Skip to main content
. 2023 Jun 7;9(6):e17051. doi: 10.1016/j.heliyon.2023.e17051

Table 1.

Effect of material parameters (concentration, viscosity, Type of Solvent, surface tension, and Conductivity) on the average fiber diameter.

Material parameters
Parameter Material Methods and Preparations Results Findings Citation
Cellulose
  • Dissolving Cellulose (0.628 g) in [C2min] [OAc], IL (5 g).

  • Adding different amounts of DMF or DMAc (5, 3.75, 2.5 g) with concentrations of (6.3, 7.2, 8.3%) (w%) Respectively.

  • Rotating wired cylinder collector.

  • Applied voltage 30 kV.

  • TCD 150 mm.

  • Immersing the spun fiber in Ethanol at 4 °C, 2 h.

  • Drying fiber at 50 °C, 1 day.

  • Average fiber diameter for different concentration of the co-solvent is about: (500, 410 and 380 nm) for DMF & (1080, 760 and 620 nm) for DMAc, respectively.

  • Degree of crystallinity for different concentration is (0.67, 0.71 and 0.71) for DMF and (0.61, 0.68 and 0.7) for DMAc, respectively.

  • The addition of the co-solvent improves the spinnability and led to more uniform and finer fibers.

  • Increasing concentration causes increasing in Degree of crystallinity.

[26]
Concentration, Viscosity and Type of Solvent (E-CE)C
  • (E-CE)C with Mn of 9.7 × 104 g/mol was prepared by a reaction of EC and Acrylonitrile with a DS of 2.1 for Ethyl and 0.37 for Cyanoethyl.

  • THF was used as the solvent.

  • (E-CE)C/THF solution concentrations of (16, 17, 18 and 19) wt% were applied.

  • Applied voltage 30 kV.

  • The diameter of orifice was 1.2 mm.

  • TCD was 150 mm.

  • Fiber will be formed only between the concentration of [15–22%], outside this range no formation for the fiber.

  • the average fiber diameter was (2200, 2000, 2900 and 3200) nm, with (16, 17, 18 and 19) wt% (E-CE)C/THF solution concentrations respectively.

  • Average fiber diameter increased, and the diameter dispersion was broadened with increases in the solution concentration

[27]
(CMC) & (PEO)
  • (PEO) with a Mw of 400000 g/mol is used in a mixture with (CMC).

  • Different types of CMC were used with different MW and DS as follow: CMC Cekol 30 (A), CMC Cekol 700 (B).

  • CMC Cekol 2000S (C), CMC Cekol 500T (D) with Mw of 120, 280, 350, 250 (g/mol) and with DS 0.72, 0.77, 1.24, 0.72 respectively

  • PEO and CMC are mixed at a ratio of 1:1 then they are dissolved in water.

  • TCD was set to 200 mm.

  • Constant voltage at 35 kV.

  • At a concentration of 8% for all CMC derivatives, the fibers are straight with an even diameter, the mean diameter of the individual fibers lies between 200 and 250 nm.

  • CMC (D) couldn’t be electro-spun at 8% conc. due to its high viscosity, so a lower conc. than 6% was used.

  • CMC (A) & (B) lead to the formation of homogenous fibers.

  • CMC (C) required a slightly higher voltage (40 kV) due to its high viscosity.

  • Nonwoven sheets and individual nanofibers were formed.

  • The electrospinning process is directly dependent on the viscosity of the liquid to be operated; high viscosities were found to be in- spinnable unless a change was made on it either concentration wise or voltage wise.

[28]
Chitosan & PVA
  • Chitosan 10 of Mv = 2.1 × 105; degree of deacetylation, 0.78 and PVA (Degree of polymerization, approximately 2000; Mn = 8.8 × 104) are used.

  • The solvent is a mixture of FA and DW.

  • A solution of PVA-DW (9 wt %) was mixed with a chitiosan10-FA solution (7 wt%) with volume ratios 90:10, 70:30, 50:50, and 30:70, respectively.

  • Experiment was performed at room temperature.

  • A 3 mL syringe with a capillary tip having an inner diameter of 0.6 mm.

  • Applied voltage was 15 kV.

  • TCD was 150 mm.

  • At a ratio of 100:0 chitosan to PVA, no jet had been obtained.

  • At a ratio of 90:10 beads started to appear on the collector.

  • At a ratio of 70:30 the size of the beads becomes smaller and thin fibers started to appear among these beads.

  • For a ratio of 50:50 homogeneous fibers with 120 nm average diameter started to appear.

  • For a ratio of 30:70, the fiber was thicker (with an average diameter of 170 nm).

  • At 0:100 chitosan to PVA, Average fiber diameter was 470 nm.

  • Homogeneity of the produced fibers increases with the decrease of the chitosan percentage in the solution.

[29]
Chitosan
  • Chitosan with ≥75% degree of d-acetylation, was used.

  • The solvent used was TFA/DCM with different volume ratios.

  • The solution was kept under massive and constant magnetic stirring until all the chitosan was dissolved.

  • The chitosan concentration was 7% (w/v).

  • Diameter of the orifice was 0.5 mm.

  • Applied voltage was 25 kV.

  • TCD was 150 mm.

  • feed rate of 2 mL/h.

  • For 60:40, 70:30, 80:20 vol ratio of TFA:DCM the average fiber diameter was 360, 410, 490 nm.

  • The increase in the TFA percentage increases the viscosity and conductivity of the solution.

  • Lower TFA percentage destroy the homogeneity of the mats.

[30]
Chitosan & PVA
  • 4% (w/v) Chitosan flakes were dissolved in 2% (w/v) acetic acid.

  • PVA powder was dissolved in deionized water at 90 °C for 2 h.

  • The two solutions were mixed.

  • Voltage was 15 kV.

  • TCD was 150 mm.

  • Feed rate was 0.03 mL/h.

  • Temperature was 20 °C

  • Humidity was 51%.

  • For different PVA: Chitosan ratios (100:0, 95:5, 90:10, 80:20, 75:25, 70:30, 50:50) (w:w) the average fiber diameter was 1059, 823.6, 799.4, 637.6, 393.6, 286.2, 119.8 nm.

  • When the Chitosan content was more than 50%, the electrospinning process couldn’t occur.

  • The increase of the chitosan content leads to the increase of the charge density, which hardens the process of fiber formation.

  • The smallest fibers can be obtained with the increasing of chitosan content.

[31]
Chitosan
  • Three samples of Chitosan were used with the following Mw (30,000, 106,000, 398,000 g/mol) with degree of deacetylation of (56%, 54%, 65%) respectively

  • The solution was inserted into a syringe with an orifice diameter of 0.58 mm.

  • The flow rate was adjusted to be 1.2 mL/h.

  • voltage up to 40 kV.

  • At acetic acid concentration of 30% (wt%) Average diameter was found to be 40 nm with large beads. But, at concentration of 90% (wt%) the fiber diameter increased to 130 nm without beads.

  • As the concentration of acetic acid increased from 10 to 90% (wt%), Surface Tension decreased from 54.6 to 31.5 dyn/cm

  • The known difficulty in electrospinning of Chitosan can be solved by dissolving Chitosan in concentrate acetic acid in water, resulting in low surface tension.

  • Acetic acid concentration was the most important parameter as it decreased surface tension and increased charge density without significant effect on viscosity.

[32]
CA
  • Cellulose acetate with 39.8% acetyl content and Mw of 30,000.

  • Acetic acid and water were mixed to make the solvent.

  • Cellulose Acetate of 17 wt% was dissolved in acetic acid solution of concentration higher than 70 wt%.

  • The applied voltage was 25 kV.

  • TCD was adjusted to 100 mm.

  • The flow rate was set to 3 mL/h.

  • The orifice diameter was 0.84 mm.

  • The viscosity of CA solutions increased by the increase of acetic acid up to 80 wt%, and then it decreased.

  • The conductivity decreased by the increase of the water content.

  • The average fiber diameter was as follow (200, 250, 300, 500, 1300 nm) for acetic acid concentration of (70, 75, 80, 90, 95 wt %)

  • The average diameters of the CA nanofibers increases by increasing concentrations of the mixed solvent.

  • The viscosity of CA solutions does not affect the average diameter of the nanofibers.

[33]
Cellulose
  • Raw cellulose fiber was used.

  • The cellulose fiber was dried at 105 °C for 24 h

  • Cellulose was dissolved in IL of BMIMAc ≥95% in concentration, (300 mg of cellulose was added to 29.7 g IL).

  • Stirred for 72 h at 90 °C and 250 rpm

  • The solution was loaded in 10 mL syringe of 0.337 mm needle inner diameter.

  • TCD was adjusted to be 25 mm.

  • The applied voltage varied from 6 to 12 kV

  • Flow rate was 1.36 and 2.38 mL/h

  • Temperature inside the syringe was (110 ± 10)

  • The process was done at constant relative humidity (65 ± 3%) and temperature of (21 ± 1 °C).

  • Stable fiber formed at 2 and 3 wt% concentration

  • In case of 1 wt% concentration the Taylor cone was interrupted with the existence of solution droplets.

  • In case of 4 wt% concentration the viscosity of the solution was too high which prevent the formation of fibers.

  • The viscosity of the tested solution affects its spinnability and fiber formation, intermediate viscosity solution allows stable fiber formation.

[34]
CA & CB
  • 12% (w/v) Cellulose acetate of 29–46% acetyl content was dissolved in DMAA with ratio of 4:1 (v/v).

  • The CA/DMAA solution was mixed with PEG for 1:1 (w/w)

  • CB of (0.7, 1.5 and 2.2 wt%) was mixed with the CA solution

  • 20 mL syringe was used

  • The applied voltage was 26 kV and −10 Kv.

  • The process was done at 24 °C and relative humidity lower than 20%.

  • TCD was 10 cm

  • Flow rate was 10 mL/h

  • The aluminum collector was on cylindrical shape.

  • Cylindrical bead free smooth fibers were formed with the following characteristics:

  • -

    The average fiber diameter was 495, 628, 727, and 831 nm for 0.7, 1.5 and 2.2 wt% of CB respectively.

  • -

    A few CB small particles were adhered to the resulted fibers.

  • -

    Pores formed on the surface of the resulted fibers.

  • The increase in CB concentration increases the average fiber diameter.

  • The pores formed on the surface of the fibers is due to the removal of PEG.

[35]
Chitosan
  • Two solutions were used in the experiment chitosan – TFA and chitosan – TFA/DCM

  • The first solution was made by mixing 1.12 g of chitosan with 14.9 g of TFA and the final solution concentration was 7 wt%.

  • The second solution was made by mixing 1.09 g of chitosan with 10.43 g of TFA dissolved in 3.99 g of DCM at a ratio of 70:30 (TFA: DCM) (v/v), the final solution concentration was 7 wt%

  • The two solutions were prepared at room temperature

  • The two solutions were left for a night to make a homogeneous solution

  • 20 mL syringe was used

  • Flow rate was 0.08 mL/h and 0.1 mL/h for the two solutions respectively

  • 25 kV was applied

  • TCD was 12 cm and 14 cm for the two solutions respectively

  • Aluminum collector was used

  • Electrospinning of the first solution yields fiber with an average diameter of 95.58 ± 39.28 nm and beads formation was observed in it.

  • Electrospinning of the second solution yields bead-free fiber with an average diameter of 907.94 ± 290.18 nm

  • The solvent used in the electrospinning process affect the average fiber diameter and the bead formation.

[36]
(PLA/CMC/GO-f-COOH)
  • 10 mL of the polymer matrix solution PLA, CMC/GO-COOH, PCGC a syringe with an orifice stainless-steel needle with a diameter of 0.6 mm

  • Voltage was 20 kV,

  • Flow rate of 0.25 mL/h.

  • The distance between the needle and the collector was 20 cm,

  • All the nanofibrous membranes exhibited uniform fiber diameter distribution sizes of 350–550 nm.

  • The PLA nanofiber had a larger diameter than the PCGC and PCGC@Ag nanofibrous materials

  • The increase of thermal treatment result in an increasing in the surface area of the planar surface

  • High difference in the morphologies of nanofibrous membranes could clearly be seen,

  • The fiber diameters were different for all the nanofibrous materials.

  • The nanofibrous membrane had a good distributed pore size, and the PLA sample was densely fibrous more than the other samples.

[37]
Chitosan & PEO
  • Chitosan (5% w/v) and PEO (2.5% w/v) solutions in 70% v/v acetic acid were mixed to obtain different Chitosan:PEO respective weight ratios of 9:1, 8:2, 7:3, 6:4, and 5:5.

  • A pure Chitosan solution (5% w/v) was tried to obtain electrospinning nanofibers.

  • 5 mL syringe with a needle (gauge 20).

  • The flow rate was 0.3 mL/h

  • The distance between the collector and the needle tip was 15 cm.

  • Voltage range of 25–28 kV

  • Nanofibers based on 8:2 Chitosan:PEO exhibited the smallest diameter (119.17 ± 22.05 nm) and the greatest mucoadhesion (22.82 ± 3.21 g/cm2)

  • A spinnable solution containing Chitosan and PEO at a respective weight ratio of 9:1 produced nanofibers with an average diameter of 135.54 ± 67.48 nm

  • The high viscosity of the pure Chitosan solution is owing to the strong hydrogen bonding between its OH and NH2 groups.

  • PEO molecules linked to chitosan backbone could disrupt chitosan chain self-association and reduce chitosan solution viscosity

  • Small and flexible PEO chains can also lie down along the rigid chitosan macromolecules smoothing their flow.

[38]
Chitosan & PEO
  • Low molecular weight chitosan with a viscosity average molecular mass Mv = 540 kDa and a degree of deacetylation DD = 78%

  • Chitosan powder was dissolved using a 5% v/v acetic acid water solution to obtain a polymer concentration of 2.5%, 3.0% and 3.5% wt

  • PEO powder was added in a Chitosan/PEO mass ratio of 50/50 to obtain a final polymer concentration of 5%, 6% and 7 % wt.

  • A solution flow rate of 0.15 mL/h

  • A voltage of 17.5 kV

  • A needle-flat collector distance of 20 cm.

  • The sample obtained by Chitosan:PEO of 50:50, 5 % wt solution with a diameter ranging from 500 nm up to 2 μm and connecting the nanofibers, by an average dimension of 150 ± 30 nm.

  • The other two samples are both characterized by a similar structure with homogenous and smooth nanofibers of around 300 ± 30 nm

  • However, the mat obtained by Chitosan:PEO of 50:50 6 % wt formulation presents a high number of defects (e.g. beads, collapsed structures, low fibre density regions), whereas the one obtained by Chitosan:PEO of 50:50, 7 % wt. formulation shows the best structure in terms of fiber homogeneity.

  • The spinnability increased with solution viscosity, as well as the improvement of homogeneity and overall morphology of nanofibers.

  • Decrease of the viscosity as the shear rate increases due to the progressive orientation and disentangle of the chains

  • The increase of viscosity of the spinning solution often leads to the increase of polymer concentration, so that the fiber diameter increases and the bead like structure disappear.

[39]
Surface Tension (E-CE)C
  • (E-CE)C with Mn weight of 9.7 × 104 g/mol, was prepared by a reaction of EC and Acrylonitrile with a DS of 2.1 for Ethyl and 0.37 for Cyanoethyl.

  • THF was used as the solvent.

  • The applied voltage is 30 kV.

  • The diameter of orifice was 1.2 mm.

  • TCD was adjusted to be 150 mm.

  • When the concentration of the (E-CE)C/THF solutions was lower than 15 wt%, the fibers could not be formed by electrospinning because of the low surface tension and viscosity.

  • At solution concentrations greater than 22 wt%, the solution jet could not erupt because of the high surface tension and viscosity.

  • Surface tension is observed to be increased by increasing the respective concentration.

  • By increasing surface tension, average diameter of the fibers increases and the diameter distribution becomes wider with increasing the concentration.

[27]
H-Chitosan
  • H-chitosan was prepared by a heterogeneous acylation reaction between Chitosan and hexanoyl Chloride.

  • H-chitosan in chloroform to produce a solution of concentration between (4–14%) (w/v)

  • Voltage ranged from 12 kV.

  • Needle was tilted at 45°.

  • TCD was 120 mm.

  • When the conc. of H-chitosan was 4% (w/v), the conductivity was 0.25 mS/cm only beads formed at this concentration.

  • At 6% conc. The conductivity was 0.27 mS/cm, and the average fiber diameter was 640 ± 360 nm.

  • At 8%, the conductivity was 0.28 mS/cm, and the average fiber diameter was 1230 ± 670 nm.

  • At 10%, conductivity was 0.35 mS/cm, and the average fiber dimeter was 1490 ± 690 nm.

  • At 14%, the conductivity was 0.4 mS/cm, and the average fiber diameter was 3930 ± 1820 nm.

  • Conductivity of the solution increases with the increase of the H-chitosan concentration, which happens as a reason of increasing the hydroxyl group in the solution.

  • The average diameter increased with the increasing of the conductivity of the solution

[40]
Conductivity
Chitosan & PEO
  • Chitosan and PEO solutions with 2–8% concentration was dissolved in acetic acid aqueous of 2 wt%.

  • Mass ratios of Chitosan:PEO were 1:1, 2:1 and 5:1.

  • Chitosan solutions with concentrations 1 wt% to 6 wt% and PEO solutions with 1 wt% to 3 wt% in aqueous 2 wt% acetic acid

  • stirred overnight at room temperature.

  • a 50 mL syringe with a metal capillary.

  • The applied voltage was set to be 15 kV.

  • The flowrate was adjusted to 0.1 mL/h.

  • TCD was adjusted to be 200 mm.

  • Conductivity of Chitosan was found to be 2.6–9.6 mS/cm, and conductivity of PEO was found to be 0.85–1.22 S/cm.

  • ● With the increase of Chitosan concentration, Conductivity of Chitosan solutions significantly increased. The viscosity also increased at concentrations of 1–6 wt%.

  • With the increase of PEO concentration, the conductivity of Chitosan/PEO solutions decreased.

  • With the increase of PEO concentrations, Surface Tension of PEO solutions reduced. Fibers were produced with an average diameter of 124 nm at 6 wt% solutions (1:1) (w/w).

  • Ultrafine fibers could only be electrospinning from chitosan solution in aqueous acetic acid when PEO was added.

  • Conductivity increases with the increase of Chitosan concentration.

[41]