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Electrospun cellulose acetate nanofibers for airborne nanoparticle filtration

Article  in  Textile Research Journal · October 2018


DOI: 10.1177/0040517518807440

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Original article
Textile Research Journal
0(00) 1–13

Electrospun cellulose acetate nanofibers ! The Author(s) 2018


Article reuse guidelines:
sagepub.com/journals-permissions
for airborne nanoparticle filtration DOI: 10.1177/0040517518807440
journals.sagepub.com/home/trj

Joerg Ahne1, Qinghai Li2, Eric Croiset1 and Zhongchao Tan1

Abstract
Reported in this paper are the effects of tip-to-collector distance, voltage, deposition time and solution concentration on
the fiber size distribution and filter quality factor of electrospun cellulose acetate (CA)-based nanofibers. Nanofibrous
filter samples were produced by electrospinning in a laboratory setting. The CA solutions were prepared by diluting
various concentrations of CA in a 2:1 (w:w) ratio of N,N-dimethylacetamide (concentration 10–20 wt.%). The electro-
spinning voltages ranged from 8–12 kV, with distances from 10–15 cm and deposition times of up to 30 minutes. The
produced nanofibrous filter samples were then analyzed in terms of fiber size distribution and filter quality factor using
nanosized sodium chloride particles ranging from 4–240 nm in diameter. The maximum filtration efficiency measured was
99.8% for filter samples obtained with an overall deposition time of 30 minutes. The maximum filter quality factor was
0.14 Pa1 for a CA concentration of 20 wt.% and a tip-to-collector distance of 15 cm. The average fiber diameters of the
fibers were between 175 and 890 nm, and CA concentrations below 15% led to the formation of beads.

Keywords
nanofiber, airborne nanoparticle filtration, filtration efficiency, electrospun cellulose acetate, fiber size distribution, filter
quality factor

Nanofibers have been used for air filtration for a few tension, etc.), applied voltage, tip-to-collector distance,
decades. Nanofibers find applications in many indus- nozzle diameter, and ambient conditions such as tem-
tries including textiles, clean energy and environment, perature and relative humidity. Beaded fibers may be
medicine and defense.1 Interest in the research and produced when the tip-to-collector distance, solvent
development of nanofibers by electrospinning has flow rate or polymer concentration is high.11
been growing in recent years due to their potential in Furthermore, a high-viscosity polymer leads to larger
producing sub-100 nm nanofibers. Among several fibers. Thinner fibers are produced at a higher tempera-
methods that are available for nanofiber production, tures, high electrospinning voltages and small flow rates
electrospinning is considered superior over others due for single jet electrospinning processes.
to its ability to produce fine fibers from a variety of Nanofibers can be produced for the filtration of air-
materials,2 for example, poly(vinyl alcohol) (PVA),1 borne nanoparticles (1–100 nm in diameter) for the pro-
polyurethane,3 polypyrrole-poly(acrylonitrile-co-vinyl tection of human health and the environment.12–16
acetate),4 polyacrylonitrile (PAN) and dimethylforma- Researchers believe that the features of nanofibers
mide,5 polypropylene,6 alumina,7 activated carbon8 and include high filtration efficiency and low pressure
polyamide-6.9 A review of multifunctional polymer
nanocomposites for multifunctional finishing of textiles
is also available.10 1
University of Waterloo, Canada
2
Electrospinning has found its way into industrial Tsinghua University-University of Waterloo Joint Research Centre for
applications over the last 8 years. A typical electrospin- Micro/Nano Energy and Environmental Technology, China
ning process is used to fabricate nanofibers with diam-
Corresponding author:
eters in the order of 100 nm. The electrospinning Zhongchao Tan, University of Waterloo, 200 University Avenue, West
process depends on multiple parameters, including Waterloo, Ontario N2L 3G1, Canada.
polymer properties (concentration, viscosity, surface Email: tanz@uwaterloo.ca
2 Textile Research Journal 0(00)

drop. PVA-, nylon 6-, cellulose acetate (CA)- and contributes to the parameter studies of CA and poly-
PAN-based nanofibers have been successfully fabri- mer nanofibers in general. Additionally, it provides
cated in laboratories for air filtration purposes. practical knowledge of air filtration, which determines
Within the area of air filtration, there is a growing the potential usability of these nanofibers. The main
interest in biodegradable nanofibers, which is mainly contribution of this paper lies in the information pro-
driven by the global promotion of sustainability and vided regarding the production of CA with various par-
related policies.17,18 Technical challenges arise in the ameters. It also enriches the available data concerning
quest to produce biodegradable polymers in a cost- the filtration mechanics of CA nanofibrous materials.
effective manner, with performance comparable to syn-
thetic polymers.19 Biodegradable nanofibers can be
made of CA, which is a natural polymer that can poten-
Experimental details
tially replace synthetic polymers. Cellulose is one of the Cellulose acetate was purchased from Sigma Aldrich,
most widely available organic compounds on Earth. USA (average Mn & 30,000). CA solutions were pre-
CA nanofibers offer relatively high modulus, flexible pared by diluting various concentrations of CA at a 2:1
and tensile strength. The properties of CA nanofibers (w:w) ratio of N,N-dimethylacetamide (Sigma Aldrich,
can also be tuned for certain contaminants by functio- 99.8%) and acetone (Sigma Aldrich, 99.7%). The
nalizing the nanofibers with chemical groups. CA nano- resultant mixtures were stirred at 35 C on a magnetic
fibers have been shown to be biocompatible, non-toxic stirring heating plate for approximately 2 hours to com-
and biodegradable, thus making them ideal candidates pletely dissolve CA into the solvent mixture. The poly-
for filtration applications.20 mer molecules were assumed to be adequately dissolved
Researchers have started to investigate the perform- in the solvent for the electrospinning process. As is typ-
ance of CA nanofibers on the filtration of airborne ical practice in this field of research, complete dissol-
nanoparticles.19 Chattopadhyay et al.21 investigated ution was confirmed through visual inspection when
the effects of the fiber diameter, solidity and membrane the solvent turned to a clear liquid. Similar formula-
thickness of electrospun CA fibers on nanoparticle fil- tions of the solvent have been reported to work well
tration. Their CA fibers were produced by electrospin- for producing CA nanofibers in the literature.23,24
ning. In their study, the tested aerosols were NaCl Three different concentrations of CA were tested for
particles in the size range of 40–270 nm and diethyl this study: 10, 15 and 20 wt.%.
hexyl sebactate at a face velocity of 45 cm/s, which is The CA solution was then placed in a 5 mL syringe
considered to be high. They found that the filtration and connected to a capillary tip (gauge 22); this solu-
performance of electrospun nanofibers was higher tion was pressed through the tube and capillary with a
than that of thin commercial filtration materials. syringe pump at a constant feed rate of 0.6 mL/h. The
Matulevicius et al.22 tested the effects of operating par- capillary needle was connected to a high-voltage supply
ameters on the fiber size and filtration performance of (maximum voltage  30 kV). The voltage varied from
electrospun polymers, including CA. They used mono- 8–12  0.1 kV and the distance between the needle
dispersed particles with sizes of 100 and 300 nm in and collector from 10–15 cm  0.1 cm. The nanofiber
diameter, which are not nanoparticles. However, the samples were deposited onto a stainless steel screen
available data for CA-based materials is still insuffi- with a wire diameter of 140 mm and opening size of
cient, especially for their application in the filtration 368 mm. The screens were placed on aluminum foil
of airborne nanoparticles. In addition, there is that covered the grounded collector. A schematic of
limited information available on the air filtration the setup can be found in Figure 1. The test conditions
performance of biodegradable filters at lower face velo- for the filter samples are listed in Table 1.
cities.22 Most of the works published to date only As described in our earlier work,15 the nanofibrous
focuses on morphology and other physical properties filter samples were first analyzed by scanning electron
of the filters. microscopy (SEM) (Zeiss Gemini Model Leo 1550) to
The primary objective of this work is to better observe their morphology. Then, fiber size distribution
understand the effects of key parameters that affect was analyzed using a MATLAB code. More details can
the filtration quality factor of CA nanofibrous filters be found the supplemental materials of our earlier
for nanoparticles. The key parameters include solvent paper.15 The same samples were tested in terms of filtra-
concentration, voltage, tip-to-collector distance and tion efficiency. The analysis steps are introduced below.
deposition time in electrospinning. The electrospun In preparation for the SEM analysis, a conductive
CA nanofibers were characterized, and tested for filtra- gold coating was sputtered onto the nanofiber surfaces
tion efficiency and quality factors to determine the opti- for 120 s to better visualize the nanofibers.
mal conditions for the fabrication of CA nanofibers Representative SEM images were obtained at magnifi-
that aim to achieve nanoparticle filtration. This paper cations from 5000–21,000. MATLAB code developed
Ahne et al. 3

Figure 1. Schematic of electrospinning setup.

Table 1. The electrospinning parameters for the nanofiber samples

Cellulose acetate Deposition Applied Tip-to-collector


Sample name concentration (wt.%) time (minutes) voltage (kV) distance (cm)

CA10_5_8_10 10 5 8 10
CA10_5_8_12.5 10 5 8 12.5
CA10_5_8_15 10 5 8 15
CA10_15_8_10 10 15 8 10
CA15_5_8_10a 15 5 8 10
CA15_5_8_12.5a 15 5 8 12.5
CA15_5_8_15a 15 5 8 15
CA15_5_10_10a 15 5 10 10
CA15_5_12_10a 15 5 12 10
CA15_15_8_10 15 15 8 10
CA15_15_10_10 15 15 10 10
CA15_15_12_10 15 15 12 10
CA15_30_8_10 15 30 8 10
CA15_30_10_10 15 30 10 10
CA20_5_8_10a 20 5 8 10
CA20_5_8_12.5a 20 5 8 12.5
CA20_5_8_15 20 5 8 15
CA20_5_10_10a 20 5 10 10
CA20_5_12_10 20 5 12 10
CA20_15_8_10 20 15 8 10
CA20_30_8_10 20 30 8 10
a
The indicated samples are also displayed in Table 2.

in-house was used to quantify the diameter of the fibers. determining the separation between fiber edges and cen-
The algorithm used for this process included image pre- terlines. Multiple images were obtained at each magni-
treatment, local threshold, smoothness, edge detection fication and from different locations to get more
and skeletonization.15 A Euclidean distance transform representative samples. An equal number of low
matrix was used to obtain fiber diameters by (factor 5000) magnification and high (factor 20,000)
4 Textile Research Journal 0(00)

magnification images were averaged out for each compare the filtration performances of the filter sam-
sample in order to get a more representative value for ples. It is a standard parameter in filtration research.
average fiber diameter. The filter quality factor (QF) can be calculated using
The filter testing apparatus is the same as the one that equation 2:
was reported in our previous studies.15,16 The same setup
is shown in Figure 2. The testing setup is comparable to lnð1  Þ
QF ¼  ð2Þ
those used by Chattopadhyay et al.21 and Matulevicius P
et al.22 A constant output atomizer (TSI model 3076)
was used to generate aerosol particles from a solution where QF is the qualify factor and P the pressure drop
composed of 0.1 g/L sodium chloride (NaCl) in distilled across the filter sample. Since the particle filtration
water. In this case, compressed air was used to form a efficiency depends on the particle size, QF is size-
high-velocity jet that atomizes the solution into polydis- dependent. To simplify the calculation, in this paper,
persed NaCl aerosol particles. The aerosol particles were total efficiency is calculated as the summation of all
then passed through a diffusion drier (TSI Model 362) to particle sizes tested.
remove water vapor from the generated aerosol.
The aerosol particles were then passed through the
filter medium at an air flow rate of 1.5 L/minute. The Results and discussion
filter medium was placed on a filter holder (BGI Inc.,
Waltham, MA). The filter sample and the filter holder
Fiber size distributions
have a diameter of 25 mm. With a flow rate of Table 2 shows the SEM images and fiber size distribu-
1.5 L/minute, the face velocity on the filter is 5.1 cm/s. tions of the samples indicated in Table 1. It is
The pressure drop across the filter medium (P) was
monitored and recorded using a differential pressure
gauge (Omegadyne, model DPG409). Each test was 1.20E+07
repeated five times. All tests were conducted in room
conditions, at normal temperature and with a relative 1.00E+07
humidity of about 50%.
dN/dlog(dp) (1/cm³)

8.00E+06
The fractional filtration efficiency was calculated
using the concentrations of particles measured with 6.00E+06
and without the presence of the nanofibrous filter (see 4.00E+06
equation 1):15
2.00E+06
Cw=o
¼ 1 ð1Þ
Cw 0.00E+00
1 10 100 1000
where Cw=o and Cw are the concentrations of nanopar- Parcle Size (nm)
ticles before and after the filter sample, respectively.
Since they have the same unit, equation 1 is dimension-
Figure 3. Particle size distribution of the NaCl particles.
less. In this paper, filter quality factor is used to

Clean, Dry, and Oil- Hygrometer


free Compressed Air HEPA Filter
Filter Holder
Fume
Hood
Diffusion Neutralizer Mass Flow
Dryer Meter

NaCl
Particles

SMPS+E (GRIMM)

Figure 2. Schematic diagram of the filtration setup.


Ahne et al. 5

Table 2. Sample scanning electron microscopy images and determined fiber size distributions

CA15_5_8_10

0.16
Mean df: 145 nm
0.14
Std: 82.8 nm
0.12

Frequency (-)
0.1
0.08
0.06
0.04
0.02
0
0 125 250 375 500 625 750 875 1000
Fiber Diameter (nm)

CA15_5_8_12.5

0.2

Mean df: 254.6 nm


0.15

Frequency (-)
Std: 238.6 nm

0.1

0.05

0
0 125 250 375 500 625 750 875 1000
Fiber Diameter (nm)

CA15_5_8_15

0.4
Mean df: 72.7 nm
0.35
Std: 176.6 nm
0.3
Frequency (-)

0.25
0.2
0.15
0.1
0.05
0
0 125 250 375 500 625 750 875 1000
Fiber Diameter (nm)

CA15_5_10_10

0.08
Mean df: 283.7 nm
0.07 Std: 254.7 nm
0.06
Frequency (-)

0.05
0.04
0.03
0.02
0.01
0
0 125 250 375 500 625 750 875 1000
Fiber Diameter (nm)

(continued)
6 Textile Research Journal 0(00)

Table 2. Continued

CA15_5_12_10

0.16
Mean df: 252.5 nm
0.14 Std: 252.2 nm
0.12

Frequency (-)
0.1
0.08
0.06
0.04
0.02
0
0 125 250 375 500 625 750 875 1000
Fiber Diameter (nm)

CA20_5_8_10

0.08
Mean df: 252.5 nm
0.07
Std: 245.4 nm
0.06

Frequency (-)
0.05
0.04
0.03
0.02
0.01
0
0 125 250 375 500 625 750 875 1000
Fiber Diameter (nm)

CA20_5_8_12.5

0.08
Meand df: 319.4 nm
0.07 Std: 491.4 nm
0.06
Frequency (-)

0.05
0.04
0.03
0.02
0.01
0
0 125 250 375 500 625 750 875 1000
Fiber Diameter (nm)

CA20_5_10_10

0.09
0.08 Mean df: 723.3 nm
Std: 751.2 nm
0.07
Frequency (-)

0.06
0.05
0.04
0.03
0.02
0.01
0

Fiber Diameter (nm)


Ahne et al. 7

noticeable that all of the distributions have a skewed temperature of the air have an impact, since both par-
log-normal shape and, depending on the production ameters can influence the conductivity or surface
parameters, the SDs and means of the samples differs tension of the solution. Based on the qualitative obser-
strongly. The impacts of the single parameters voltage, vations above, only 15 and 20 wt.% samples were ana-
tip-to-collector distance and concentration on the fiber lyzed from this point on for fiber diameter, filtration
distributions are discussed in the following sections. efficiency and filtration quality.
A higher CA solution ultimately leads to higher vis-
Effects of CA concentration on the sizes and cosity of the solution, and consequent higher resistance
of the liquid being precipitated by the electric field. This
morphologies of the nanofibers resistance leads to lower bending instabilities and ultim-
The SEM images in Figure 4 are for samples with ately thicker nanofibers. Similar trends have been
10 wt.% CA. They clearly show the beading of poly- observed for CA nanofibers by other research-
mers. Droplet formation was observed when the poly- ers.20,23,24,26 The increased range of fiber sizes is also
mer concentration was below a certain point or a common for increased polymer concentrations.21 In the
critical chain entanglement concentration, ce.25 Such study by Chattopadhyay et al., the concentration of
defects were not observed above this critical concentra- 15% CA resulted in a fiber diameter of 302  127 nm,
tion. Similar findings have been reported by others.21 It whereas the fiber diameters corresponding to 20% CA
has been reported that the magnitude of ce is dependent were 669  341 nm.
on solvent–polymer interactions.24 Bead-free nanofi-
bers are expected at high CA concentrations, that is,
Effects of tip-to-collector distance on fiber diameter
over 15 wt.%. Higher DMAc content in the solvent
leads to strong hydrogen-bonding interactions between Tip-to-collector distance can impact the quality of the
the solvent and the CA molecules. For the 2:1 DMAc/ fibers; beads can be observed if the tip-to-collector dis-
acetone formulation, the evaporation of the solvent is tance is either too short or too long.27 Tip-to-collector
expected to be slower, resulting in a wet jet landing on distances of 10, 12.5 and 15 cm were considered for the
the collector. In order to minimize surface tension, the following study. No beading was observed for these
solution on the collector forms spherical beads. three tip-to-collector distances.
Note that, in an earlier study24 using a 2:1 DMAc/ As seen in Table 3, for the concentration of 15 wt.%
acetone solvent solution, the beading phenomenon was CA, the general trend indicates an increase in fiber
observed at concentrations as high as 20 wt.%. Bead- diameter with increasing the tip-to-collector distance
free nanofibers were only obtained at a CA concentra- up to 12.5 cm, after which it reaches a plateau. For
tion of 25 wt.%.24 In the current work, the absence of the concentration of 20 wt.% CA, the average fiber
droplets in the 15 wt.% micrographs indicates that the diameter increased from 327  245 to 466  262 nm
critical chain entanglement concentration for the 2:1 when the tip-to-collector distance changed from 10 to
DMAc/acetone solvent mixture is somewhere between 12 cm. A further increase of 2.5 cm in the tip-to-collec-
10 and 15 wt.% of CA. This also indicates that other tor distance resulted in an increase in fiber diameter to
factors may have played an important role in bead for- 836  690 nm. The wide uncertainty associated with
mation. It is likely that the relative humidity or the diameter indicates a poor correlation between

Figure 4. Scanning electron microscopy images of the nanofibers produced with different cellulose acetate concentrations.
(a) 10 wt.%, (b) 15 wt.% and (c) 20 wt.%.
8 Textile Research Journal 0(00)

Table 3. Fiber size distributions at different concentrations and Table 4. Fiber diameters at different concentrations and
tip-to-collector distances applied voltages

Cellulose acetate Tip-to-collector Average nanofiber Cellulose acetate Voltage Average nanofiber
concentration distance (cm) diameter (nm) concentration (kV) diameter (nm)

15 wt% 10 175  82 15 wt.% 8 175  82


12.5 343  175 10 330  254
15 344  174 12 318  259.
20 wt% 10 327  245 20 wt.% 8 466  262
12.5 466  262 10 836  690
15 836  690 12 879  783

tip-to-collector distance and average fiber diameter. The experimental results are summarized in Table 4.
Other researchers have observed that a larger For both CA solutions, an increasing trend is observed
tip-to-collector distance results in thinner nanofibers. for the average fiber diameter with applied voltage. The
A larger distance provides a longer time period for sharp increase in the average fiber diameter can be
the solvent to evaporate. Therefore, the jet undergoes seen when the voltage was increased from 8 to 10 kV
increased elongation due to greater bending instabilities for both CA concentrations. For the concentration of
in the system. Hence, thinner fibers can be obtained. 20 wt.%, the average fiber diameter increases by 369 nm
The increased range of fiber diameters could also be when the voltage increased from 8 to 10 kV. When
attributed to the increase of bending instability. The the applied voltage increased from 10 to 12 kV, the
whipping continuously alters the traveling distance of increase in average fiber diameter was only 43 nm.
the fibers, which has a direct impact on the final A similar trend was also observed when the concentra-
fiber size. However, a similar study concluded that tion was 15 wt.%. However, a marginal decrease
the diameter size and morphology of the fibers were in fiber diameter was observed when the voltage was
not significantly influenced by the deposition range changed from 10 to 12 kV for the concentration of
between 5 and 15 cm.20 Similarly, another study saw 15 wt.% CA.
a minimal impact of the tip-to-collector distance of The effects of the applied voltage on fiber diameter
15–30 cm on the corresponding SEM images.20 It were not conclusive based on earlier studies.20,21 In a
would be desirable to have some data at a shorter dis- separate study on CA nanofibers, other researchers
tance, but no fibers could be formed and collected at found an inverse effect of applied voltage on the
distances of 10 cm. An advanced experimental setup mean fiber diameter.27 This was attributed to stronger
shall be developed for nanofiber fabrication at short electrostatic forces at higher voltages, which caused
distances. It is worth noting that it is very normal to the fibers to stretch more and become thinner.
have a wide range of fiber sizes. The fiber sizes depend Another study showed that voltage had a negligible
not only on the operation of the setup (voltage, distance effect on the diameter of CA nanofibers.28 Increasing
and concentration), but also on the experimental setup the applied electric field resulted in a slight decrease in
itself. Chattopadhyay et al.21 used a drum collector, mean fiber diameter for ethylcellulose nanofibers.
and Christoforou et al.20 used a horizontal setup with However, an increase in fiber diameter may also be
a plate sized 24  24 cm. They all demonstrated that attributed to a stronger electric field, which can result
collector size directly impact the strength of the electric in the solution being ejected more quickly from the
field and the final fiber morphology. capillary tip.
Table 5 shows the results of similar studies in the
literature. It can be seen that the variance of the pro-
Effects of applied voltage on fiber size duced fibers strongly depends on the operating param-
Samples were produced at different applied voltages eters. The parameters also varied between studies for
with two CA concentrations of 15 and 20 wt.% CA, different setups, especially the collector shape and
but with the same deposition time of 5 minutes and dimension. Furthermore, it can be seen that a higher
same tip-to-collector distance of 10 cm. These two polymer concentration leads to a greater mean fiber
groups of samples were used to study the effects of diameter. The fiber sizes produced in our study herein
applied voltage, which were 8, 10 and 12 kV, on the for concentrations of 15 wt.% are comparable with
fiber diameter. those produced by others.
Ahne et al. 9

Table 5. Fiber diameters and production parameters of other research

Cellulose acetate
concentration Mean fiber diameter Voltage (kV) Distance (cm) Reference
21
11% 0.12  0.07 mm (beading) 75–80 20
21
15% 0.3  0.01 mm 75–80 20
21
17% 0.5  0.019 mm 75–80 20
24
15% 275  195 mm (different molecular weight) 8 15
24
15% 241  111 nm 8 15
24
15% 287  165 nm 8 15
22
11% 350  129 nm (different solvent) 18 16
22
11% 363  131 nm 18 16

(a) (b)
1 0.1
CA15_5_8_10 CA15_5_8_10
0.9 CA20_5_8_10 0.09
CA20_5_8_10
0.8 CA15_15_8_10 0.08
CA15_15_8_10
Quality Factor [Pa-1]
0.7 CA20_15_8_10 0.07 CA20_15_8_10
Efficiency [-]

0.6 CA15_30_8_10 0.06 CA15_30_8_10


CA20_30_8_10 CA20_30_8_10
0.5 0.05
0.4 0.04
0.3 0.03
0.2 0.02
0.1 0.01
0 0
10 100 1000 10 100 1000
Parcel size [nm] Parcel size [nm]

Figure 5. (a) Filtration efficiencies and (b) quality factors at different cellulose acetate concentrations.

Air filtration performance polymer concentration of the solution. A higher con-


centration of polymer in the solution leads to relatively
Effect of CA concentration on filtration performance
less volatile solvent in the jet, which results in a higher
Figure 5 shows the effects of CA concentration on the polymer mass deposition rate and solidity of the pro-
filtration efficiencies and quality factors corresponding duced filters. The higher filtration quality is connected
to deposition times of 5–30 minutes. The tip-to-collec- to the higher filtration efficiency with an equal pressure
tor distance and applied voltage were kept constant at drop or less. The slipping effect enabled by the very fine
10 cm and 8 kV, respectively. Since obvious beading of fibers enables a better filtration performance with a
the polymer was observed for 10 wt.% CA, only sam- lower pressure drop. Slip flow occurs when the size of
ples for the concentrations of 15 and 20 wt.% are con- the fiber approaches the mean free path of the air. As a
sidered in this paper. At all deposition times, except for result, the air molecules ‘‘slip’’ over the fiber surface,
15 minutes, filtration efficiency and quality factor which leads to a lower pressure drop. As a result, the
increased when the CA concentration increased from deposited mass does not impact the pressure drop
15 to 20 wt.%. For example, in the case of 30 minutes significantly.
of deposition time, increasing the CA concentration
from 15 to 20 wt.% led to an increase in average filtra- Effects of tip-to-collector distance on filtration
tion efficiency from 14.8 to 60.4%. Under the same
performance
conditions, the quality factor increased from 0.0214 to
0.027 Pa1. Figure 6 shows the effects of tip-to-collector distance on
The higher filtration efficiency can be explained by the filtration efficiency and quality factor of filter sam-
the increased mass deposition of fibers due to the higher ples obtained with 15 and 20 wt.% CA. The deposition
10 Textile Research Journal 0(00)

(a) 0.5 (b) 0.2


CA15_5_8_10 CA15_5_8_10
0.45 CA15_5_8_12.5 0.18 CA15_5_8_12.5
0.4 CA15_5_8_15 0.16 CA15_5_8_15
CA20_5_8_10 CA20_5_8_10

Quality Factor [Pa-1]


0.35 0.14
CA20_5_8_12.5 CA20_5_8_12.5
Efficiency [-]

0.3 CA20_5_8_15 0.12 CA20_5_8_15


0.25 0.1
0.2 0.08
0.15 0.06
0.1 0.04
0.05 0.02
0 0
10 100 1000 10 100 1000
Parcel size [nm] Parcel size [nm]

Figure 6. (a) Filtration efficiencies and (b) quality factors at different tip-to-collector distances.

(a) (b)
1 0.1
CA15_5_8_10 CA15_5_8_10
0.9 CA15_15_8_10 0.09
CA15_15_8_10
0.8 CA15_30_8_10 0.08 CA15_30_8_10
Quality Factor [Pa-1]

0.7 CA20_5_8_10 0.07 CA20_5_8_10


Efficiency [-]

CA20_15_8_10 CA20_15_8_10
0.6 CA20_30_8_10 0.06
CA20_30_8_10
0.5 0.05
0.4 0.04
0.3 0.03
0.2 0.02
0.1 0.01
0 0
10 100 1000 10 100 1000
Parcel size [nm] Parcel size [nm]

Figure 7. (a) Filtration efficiencies and (b) quality factors at different deposition times.

time and applied voltage were kept constant at 5 min- obtained between tip-to-collector distance and both fil-
utes and 8 kV, respectively. For both CA concentra- tration efficiency and filter quality factor.
tions, positive trends are observed for filtration
efficiency and quality factor with increasing tip-to-col-
Effects of deposition time on filtration performance
lector distance. There was generally an increase in aver-
age fiber diameter with increasing tip-to-collector The effects of deposition time on the total filtration
distance. Typically, thinner nanofibers correspond to efficiency and quality factor are shown in Figure 7
higher filtration efficiency. However, this trend was below. All data points were for 15 and 20 wt.% CA
not observed in the study herein. As seen in Table 2, solutions with a tip-to-collector distance of 10 cm
although the mean sizes of certain samples were rela- when the applied voltage was 8 kV. It was observed
tively large, these samples have many fibers that are for both concentrations that both the filtration effi-
smaller than the measured fiber diameter. Therefore, ciency and quality factor increased with deposition
the effects of nanosized fibers can be observed for sam- time. The filtration performance was relatively poor
ples with a high mean fiber size. In a separate study when the deposition time was 5 minutes for all tested
using PVA nanofibers,15 a similar correlation was samples. As shown in Figure 6(a), the filtration
Ahne et al. 11

efficiency hovered around 10% for all samples. to have a quality factor as high as 0.007 Pa1.30 Thus,
However, an increase in deposition time obviously pro- the nanofibers in this study outperformed these com-
moted the filtration performance. Increasing the depos- mercial products.
ition time from 5 to 30 minutes led to a jump of average Figure 8 illustrates the relationship between the fil-
filtration efficiency from 1.8 to 60.4%. As discussed tration efficiency and the pressure drop. The pressure
above, slip flow regime was observed when nanofiber drop increased so much for 10 kV that the rise of the
diameter was less than 1 mm. Thicker nanofibers may be filtration efficiency was negligible. From the results in
one factor that led to low filtration efficiency. Table 4, we knew that a higher voltage led to a greater
It can be seen from Figure 7 that the filtration qua- average fiber diameter. It also led to the increase in
lities corresponding to the 15% CA sample and 20% pressure drop. The same was true for 12 kV, which
CA concentrations are close to each other. Table 3 and showed a sharp increase in filtration efficiency but a
Table 4 show that a lower concentration resulted in relatively small increase in filter quality factor. On the
finer fibers. Thinner fibers can be deposited for a other hand, the increase in the filtration efficiency of the
longer time than thick ones without restricting the air thinner fibers for 8 kV led to an equivalent increase of
flow to a point that the pressure drop overcomes the the filtration quality factor. All these results suggest
gain in filtration efficiency. that the filter with thicker fibers may be more efficient
in capturing nanoparticles, but they also have
high solidity, which led to a high pressure drop.
Effects of applied voltage on filtration performance Furthermore, the slipping effect reduces the pressure
Figure 8 shows the effects of applied voltage on the drop for finer fibers. This finding matches the theory
total filtration efficiency and quality factor. For a described by the models summarized by Hinds.29,31
given deposition time, the filtration efficiency increases Notable differences are samples CA15_5_12_10 and
with increasing applied voltage. The corresponding CA15_15_12_10, which show consistently high filtra-
concentration was 15 wt.% with a tip-to-collector dis- tion efficiencies with only a minor dip at 100 nm.
tance of 10 cm. A similar trend was also observed in Figures 6 to 8 also show the effects of deposition
terms of the quality factor of the media. This trend in time on filtration performance. The circles, squares
filtration efficiency is clearly observed for all deposition and rectangles stand for short, medium and long depos-
times. As the voltage increased from 8 to 12 kV, the ition times, respectively. All three graphs show that a
filtration efficiency approached 100%. For example, short deposition time corresponds to low filtration effi-
for the deposition time of 15 min, the filtration effi- ciencies, while a long deposition time corresponds to
ciency for the 10 kV sample was 36.7% and was high filtration efficiencies. The higher filtration effi-
99.3% for the 12 kV sample. As seen in Figure 8, ciency is attributed to the thicker filter resulting from
higher applied voltages require shorter deposition a longer electrospinning time. However, as expected,
times to make filters with filtration efficiencies > 99%. the increased amounts of deposited fibers lead to a
The local maximum filtration quality factor was higher pressure drop. Nonetheless, the overall filtration
0.06 Pa1, while the maximum quality factor for all quality is still the highest for all samples made with a
was 0.027 Pa1. Commercial filters have been found long deposition time.

(a) (b)
1 0.1
CA15_5_8_10
CA15_5_8_1
Quality Factor [Pa-1]

0.8 0.08
0 CA15_15_8_1
Efficiency [-]

CA15_15_8_
0.6 0.06 0
10
CA15_30_8_ CA15_30_8_1
0.4 10 0.04 0
CA15_5_10_
0.2 10 0.02

0 0
10 100 1000 10 100 1000
Parcel size [nm] Parcel size [nm]

Figure 8. (a) Filtration efficiency and (b) quality factor depending on applied voltage.
12 Textile Research Journal 0(00)

Conclusions 4. Cetiner S, Kalaoglu F, Karakas H, et al. Electrospun


The results of this paper show that applied voltage, tip- nanofibers of polypyrrole-poly (acrylonitrile-co-vinyl
to-collector distance, CA concentration and deposition acetate). Text Res J 2010; 80: 1784–1792.
time in electrospinning affects the size of the resulting 5. Bagherzadeh R, Latifi M, Najar SS, et al. Transport
nanofibers and the consequent filtration quality factors. properties of multi-layer fabric based on electrospun
nanofiber mats as a breathable barrier textile material.
With CA concentrations of 15% or less, beads were
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formed during the electrospinning process, regardless
6. Nayak R, Padhye R, Kyratzis IL, et al. Effect of viscosity
of other electrospinning parameters. A higher CA con- and electrical conductivity on the morphology and fiber
centration resulted in larger fiber diameters, likely due diameter in melt electrospinning of polypropylene. Text
to the increased viscosity. Res J 2013; 83: 606–617.
Furthermore, a longer tip-to-collector distance and 7. Kang W, Cheng B, Li Q, et al. A new method for pre-
higher applied voltage also led to larger fiber diameters. paring alumina nanofibers by electrospinning technology.
The impacts of the tip-to-collector distance and voltage Text Res J 2011; 81: 148–155.
are comparable with respect to the increase in fiber 8. Liu W and Adanur S. Properties of electrospun polyacry-
diameter. lonitrile membranes and chemically-activated carbon
Finally, the larger the fiber diameters the higher the nanofibers. Text Res J 2010; 80: 124–134.
filtration efficiency. The increased filtration efficiency 9. Hekmati AH, Rashidi A, Ghazisaeidi R, et al. Effect of
did not necessarily mean a higher filtration quality needle length, electrospinning distance, and solution
factor, especially for filters obtained via a longer depos- concentration on morphological properties of polya-
mide-6 electrospun nanowebs. Text Res J 2013; 83:
ition time. The maximum filtration efficiency was
1452–1466.
99.8% for filters made with an overall deposition time
10. Gowri S, Almeida L, Amorim T, et al. Polymer nano-
of 30 minutes. The maximum filter quality factor was composites for multifunctional finishing of textiles -
0.05 Pa1 for a filter corresponding to a CA concentra- A review. Text Res J 2010; 80: 1290–1306.
tion of 20 wt.%, a tip-to-collector distance of 12.5 cm, a 11. Angammana CJ. A study of the effects of solution and
voltage of 8 kV and a deposition time of 5 minutes. process parameters on the electrospinning process and
nanofibre morphology. PhD Thesis, University of
Waterloo, Canada, 2011.
Declaration of conflicting interests
12. Liang H-W, Wang L, Chen P-Y, et al. Carbonaceous
The authors declared no potential conflicts of interest with nanofiber membranes for selective filtration and separ-
respect to the research, authorship and/or publication of this ation of nanoparticles. Adv Mater 2010; 22: 4691–4695.
article. 13. Wang C-S and Otani Y. Removal of nanoparticles from
gas streams by fibrous filters: A review. Ind Eng Chem
Funding Res 2012; 52: 5–17.
14. Givehchi R. Filtration of NaCl and WOx nanoparticles
The authors disclosed receipt of the following financial
using wire screens and nanofibrous filters. PhD Thesis,
support for the research, authorship, and/or publication of
University of Waterloo, Canada, 2016.
this article: This work was supported by the Natural
15. Givehchi R, Li Q and Tan Z. Quality factors of PVA
Sciences and Engineering Research Council of Canada,
nanofibrous filters for airborne particles in the size
the Canadian Foundation for Innovation, the International
range of 10–125 nm. Fuel 2016; 181: 1273–1280.
S&T Cooperation Program of China (Grant Number
16. Givehchi R and Tan Z. The effect of capillary force on
2015DFG61910) and the OntarioChina Research and
airborne nanoparticle filtration. J Aerosol Sci 2015; 83:
Innovation Fund (OCRIF-2014).
12–24.
17. Ding B, Kimura E, Sato T, et al. Fabrication of blend
ORCID iD biodegradable nanofibrous nonwoven mats via multi-jet
Zhongchao Tan http://orcid.org/0000-0001-7922-8291 electrospinning. Polymer 2004; 45: 1895–1902.
18. Satyanarayana KG, Arizaga GG and Wypych F.
Biodegradable composites based on lignocellulosic
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