fluoride
Main Solvents: DMAC + 3%TEAB in DMF
Solution concen. w/v (%)1012.515
Ratio of solvents50/1
DMAC/TEAB in DMF		50/1
DMAC/TEAB in DMF		50/1
DMAC/TEAB in DMF
SEM Image
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i064Polymers 17 03019 i065Polymers 17 03019 i066
Fiber diameters (nm)225 ± 124325 ± 167440 ± 189
Solution concen. w/v (%)17.520
Ratio of solvents50/1
DMAC/TEAB in DMF		50/1
DMAC/TEAB in DMF
SEM Image
Magnifications
10k×–10k×		Polymers 17 03019 i067Polymers 17 03019 i068
Fiber diameters (nm)
★ Best conditions		495 ± 185 ★590 ± 210
Table 16. Process parameters of PU nanofibers electrospinning.
Table 16. Process parameters of PU nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−30/+70kV
Distance between electrodes320mm
Solution feeding rates100–200mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature28/22Rh%/°C
Table 17. Solution parameters, SEM images, and fiber diameters of PU nanofibers.
Table 17. Solution parameters, SEM images, and fiber diameters of PU nanofibers.
Polymer: Polyurethane
Main Solvents: DMF + 3%TEAB in DMF
Solution concen. w/v (%)101520
Ratio of solventsDMFDMFDMF
SEM Image
Magnifications
5k×–5k×–5k×		Polymers 17 03019 i069Polymers 17 03019 i070Polymers 17 03019 i071
Fiber diameters (nm)445 ± 138680 ± 1651410 ± 215
Solution concen. w/v (%)10 12.515
Ratio of solventsDMF/TEAB in DMF
50/1		DMF/TEAB in DMF
50/1		DMF/TEAB in DMF
50/1
SEM Image
Magnifications
5k×–10k×–10k×		Polymers 17 03019 i072Polymers 17 03019 i073Polymers 17 03019 i074
Fiber diameters (nm)
★ Best conditions		470 ± 174560 ± 186665 ± 242 ★
Solution concen. w/v (%)17.515 PU/PVB
10/1
Ratio of solventsDMF/TEAB in DMF
50/1		DMF
SEM Image
Magnifications
10k×–5k×		Polymers 17 03019 i075Polymers 17 03019 i076
Fiber diameters (nm)
★ Best conditions		720 ± 255 ★450 ± 195
Table 18. Process parameters of PVB nanofibers electrospinning.
Table 18. Process parameters of PVB nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−25/+70kV
Distance between electrodes290Mm
Solution feeding rates80–120mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature30/25Rh%/°C
Table 19. Solution parameters, SEM images, and fiber diameters of PVB nanofibers.
Table 19. Solution parameters, SEM images, and fiber diameters of PVB nanofibers.
Polymer: Polyvinyl Butyral
Main Solvents: Ethanol
Solution concen. w/v (%)1012.515
Ratio of solvents1/1 EtOH/CH1/1 EtOH/CH1/1 EtOH/CH
SEM Image
Magnifications
5k×–5k×–		Polymers 17 03019 i077Polymers 17 03019 i078Too viscous polymer solution—no fibers
Fiber diameters (nm)1455 ± 3581580 ± 377
Solution concen. w/v (%)1012.515
Ratio of solvents1/1 EtOH/(AA:FA)1/1 EtOH/(AA:FA)1/1 EtOH/(AA:FA)
SEM Image
Magnifications
5k×–10k×–5k×		Polymers 17 03019 i079Polymers 17 03019 i080Polymers 17 03019 i081
Fiber diameters (nm)
★ Best conditions		720 ± 203 ★890 ± 2742640 ± 298
Solution concen. w/v (%)1012.515
Ratio of solvents1/1 EtOH/EtAC1/1 EtOH/EtAC1/1 EtOH/EtAC
SEM Image
Magnifications
10k×–5k×–5k×		Polymers 17 03019 i082Polymers 17 03019 i083Polymers 17 03019 i084
Fiber diameters (nm)510 ± 1651630 ± 2482150 ± 313
Table 20. Process parameters of PVA nanofibers electrospinning.
Table 20. Process parameters of PVA nanofibers electrospinning.
ParametersValuesUnits
Applied voltage−25/+70kV
Distance between electrodes350mm
Solution feeding rates100–250mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature20/30Rh%/°C
Table 21. Solution parameters, SEM images, and fiber diameters of PVA nanofibers.
Table 21. Solution parameters, SEM images, and fiber diameters of PVA nanofibers.
Polymer: Polyvinyl Alcohol
Main Solvents: DW, EtOH, AA/FA (1/1), DMF
Solution concen. w/v (%)101214
Ratio of solventsDemi-waterDemi-waterDemi-water
SEM Image
Magnifications
1k×–10k×–5k×		Polymers 17 03019 i085Polymers 17 03019 i086Polymers 17 03019 i087
Fiber diameters (nm)
★ Best conditions		360 ± 103435 ± 152 ★690 ± 194
Solution concen. w/v (%)101214
Ratio of solventsEtOHEtOHEtOH
SEM Image
Magnifications
5k×–5k×–5k×		Polymers 17 03019 i088Polymers 17 03019 i089Polymers 17 03019 i090
Fiber diameters (nm)1160 ± 2341280 ± 2532430 ± 279
Solution concen. w/v (%)101214
Ratio of solventsAA/FA (1/1)AA/FA (1/1)AA/FA (1/1)
SEM Image
Magnifications
–20k×–5k×		Low viscosity, wet surfacePolymers 17 03019 i091Polymers 17 03019 i092
Fiber diameters (nm)
★ Best conditions		 245 ± 87 ★1965 ± 268
Solution concen. w/v (%)101214
Ratio of solventsDMFDMFDMF
SEM Image
Magnifications
–10k×–5k×		Low viscosity, wet surfacePolymers 17 03019 i093Polymers 17 03019 i094
Fiber diameters (nm) 570 ± 1641090 ± 236
Table 22. Process parameters of PA6 nanofibers containing nanoparticles during electrospinning.
Table 22. Process parameters of PA6 nanofibers containing nanoparticles during electrospinning.
ParametersValuesUnits
Applied voltage−27/+70kV
Distance between electrodes320mm
Solution feeding rates80–100mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature35/22Rh%/°C
Table 23. Solution parameters, SEM images of PA6 nanofibers containing nanoparticles.
Table 23. Solution parameters, SEM images of PA6 nanofibers containing nanoparticles.
Polymer: 15 w/v % PA6
Main Solvents and Ratio: AA/FA/CH 1/1/1
Type of NanoparticleTiO2 200 nm
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
20k×–20k×–20k×		Polymers 17 03019 i095Polymers 17 03019 i096Polymers 17 03019 i097
Type of NanoparticleZnO 30–50 nm
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
20k×–10k×–20k×		Polymers 17 03019 i098Polymers 17 03019 i099Polymers 17 03019 i100
Type of NanoparticleMgO 55 nm
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i101Polymers 17 03019 i102Polymers 17 03019 i103
Type of NanoparticleMgO 500–1500 nm
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
10k×–5k×–10k×		Polymers 17 03019 i104Polymers 17 03019 i105Polymers 17 03019 i106
Type of NanoparticleCuO 38 nm
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
10k×–5k×–5k×		Polymers 17 03019 i107Polymers 17 03019 i108Polymers 17 03019 i109
Type of NanoparticleCuO 78 nm
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
10k×–5k×–5k×		Polymers 17 03019 i110Polymers 17 03019 i111Polymers 17 03019 i112
Type of NanoparticleCuO 20 micron
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
5k×–5k×–5k×		Polymers 17 03019 i113Polymers 17 03019 i114Polymers 17 03019 i115
Type of NanoparticleAg
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
10k×–5k×–10k×		Polymers 17 03019 i116Polymers 17 03019 i117Polymers 17 03019 i118
Type of NanoparticleGraphene Oxide
Nanoparticle concen. w (%)51530
SEM Images
Magnifications
5k×–10k×–10k×		Polymers 17 03019 i119Polymers 17 03019 i120Polymers 17 03019 i121
Type of NanoparticleCeO2
Nanoparticle concen. w (%) 1530
SEM Images
Magnifications
–5k×–5k×		 Polymers 17 03019 i122Polymers 17 03019 i123
Type of NanoparticleCeO2/TiO2
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
15k×–10k×–25k×		Polymers 17 03019 i124Polymers 17 03019 i125Polymers 17 03019 i126
Type of NanoparticleCeO2/ZnO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i127Polymers 17 03019 i128Polymers 17 03019 i129
Type of NanoparticleEr2O3
Nanoparticle concen. w (%) 1530
SEM Images
Magnifications
–10k×–10k×		 Polymers 17 03019 i130Polymers 17 03019 i131
Type of NanoparticleEr2O3/TiO2
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
20k×–20k×–20k×		Polymers 17 03019 i132Polymers 17 03019 i133Polymers 17 03019 i134
Type of NanoparticleEr2O3/ZnO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i135Polymers 17 03019 i136Polymers 17 03019 i137
Type of NanoparticleWO3
Nanoparticle concen. w (%) 1530
SEM Images
Magnifications
–10k×–10k×		 Polymers 17 03019 i138Polymers 17 03019 i139
Type of NanoparticleWO3/TiO2
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
20k×–20k×–10k×		Polymers 17 03019 i140Polymers 17 03019 i141Polymers 17 03019 i142
Type of NanoparticleWO3/ZnO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i143Polymers 17 03019 i144Polymers 17 03019 i145
Type of NanoparticleMnO2
Nanoparticle concen. w (%) 1530
SEM Images
Magnifications
–10k×–10k×		 Polymers 17 03019 i146Polymers 17 03019 i147
Type of NanoparticleMnO2/GO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i148Polymers 17 03019 i149Polymers 17 03019 i150
Type of NanoparticleTiO2/GO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
20k×–10k×–10k×		Polymers 17 03019 i151Polymers 17 03019 i152Polymers 17 03019 i153
Type of NanoparticleCeO2/GO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i154Polymers 17 03019 i155Polymers 17 03019 i156
Type of NanoparticleWO3/GO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i157Polymers 17 03019 i158Polymers 17 03019 i159
Type of NanoparticleEr2O3/GO
Nanoparticle concen. w (%)(15/15)(30/15)(15/30)
SEM Images
Magnifications
10k×–10k×–10k×		Polymers 17 03019 i160Polymers 17 03019 i161Polymers 17 03019 i162
Type of NanoparticleHyperbranched polymer
Nanoparticle concen. w (%)1% HBPG4-OH1% HBPG4-NH
SEM Images
Magnifications
10k×–10k×–		Polymers 17 03019 i163Polymers 17 03019 i164
Table 24. Process parameters of PAN nanofibers containing nanoparticles during electrospinning.
Table 24. Process parameters of PAN nanofibers containing nanoparticles during electrospinning.
ParametersValuesUnits
Applied voltage−30/+70kV
Distance between electrodes350mm
Solution feeding rates100–150mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature21/23Rh%/°C
Table 25. Solution parameters, SEM images of PAN nanofibers containing nanoparticles.
Table 25. Solution parameters, SEM images of PAN nanofibers containing nanoparticles.
Polymer: 15 w/v % PAN
Main Solvents and Ratio: DMF
Type of NanoparticleTiO2 NP—200 nmZnO—30–50 nmMgO NP—55 nm
Nanoparticle concen. w (%)151515
SEM ImagesPolymers 17 03019 i165Polymers 17 03019 i166Polymers 17 03019 i167
Type of NanoparticleMgO/TiO2 NPMgO/ZnO
Nanoparticle concen. w (%)15/1515/15
SEM ImagesPolymers 17 03019 i168Polymers 17 03019 i169
Type of NanoparticleCeO2CeO2/TiO2CeO2/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i170Polymers 17 03019 i171Polymers 17 03019 i172
Type of NanoparticleEr2O3Er2O3/TiO2Er2O3/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i173Polymers 17 03019 i174Polymers 17 03019 i175
Type of NanoparticleWO3WO3/TiO2WO3/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i176Polymers 17 03019 i177Polymers 17 03019 i178
Type of NanoparticleMnO2MnO2/TiO2MnO2/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i179Polymers 17 03019 i180Polymers 17 03019 i181
Type of NanoparticleGOGO/TiO2GO/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i182Polymers 17 03019 i183Polymers 17 03019 i184
Table 26. Process parameters of PU nanofibers containing nanoparticles during electrospinning.
Table 26. Process parameters of PU nanofibers containing nanoparticles during electrospinning.
ParametersValuesUnits
Applied voltage−30/+70kV
Distance between electrodes350mm
Solution feeding rates100–150mbar/h
Solution feeding rates100mL/h
Nonwoven winding speed1mm/s
Humidity/Temperature21/23Rh%/°C
Table 27. Solution parameters, SEM images of PU nanofibers containing nanoparticles.
Table 27. Solution parameters, SEM images of PU nanofibers containing nanoparticles.
Polymer: 14.5 w/v % PU
Main Solvents and Ratio: DMF
Type of NanoparticleTiO2 NP—200 nmZnO—30–50 nmMgO NP—55 nm
Nanoparticle concen. w (%)151515
SEM ImagesPolymers 17 03019 i185Polymers 17 03019 i186Polymers 17 03019 i187
Type of NanoparticleMgO/TiO2 NPMgO/ZnO
Nanoparticle concen. w (%)15/1515/15
SEM ImagesPolymers 17 03019 i188Polymers 17 03019 i189Polymers 17 03019 i190
Type of NanoparticleCeO2CeO2/TiO2CeO2/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i191Polymers 17 03019 i192Polymers 17 03019 i193
Type of NanoparticleWO3WO3/TiO2WO3/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i194Polymers 17 03019 i195Polymers 17 03019 i196
Type of NanoparticleMnO2MnO2/TiO2MnO2/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i197Polymers 17 03019 i198Polymers 17 03019 i199
Type of NanoparticleGrOGrO/TiO2GrO/ZnO
Nanoparticle concen. w (%)1515/1515/15
SEM ImagesPolymers 17 03019 i200Polymers 17 03019 i201Polymers 17 03019 i202
Table 28. Applications of all the mentioned polymeric nanofibers and their summary.
Table 28. Applications of all the mentioned polymeric nanofibers and their summary.
PolymerApplications of NanofibersSummary
PA6Filtration membranes [112], sportwear and protective textiles [17], biomedical scaffolds [113], air and water purification [114]Widely used in filtration thanks to the small fiber diameter.
PA11Biomedical devices, sensors [115], membrane separation, eco-friendly engineering applications [116]Bio-based polymer for sustainable applications.
PA12Oil-water separation membranes, biomedical materialsIndustrial filters due to low water absorption.
PVBAir filtration [117], battery separators [118], sound-insulating materials [119]Versatile and flexible nanofibers.
PCLTissue engineering scaffolds [60], drug delivery systems [61], wound healing applications [82]Medical applications, thanks to biodegradability.
PANFiltration membranes [120], energy storage [121](supercapacitors), carbon nanofiber precursors [122], protective textiles [107]Excellent thermal stability and chemical resistance for challenging applications.
PVDFBattery separators [123], piezoelectric sensors [124,125], water treatment membranes [126], energy harvesting devices [127], food packaging [128]Excellent weathering and chemical resistance.
PUWound dressings [129], biomedical scaffolds [130], breathable protective clothing [131], filtration membranes [132]Flexible, elastic, suitable for apparel and wound healing.
PVABiomedical applications [133] (drug delivery, wound healing), food packaging [134], water filtration membranes [135]hydrophilic, biodegradable, and non-toxic, widely used in biomedical fields.
CAAir and water filtration [136], biodegradable packaging [137], drug delivery systems [138], membrane separation [139]Exhibit excellent biocompatibility and biodegradability.
PA6/NPAntibacterial textiles [140], photocatalytic membranes [141], self-cleaning surfaces [142], heavy metal removal from wastewater [143]Enhances antibacterial, photocatalytic, and self-cleaning properties
PAN/NPFiltration membranes [144], antibacterial materials [145], enhanced adsorption capacity [146], UV protection [147]Provides enhanced photocatalytic activity, antibacterial behavior, and pollutant adsorption
PU/NPAntimicrobial wound dressings [148], UV-resistant coatings [149], smart textiles [150], gas sensors [151]Provides antimicrobial activity, UV resistance
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Yalcinkaya, B.; Buzgo, M. A Guide for Industrial Needleless Electrospinning of Synthetic and Hybrid Nanofibers. Polymers 2025, 17, 3019. https://doi.org/10.3390/polym17223019

AMA Style

Yalcinkaya B, Buzgo M. A Guide for Industrial Needleless Electrospinning of Synthetic and Hybrid Nanofibers. Polymers. 2025; 17(22):3019. https://doi.org/10.3390/polym17223019

Chicago/Turabian Style

Yalcinkaya, Baturalp, and Matej Buzgo. 2025. "A Guide for Industrial Needleless Electrospinning of Synthetic and Hybrid Nanofibers" Polymers 17, no. 22: 3019. https://doi.org/10.3390/polym17223019

APA Style

Yalcinkaya, B., & Buzgo, M. (2025). A Guide for Industrial Needleless Electrospinning of Synthetic and Hybrid Nanofibers. Polymers, 17(22), 3019. https://doi.org/10.3390/polym17223019

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