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Current Applied Physics 6 (2006) 1030–1035

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Development of high efficiency nanofilters made of nanofibers


a,b
Y.C. Ahn , S.K. Park b, G.T. Kim b, Y.J. Hwang b, C.G. Lee b, H.S. Shin b, J.K. Lee b,*

a
Research Institute of Mechanical Technology, Pusan National University, San 30, Jangjeon-dong, Keumjeong-ku, Busan 609-735, Republic of Korea
b
Department of Mechanical Engineering, Pusan National University, San 30, Jangjeon-dong,
Keumjeong-ku, Busan 609-735, Republic of Korea

Received 4 September 2004; received in revised form 19 March 2005


Available online 11 August 2005

Abstract

Electrospinning is a fabrication process that uses an electric field to control the deposition of polymer fibers onto a target sub-
strate. This electrostatic processing strategy can be used to fabricate fibrous polymer mats composed of fiber diameters ranging from
several microns down to 100 nm or less. In this study, optimized conditions to produce nanofibers using Nylon 6 are investigated
and the Nylon 6 nanofilters using nanofibers of 80–200 nm in diameter are designed and evaluated the filtration efficiency and pres-
sure drop across the filter. When the Nylon 6 concentration is 15 wt.%, electrospun fibers have an average diameter of 80 nm, but
there are many beads, and the concentration increases to 24 wt.%, the fiber diameter gradually thickens to 200 nm, but there are not
any beads. When the spinning distance is small, the thinner nanofibers are produced and the more fibers are collected on the
grounded electrode. The filtration efficiency of Nylon 6 nanofilters is 99.993% superior to the commercialized HEPA filter at the
face velocity of 5 cm/s using 0.3 lm test particles. Even though the high pressure drops across the nanofilter, they show the potential
to have the application of HEPA and ULPA grade high efficiency filter.
Ó 2005 Elsevier B.V. All rights reserved.

PACS: 81.05.L

Keywords: Electrospinning; Nanofibers; Nanofilter; Nylon 6; HEPA

1. Introduction scale diameters. Fig. 1 shows the classification by the fi-


ber diameter. Nanofibers have a large specific surface
Since the beginning of the nineteenth century, poly- area and a small pore size in comparison with commer-
mers have replaced metals in various applications for cial textiles. So polymer nanofibers are being used or
their lightweight and flexibility. Commercially, most finding uses in filtration, protective clothing, biomedical
synthetic manufactured fibers are created by extrusion, applications including wound dressings and drug deliv-
which consists of forcing a thick, viscous liquid through ery systems, as structural elements in artificial organs,
the tiny holes of a device called a spinneret to form con- and in reinforced composites. Recently, there has been
tinuous filament of semi-solid polymer. a renewed interesting in these commercially variable pro-
Electrospinning is a process of electrostatic fiber cesses, making literature involving the quantitative tech-
formation by which uses electrical forces to produce nical and scientific information of the process and
polymer fibers from polymer solution, with nanometer- product characterization extremely limited. Polymer fi-
bers encouraged the invention of technology for manu-
*
Corresponding author. Tel.: +82 51 510 2455; fax: +82 51 582
facturing nanofibers such as electrospinning [2,3].
6368. This paper derives an optimum condition to form
E-mail address: jklee@pusan.ac.kr (J.K. Lee). Nylon 6 nanofibers by electrospinning process and

1567-1739/$ - see front matter Ó 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.cap.2005.07.013
Y.C. Ahn et al. / Current Applied Physics 6 (2006) 1030–1035 1031

Table 1
Experimental conditions to produce Nylon 6 nanofibers by
electrospinning
Parameters Values
Polymer Nylon 6
Solvent Formic acid
Concentration (wt.%) 15–24
Electric voltage (kV) 25
Tip to collector distance (cm) 5–14
Collector Steel mesh
Capillary diameter (mm) 0.7
Fiber diameter range (nm) 80–200
Temperature (°C) 25
Relative humidity (%) 40

polymer fluid contained in a glass syringe and a metallic


collector. The hemispherical shape of pendant droplet at
the end of syringe tip is changed into a conical shape
with increasing voltage, which is known as the Taylor
Fig. 1. Classification by the fiber diameters [1]. cone. When the voltage reaches a critical value, the elec-
tric force overcomes the surface tension of the deformed
develops nanofilters. The important parameters in the drop of the suspended polymer solution formed on the
forming of electrospun Nylon 6 nanofilters such as con- tip of the syringe, and a jet is produced. A jet travels
centration, and electric field strength are investigated through the air, the solvent evaporates leaving behind
experimentally. Also the filtration characteristics of the polymer fibers to be collected on an electrically
Nylon 6 nanofilters such as collection efficiency and grounded target. This means that the electrospinning
pressure drop are evaluated. jet can be thought of as string of charge elements con-
nected by a viscoelastic medium, with one end fixed at
the point of origin and the other end free. The free
2. Experimental end of the electrospinning jet follows a chaotic path as
it travels toward the grounded collector [4–6]. This cha-
2.1. Electrospinning to develop Nylon 6 nanofilters otic motion is the result of a complicated interaction of
variables that involve viscosity, conductivity, surface
Fig. 2 shows a schematic diagram of the electrospin- tension, electrostatic force, air friction, gravity and
ning process. It consists of the syringe feeder system, the ambient parameters [7–9].
collector system, and the high voltage power supply sys- Table 1 shows the experimental conditions to develop
tem. High electric field strength is generated between a Nylon 6 nanofilters. Nylon 6 solutions are prepared
from Nylon 6 pellet (Aldrich) and it is dissolved by for-
mic acid in the ultrasonicator. The concentration of the
Nylon 6 solution tested ranges from 15 to 24 wt.%. Spin-
ning occurs from the droplet of solution protruding
from the 0.7 mm internal diameter of the tip. A positive
electric potential is applied to the polymer blend solu-
tion, by attaching the lead to the variable high voltage
power supply (Chung-pa Co., EMT) directly to the cop-
per wire, to the solution inside a syringe. The electric
voltage is 25 kV. A drum collector covered with steel
mesh is placed 5–14 cm vertically from the tip of the syr-
inge as a grounded collector. The morphology and
diameter of the electrospun fibers aggregates are deter-
mined with a scanning electron microscope (HITACHI,
4200) and image analyzer (IMT, IMT-2000).

2.2. Performance evaluation of the nanofilters

Fig. 3 is a schematic diagram of the filter testing


Fig. 2. Schematic diagram of the electrospinning set-up. apparatus used. The system is comprised of an atomizer,
1032 Y.C. Ahn et al. / Current Applied Physics 6 (2006) 1030–1035

Compressed
Air Excess
Aerosol
HEPA HEPA Filter ΔP
Diffusion Flow
Filter Flow HEPA
Dryer meter meter
Filter

Test Filte

Atomizer Kr-85
HEPA Neutralizer
Filter
Vacuum
Dilution Air
Pump
Condensation
Particle Counter

Fig. 3. Schematic diagram for the performance evaluation of nanofilters.

a diffusion dryer, a charge neutralizer, a filter holder, 3. Results and discussions


and a condensation particle counter. In the atomizer,
PSL (Polystyrene Latex) particles which have known 3.1. Effects of Nylon 6 concentration on fibers morphology
sizes are dissolved in a distilled water and the solution
is atomized. Much moisture are on the surfaces of the Fig. 4 shows the SEM images of Nylon 6 nanofibers
monodisperse particles, however, they are eliminated as a function of Nylon 6 concentration at the applied
during passing through the diffusion dryer. In order to voltage of 25 kV. When the concentration is 15 wt.%,
avoid unwanted electrostatic effects, a charge neutralizer electrospun fibers have an average diameter of 80 nm,
(TSI, 3054) is used. Electrical charges on the aerosols are but as the concentration of Nylon 6 increases to
neutralized by exposing the aerosols to a cloud of bipo- 24 wt.%, the fiber diameter gradually thickens to
lar ions produced by a radioactive source. The 10 mCi 200 nm. The higher concentration of the polymer solu-
Kr85 source is placed inside an aluminum tube and the tion tries to form thicker fibers by preventing the
aerosol is passed through the tube. The particles are thus stretching of fibers. Polymer concentration also has an
brought to a state of Boltzmann charge equilibrium. The effect on bead formation and bead density. Fibers pro-
filter to be tested is placed in a filter holder and the par- duced from lower concentrated solution exhibit more
ticle concentration upstream and downstream of the fil- beads while other parameters remain constant. A mix-
ter is measured using the condensation particle counter ture of large beads and fibers is generated by electrospin-
(TSI, 3010). The condensation particle counter can mea- ning Nylon 6 solution at the concentrations below
sure the number concentration of nano-sized particles to 18 wt.%. The reason is that at lower concentrations,
grow to micro-sized droplets in a supersaturated electrospun fibers are harder to dry before they reach
environment. the collection drum. When solidification process is
Table 2 shows the experimental conditions for perfor- undergoing on the surface of the collection drum, sur-
mance evaluation of nanofilters. The diameter of the test face tension makes bead spherical shape. At low concen-
filters is 47 mm and the face velocity is varied from 3 to tration, surface tension becomes dominant influence
10 cm/s. Nylon 6 nanofilters are prepared two samples over viscosity and form more beads. But as the viscosity
according to the base weight of 5.75–10.75 g/m2 and fil- increases in the solution, surface tension becomes dom-
tration efficiency is evaluated using test particles of inated by viscosity and results in less number of beads,
0.085–2.0 lm in diameter. while the other variables are maintained constant.

3.2. Effects of spinning distance on fibers morphology

Table 2 Fig. 5 shows SEM images of Nylon 6 nanofibers as a


Experimental conditions for evaluating the filtration efficiency of function of spinning distance at the Nylon 6 concentra-
nanofilters tion of 24%. In general, the spinning distance performed
Parameters Values a role on the fiber structure and morphology [3]. The
Face velocity (cm/s) 3–10 electric field strength is increased when the spinning dis-
Particle size (lm) 0.085–2.0 tance is decreased, and the polymer jet is discharged
Test filter size (mm) 47 with a greater electrostatic repulsion that causes it to un-
Base weight (g/m2) Sample 1 5.75 dergo higher levels of drawing stress and the jet velocity
Sample 2 10.75
increases. The increasing electrostatic force reinforces
Y.C. Ahn et al. / Current Applied Physics 6 (2006) 1030–1035 1033

Fig. 4. Scanning electron micrographs of Nylon 6 nanofibers as a function of concentration (applied voltage = 25 kV, spinning distance = 5 cm).

Fig. 5. Scanning electron micrographs of Nylon 6 nanofibers as a function of spinning distance (applied voltage = 25 kV, Nylon 6
concentration = 24%).

the stretch ability of a droplet. During the travel of strength has the opportunity to stretch the fibers
the fibers towards the target, the higher electric field more and results in thin fibers. The morphology of the
1034 Y.C. Ahn et al. / Current Applied Physics 6 (2006) 1030–1035

nanofibers at the spinning distance of 5 cm shows thin-


100.00
ner fibers and the collection efficiency to the grounded

Filtration Efficiency (%)


electrode is slightly high compared with the other cases. 99.98

Therefore, the optimum conditions for mass production


of nanofilters are selected as 25 kV of electric potential 99.96

at 5 cm of spinning distance using solution of 24%


99.94
Nylon 6 concentration. Particle Size : 0.3 μ m
HEPA Filter
2
99.92 Nano filter, Sample 1 (Base Weight: 5.75 g/m )
3.3. Performance evaluations of Nylon 6 nanofilters 2
Nano filter, Sample 2 (Base Weight: 10.75 g/m )

99.90
2 3 4 5 6 7 8 9 10 11
Three samples of filters are used in this study. The Face Velocity (cm/s)
one is HEPA(High Efficiency Particulate Air) filter to Fig. 7. Filtration efficiency of the HEPA filter and the Nylon 6
measure reference values and others are Nylon 6 nano- nanofilters as a function of face velocity.
filters to evaluate the performances such as filtration effi-
ciency and pressure drop. The HEPA filter is used as a
commercialized one (Hollingsworth & Vose, HB5443), Fig. 7 shows the filtration efficiency of the HEPA filter
and Nylon 6 nanofilters are prepared by electrospinning. and the Nylon 6 nanofilters as a function of face velocity.
The homogeneity of the Nylon 6 nanofilters are con- The filtration efficiency of test particle can be calculated
firmed as following methods. Several sample filters with by comparing with the particle number concentration be-
the same nominal base weight and dimensions are pre- tween upstream and downstream of the test filter medium
pared and the pressure drop across each filter is mea- for the size range of each particle. The nanofilter sample 1
sured as a function of face velocity. The results show shows a good filtration efficiency to satisfy the criterion of
that the filters are the same. HEPA filter for the filtration efficiency of 99.97% at
Fig. 6 shows the pressure drop of the HEPA filter and 0.3 lm particle size. At the condition of 10 cm/s of face
the Nylon 6 nanofilters as a function of face velocity. velocity, the filtration efficiency of nanofilter sample 1 is
The normal criteria of the HEPA filter media show decreased to 99.96% while the other filters still satisfy
that the filtration efficiency is over 99.97% at 0.3 lm the criterion of HEPA filter. As the velocity is increased,
particles and the pressure drop is lower than 40 mmAq collection by diffusion is reduced, but collection by
at 5 cm/s face velocity [10]. The test results show the impaction rises. In the high velocity conditions, some
pressure drop of the HEPA filter is in the normal particles, acquired more momentum, pass through the fil-
range, however, the pressure drops of the Nylon 6 nano- ters because of extremely thin thickness of the nanofilter
filters are higher than that of HEPA filter. The pore sample 1. On the other hand, the nanofilter sample 2,
size of the HEPA filter is 1.7 lm and the Nylon 6 nano- which has double thickness to the sample 1, shows better
filters are 0.24 lm and the thickness of the HEPA filter filtration efficiency than commercialized HEPA filter and
is 500 lm and the Nylon 6 nanofilters are 50 lm 99.993% at 5 cm/s using 0.3 lm particle.
(base weight: 5.75 g/m2) and 100 lm (base weight:
10.75 g/m2). When it is considered that the base weight
of HEPA filter is 78.2 g/m2 and the Nylon 6 nanofilters 4. Conclusions
are 5.75 and 10.75 g/m2, the Nylon 6 nanofilters are
formed just like a thin film with very fine sized pores. Electrospinning is a process of electrostatic fiber
formation by which uses electrical forces to produce
polymer fibers from polymer solution, with nanometer-
300
scale diameters. Nanofibers have a large specific surface
HEPA Filter
250
2
Nano Filter, Sample 1 (Base Weight: 5.75 g/m )
area and a small pore size in comparison with conven-
2
Nano Filter, Sample 2 (Base Weight: 10.75 g/m ) tional commercial textiles. Therefore, polymer nanofi-
Pressure Drop (mmAq)

200 bers are being used or finding uses in the industrial and
the biomedical fields. Especially, in this study, the appli-
150
cation for the filtration medium is evaluated using nano-
100 filters made by electrospun Nylon 6 nanofibers.
The concentration of the polymer solution has shown
50 a great influence on the fiber diameter as well as on
bead. When the Nylon 6 concentration is 15 wt.%, elec-
0
2 3 4 5 6 7 8 9 10 11 trospun fibers have an average diameter of 80 nm, but
Face Velocity (cm/s) there are many beads, and the concentration of Nylon
Fig. 6. Pressure drop measurements across the HEPA filter and the 6 increases to 24 wt.%, the fiber diameter gradually
Nylon 6 nanofilters as a function of face velocity. thickens to 200 nm, but there are not any beads. When
Y.C. Ahn et al. / Current Applied Physics 6 (2006) 1030–1035 1035

the spinning distance is small, the thinner nanofibers are References


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