Startseite Temperature effects on electrospun chitosan nanofibers
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Temperature effects on electrospun chitosan nanofibers

  • Dan-Thuy Van-Pham , Tran Thi Bich Quyen , Pham Van Toan , Chanh-Nghiem Nguyen , Ming Hua Ho und Doan Van Hong Thien EMAIL logo
Veröffentlicht/Copyright: 22. September 2020
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Green Processing and Synthesis
Aus der Zeitschrift Green Processing and Synthesis Band 9 Heft 1

Abstract

Effects of the temperature of chitosan (CS) solutions as well as the temperature of the chamber on an electrospinning process were investigated. CS with a low molecular weight was dissolved in the solvent of trifluoroacetic acid/dichloromethane (70/30 v/v) at a concentration of 80 mg/mL for electrospinning. Both CS solution and chamber temperatures strongly affected the morphology of electrospun CS nanofibers. At the solution temperature and chamber temperature of 32°C, uniform CS nanofibers with an average diameter of 200 nm could be obtained. Although the chamber temperature is generally regarded as an unimportant parameter in the electrospinning of polymers, the experimental results demonstrated its critical effect on the electrospinning of CS.

Keywords: chitosan; electrospinning; nanofibers; temperature effects

1 Introduction

Chitosan (CS) is a biodegradable, biocompatible, and nontoxic polymer that is abundant in nature [1,2,3,4,5]. Besides the above advantages of CS, nanofibrous CS substrates can provide a high surface area for adsorption and cell attachment [1,6]. Thus, CS nanofibers should have a high potential use for tissue-engineering scaffolds as well as adsorption processes [1,2,7]. However, electrospinning of CS is limited due to its high viscosity, the limitation of solvents, and the positive charges of amino groups [8]. Although there are a few reports about the electrospinning of pure CS, important operational parameters for the electrospinning of CS have not been investigated thoroughly. Ohkawa et al. (2004) reported the first successful preparation of pure CS fibers by the electrospinning technique. By using trifluoroacetic acid (TFA) as the solvent, homogeneous CS nanofibers were successfully prepared [9]. High volatility of TFA plays a crucial role in the formation of uniform nanofibers. Moreover, TFA can block the positive charges of the amino groups on CS, which can decrease the electrostatic forces and enable the production of continuous fibers [9,10]. Therefore, the effectiveness of the TFA fostered further studies on electrospinning CS with various molecular weights where TFA was utilized as the solvent [11,12].

Electrospinning can create very fine fibers from a liquid by using an electrostatic force. When the electrical field is applied, charges on the surface of a polymer solution repulse each other. Meanwhile, surface tension causes forces opposite to the electrical force. With counteraction between mutual repulsive force between charges and the force from surface tension, the liquid is bended to form an electrospun jet. The eruption of the liquid has a conical shape, called as the Taylor cone [13,14,15,16]. Then, the jet is continuously elongated, and the solvent is also evaporated to form fibers if the entanglement force in the liquid is high enough to prevent the breaking of the stream. Finally, fibers are deposited on the collector. Electrospinning is a simple process to produce micro- and nanofibers. However, the effects of parameters are very complicated [13,17]. The electrospinning parameters are usually divided into three groups: the properties of a polymer solution (e.g., polymer concentration, polymer molecular weight, the type of solvent); operational parameters (e.g., the applied voltage, the distance between the needle tip and collector, feeding rate); and ambient conditions (e.g., temperature, humidity, velocity of air chamber) [13,17,18].

While various studies focused on polymer solution and operational parameters, ambient parameters are generally considered to contribute an insignificant effect to the electrospinning process. However, it should be noted that an increase in the temperature of a polymer solution might lead to a decrease in the viscosity of that solution and an increase in the evaporation of the solvent [19]. Thus, an increase in temperature of a polymer solution could lead to a decrease in diameters of electrospun fibers. Therefore, there are several studies on the effects of the polymer solution temperature on electrospinning. The results show that increasing the temperature is often beneficial to the process of electrospinning [19,20,21,22]. In addition, melting electrospinning is also an attractive issue because there is no need to use solvents for electrospinning [23,24,25].

Although uniform CS nanofibers could be prepared by using the TFA/dichloromethane (DCM) as the solvent, the temperature effect of the CS solution has not been investigated. Also, it is questionable whether the temperature of the electrospinning chamber might have a significant effect on the evaporation of the solvent. To address this knowledge gap, this research work investigated the effects of both solution temperature and chamber temperature on electrospun CS nanofibers. Rigorous experimentation on the impact of various types of solvents on the nanofiber morphology was also conducted to reconfirm the effectiveness of TFA/DCM for the successful electrospinning of pure CS nanofibers.

2 Materials and methods

2.1 Materials

Ascorbic acid, glycolic acid, malic acid, succinic acid, TFA, ethanol, hexane, tetrahydrofuran (THF), and CS with a low molecular weight were purchased from Sigma-Aldrich. DCM was obtained from TEDIA.

2.2 Methods

2.2.1 Electrospinning of CS

In this study, we developed a customized electrospinning setup, as shown in Figure 1. There are three main components in the electrospinning equipment: a syringe pump (KD Scientific, KDS 100) with a metallic needle (0.65 × 32 mm), where the temperature of the solution is controlled; a high voltage generator; and a collector covered by an aluminum foil.

Figure 1 Electrospinning setup.
Figure 1

Electrospinning setup.

The solution temperature was controlled by surrounding the needle and the syringe with a tube that allowed a continuous flow of water from a temperature-controlled water bath (as illustrated in Figure 1, Section I). An electric heater attached on both sides of the chamber was used to warm up the chamber to the desired chamber temperature measured by a thermocouple that was placed close to the workspace of the collector (as illustrated in Figure 1).

In this study, CS solutions were prepared for electrospinning using various solvents with different levels of volatility. First, low-volatility acids (i.e., ascorbic acid, glycolic acid, malic acid, succinic acid) were utilized to produce CS solutions of 2–5% concentration for electrospinning. Second, acetic acid, a moderate-volatility acid, was also used to produce CS solutions of 5–7% concentration for electrospinning. Co-solvents (i.e., ethanol, hexane, THF) were also added into the solution to analyze their effect on electrospinning products. Finally, CS was dissolved by strong and high-volatility TFA with DCM as the co-solvent, as described by the previous report for preparing pure CS nanofibers [9]. CS was dissolved in TFA/DCM (70/30 v/v) at a concentration of 80 mg/mL. After stirring for 12 h, the CS solution was placed in a 3 mL syringe for electrospinning. The distance and the applied voltage between the tip and the collector were 120 mm and 17 kV, respectively. The flow rate of CS solution was fixed at 0.2 mL/h. The electrospinning experiments were carried out at a humidity of 70–75% for 45 min. To study the temperature effects of the solution, the solution temperatures of 20°C, 22°C, 27°C, and 32°C were observed under experimentation after the chamber temperature had been fixed at 32°C. To investigate the chamber temperature, the experiments were conducted at the chamber temperatures of 24°C, 29°C, 32°C, and 37°C after the solution temperature had been controlled at 32°C.

2.2.2 Characterizations of electrospun CS nanofibers

Surface morphology of the CS nanofibers was observed by a scanning electron microscope (SEM, JSM-6390LV, JEOL, Japan) at an accelerating voltage of 20 kV after gold coating.

From the SEM image results, the diameters of CS fibers and the distribution of fiber diameters were analyzed by ImageJ software. A hundred fibers were randomly selected from different areas of a SEM image to determine the mean diameter and its standard deviation of the obtained nanofibers.

3 Results and discussion

3.1 Effects of the solvent

Besides TFA, various solvents for CS including low-volatility acids such as ascorbic acid, glycolic acid, malic acid, and succinic acid; and a moderate-volatility acid (i.e., acetic acid and its mixtures with various co-solvents) were experimented in this study. Figure 2 shows the SEM images of electrospinning CS using solvents of the former type. No uniform structure could be observed. It was known that TFA could change the viscosity of a CS solution and the interaction between the amino groups of CS [9], resulting in the electrospinnability of pure CS. For ascorbic acid, succinic acid, and malic acid, they increased the viscosity of a CS solution, revealing the enhancement in the entanglement force between the polymer chains of CS [26]. Thus, no homogeneous and continuous fibers could be formed by using these solvents.

Figure 2 SEM images of electrospun CS with 30 mg/mL of CS concentration in various solvents: (a) ascorbic acid, (b) glycolic acid, (c) malic acid, and (d) succinic acid.
Figure 2

SEM images of electrospun CS with 30 mg/mL of CS concentration in various solvents: (a) ascorbic acid, (b) glycolic acid, (c) malic acid, and (d) succinic acid.

Figure 3 shows the SEM images of electrospun CS with acetic acid and the mixture of acetic acid with co-solvents including hexane, ethanol, and THF. These co-solvents were chosen due to their low surface tension, low dielectric constant, and high volatility (Table 1). It was found that the bead-in-string morphology existed, and the homogeneity of CS nanofibers was not improved using different co-solvents. These factors agreed well with the previous reports in ref. [9,27], which supported the use of TFA as a high-volatility solvent to suppress the positive charges of CS for the successful electrospinning of pure CS.

Figure 3 SEM images of electrospun CS with 70 mg/mL of CS concentration in various co-solvents: (a) acetic acid, (b) acetic acid and hexane, (c) acetic acid and ethanol, and (d) acetic acid and THF.
Figure 3

SEM images of electrospun CS with 70 mg/mL of CS concentration in various co-solvents: (a) acetic acid, (b) acetic acid and hexane, (c) acetic acid and ethanol, and (d) acetic acid and THF.

Table 1

Physical properties of the main solvents for the electrospinning of CSa

SolventSurface tension (mN m−1, at 20°C)Relative density (g/cm3, at 25°C)Viscosity (cP, at 25°C)Vapor pressure (hPa, at 25°C)Boiling point (°C, at 760 mm Hg)Dielectric constant at 20°C
TFA72.501.479 0.81315871.808.55ε0
DCM26.501.3170.41358439.758.93ε0
Acetic acid27.601.0491.15520.791186.15ε0
THF27.300.8800.480255657.60ε0
Ethanol22.100.7871.09588.4478.2925.30ε0
Hexane18.430.659 0.297100691.89ε0
  1. a

    The values of physical properties refer to the Safety Data Sheet of Sigma-Aldrich for the solvents.

3.2 Effects of the solution temperature

Figure 4 shows the SEM images of the electrospun fibers when the solution temperatures were varied from 20°C, 22°C, 27°C, and 32°C. Remarkably, morphology change from bead-connected fibers to uniform fibers was observed, following the increase in solution temperature. This finding could be very useful for the formation of uniform electrospun fibers and was consistent with previous research works on the electrospinning of CS/poly(acrylamide) [20], CS/polyethylene oxide [19], and nylon 6 [21].

Figure 4 SEM images of electrospun CS with 80 mg/mL of CS concentration in the solvents TFA/DCM (70/30 v/v) at different temperatures of the solution: (a) 20°C, (b) 22°C, (c) 27°C, and (d) 32°C.
Figure 4

SEM images of electrospun CS with 80 mg/mL of CS concentration in the solvents TFA/DCM (70/30 v/v) at different temperatures of the solution: (a) 20°C, (b) 22°C, (c) 27°C, and (d) 32°C.

Because the high viscosity of CS solution may limit the electrospinning process, a high concentration of CS with a low molecular weight was used as a trade-off between lowering viscosity (i.e., using low-molecular weight CS) and allowing the successful electrospinning of CS nanofibers (i.e., increasing concentration to provide enough CS material). Therefore, an increase in the solution temperature might lead to a decrease in the viscosity of CS solution. As a consequence, the entanglement force could be reduced and the electrospinning process could get accelerated to produce uniform CS nanofibers.

The solution temperature increase could also result in an increase in chain mobility and repulsive interaction among polymer chains. Thus, increasing solution temperature could partially promote the formation of fibers and limit the formation of beads. These tendencies could have facilitated the formation of uniform electrospun fibers.

3.3 Effect of the chamber temperature

Figure 5 shows the SEM images of the electrospun CS fibers at various chamber temperatures (24°C, 29°C, 32°C, and 37°C). Uniform CS nanofibers were obtained at the chamber temperature of 32°C. An increase in the chamber temperature could have resulted in a higher evaporation rate of the solvent; thus, the electrical forces could be reduced during the electrospinning process. However, at a higher chamber temperature (i.e., 37°C), the electrospinning jet was solidified, which resulted in the production of inhomogeneous fibers. Therefore, chamber temperature should be considered as a crucial electrospinning parameter for obtaining uniform CS nanofibers.

Figure 5 SEM images of electrospun CS with 80 mg/mL of CS concentration in the solvents TFA/DCM (70/30 v/v) at different temperatures of the chamber: (a) 24°C, (b) 29°C, (c) 32°C, and (d) 37°C.
Figure 5

SEM images of electrospun CS with 80 mg/mL of CS concentration in the solvents TFA/DCM (70/30 v/v) at different temperatures of the chamber: (a) 24°C, (b) 29°C, (c) 32°C, and (d) 37°C.

Figure 6 shows the distribution of the CS nanofiber diameters obtained under the optimal temperature conditions. The diameter of the obtained CS nanofibers had a mean value of about 200 nm with a standard deviation of 86 nm.

Figure 6 Diameter distribution of electrospun CS nanofibers using 80 mg/mL of CS concentration in the solvents TFA/DCM (70/30 v/v) at the optimal chamber and solution temperature of 32°C.
Figure 6

Diameter distribution of electrospun CS nanofibers using 80 mg/mL of CS concentration in the solvents TFA/DCM (70/30 v/v) at the optimal chamber and solution temperature of 32°C.

4 Conclusion

Uniform nanofibers with an average diameter of 200 nm were successfully obtained from pure CS by the electrospinning technique. The TFA/DCM (70/30 v/v) solvents were the best choice for the electrospinning process. The temperature of the CS solution and the chamber had significant effects on the morphology of CS nanofibers. The proper temperatures of the solution and the chamber were 32°C for preparing pure CS nanofibers, which would be a potential factor for various applications in biomaterials, adsorbents, and carriers.

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Acknowledgment

This work was financially supported by the Can Tho University Improvement Project VN14-P6, supported by a Japanese ODA loan.

  1. Conflict of interest: The authors declare that there is no conflict of interest.

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Received: 2020-06-28
Revised: 2020-07-30
Accepted: 2020-08-02
Published Online: 2020-09-22

© 2020 Dan-Thuy Van-Pham et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/gps-2020-0050
Schlagwörter für diesen Artikel
chitosan; electrospinning; nanofibers; temperature effects
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Artikel in diesem Heft

  1. Obituary for Prof. Dr. Jun-ichi Yoshida
  2. Regular Articles
  3. Optimization of microwave-assisted manganese leaching from electrolyte manganese residue
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  9. Efficient synthesis of palladium nanoparticles using guar gum as stabilizer and their applications as catalyst in reduction reactions and degradation of azo dyes
  10. Isolation of biosurfactant producing bacteria from Potwar oil fields: Effect of non-fossil fuel based carbon sources
  11. Green synthesis, characterization and photocatalytic applications of silver nanoparticles using Diospyros lotus
  12. Dielectric properties and microwave heating behavior of neutral leaching residues from zinc metallurgy in the microwave field
  13. Green synthesis and stabilization of silver nanoparticles using Lysimachia foenum-graecum Hance extract and their antibacterial activity
  14. Microwave-induced heating behavior of Y-TZP ceramics under multiphysics system
  15. Synthesis and catalytic properties of nickel salts of Keggin-type heteropolyacids embedded metal-organic framework hybrid nanocatalyst
  16. Preparation and properties of hydrogel based on sawdust cellulose for environmentally friendly slow release fertilizers
  17. Structural characterization, antioxidant and cytotoxic effects of iron nanoparticles synthesized using Asphodelus aestivus Brot. aqueous extract
  18. Phase transformation involved in the reduction process of magnesium oxide in calcined dolomite by ferrosilicon with additive of aluminum
  19. Green synthesis of TiO2 nanoparticles from Syzygium cumini extract for photo-catalytic removal of lead (Pb) in explosive industrial wastewater
  20. The study on the influence of oxidation degree and temperature on the viscosity of biodiesel
  21. Prepare a catalyst consist of rare earth minerals to denitrate via NH3-SCR
  22. Bacterial nanobiotic potential
  23. Green synthesis and characterization of carboxymethyl guar gum: Application in textile printing technology
  24. Potential of adsorbents from agricultural wastes as alternative fillers in mixed matrix membrane for gas separation: A review
  25. Bactericidal and cytotoxic properties of green synthesized nanosilver using Rosmarinus officinalis leaves
  26. Synthesis of biomass-supported CuNi zero-valent nanoparticles through wetness co-impregnation method for the removal of carcinogenic dyes and nitroarene
  27. Synthesis of 2,2′-dibenzoylaminodiphenyl disulfide based on Aspen Plus simulation and the development of green synthesis processes
  28. Catalytic performance of the biosynthesized AgNps from Bistorta amplexicaule: antifungal, bactericidal, and reduction of carcinogenic 4-nitrophenol
  29. Optical and antimicrobial properties of silver nanoparticles synthesized via green route using honey
  30. Adsorption of l-α-glycerophosphocholine on ion-exchange resin: Equilibrium, kinetic, and thermodynamic studies
  31. Microwave-assisted green synthesis of silver nanoparticles using dried extracts of Chlorella vulgaris and antibacterial activity studies
  32. Preparation of graphene oxide/chitosan complex and its adsorption properties for heavy metal ions
  33. Green synthesis of metal and metal oxide nanoparticles from plant leaf extracts and their applications: A review
  34. Synthesis, characterization, and electrochemical properties of carbon nanotubes used as cathode materials for Al–air batteries from a renewable source of water hyacinth
  35. Optimization of medium–low-grade phosphorus rock carbothermal reduction process by response surface methodology
  36. The study of rod-shaped TiO2 composite material in the protection of stone cultural relics
  37. Eco-friendly synthesis of AuNPs for cutaneous wound-healing applications in nursing care after surgery
  38. Green approach in fabrication of photocatalytic, antimicrobial, and antioxidant zinc oxide nanoparticles – hydrothermal synthesis using clove hydroalcoholic extract and optimization of the process
  39. Green synthesis: Proposed mechanism and factors influencing the synthesis of platinum nanoparticles
  40. Green synthesis of 3-(1-naphthyl), 4-methyl-3-(1-naphthyl) coumarins and 3-phenylcoumarins using dual-frequency ultrasonication
  41. Optimization for removal efficiency of fluoride using La(iii)–Al(iii)-activated carbon modified by chemical route
  42. In vitro biological activity of Hydroclathrus clathratus and its use as an extracellular bioreductant for silver nanoparticle formation
  43. Evaluation of saponin-rich/poor leaf extract-mediated silver nanoparticles and their antifungal capacity
  44. Propylene carbonate synthesis from propylene oxide and CO2 over Ga-Silicate-1 catalyst
  45. Environmentally benevolent synthesis and characterization of silver nanoparticles using Olea ferruginea Royle for antibacterial and antioxidant activities
  46. Eco-synthesis and characterization of titanium nanoparticles: Testing its cytotoxicity and antibacterial effects
  47. A novel biofabrication of gold nanoparticles using Erythrina senegalensis leaf extract and their ameliorative effect on mycoplasmal pneumonia for treating lung infection in nursing care
  48. Phytosynthesis of selenium nanoparticles using the costus extract for bactericidal application against foodborne pathogens
  49. Temperature effects on electrospun chitosan nanofibers
  50. An electrochemical method to investigate the effects of compound composition on gold dissolution in thiosulfate solution
  51. Trillium govanianum Wall. Ex. Royle rhizomes extract-medicated silver nanoparticles and their antimicrobial activity
  52. In vitro bactericidal, antidiabetic, cytotoxic, anticoagulant, and hemolytic effect of green-synthesized silver nanoparticles using Allium sativum clove extract incubated at various temperatures
  53. The green synthesis of N-hydroxyethyl-substituted 1,2,3,4-tetrahydroquinolines with acidic ionic liquid as catalyst
  54. Effect of KMnO4 on catalytic combustion performance of semi-coke
  55. Removal of Congo red and malachite green from aqueous solution using heterogeneous Ag/ZnCo-ZIF catalyst in the presence of hydrogen peroxide
  56. Nucleotide-based green synthesis of lanthanide coordination polymers for tunable white-light emission
  57. Determination of life cycle GHG emission factor for paper products of Vietnam
  58. Parabolic trough solar collectors: A general overview of technology, industrial applications, energy market, modeling, and standards
  59. Structural characteristics of plant cell wall elucidated by solution-state 2D NMR spectroscopy with an optimized procedure
  60. Sustainable utilization of a converter slagging agent prepared by converter precipitator dust and oxide scale
  61. Efficacy of chitosan silver nanoparticles from shrimp-shell wastes against major mosquito vectors of public health importance
  62. Effectiveness of six different methods in green synthesis of selenium nanoparticles using propolis extract: Screening and characterization
  63. Characterizations and analysis of the antioxidant, antimicrobial, and dye reduction ability of green synthesized silver nanoparticles
  64. Foliar applications of bio-fabricated selenium nanoparticles to improve the growth of wheat plants under drought stress
  65. Green synthesis of silver nanoparticles from Valeriana jatamansi shoots extract and its antimicrobial activity
  66. Characterization and biological activities of synthesized zinc oxide nanoparticles using the extract of Acantholimon serotinum
  67. Effect of calcination temperature on rare earth tailing catalysts for catalytic methane combustion
  68. Enhanced diuretic action of furosemide by complexation with β-cyclodextrin in the presence of sodium lauryl sulfate
  69. Development of chitosan/agar-silver nanoparticles-coated paper for antibacterial application
  70. Preparation, characterization, and catalytic performance of Pd–Ni/AC bimetallic nano-catalysts
  71. Acid red G dye removal from aqueous solutions by porous ceramsite produced from solid wastes: Batch and fixed-bed studies
  72. Review Articles
  73. Recent advances in the catalytic applications of GO/rGO for green organic synthesis
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Heruntergeladen am 22.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/gps-2020-0050/html
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