Tekstil Teknolojileri Elektronik Dergisi

Cilt: 8, No: 3, 2014 (49-60)

Electronic Journal of Textile Technologies
Vol: 8, No: 3, 2014 (49-60)

TEKNOLOJK
ARATIRMALAR
www.teknolojikarastirmalar.com
e-ISSN:1309-3991

Derleme
(Review)

Nanofiber Production Methods

*

Yasar Emre KIYAK*, Enes Cakmak*,

North Carolina State University, College of Textiles, Raleigh, NC, 27606, USA
kiyakest@gmail.com

Abstract
Nanofiber technologies are appealing huge interest as a functional fabrication method for one dimensional structured
organic, inorganic and hybrid nanomaterials with controlled dimensions. Nanofibers are generated as haphazardly or
oriented continuous nanofibers with possibilities of ordered internal morphologies such as coresheath, hollow or porous
fiber, or even multi channeled microtube arrangements. These various type of materials can be obtained by different
fabrication techniques. Undoubtedly, most appropriate and controllable is method electrospinning.
Keywords : Nanofibers, Electropsinning, Fiber Production

Nanolif retim Yntemleri

zet
Lif aplarnn kontrol edilebilmesi, organik- inorganik ve hibrid nanometaryallerin retilebilmesi nanolif retim
teknolijilerine olan ilgiyi artrmtr. Nanolifler geliigzel veya oryante olmu, kabuk-z, ii bos, gzenekli ve ok
kanall mikro-tp olarak kullanlabilmektedir. Bu ok deiik zellikli malzemeler yine ok eitli lif retim teknikleri
sayesinde retilebilmektedir. Hi phesiz ki, bunlarn arasnda en uygunu elektrolit ekim metodudur.
Anahtar Kelimeler: Nanolif, Elektrolif ekim, retim Yntemleri

Bu makaleye atf yapmak iin

Kiyak E.Y., Cakmak E., Nanolif Uretim Yontemleri Tekstil Teknolojileri Elektronik Dergisi 2014, 8(3) 49-60
How to cite this article
Kiyak E.Y., Cakmak E., Nanofiber Production Methods Electronic Journal of Textile Technologies, 2014, 8 (3) 49-60

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Nanofiber Production Methods

1. INTRODUCTION
Up to now, much research about nanofiber based composites has been carried out. Because nanofibers
have unique mechanical, electrical and chemical properties, they are accepted as advanced materials.
Nanofibrous mats can be produced intentionally and in desired conditions, which means they can be
regarded as nanomaterial, as well. Since it is very hard to get a single nanofiber, they are produced as
membrane or non-woven form. Countless applications of nanofiber makes itself an attractive material.
Therefore, understanding different production methods and utilizing the methods according to specific
application is crucial for the success of the application. There have been many different ways for
producing nanofibers, such as drawing, phase separation, self-assembly, template synthesis,
electroblowing, centrifugal and electrospinning [1].In this paper, different techniques of nanofiber
production methods are briefly reviewed.
2. ELECTROSPNNNG & CONFGURATONS
From the beginning of this century, researchers have been reinventing an old process known as
electrospinning [2]. It is able to fabricate continual nanofibers from different types of material when
regarding manageability [2]. Moreover, electrospinning is a more inexpensive method than others. Today,
low-cost, high-strength, high-value added nanofibers can be produced in diameter ranging from 20 nm to
1 micron [3,4].
2.1. Basic Electrospinning
First, the technique produces dimension controlled fibers down to nanometer range. A melt or solution of
polymer is fed through a narrow needle or nozzle. The nozzle or needle perform as an electrode
simultaneously applying typically high voltage from 20 to 100 kV. Generally, the distance from electrode
to collector is 10-25 cm in typical laboratory set-up The current varies from nanoamper to microampere
during the electrospinning process. The design of typical electrospinning can be from top to bottom or
bottom to top [4].
If high voltage is applied to an electrode, an electric field is generated between collectorandelectrode.
After critical voltage value, electrostatic force overcomes the surface tension and the charged polymer
solution is forced to leave from the tip of thenozzle or needle. The pulled polymer solution jet passes
through an elongation and instability phase due to the effects of electrostatic force, which makes the jet
very thinandlong. Simultaneously, solvent evaporates and solidification takes place, and an
interconnected layer of fibers on the surface of the collectoris created. In the case of melt, ejected jet
solidifies while traveling in the air [5].
2.2. Melt Electrospinning
Most of the electrospun nanofibers are based on solution spinning. Risky chemicals are used to dissolve
plentiful polymers. These solvents may leave residue that is not compatible withhealth issues. There has
been adesire to produce fibers by concentrating on a cleaner process, through being environmentally safe
and productive. Thus, an electrospinning system that uses molten polymer has gathered great excitement.
Despite many promising applications, little development has been made in the past 20 years [6].
Figure 1 shows the design of typical meltelectrospinning. When high voltage is applied to a spinneret, a
cone is formed. At the critical voltage, electro static forces overcome the surface tension. Viscoelastic
behavior of the melt result in a fine fiber extruded from the orifice residing at small holes. Rheology of
the molten state is critical for the stable spinning [6].

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Figure 1. Melt electrospinning technique

In the melt electrospinning, there must be a constant heat supply to the reservoir containing the polymer
solution so that the polymer remains in a molten state. The distance from nozzle to collector is typically
smaller than basic electrospinning. Because the polymer is in a molten form, greater charge is required for
jet initiation [1].
2.3. Gas-Jacket Electrospinning

Figure 2. Gasassisted electrospinning .

In some circumstances, electro static force may not be sufficient alone to stretch the solution for
producing nanofibers. The reason can be because ofexcessive surface tension of the solutionor high
viscosity. If easily evaporated solvents are preferred, exposure to the environment and fast evaporation of
the solvent may make the solution hard to spin [7]. Therefore, a gas jacket that hits and brings into play a
stretching force on the solution can be used at the spinneret tip in order to initiate the spinning,as shown
in Figure 2 [8]. For example, hyaluronic acid that has a high viscosity can be electrospun in this system.
Fiber fabrication can be advanced by using a heated gas because the higher temperature decreases the
viscosity of the solution [9].The inert gas is brought up from the basin and passed through the buffer
reservoir, which stabilizes the gas flow in the shape of the laminar flow. The gas flow additionally
contributes to stretch the jet of the polymer solution, which was slowly injected into a capillary by
injector and flowed through a capillary with a definite length. In order to actualize the gas electrospinning
process, the polymer solution with a certain concentration is deduced by spinneret, which is connected to
the anode of a high-voltage supplier. The cathode is the metal collector or coagulating bath and connected
to the ground [10]. Moreover, the electroblowing technique can be regarded as the same production
method [11-14]
2.4. Bubble Electrospinning
An innovative technique mimicking the spider spinninghas been designed to minimize the surface tension
of solution. This novel system which is patented [15] includes a vertical solution reservoir with a gas tube
feeding from the bottom with a metal electrode fixed along the middle of the tube. A grounded collector
is mounted above the reservoir (Fig. 3).

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Nanofiber Production Methods

Figure 3. Bubble Electrospinning

The mechanism of this innovative electrospinning process is certainly simple. In the absence of an
electric field, the aeration system generates various bubbles on the surface. When an electric field is
created, it induces charges into the bubble surface. The coupling of surface charge and external electric
field create a tangential stress, resulting in the transformation of the little bubbles into protuberanceinduced upward-directed reentrant jets. Once the electric field surpasses the critical value needed to
overcome the surface tension, a fluid jet distracts from the zenith of the conical bubble. The threshold
voltage needed to overcome the surface tension depends upon the size of the bubble and the inlet air
pressure. The most attractive property of this bubble electrospinning technique is that it is independent of
the properties of the the solution such as viscosity. This novel technology has critical importance for the
new generation of electrospinning, [3].
2.5. Magneto Electrospinning
A magnetic field is utilized in the electrospinning process by generating ampere force. If a magnetic field
is applied,magneto electrospinning(Fig. 4) can be conducted completely [3].The resultant electrical force
and the viscous force of the jet flow increases the radius of the whipping circle.

Figure 4. Magnetic field electrospinning

A mathematical model of the magnetic electrospinning technique and the moving behavior of the jet are
investigated. The results show that the magnetic field creates a radial Lorenz Force resulting in jet
shrinking. The relationship of the swing of the jet and its distance with different excitation currents are
obtained. From the relationship, it is known that the swing with a magnetic field is smaller than that
without a magnetic field. The simulation results do not agree well with the experimental data and show
that the magnetic field can influence the jet at an appropriate distance [17]. It seems hard to adapt this
technique for mass production.
2.6. Conjugate Electrospinning
The system used in conjugate electrospinning is illustrated in Figure 5. It consists of two or three high
voltage power supplies with opposite polarity, two or three spinnerets and a receiver drum. Two or three
programmable pumps are used to control the delivery rate of solutions. Power supplies are connected with
spinnerets, respectively. Spinnerets are arranged in opposite positionson the same horizontal line. The
distance between spinnerets are designed as adjustable. The solution is separately delivered by syringes to
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two or three spinnerets. The receiver is a rotating drum controlled by a stepping motor. The fibers from
the two or three oppositely charged electrospinning spinnerets were collected and stretched by the drum
receiver with a constant speed. The nanofiber yarns,which can be produced by this technique, are dried
under vacuum at room temperature [18].

Figure 5. Conjugate electrospinning [18].

2.7. Co-axial Electrospinning

Figure 6. Co-axial electrospinning

In the co-axial electrospinning technique (Fig. 6), twoliquids distract from the core and surrounding
concentric nozzles in the form of polymer solution or melt. The liquids contact each other only at the tip
of the coaxial needle or capillary [16].Taylor cone formation is achieved through the nozzle. During the
spinning process, solvents evaporate and compound jet solidify. As a result of this solidification, coreshell nanofiber is produced. n this technique, preventing the mixing of polymer solutions is
critical.Here, shell polymer serves as a template for the core material leading to cable-type structures.
With this technique, polymer that cannot be electrospun by basic electrospinning is preferred to obtain
core-shell nanofiber.These types of fibers have potential applications in microelectronics, optics, and
medicine. Furthermore, polymer nanotubes can be generated [20].
2.8. Needless Electrospinning
The needless electrospinning technology was first patented at the Technical University of Liberec in 2003
[21]. The idea comes from the industrial application. Needle system is regarded as inappropriate for mass
production. In 2004, with the help of Elmarco Company, the process was attempted to be commercialized
for the production of nanofibers.

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Nanofiber Production Methods

Figure 7. Needleless Electrospinning

Jirsak found a needleless electrospinning setup via a rotating roller. When the roller revolving slowlyis
partially submerged into a polymer solution, the polymer solution is loaded onto the higher roller surface
[22].As applying a high voltage to the reservoir, a gigantic number of solution jets can be generated from
the roller surface upward (Fig. 7). This setup has been commercialized by Elmarco Co. with the brand
name NanospiderTM [24]. The rotation of spinneret loads a small layer of polymer solution onto the
spinneret surface. The rotation and perturbance create conical spikes on the surface. When a high voltage
is applied, these spikes collect charges and amplify the perturbance and, as a result of this, the fluid
around the spikes is spun. Therefore, Taylor cones are generated. Slim electrospinning jets are then
ejected from the tips when the electric force is adequate [24-25].
2.9. Centrifugal Electrospinning
The centrifugal electrospinning(Fig. 8)process is the combination of centrifugal spinning
andelectrospinning. Polymer solution is fed and placed centrally onto a very high speed rotating spinning
disc. The polymer solution is moved radial towards the rim of the rotating disc where the surface tension
is overcomedue to the centrifugal forces. The electric field contributes to stretch the jets to very small
dimensions under simultaneous evaporation of the solvent, leaving a dry nanofibrous coating on the
substrate.The method is independent of ambient conditions such as temperature and humidity. This is a
definite advantage when compared to needle based or needleless processes, which sometimes are affected
severely by relative humidity. Bead and holes are possible defects that can be seen in this technique [26].

Figure 8. Centrifugal electrospinning

3. CENTRIFUGAL SPINNING
Centrifugal spinning method is similar to the cotton-candy spinning method. In a cotton candy machine,
sugars are melted by heating and extruded by centrifugal spinning through nozzles, resulting in sucrose
fibers randomly distributed in the free space near the spinneret. Recently, the fabricated sucrose fibers
have been used as a mold for porous polymer forming [27]. This process has been patented by Huang in
2007 [28]. Centrifugal production method is quite similar to centrifugal electrospinning. But, in this
method no electrical charge is used. Instead, it consists ofdropping of a polymer solution onto a typical
spin coater followed by a very fast rotatingspinneret. Moreover, the spinning procedure offers many
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technologically relevant opportunities, such as yielding hollow polymer beads,and being applicable to
different types of polymers [29].
Today, a company has improved a new method called ForcespinningTM(Fig 9.) for the nanofiber
production via this technique. ForcespinningTM is applicable for solutions and molten materialsvia
centrifugal force. Because Forcespinning uses less solvent or no solvent at all, it is more productive in
terms of cost when compared to electrospinning. No heated air jets or no heating make it more cost
effective than meltblown. [30].A spinneret with a reservoir containing liquid material is rotated
centrifugally on an axis at high rpm. While the spinneret rotates, liquid material is pushed to the outer
wall through an orifice. In this process, centrifugal and hydrostatic forces together initiate the jet [30].

Figure 9. ForcespinningTM [30]

4. WET SPINNING
This technique is derived from a conventional and commercial wet spinning technique that can fabricate
polymer nanofibers with diameter ranges from 10 microns down to 400 nanometers.

Figure 10. Wet-spinning setup for nanofiber production

Fiber spinning succeed via injection of a polymer solution precursor passing through a very small
aperture into a moving and highly viscous medium (Fig. 10). The medium is moved by a spinning
mandrel, which serves to perform the extruded fiber away from the pinhole. The mandrel pulls the
nanofiber. If the extrusion tip is appropriately positioned, the extruded fiber moves in a spiral trajectory
and is deposited continuously around the mandrel. Polymer solidifies in the viscous medium. This
modified wetspinning technique can spin fibers that would be considered unspinnable by any other
method. Furthermore, some materials that have low viscosity can be used in this process [31].
5. DRAWING
The drawing technique provides simple and cost effective photonic wire manufacturing. But a steady
temperature distribution is needed in the drawing zone and the lengths of the fabricated wires are limited
to tens of millimeters. PTT nanofibers with diameters down to 60 nm and lengths up to 500 mm can be
fabricated by the drawing process, as described in Figure 11. PTT is retracted at a speed of 0.11 m/s.
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Nanofiber Production Methods

The extended PTT wire is quickly cooled in air and finally an unclad amorphous PTT nanofiber is created
[32]. Fibers fabricated by this technique not only show low optical losses but also offer good flexibility
[33].

Figure 11. Drawing process

6. ISLAND IN THE SEA
There have been several configurations and patents about the island in the sea process [34-35]. Typical
island in the sea fiber can be seen in the Figure 12. This method allows the melt and solution processing
of plural component fibers. Basically, two different polymers are spun together after that sea polymer is
dissolved. Also, before dissolving the sea polymer, a drawing can be conducted in order to reduce the
fiber diameter. Moreover, Hills spin pack offers some attractive features, such as high spinneret density
for complex bicomponent cross sections, flexibility in selection of polymer types and bicomponent crosssections. In the production of the Island in the Sea filaments, the spinneret design and the distribution
plates are crucial because the fiber diameter, the cross sectional area and the number of islands depend on
the diameter and the shape of the spinneret orifice and the polymer distribution in the distribution plates.
Furthermore, the same method can be applied to spunbond process [36].

Figure 12. Typical island-in-sea fiber

Island and sea polymers have to be selected according to their ability to be spun in the island in the sea
configuration. It has been shown that the polymer viscosities are the most profound factors influencing
the spinnability of the two components in the configuration. The difference in the viscosity of polymers
can cause serious migration and deformation of an interface between polymers resulting from unequal
concentration of stresses in the spinline. The spinline tension is mainly concentrated on the component
having higher viscosity [37].
8. OTHER TECHNIQUES
From the wide aspect of nanofiber production, there have been several techniques that are used rarely.
Some of them will be given very briefly.
Template Synthesis
The template method is an effective approach for the controlled synthesis of nano materials with
various morphologies and has attracted a lot of efforts [38]. Henceforward the casting method and DNA
replication can be considered as template-based synthesis. For the case of nanofiber production by the
template refers to a metal oxide membrane with pores of nano-scale diameter. Under the application of
water pressure on one side, restraining from the porous membrane causes extrusion of the polymer
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which comes into contact with a solidifying solution giving rise to nanofibers whose diameters are
determined by the pores [1].
Phase Separation
In phase separation, a polymer is firstly mixed with a solvent before undergoing gelation. The main
mechanism in this process is (as the name suggests) the separation of phases due to physical
incompatibility. One of the phases which is the solvent is extracted resulting in leaving behind the other
remaining phase [1]. In other words, the process can be described subsequently as: dissolution of
polymer, liquid-liquid phase separation, polymer gelation, extraction of solvent from gel and quenching,
respectively [39].
Self- Assembly
The main mechanism for a generic self-assembly is the intermolecular forces that bring the smaller units
together. The shape of the smaller units of molecules determine the overall shape of the macromolecular
nanofiber. Molecular self-assembly provides an innovative way to design and produce novel materials at
multiple levels (nanomicromacro) [1].
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