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DOI: 10.1016/j.jmrt.2019.10.001
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Available online 19 October 2019
Fabrication and characterization of PEBA fibers by melt and solution electrospinning
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Zahid Sarwar, Edvinas Krugly, Paulius Pavelas Danilovas, Darius Ciuzas, Violeta Kauneliene, Dainius Martuzevicius
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daimart@ktu.lt

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Kaunas University of Technology, Faculty of Chemical Technology, Radvilenu pl. 19, Kaunas, Lithuania
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Received 06 June 2019. Accepted 01 October 2019
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Table 1. Design of Experiment of melt electrospinning.
Table 2. Design of experiment of solution electrospinning.
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Abstract

Poly(ether-block-amide), often abbreviated as PEBA, is a novel polymer which is a combination of polyamide and poly ether group. The present study aimed at the fabrication of PEBA fibers by both melt and solution electrospinning. The effects of process parameters of both electrospinning techniques on fiber diameters and morphology were researched. The obtained fiber substrates were characterized for their morphology, changes in chemical composition, thermal properties, crystallinity, and hydrophobicity. Optimum results (as minimum average fiber diameter of 1.92 ± 3.31 µm) in case of melt electrospinning were obtained at tip-to-collector distance (TTCD) of 60 mm, voltage 20.0 kV, collector speed 55 rpm, and melt temperature 270 °C, whereas in case of solution electrospinning TTCD of 200 mm distance and voltage of 20 kV yielded the lowest average fiber diameter of 0.37 ± 0.34 μm.

Keywords:
PEBA
Melt electrospinning
Solution electrospinning
Hydrophobic membranes
Full Text
1Introduction

PEBA is an emerging elastomer which has many versatile applications. It is a copolymer of polyamide and polyether segments [1,2]. Polyamide is a hard hydrophilic segment that is responsible for higher mechanical strength. On the other side polyether is soft hydrophobic part that gives flexibility [3–5]. Thus, it offers a balanced combination of mechanical strength, breathability, flexibility, chemical resistance, and ease of processing. Therefore, it can be applied in many fields, such as medical materials, sports market, daily life, environmental, etc. [5–7]. Specific applications of PEBA extend to separation of organic compounds [8–10] and gases [11–15], recovery of alcohols from aqueous streams [16,17], and storing of food materials in modified atmosphere [18].

The applications taking advantage on the affinity of PEBA for certain compounds are of a specific interest in chemical engineering. Sridhar et al. [19] synthesized and characterized membranes of PEBA loaded with activated carbon for the permeability of carbon dioxide and methane gas. Sole et al. [4] developed non porous modified membranes of PEBA by using mercaptoethanol for different biomedical applications. Thanakkasaranee et al. [2] reported preparation of composite membrane of PEBA and poly ethylene glycol using solution casting technique for temperature dependent permeability of gases. Cheshomi et al. [6] fabricated thin film composite membranes for waste water treatment by coating polysulfone and polyethersulfone (PSf-PES) membrane with PEBA and using TiO2 nanoparticles to modify the membrane.

While above studies report PEBA applications in the form of coated membranes, there are very few attempts to produce fibrous membranes. High surface area to volume ratio, easy process for various functionalities, mechanical strength, high speed & low cost, large porosity, and control of fiber diameter are the some major advantages over the traditional coated membranes [20–25].

Some of the most popular techniques to produce polymer fibers includes electrospinning. It is a versatile technique which is abundantly used for the production of fibers from micrometer to nanometric scale [26]. The key feature of electrospun fiber is high aspect ratio [27] that made it suitable for many potential applications in various fields such as tissue engineering, drug delivery, biomedical, textiles, filtration, sensors, catalysis, electronic devices, energy storage, and environmental applications [28–33].

The stretching of polymer cone or jet through a small nozzle with the help of electrostatic force for the generation of fiber is known as electrospinning [34,35]. Electrospinning gained rapid attention since its start from 1887 [36]. The process of electrospinning is relatively simple in which a syringe with capillary or needle, feed pump, high supply voltage source and collector are used to produce fibers. One terminal of voltage supply is attached with syringe and other is with collector. The polymer is forced through the nozzle due to the electrostatic force of repulsion of similar charges and charged species accumulate at the tip of nozzle. When this repulsion force dominates the surface tension, these charged species came out from the nozzle in the form of conical shape that is called Taylor cone [34]. The Taylor cone is elongated due the attractive force of opposite charged collector and solidify on collector in the form of fiber [37,38]. A variety of materials including polymers, ceramics, and composites can be used in electrospinning for the fabrication of fine fibers [39]. By using this technique, hollow and solid interior structures of fibers can also be developed [40].

Electrospinning is categorized into two types based on polymer state used for the formation of fiber, namely melt and solution electrospinning [41]. Melt electrospinning is also known as solvent free electrospinning [42]. Toxicity, selectivity, environmental concerns, cost of solvents, and low production are the some major drawbacks of solution electrospinning [43,44]. The absence of solvents and its residues made melt electrospinning a safer, reliable, and greener method for the production of fibers for various applications [45] but larger diameter, complex apparatus and deficiency of suitable materials are the few drawbacks of it [46]. In melt electrospinning polymer is directly heated for the formation of fibers. The produced fibers have fewer defects and better physio mechanical properties besides higher yield [47,41].

Only one study to produce PEBA fibers by solution electrospinning was reported by Liang et al. [48]. Here PEBA was dissolved in isopropanol along with silver nanoparticles of diameter 200 nm to impart antimicrobial functionality. The diameter of resultant fibers was in micrometer range. Antibacterial results indicate that very low content of silver nanoparticles (0.15%) in PEBA fibers show excellent inhibition rate (>99.9%) against E. coli and S. aureus. Buivydiene et al. recently reported applications of melt electrospun PEBA for air filtration, however, due to issues in polymer feeding, obtained morphologies were less consistent, compared to polyamide [49], allowing for the further optimization of the spinning process.

This research presents an attempt to produce PEBA fibres by melt and solution electrospinning. Effects of process parameters such as applied voltage, tip to collector distance, melting temperature, feed rate, and collector speed on fiber morphology were investigated. The obtained fibrous mats were tested for thermal stability and changes in chemical composition.

2Experimental2.1Materials

Poly(ether-block-amide) in the form of pellets was obtained from Arkema Group, France (product No Pebax 3533SP-01). This grade of Pebax has been selected due to its relatively high melt flow rate among the product line.

Butanol (71-36-3) and acetic acid (glacial) were purchased from Merck KGaA (Germany) and used it as received without further purification.

2.2Preparation of filament for melt electrospinning

The pellets of PEBA were converted into filament form by using a filament extruder, which included steps of grinding, melting, extruding, cooling in cold water bath, and stretching in a roller system. This filament (diameter 1.5 mm) was the input material for melt electrospinning. The viscosity of the melt of such filament ranged from 706 Pa·s at 300 ℃ to 792 Pa·s at 240 °C.

2.3Preparation of solution

The solution for electrospinning has been prepared by dissolving pellets in either glacial acetic acid or butanol. A homogenized solution of 15% w/v was prepared at 60 °C with magnetic stirring at 250 rpm for 5 h. The viscosity of solution was 17.9 Pa.s in case of butanol and 12.3 Pa.s in case of acetic acid.

2.4Electrospinning apparatus and process

Electrospinning setups used in this study were developed in KTU and reported by Buivydiene et al. [49] and Matulevicius et al. [50].

Filament of PEBA was fed to the melt electrospinning machine by using a nozzle of 0.4 mm with a feed rate of 5 mm/min.

Solution was fed into solvent electrospinning machine by using a needle of 21 G, flow rate of 3 ml/h and collector speed of 15 rpm. The process of electrospinning was carried out in a closed chamber at the temperature of 22 °C and relative humidity of 40%.

2.5Design of experiment and data analysis

The experiment was conducted following a full factorial design (MODDE 10, Umetrics, Sweden) as shown in Tables 1 and 2. Fiber morphology and characteristics mainly depend upon the process parameters [57]. Thus, experimental variables including voltage, tip-to-collector distance, temperature, and collector speed were varied in order to research their effects to the fiber morphology (represented as a mean fiber diameter).

Table 1.

Design of Experiment of melt electrospinning.

Sample code  Tip-to-collector distance(mm)  Voltage (kV)  Collector speed, rpm  Temperature, o
M1  20  10  10  300 
M2  20  10  100  300 
M3  20  30  100  300 
M4  20  30  10  300 
M5  20  30  10  240 
M6  20  30  100  240 
M7  20  10  100  240 
M8  20  10  10  240 
M9  60  20  55  270 
M10  100  10  10  240 
M11  100  10  100  240 
M12  100  30  10  240 
M13  100  30  100  240 
M14  100  30  10  300 
M15  100  30  100  300 
M16  100  10  100  300 
M17  100  10  10  300 
Table 2.

Design of experiment of solution electrospinning.

Sample code  Tip-to-collector Distance (mm)  Voltage (kV) 
Solvent acetic acid
SA1  100  12 
SA2  100  20 
SA3  200  20 
SA4  200  12 
SA5  150  16 
SA6  150  16 
SA7  150  16 
Solvent Butanol
SB1  100  12 
SB2  100  20 
SB3  200  20 
SB4  200  12 
SB5  150  16 
SB6  150  16 
SB7  150  16 
2.6Characterization

The morphology of electrospun samples was observed by scanning electron microscopy (EVO MA10, Carl Zeiss, Germany). Image J (NIH, USA) software was used for the calculation of diameter of fibers from SEM images. 50 readings for each sample were taken and then average diameters were calculated.

Thermal stability of the produced fibers was analyzed by the thermogravimetric analysis (TGA), using by the TG analyzer (TGA 400, Perkin Elmer, USA) under nitrogen atmosphere. The temperature range is between 0 and 700 °C with a heating rate of 10 °C·min1.

The chemical composition (polymer functional groups) of the fibers (melt & solution) were characterized by infrared spectrometer (Spectrum, Perkin Elmer, USA), within the wavelength ranging from 4000–500cm−1.

The crystallinity of electrospun fibers was assessed by XRD analysis (D8 Advance, Bruker-AXS, Germany) with Cu-Kα1 source. The analysis was conducted at a room temperature by scanning speed 6°/min from 5° to 90°(2θ).

The wetting behavior of electro spun fibers was evaluated by contact angle, measured with the optical tensiometer (Theta Lite, Biolin Scientific, UK). A 5 µL water droplet of deionized water was pipetted and contact angle was measured according to sessile method. This procedure was repeated at three different places for each sample and average (arithmetic mean) was taken from these results.

3Results and discussion3.1Morphology of melt electro spun fibers

The obtained fibrous mats displayed a relatively large variation in fiber diameters, ranging from 1.92 to 61.70 μm (Fig. 1). The majority of diameters of the samples ranged from 1 to 10–15 μm. Generally, fiber diameter distributions were narrow, with the interquartile range spanning between 2 and 7 μm. The smallest fiber diameter with low dispersion has been featured in sample M4 (Fig. 2a and b), obtained at conditions of high voltage (30 kV), small TTCD (20 mm), high heating temperature (300 °C) and slow rotation of collector drum (20 rpm). Specific cases were noted in samples M6 and M17, where both fiber average diameter and the dispersion were higher. M6 was a combination of low temperature (240 °C), and high voltage (30 kV), which resulted in poor spinning conditions and large randomly oriented fibers. On the contrary, most samples were featuring a core of highly oriented larger fibers, interlinked with smaller whipped ones. Similar morphology has been obtained in recent study [49], where major part of obtained samples were referred to as “parallel/disperse/thick”. Such formation has been reported to occur under low-voltage conditions and a high polymer feed rate, suggesting that in cases of overly high polymer viscosity, the electric field is not capable of initiating sufficient formation of fiber jets or whipping, thereby resulting in a process of simple drawing of the melt as opposed to electrospinning. Interestingly, we did not observe ribbon like structure, previously reported at medium or large nozzle tip diameters (0.4–0.5 mm) and high feed rate (20 mm/min). But generally, we were able to obtain fibers of smaller diameter, having majority at below 10 µm, as opposed to those reported by Buivydiene et al., 2019 in the range of 10-40 μm.

Fig. 1.

Fiber diameter distribution of melt electro spun fibers.

(0.12MB).
Fig. 2.

SEM images of melt electrospun samples: M4 (TTCD = 20 mm, U = 30 kV, S = 10 rpm, T = 300 °C) and M13 (TTCD = 100 mm, U = 30 kV, S = 100 rpm, T = 240 °C) at magnification of ×50 (A and C), and ×100 (B and D), respectively.

(0.57MB).

Effects of process parameters on the mean fiber diameter are shown in Fig. 3. It can be observed that as the collector distance increased from 20 to 60 mm, the resultant fiber diameter decreased from 12.5 to 5 μm. It is potentially due to the fact that at larger collector distance, the jet of polymer has enough time for thinning to reach the collector. The further increase of the distance to 100 mm resulted in the increase of fiber diameter to 7.5 μm. The further increase in distance reduced the electrostatic field and jet solidified before reaching the collector, as suggested by [51], who observed similar phenomenon by electrospinning low-density polyethylene.

Fig. 3.

Effect of Process parameters on fiber diameter melt electro spun fibers.

(0.18MB).

The increasing voltage from 10 to 20 kV resulted in the decreasing fiber diameter from 7 to 5 μm, due to more intensive stretching of a fiber by an oppositely charged collector [52]. However, the further increase in voltage to 30 kV caused fiber diameter to increase to the average of 13 μm. The possible reason is that polymer jet is solidifies in the way before reaching the collector due to less time available for cooling under extensive applied voltage. Similar observation has been reported during melt electrospinning of polypropylene, where fiber diameter increased from 8 to 10 μm, following the increase of the voltage from 70 to 90 kV [53].

Increase in collector speed to a specific value decreased the fiber diameter. Further increase in the collector speed from that specific value increase the diameter of fiber. These results agree with those reported by [54]. Increase in temperature from 240 to 270 °C decreased the diameter of fiber from ∼15 to ∼5 μm. This is because increase in temperature decreased the viscosity of polymer and jet of polymer is easily stretched by electrical force and it became thin. When temperature is further increased to 300 °C, the diameter of fiber is increased to 5.50 μm. This is may be due to very low viscosity of polymer at this temperature that increase the falling speed of jet and ultimately higher feed rate that generate beaded fibers [55].

3.2Morphology of solution electrospun fibers

As expected, the solution electrospinning produced fiber diameter by an order of magnitude lower compared to melt electrospinning, with majority of fibers falling within 0.2–1 μm. The dispersion of fiber diameters was relatively low, with interquartile range varying within 0.5–0.8 μm. The smallest average diameter (0.37 ± 0.34 μm) has been obtained with the sample SB4 (TTCD = 200 mm, V = 12 kV), while the largest (0.78 ± 1.25 μm) with sample SB5 (TTCD = 150, V = 16 kV) (Fig. 4).

Fig. 4.

Fiber diameter distributions of solution electro spun fibers.

(0.14MB).

The solvent selection (acetic acid vs. butanol) did not significantly affect fiber diameter (p < 0.05 based on Mann–Whitney U test). At the same time, the selection of solvent for electrospinning of PEBA is critical due to its chemical resistant nature. Butanol has proved as good choice as a solvent producing smooth and uniform fibers, but solution of PEBA in butanol tends becoming very viscous and blocking the needle of syringe. The use of acetic acid as a solvent helped overcoming the problem of needle blockage due to being of lower viscosity at the same concentration of PEBA but resulted in the formation of beaded fibers (Fig. 5). Yener et al. explored this phenomenon with polyvinyl butyral and came to conclusion that lower conductivity of acetic acid as opposed to butanol causes the formation of beads [56].

Fig. 5.

SEM images of solution electrospun mat sample: SA2 (TTCD = 100 mm, U = 20 kV and SB4 (TTCD = 200 mm, U = 12 kV at magnification of ×100 (A and C), and ×20 (B and D), respectively.

(0.62MB).

Effects of tip to collector distance and voltage on the mean fiber diameter are presented in Fig. 6. Both parameters had an reverse effect to the fiber diameter. As the collector distance increased from 100 to 200 mm, the resultant fiber diameter decreased from 0.62 to 0.39 μm. At a larger TTCD, the jet of polymer has enough time for the evaporation of solvent and thus reaching collector at a low diameter. This is a well established phenomenon in solution electrospinning [57].

Fig. 6.

Effect of process parameters (tip-to-collector distance and voltage) on fiber diameter for solution electro spun fibers.

(0.13MB).

The effects of increasing voltage to the decreasing fiber diameter has been also well researched. Charge repulsion within the polymer jet has been indicated as the main principle [58]. In our study, increasing the voltage from 12 to 20 kV resulted in the fiber diameter decrease from 0.59 to 0.42 μm, respectively.

3.3Thermal stability

The PEBA material has a one-step thermal degradation pattern (Fig. 7). The degradation starts at 300 °C and ends at 480 °C. Similar thermogram pattern was reported previously [59]. PEBA is known by its relatively high thermal stability which is attributed to a random chain scission mechanism in the structure [60,61]. At the same time, electrospun fibrous material has not changed the core properties of raw polymer. The melt electrospun sample provided a sharper (although not significantly) degradation curve (Tables 1 and 2).

Fig. 7.

Thermogram of raw PEBA material, melt and solution electrospun fibers.

(0.13MB).
3.4Chemical composition

Fig. 8 displays FTIR spectra, which indicate characteristic peaks for PEBA polymer. The peak at 3300 cm−1 occurs due to due NH stretching, peaks at 2923 and 2850 cm−1 correspond to the asymmetric and symmetric stretching of the CH bond in amide segment. The peak at 1736 cm−1 corresponds to the ester carbonyl group that bond the polyamide and polyether segments together, whereas peak at 1637 cm−1 indicates the amide carbonyl group. Intensive peaks at 1372 and 1108 cm−1 represents the CH bending and stretching vibration in ether group. Similar spectra have been reported by [62,63]. Processing of raw material by melt and solution electrospinning does not indicate any changes in chemical structure, confirming that these techniques are suitable for production of PEBA fibers without losing chemical properties (Figs. 9 and 10).

Fig. 8.

FTIR spectra of raw PEBA, melt & solution electrospun fibers.

(0.23MB).
Fig. 9.

Contact angle of melt and solution electrospun fibers.

(0.12MB).
Fig. 10.

X-Ray diffraction patterns for raw PEBA, melt electrospun fibres, and solution electrospun fibres on aluminum substrate.

(0.19MB).
3.5Wetting properties

The produced fibers were highly hydrophobic, with the measured contact angle in the range between 105 and 130 degrees (Fig 9). The contact angle increased with the decreasing diameter of fibers. The relationship was log linear, with the regression model of CAmelt = 119.2–18.9*log(df), R2 = 0.86 and CAsolution = 120.4–10.3*log(df), R2 = 0.81. This opposite relationship is expected, owing to the fact that when diameter of fiber is reduced, the orientation of molecular chains and degree of crystallinity is increased [64]. The structure of higher crystallinity results in the decreased water absorbency, thus increasing the contact angle. Similar results were reported previously by [65] and [66] who observed this with solution spun polycaprolactone, although the decrease in contact angle with the increase of fiber diameter has not been so sharp as compared to our study. Electrospun membranes of polyvinylidene fluoride-co-hexafluoropropylene (PcH) reached CA of 119 ° [67]. Electrospinning also results in porous and relatively rough surfaces, thus increasing the contact angle, owing to the trapped air channels in the porous membrane with heterogeneous surface [68].

Combining natural hydrophobic properties of PEBA and the structural composition of electrospun membranes, a further exploration of these applications should be sought for separation processes (oil/water, organic mixtures, gas/liquid).

3.6Crystallinity

Raw polymer and melt electro spun fibers show diffraction peak at 2θ = 20° (Fig. 10), which is similar to previous studies with PEBA as substrate for electrospinning [48] or membranes [59]. After solution electrospinning the peak is shifted at 2θ = 17° due to higher orientation of molecular chains in small fiber diameter [69]. These peaks are overshadowed by the signal from aluminum foil which was used as a substrate for the collection of fibers.

4Conclusions

Electrospun fibers of Poly(ether‐block‐amide) (PEBA) were successfully fabricated by using melt and solution electrospinning techniques. In both type of spinning techniques, the effect of process parameters on fiber diameter was studied and it was found that fiber diameter decreased by increasing voltage, distance, collector speed and melting temperature up to a certain limit, while further increase results in increasing fiber diameter in melt electrospinning. In solution electrospinning, the diameter of fiber is decreased by increasing voltage and distance. The fibers obtained by melt electrospinning were approx. an order of magnitude larger, compared to solution electrospinning (minimum average fiber diameters 1.92 ± 3.31 and 0.37 ± 0.34 μm, respectively). While melt electrospinning produces larger fibres, it has an advantage of not using solvents in the process thus more suitable for higher throughput production, especially when supermicrometer fibers are sufficient.

The selection of solvent for electrospinning of PEBA is important due to its chemically resistant nature. Butanol was determined as efficient solvent, resulting in smooth and uniform fibers, but causing issues in electrospinning due to increasing viscosity and blocking the needle. The use of acetic acid as a solvent can overcome this problem of needle blockage, but decreased viscosity may result in the formation of beaded fibers.

The processing of PEBA by electrospinning does not alter its thermal and chemical properties, while produced membranes have high hydrophobicity, which increases with decreasing fiber diameter. Applications of such membranes for hydrophobic packaging, separation membranes, osmotic evaporation may be sought after.

Data availability

The raw/processed data required to reproduce these findings cannot be shared at this time as the data also forms part of an ongoing study.

Conflict of interests

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgements

Authors are grateful for Arkema Group for providing samples of PEBAX for research. We would like to thank Dr. Martynas Tichonovas for the assistance in electrospinning setup preparations.

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