nanomaterials

Article
Effects of Electrospinning Parameters on the Microstructure of
PVP/TiO2 Nanofibers
Wan-Tae Kim 1,2 , Dong-Cheol Park 1,3 , Wan-Hee Yang 3 , Churl-Hee Cho 4, * and Won-Youl Choi 1,2, *

1 Department of Advanced Materials Engineering, Gangneung-Wonju National University, Gangneung,

Gangwon 25457, Korea; kwt3809@gmail.com (W.-T.K.); cufe2000@naver.com (D.-C.P.)
2 Research Institute for Dental Engineering, Gangneung-Wonju National University, Gangneung,
Gangwon 25457, Korea
3 WITH M-TECH Co., Ltd., Suwon, Gyeonggi 16229, Korea; dangchan74@empas.com
4 Graduate School of Energy Science and Technology, Chungnam National University, Daejeon 34134, Korea
* Correspondence: choch@cnu.ac.kr (C.-H.C.); cwy@gwnu.ac.kr (W.-Y.C.);
Tel.: +82-42-821-8606 (C.-H.C.); +82-33-640-2483 (W.-Y.C.)

Abstract: Titanium dioxide has excellent chemical, electrical, and optical properties, as well as
good chemical stability. For that reason, it is widely used in many fields of study and industry,
such as photocatalysts, organic solar cells, sensors, dental implants, and other applications. Many
nanostructures of TiO2 have been reported, and electrospinning is an efficient practical technique
that has a low cost and high efficiency. In various studies on improving performance, the researchers
created nanofibers with suitable microstructures by changing various properties and the many
process parameters that can be controlled. In this study, PVP/TiO2 nanofibers were fabricated by the
electrospinning process. The diameters of the nanofibers were controlled by various parameters. To



understand the effects on the diameter of the nanofibers, various process parameters were controlled:


the molecular weight and concentration of the polymers, deionized water, applied voltage, fluid
Citation: Kim, W.-T.; Park, D.-C.;
velocity, and concentration of titanium precursor. The average diameter of the PVP nanofibers was
Yang, W.-H.; Cho, C.-H.; Choi, W.-Y.
controlled in a range of 42.3 nm to 633.0 nm. The average diameter of the PVP/TiO2 nanofibers was
Effects of Electrospinning Parameters
also controlled in a range of 63.5 nm to 186.0 nm after heat treatment.
on the Microstructure of PVP/TiO2
Nanofibers. Nanomaterials 2021, 11,
Keywords: electrospinning; TiO2 ; PVP; nanofiber
1616. https://doi.org/10.3390/
nano11061616

Academic Editor: Vincenzo Vaiano

1. Introduction
Received: 26 May 2021 Titanium dioxide has excellent chemical, electrical, and optical properties, as well as
Accepted: 18 June 2021 chemical stability. For that reason, it is widely used in many fields of study and industry,
Published: 20 June 2021 such as photocatalysts, organic solar cells, sensors, dental implants, and other applica-
tions [1–14]. It is a very useful material and is commonly used for photocatalysts due to its
Publisher’s Note: MDPI stays neutral photoactivity, high stability, low cost, and safety for the environment and humans [7,15,16].
with regard to jurisdictional claims in Many nanostructures of TiO2 have been reported with improved properties, for example,
published maps and institutional affil- nanoparticles, nanofibers, and nanotubes [4,5,7,9–12,17–23]. These nanostructures are
iations.
fabricated by the sol-gel method, hydrothermal treatment, anodic oxidation, and electro-
spinning [13,17,18,23–28]. With their large specific area and semiconductor properties,
electrospun TiO2 nanofibers are being researched in many fields, such as photocatalysts,
solar cells, and metal oxide gas sensors [4,9,18,29–35]. Electrospinning is an efficient practi-
Copyright: © 2021 by the authors. cal technique that is low cost and has a high efficiency, and many studies have reported
Licensee MDPI, Basel, Switzerland. the production of various nanofibers [4,9,18–23,36–38]. In electrospinning, the precursor
This article is an open access article solution flows at a constant rate through a pump, in such a way as to create a continuous
distributed under the terms and nanofiber, and then electrodes are connected to the inflowing electrospinning solution,
conditions of the Creative Commons
while other electrodes are connected to the appliance plate. At this time, if a high voltage is
Attribution (CC BY) license (https://
applied, it is emitted in a conical shape by surface tension at the end of the electrospinning
creativecommons.org/licenses/by/
solution [23,26–28,39]. The charge is subsequently stored in the electrospinning solution,
4.0/).

Nanomaterials 2021, 11, 1616. https://doi.org/10.3390/nano11061616 https://www.mdpi.com/journal/nanomaterials

Nanomaterials 2021, 11, 1616 2 of 15

and mutual repulsion causes the cone to be radiatively stretched to a jet when the surface
tension of the electrospinning solution is exceeded. In the radiation-stretched electrospin-
ning solution, volatilization of the solvent occurs before it collects in the plate, which can
result in disorderly arranged nanofibers in the plate. The diameter of nanofibers is con-
trolled by the influence of these various instabilities. When applying nanofibers to be used
in various studies, to improve performance, nanofibers with suitable microstructure are
needed to change various properties, and many process parameters need to be controlled.
In this study, polyvinyl pyrrolidone (PVP)/TiO2 nanofibers were fabricated by an elec-
trospinning process. To understand their effects on the diameter of the nanofibers, various
process parameters were controlled: the molecular weight and concentration of polymer
and deionized water (DI water), applied voltage, fluid velocity, and concentration of the
titanium precursor. For a rheological study, viscosity was observed using a viscometer. The
morphology, diameter, and properties of the nanofibers were measured and compared by
field emission scanning electron microscope (FE-SEM), thermogravimetric analysis (TGA),
and X-ray diffractometer (XRD).

2. Materials and Methods

PVP (molecular weight 8000 g/mol, 58,000 g/mol, 1,300,000 g/mol) was purchased
from Alfa Aesar Korea Co., Ltd. (Incheon, Korea). Ethanol (EtOH) was purchased
from Samchun Chemical Co., Ltd. (Seoul, Korea). Acetyl acetone (ACAC) and titanium
4-isopropoxide (TTIP) were purchased from Junsei Co., Ltd. (Tokyo, Japan).
To compare the microstructure of different molecular weights of PVP, electrospinning
solutions containing 10 wt% PVP with three different molecular weights (8000 g/mol,
58,000 g/mol, and 1,300,000 g/mol) in EtOH were prepared. After solution preparation,
the samples were loaded into a plastic syringe and connected to a needle. The spinning
needle diameter was about 0.337 mm, the fluid velocity was maintained at 0.2 mL/h,
and a voltage of 20 kV was applied to the spinning solution by a direct current power
supply. To compare the microstructure with different PVP concentrations, 5 ethanol
solutions containing 2~10 wt% PVP (1,300,000 g/mol) samples were loaded into a plastic
syringe and connected to the needle. The spinning needle diameter was about 0.337 mm,
the fluid velocity was maintained at 0.2 mL/h, and a voltage of 20 kV was applied to
the spinning solution. Viscosities of PVP solutions were measured and compared by
viscometer (LVT, AMETEK Brookfield, Middleboro, MA, USA) with different molecular
weight and concentrations.
To compare the microstructure for different DI water concentrations, a 10:0~0:10 ratio
of EtOH and DI water solution containing 10 wt% PVP (1,300,000 g/mol) was electrospun
under the following conditions: 20 kV applied voltage, 0.337 mm needle diameter, and
0.2 mL/h fluid velocity. Viscosities were measured and compared with a viscometer.
To compare the microstructure with different applied voltages and fluid velocities, PVP
nanofibers were prepared under the conditions of 10 wt% PVP (1,300,000 g/mol) in ethanol
and 0.337 mm nozzle inner diameter by varying the process voltage from 10~20 kV and
the flow rate from 0.2~1.0 mL/h.
Raw PVP (1,300,000 g/mol), PVP nanofibers, and PVP/TiO2 nanofibers were com-
pared by TGA (STA 409, Q500, NETZSCH Korea Co., Ltd., Paju, Korea) analysis in a
nitrogen atmosphere up to 600 ◦ C, and PVP/TiO2 nanofibers up to 600 ◦ C in nitrogen and
oxygen atmospheres. PVP nanofibers were prepared by electrospinning under conditions
of 10 wt% PVP (1,300,000 g/mol) in ethanol, a 0.337 mm nozzle inner diameter, 20 kV
voltage, and 1.0 mL/h fluid velocity; and PVP/TiO2 nanofibers were prepared by electro-
spinning under conditions of 5 wt% TTIP, 5 wt% ACAC and 10 wt% PVP in 8:2 mixtures of
EtOH and DI water, a 0.337 mm nozzle inner diameter, 20 kV voltage, and 0.2 mL/h fluid
velocity. The heat treatment temperature was determined through TGA analysis and heat
treatment was performed at 450 ◦ C for 3 h in an air atmosphere. After heat treatment and
crystallization, the crystal structures were analyzed by XRD (AXS-D8, Bruker Korea Co.,
Ltd., Gyeonggi, Korea).
Nanomaterials 2021, 11, 1616 3 of 15

To observe the changes in the microstructure of PVP/TiO2 nanofibers by the differ-

ence in fluid velocity and titanium precursor concentration, PVP/TiO2 nanofibers were
fabricated by electrospinning under conditions of 5 wt% TTIP, 5 wt% ACAC and 10 wt%
PVP (1,300,000 g/mol) in 8:2 mixtures of EtOH and DI water, a 0.337 mm nozzle inner
diameter, 20 kV voltage, and 0.1~1.0 mL/h fluid velocity. By varying the weight ratio
of TTIP and ACAC to 5:5, 3:7, and 1:9, an 8:2 ratio of ethanol and DI water solution con-
taining 10 wt% TTIP/ACAC and 10 wt% PVP (1,300,000 g/mol) was used at a voltage of
20 kV, fluid velocity of 0.1 mL/h, and nozzle inner diameter of 0.337 mm under conditions
of electrospinning.
After electrospinning and heat treatment, microstructural changes were measured
and compared before and after heat treatment by FE-SEM (Inspect F, FEI Korea Co., Ltd.,
Gyeonggi, Korea).

3. Results and Discussion

Figure 1 shows FE-SEM images of nanoparticles, nanofibers, and viscosities with
different PVP molecular weights of electrospinning solution. When the electrospinning
solution contained PVP with a molecular weight of 8000 g/mol and 58,000 g/mol, it formed
a shape close to spherical particles, and their average diameters were about 1850.8 nm and
527.6 nm, respectively. When the electrospinning solution contained PVP with a molecular
weight of 1,300,000 g/mol, it formed in the shape of nanofibers, and their average diameter
was about 339.0 nm. The viscosities of PVP solution of 8000 g/mol, 58,000 g/mol, and
1,300,000 g/mol PVP molecular weight were 3.5 cP, 7.8 cP, and 184.0 cP, respectively.

Figure 1. FE-SEM images of nanoparticles and nanofibers with different PVP molecular weights: (a) 8000 g/mol,
(b) 58,000 g/mol, (c) 1,300,000 g/mol, and (d) dynamic viscosity.

Figure 2 shows FE-SEM images of mixed microstructures with beads and nanofibers
as the PVP (1,300,000 g/mol) concentration changes from 2 wt% to 10 wt%, and Figure 3
021, 11, x FOR PEER REVIEW 4 of 15

Nanomaterials 2021, 11, 1616 4 of 15

shows the average diameters of the beads and nanofibers, and viscosities. In a PVP con-
centration range of 2 wt% to 8 wt%, beads formed, and their number decreased with in-
creasing PVP concentration. The average diameters of the beads in 2 wt%, 4 wt%, 6 wt%,
shows the average
and 8 wt% PVP concentrations were diameters
702.3 nm, of the beadsnm,
1118.0 and 1163.1
nanofibers,
nm,and
andviscosities.
1419.3 nm, In are-
PVP concen-
spectively. The average diameters of the nanofibers increased with increased PVP concen- increasing
tration range of 2 wt% to 8 wt%, beads formed, and their number decreased with
PVP concentration. The average diameters of the beads in 2 wt%, 4 wt%, 6 wt%, and 8 wt%
tration. The values at 2 wt%, 4 wt%, 6 wt%, 8 wt%, and 10 wt% PVP concentration were
PVP concentrations were 702.3 nm, 1118.0 nm, 1163.1 nm, and 1419.3 nm, respectively.
66.5 nm, 114.8 nm,The 202.8 nm, 278.7 nm, and 305.7 nm, respectively. The viscosities of PVP
average diameters of the nanofibers increased with increased PVP concentration. The
solution at 2 wt%,values
4 wt%, at62wt%,
wt%, 84 wt%,
wt%, and6 wt%,10 wt%
8 wt%, PVP
andconcentration were 8.5 cP, 19.0
10 wt% PVP concentration were 66.5 nm,
cP, 44.0 cP, 86.0 cP,
114.8 nm, 202.8 nm, 278.7 nm, and 305.7 nm, respectively. The viscositiessolution
and 184.0 cP, respectively. The viscoelasticity of the polymer of PVP solution at
competes with the2 Rayleigh
wt%, 4 wt%, instability
6 wt%, 8 and wt%,isandconventionally determined by
10 wt% PVP concentration werethe8.5polymer
cP, 19.0 cP, 44.0 cP,
concentration or 86.0
molecular weight.
cP, and 184.0 Increasing The
cP, respectively. theviscoelasticity
polymer concentration
of the polymerorsolution
entangle-
competes with
the Rayleigh instability and is conventionally determined by
ments in the solution causes particle electrospray to transit to fiber electrospinning, with the polymer concentration or
molecular weight. Increasing the polymer concentration
beads-on-strings morphologies, as a result of the incomplete suppression of the Rayleigh or entanglements in the solution
causes particle electrospray to transit to fiber electrospinning, with beads-on-strings mor-
instabilities [40]. The molecular weight of the polymer has a significant effect on the rhe-
phologies, as a result of the incomplete suppression of the Rayleigh instabilities [40]. The
ological and electrical properties, such as viscosity, surface tension, conductivity, and di-
molecular weight of the polymer has a significant effect on the rheological and electrical
electric strength. This is another
properties, suchimportant
as viscosity,solution parameter
surface tension, that affects
conductivity, andthe morphology
dielectric strength. This is
of electrospun fibers,
another important solution parameter that affects the morphologyhave
and generally high molecular weight polymer solutions been
of electrospun fibers,
used in electrospinning as they
and generally provide
high molecularthe weight
desiredpolymer
viscosity for fiber
solutions havegeneration.
been used inItelectrospinning
has
been observed that asathey
solution with
provide thetoo low aviscosity
desired molecular forweight tends to form
fiber generation. beads
It has beenrather
observed that a
solution with too low a molecular weight tends to form
than fibers, and a high molecular weight solution gives fibers with larger average diame- beads rather than fibers, and a
ters. The molecular weight of the polymer reflects the number of entanglements of the molecular
high molecular weight solution gives fibers with larger average diameters. The
polymer chains inweight of the polymer reflects the number of entanglements of the polymer chains in a
a solution, and thus solution viscosity. Chain entanglement plays an
solution, and thus solution viscosity. Chain entanglement plays an important role in the
important role in the process of electrospinning. To fabricate nanofiber, the entanglement
process of electrospinning. To fabricate nanofiber, the entanglement of the polymer chains
of the polymer chains
must be must be of sufficient
of sufficient viscosity to viscosity to createjet,a otherwise
create a uniform uniform particles
jet, otherwise
and bead shapes
particles and beadwillshapes will be [26,41,42].
be produced produced [26,41,42].

2. FE-SEM
FigureFigure images of
2. FE-SEM mixed of
images microstructures with beads and
mixed microstructures nanofibers,
with beads and with different PVP
nanofibers, concentrations:
with different PVP(a) 2 wt%,
(b) 4 wt%, (c) 6 wt%, (d) 8 wt%, and (e) 10 wt%.
concentrations: (a) 2 wt%, (b) 4 wt%, (c) 6 wt%, (d) 8 wt%, and (e) 10 wt%.
 Nanomaterials 2021, 11, x FOR PEER REVIEW
Nanomaterials 2021, 11, 1616 5 of 15

Figure 3. (a)
Figure 3. (a) Average Averageof
diameter diameter
beads of
andbeads and nanofibers,
nanofibers, (b) viscosities
(b) viscosities withwith differentPVP
different PVP concentrations.
concentrations.
Figure 4 shows FE-SEM images of mixed microstructures with beads and nanofibers
with variousFigure
weight 4ratios
shows FE-SEM
of EtOH to DIimages
water inofsolvents,
mixed and microstructures
Figure 5 showswith their beads
averageand nano
withand
diameters various weight
viscosities ratios
of PVP of EtOH
solution. Theto DI water
diameter in solvents,
of the nanofibersand Figurewith
decreased 5 shows th
erage diameters
an increasing ratio of DIandwaterviscosities of PVPfrom
in the solvents solution. TheThe
0 to 10. diameter
averageofdiameters
the nanofibers
of dec
nanofibers
withinan10:0, 8:2, 5:5, 2:8,
increasing and
ratio of 0:10 were 314.6
DI water in thenm, 227.0 nm,
solvents from140.3
0 tonm,
10.75.0
Thenm, and diame
average
42.3 nm, respectively. The viscosities of PVP solution in 10:0, 8:2,
nanofibers in 10:0, 8:2, 5:5, 2:8, and 0:10 were 314.6 nm, 227.0 nm, 140.3 nm, 5:5, 2:8, and 0:10 of 75.0 nm
solution weight ratio were 184.0 cP, 375.0 cP, 329.0 cP, 280.0 cP, and 134.0 cP,
42.3 nm, respectively. The viscosities of PVP solution in 10:0, 8:2, 5:5, 2:8, and 0:10 orespectively.
When the ratio of DI water was increased, the diameters of the nanofibers were decreased.
tion weight ratio were 184.0 cP, 375.0 cP, 329.0 cP, 280.0 cP, and 134.0 cP, respec
When the ratio of DI water was greater than 5:5, beads formed, and the number of beads
When
increased withtheanratio of DI water
increasing amount was increased,
of DI water. Waterthe diameters
has a higher of dielectric
the nanofibers were decr
constant
When
and dipole the ratio
moment thanofethanol,
DI water whichwasmeans
greater
the than 5:5,water
jet using beadsasformed,
a solventand the number of
is subjected
increased with an increasing amount of DI water. Water has
to a stronger elongation force. On the other hand, the dryness of the electrospun fibers a higher dielectric co
andwith
increases dipole
the moment
decreasing than ethanol,
density which point
and boiling means ofthe
the jet using water
solvents. as a solvent is sub
The evaporation
of the solvent systemselongation
to a stronger richer in water wasOn
force. much
the slower than those
other hand, the richer
dryness in ethanol, due
of the electrospun
to the higher
increases with the decreasing density and boiling point of the solvents. the
density and boiling point of water. Thus, the viscoelastic force acting on The evapo
chargedof jet
therapidly
solvent increased
systemswith increasing
richer in water ethanol content
was much in a mixed
slower than solvent, due toin ethano
those richer
to the higher density and boiling point of water. Thus, the viscoelastic force acting
charged jet rapidly increased with increasing ethanol content in a mixed solvent,
the extremely rapid solvent evaporation. As soon as the viscoelastic force exceed
 Nanomaterials 2021, 11, 1616 6 of 15
Nanomaterials 2021, 11, x FOR PEER REVIEW 6 of 15

the extremely rapid solvent evaporation. As soon as the viscoelastic force exceeded the
Coulomb
Coulomb force,
force,the
thejets
jets could notbebestretched
could not stretchedanyany further,
further, andfibers
and the the fibers were subjected
were subjected to
to aa smaller elongation
smaller elongation force
force forfor a shorter
a shorter timetime [43,44].
[43,44].

Figure
Figure 4. FE-SEM
4. FE-SEM images
images ofofmixed
mixedmicrostructures
microstructures with beads
with andand
beads nanofibers in various
nanofibers weight ratios
in various weight of EtOH
ratiostoofDIEtOH
water to DI
in solvents (a) 10:0, (b) 8:2, (c) 5:5, (d) 2:8, and (e) 0:10.
water in solvents (a) 10:0, (b) 8:2, (c) 5:5, (d) 2:8, and (e) 0:10.
Figure 6 shows FE-SEM images of electrospun nanofibers with different voltages and
fluid velocities, and Figure 7 shows their average diameters. At an applied voltage of
10 kV, the average diameters of the nanofibers in 0.2 mL/h, 0.4 mL/h, 0.6 mL/h, 0.8 mL/h,
and 1.0 mL/h were 449.7 nm, 515.4 nm, 582.4 nm, 633.0 nm, and 560.0 nm, respectively.
At an applied voltage of 15 kV, the average diameters of the nanofibers in 0.2 mL/h,
0.4 mL/h, 0.6 mL/h, 0.8 mL/h, and 1.0 mL/h were 338.6 nm, 379.2 nm, 406.0 nm, 418.2 nm,
and 484.8 nm, respectively. At an applied voltage of 20 kV, the average diameters of the
nanofibers in 0.2 mL/h, 0.4 mL/h, 0.6 mL/h, 0.8 mL/h, and 1.0 mL/h were 338.1 nm,
369.5 nm, 425.7 nm, 381.0 nm, and 420.7 nm, respectively. When the voltages were 15 kV
and 20 kV, the diameter change of the nanofibers was not large, but the diameter increased
significantly as the voltage decreased to 10 kV. In the electrospinning process, above a
critical voltage, the effect of voltage on the formation of fibers was small. However, at
lower voltage, the instability resulting from the electric field was small and the charge
stress contributing to the elongation of the fibers occurring simultaneously with solvent
volatilization was small. As the fluid velocity decreased, the average diameter of the
nanofibers tended to decrease.
Nanomaterials 2021, 11, 1616 7 of 15
Figure 4. FE-SEM images of mixed microstructures with beads and nanofibers in various weight ratios of EtOH to DI
water in solvents (a) 10:0, (b) 8:2, (c) 5:5, (d) 2:8, and (e) 0:10.

Nanomaterials 2021, 11, x FOR PEER REVIEW 7 of 15

Figure 5. (a) Average diameter of nanofibers, and (b) viscosities with different EtOH and DI water
Figure 5. (a) Average diameter of nanofibers, and (b) viscosities with different EtOH and DI water weight ratios in sol-
vents. weight ratios in solvents.

Figure 6 shows FE-SEM images of electrospun nanofibers with different voltages and
fluid velocities, and Figure 7 shows their average diameters. At an applied voltage of 10
kV, the average diameters of the nanofibers in 0.2 mL/h, 0.4 mL/h, 0.6 mL/h, 0.8 mL/h, and
1.0 mL/h were 449.7 nm, 515.4 nm, 582.4 nm, 633.0 nm, and 560.0 nm, respectively. At an
applied voltage of 15 kV, the average diameters of the nanofibers in 0.2 mL/h, 0.4 mL/h,
0.6 mL/h, 0.8 mL/h, and 1.0 mL/h were 338.6 nm, 379.2 nm, 406.0 nm, 418.2 nm, and 484.8
nm, respectively. At an applied voltage of 20 kV, the average diameters of the nanofibers
in 0.2 mL/h, 0.4 mL/h, 0.6 mL/h, 0.8 mL/h, and 1.0 mL/h were 338.1 nm, 369.5 nm, 425.7
nm, 381.0 nm, and 420.7 nm, respectively. When the voltages were 15 kV and 20 kV, the
diameter change of the nanofibers was not large, but the diameter increased significantly
as the voltage decreased to 10 kV. In the electrospinning process, above a critical voltage,
the effect of voltage on the formation of fibers was small. However, at lower voltage, the
instability resulting from the electric field was small and the charge stress contributing to
the elongation of the fibers occurring simultaneously with solvent volatilization was
small. As the fluid velocity decreased, the average diameter of the nanofibers tended to
decrease.
Nanomaterials 2021, 11, 1616 8 of 15
Nanomaterials 2021, 11, x FOR PEER REVIEW 8 of 15

Figure 6.
Figure 6. FE-SEM
FE-SEM images
images of
of electrospun
electrospun nanofibers
nanofibers with
with different
different voltages
voltages and
andfluid
fluidvelocities.
velocities.
Nanomaterials 2021,
Nanomaterials 11, x1616
2021, 11, FOR PEER REVIEW 99 of
of 15
15

Figure 7. Average diameter of nanofibers with different voltages and fluid velocities.
Figure 7. Average diameter of nanofibers with different voltages and fluid velocities.
Figure 8 shows TGA curves of raw PVP, PVP nanofibers, PVP/TiO2 nanofibers in
Figure atmosphere,
a nitrogen 8 shows TGA andcurves of rawnanofibers
PVP/TiO PVP, PVP in nanofibers,
a nitrogenPVP/TiO 2 nanofibers in a
and oxygen atmosphere.
2
nitrogen atmosphere, and PVP/TiO 2 nanofibers in a nitrogen and oxygen atmosphere.
Compared with raw PVP, electrospun nanofibers contained moisture and organic solvents,
Compared
so the initialwith raw PVP,
weight electrospun
reduction nanofibers
was large. PVP/TiO contained moisture and organic sol-
2 nanofibers containing TTIP and
vents, so the initial weight reduction was large. PVP/TiO 2 nanofibers containing TTIP and
ACAC showed weight loss due to desorption of hydroxyl groups from about 140 ◦ C,
ACAC showed weight
and crystallization loss due
appeared to desorption
from 210 ◦ C. In of
allhydroxyl
the samples,groups
the from about
largest weight 140loss
°C, and
was
crystallization appeared from 210 °C.
◦ In all the
◦ samples, the largest
observed in the range of about 350 C to 450 C, due to PVP decomposition. In addition, weight loss was ob-
served in the range of about 350 °C to 450 °C, due to PVP decomposition.
in a nitrogen atmosphere, PVP was thermally decomposed, and about 5 wt% remained, In addition, in
awhile
nitrogen atmosphere,
PVP/TiO PVP was thermally decomposed, and about 5 wt% remained,
2 nanofibers containing TTIP and ACAC showed a weight reduction of
while
about PVP/TiO
75 wt%. In 2 nanofibers containing
both the nitrogen TTIP and
and oxygen ACAC showed
atmospheres, a weight
the weight reduction
initially of
decreased
about 75 wt%. In both the nitrogen and oxygen atmospheres, the
due to volatilization of the water and organic solvents, and the weight decreased from weight initially de-
creased
about 140 due◦ C
todue
volatilization
to desorptionof theof water
hydroxyland groups,
organic while
solvents, and the weight
crystallization decreased
occurred from
from ◦ about 140 °C due to desorption of hydroxyl groups, while crystallization
210 C. In the nitrogen atmosphere, the weight was reduced by the thermal decomposition occurred
from
of PVP,210and
°C. in
In the oxygen
nitrogenatmosphere,
atmosphere,the thePVP
weightwaswas reduced at
combusted bythe
thesame
thermal timedecom-
as the
position
thermal of PVP, and in the
decomposition, and oxygen atmosphere,
the weight decreased.the These
PVP was combusted atagreed
transformations the samewithtime
the
as the thermal
literature decomposition,
[45–47]. Figure 9 shows andthethe
XRDweight decreased.
spectrum These transformations
of heat-treated agreed
PVP/TiO2 nanofibers.
with the literature
The peaks [45–47].were
of TiO2 anatase Figure 9 shows the XRD spectrum of heat-treated PVP/TiO2
identified.
nanofibers. The peaks of TiO2 anatase were identified.
Nanomaterials
Nanomaterials2021,
2021,11,
11,x1616
FOR PEER REVIEW 1010ofof1515

Figure
Figure8.8.TGA
TGAcurves
curvesof
of(a)
(a)raw
raw PVP, nanofibers,PVP/TiO
PVP, PVP nanofibers, PVP/TiO22 nanofibers
nanofibers in
inaanitrogen
nitrogenatmosphere,
atmos-
phere, and
and (b) (b) PVP/TiO
PVP/TiO 2
2 nanofibers
nanofibers in a in a nitrogen
nitrogen and and
oxygenoxygen atmosphere.
atmosphere.
021, 11, x FOR PEER REVIEW 11 of 15

Nanomaterials
Nanomaterials 2021,
2021, 11,
11, x1616
FOR PEER REVIEW 11
11 of
of 15
15

Figure 9. XRD spectrum of heat-treated PVP/TiO2 nanofibers.

Figure 9.
Figure XRD spectrum
9. XRD spectrum of
of heat-treated
heat-treated PVP/TiO
PVP/TiO2 2nanofibers.
nanofibers.
Figure 10 shows FE-SEM images of PVP/TiO2 nanofibers with different fluid veloci-
Figure
ties before and after heat
Figure 10 shows
10 shows FE-SEM
treatment, and images
Figure
FE-SEM 11 of
images ofPVP/TiO
shows their
PVP/TiO 2 2nanofibers
average
nanofibers with
withdifferent
diameter. Thefluid
different av- velocities
fluid veloci-
before
erage diameter ofties andand
nanofibers
before after heatheat
decreased
after treatment,
with the
treatment,andfluid
Figure
and 11 shows
velocity.
Figure theirtheir
Before
11 shows average diameter.
heataverage
treatment, The average
the
diameter. The av-
diameter of nanofibers
average diametererage diameter
of the nanofibers at decreased
of nanofibers with the
decreased
fluid velocities offluid
with velocity.
0.1the fluid 0.5
mL/h, Before heat
velocity.
mL/h,Before
andtreatment,
heatmL/h
1.0 the average
treatment, the
diameter
average of the
diameter nanofibers at fluid velocities of 0.1 mL/h, 0.5 mL/h, and 1.0 mL/h were
were 311.4 nm, 364.1, and 376.5 of nm,therespectively.
nanofibers at fluid velocities
The values of 0.1
after mL/h,
heat 0.5 mL/h,were
treatment and 1.0 mL/h
311.4 311.4
were nm, 364.1,
nm, and 376.5
364.1, andnm,
376.5 respectively.
nm, The values
respectively. The after heatafter
values treatment
heat were decreased
treatment were
decreased to 120.5tonm,
120.5172.1, and 186.0
nm, 172.1, nm nm
and 186.0 duedue to calcination
to calcination ofofthe
thePVP.
PVP.
decreased to 120.5 nm, 172.1, and 186.0 nm due to calcination of the PVP.

Figure 10. FE-SEM images of PVP/TiO2 nanofibers with different fluid velocities before (a) 0.1
mL/h,
Figure 10. FE-SEM images of (b) 0.5
PVP/TiO mL/h, (c) 1.0
nanofibers mL/h
with and after
different fluidheat treatment
velocities (d) (a)
before 0.10.1
mL/h, (e) 0.5
mL/h, (b) mL/h, (f) 1.0
0.5 mL/h, (c)mL/h.
1.0
Figure 10. FE-SEM images of 2PVP/TiO 2 nanofibers with different fluid velocities before (a) 0.1
mL/h and after heat treatment (d) 0.1 mL/h, (e) 0.5 mL/h, (f) 1.0 mL/h.
mL/h, (b) 0.5 mL/h, (c) 1.0 mL/h and after heat treatment (d) 0.1 mL/h, (e) 0.5 mL/h, (f) 1.0 mL/h.
021, 11, x FOR PEER REVIEW 12 of 15

Nanomaterials
Nanomaterials2021,
2021,11,
11,x1616
FOR PEER REVIEW 12
12of
of15
15

Figure 11. Average diameter of PVP/TiO2 nanofibers with different fluid velocities before and after
heat treatment. Figure11.
Figure Averagediameter
11.Average diameterof
ofPVP/TiO
PVP/TiO nanofiberswith
nanofibers
22 withdifferent
differentfluid
fluidvelocities
velocitiesbefore
beforeand
andafter
after
heattreatment.
heat treatment.
Figure 12 shows FE-SEM images of PVP/TiO2 nanofibers with different weight ratios
Figure12
Figure 12 showsFE-SEM
FE-SEMimages
imagesof ofPVP/TiO
PVP/TiO2 2nanofibers
nanofibers withdifferent
differentweight
weightratios
ratios
of TTIP and ACAC before andshows
after annealing, and Figure 13 shows theirwithaverage diame-
of TTIP and ACAC before and after annealing, and Figure 13 shows their average
of TTIP and ACAC before and after annealing, and Figure 13 shows their average diame- diameters.
ters. Before heat treatment,
Before heatthe average
treatment, diameters
the average of the nanofibers
diameters at TTIP
of theofnanofibers at weight
TTIP ratios
weight ratiosratios
of 1:9,
ters. Before heat treatment, the average diameters the nanofibers at TTIP weight
of 1:9, 3:7, and 5:53:7,
wereand 279.7
5:5 nm,279.7
were 309.3nm,
nm,309.3
and nm,
381.5
andnm, respectively.
381.5 nm, The values
respectively. The after after heat
values
of 1:9, 3:7, and 5:5 were 279.7 nm, 309.3 nm, and 381.5 nm, respectively. The values after
heat treatment wereheat
63.5
treatment nm,
were
treatment
102.2
63.5nm,
were nm, and
63.5
126.6
102.2102.2
nm, nm, andnm.and
The126.6
nm, 126.6
reduction
nm. The was due
nm. reduction was
The reduction
todue
the due
was to
calci-
thetocalcination
the calci-
nation of PVP through
of PVP heat treatment.
through heat The average
treatment. The diameters
average decreased
diameters with
decreased decreasing
with decreasing
nation of PVP through heat treatment. The average diameters decreased with decreasing TTIP
TTIP weight ratio. weight ratio.
TTIP weight ratio.

Figure 12. FE-SEM images of PVP/TiO2 nanofibers with different weight ratios of TTIP and ACAC
before (a) 1:9, (b) 3:7, (c) 5:5 and after annealing (d) 1:9, (e) 3:7, (f) 5:5.
FigureFigure 12. FE-SEM
12. FE-SEM images ofimages
PVP/TiOof PVP/TiO 2 nanofibers with different weight ratios of TTIP and ACAC
2 nanofibers with different weight ratios of TTIP and ACAC before (a) 1:9, (b) 3:7,
before (a) 1:9, (b) 3:7, (c) 5:5 and after
(c) 5:5 and after annealing (d) 1:9, (e) 3:7, (f) 5:5. annealing (d) 1:9, (e) 3:7, (f) 5:5.
Nanomaterials
Nanomaterials 2021,
2021, 11,
11, x1616
FOR PEER REVIEW 13
13 of
of 15
15

Figure13.
Figure Average diameter
13.Average diameter of
of PVP/TiO nanofibers with
PVP/TiO22 nanofibers with different
different weight
weight ratios
ratiosof
ofTTIP
TTIPand
andACAC
before before
ACAC and after
andheat treatment.
after heat treatment.

Many process
Many process parameters
parameterscan affect
can the the
affect microstructure of PVP/TiO
microstructure 2 nanofibers.
of PVP/TiO More-
2 nanofibers.
over, the microstructure of TiO
Moreover, the microstructure of nanofibers can affect their optical, mechanical, and photo-
2 TiO2 nanofibers can affect their optical, mechanical, and
catalytic properties [48–51].
photocatalytic properties [48–51].
4. Conclusions
4. Conclusions
To fabricate various nanostructured PVP and PVP/TiO2 nanofibers by electrospinning,
To fabricate
we controlled somevarious
process nanostructured PVP and
parameters, namely, PVP/TiO2 weight
the molecular nanofibers by electrospin-
and concentration of
ning,
PVP, DI water weight ratio in the solvent, applied voltage, fluid velocity, and and
we controlled some process parameters, namely, the molecular weight TTIPconcen-
weight
tration of PVP,
ratio. With DI waterinweight
an increase the DI ratio
waterinratio
the solvent, appliedinvoltage,
and a decrease fluid velocity,
the molecular weight and
and
TTIP weight ratio.
concentration Withthe
of PVP, anaverage
increasediameters
in the DI water
of theratio
PVP and a decrease
nanofibers andinspherical
the molecular
shape
weight and concentration
formations decreased. With of PVP, the average
a decrease diameters
in fluid ofand
velocity the PVP nanofibers
an increase andapplied
in the spher-
ical shape formations decreased. With a decrease in fluid velocity and
voltage, the average diameter of the PVP nanofibers decreased. The average diameter an increase in the
applied
was reduced due to the calcination of PVP through heat treatment. The diameter of di-
voltage, the average diameter of the PVP nanofibers decreased. The average the
ameter
PVP/TiO was nanofibers
reduced due wasto decreased
the calcination
by a of PVP through
decrease in the heat
fluidtreatment.
velocity TheTTIP
and diameter
ratio.
2
of
Wethe PVP/TiO2innanofibers
succeeded controlling wasthedecreased by a decrease
nanostructure in the fluid
of the PVP/TiO velocity and TTIP
2 nanofibers using the
ratio. Weparameters,
process succeeded inandcontrolling the nanostructure
the resulting nanofibers are of the PVP/TiO2appropriate
nanostructures nanofibers using the
for many
process parameters, and the resulting nanofibers are nanostructures
applications, such as photocatalysts, solar cells, sensors, and filters. appropriate for many
applications, such as photocatalysts, solar cells, sensors, and filters.
Author Contributions: Conceptualization, D.-C.P. and W.-Y.C.; methodology, W.-T.K.; validation,
Author
W.-T.K.;Contributions:
formal analysis,Conceptualization, D.-C.P.
W.-T.K.; investigation, and resources,
W.-T.K.; W.-Y.C.; methodology, W.-T.K.;
W.-H.Y. and W.-Y.C.; validation,
data curation,
W.-T.K.;
W.-T.K.; formal analysis, W.-T.K.;
writing—original investigation,W.-T.K.;
draft preparation, W.-T.K.;writing—review
resources, W.-H.Y.andand W.-Y.C.;
editing, data and
C.-H.C. cu-
ration, W.-T.K.;
W.-Y.C.; writing—original
visualization, draft preparation,
W.-T.K.; supervision, W.-T.K.;
C.-H.C. and writing—review
W.-Y.C.; and editing,
project administration, C.-H.C.
W.-H.Y. and
and W.-Y.C.;
W.-Y.C.; visualization,
funding W.-T.K.;
acquisition, D.-C.P. supervision, C.-H.C.
and W.-Y.C. All andhave
authors W.-Y.C.; project
read and administration,
agreed W.-
to the published
H.Y. andofW.-Y.C.;
version funding acquisition, D.-C.P. and W.-Y.C. All authors have read and agreed to the
the manuscript.
published version of the manuscript.
Funding: This work was supported by the Korea Institute of Energy Technology Evaluation and
Funding: This workthe
Planning (KETEP), was supported
Ministry by the
of Trade, Korea and
Industry Institute of (MOTIE)
Energy Energy Technology Evaluation and
(Grant No. 20181110200070)
Planning (KETEP),
and the National the Ministry
Research Foundation ofof Trade, Industry
Korea (Grant and Energy (MOTIE) (Grant No.
No. 2019R1I1A3A01057765).
20181110200070) and the National Research Foundation of Korea (Grant No.
Institutional Review Board Statement: Not applicable.
2019R1I1A3A01057765).
Informed Consent
Institutional Statement:
Review Not applicable.
Board Statement: Not applicable.
Acknowledgments:
Informed The authors
Consent Statement: Notthank the researcher (Jung-Woo Lee) of WITH M-TECH Co., for
applicable.
their time and contributions to the study.
Acknowledgments: The authors thank the researcher (Jung-Woo Lee) of WITH M-TECH Co., for
Conflicts
their of Interest:
time and The authors
contributions to the declare
study. no conflict of interest.
Conflicts of Interest: The authors declare no conflict of interest.
Nanomaterials 2021, 11, 1616 14 of 15

References
1. Kubiak, A.; Siwińska-Ciesielczyk, K.; Bielan, Z.; Zielińska-Jurek, A.; Jesionowski, T. Synthesis of highly crystalline photocatalysts
based on TiO2 and ZnO for the degradation of organic impurities under visible-light irradiation. Adsorption 2019, 25, 309–325.
[CrossRef]
2. Shayegan, Z.; Lee, C.-S.; Haghighat, F. TiO2 photocatalyst for removal of volatile organic compounds in gas phase—A review.
Chem. Eng. J. 2018, 334, 2408–2439. [CrossRef]
3. Ohno, T.; Sarukawa, K.; Tokieda, K.; Matsumura, M. Morphology of a TiO2 photocatalyst (Degussa, P-25) consisting of anatase
and rutile crystalline phases. J. Catal. 2001, 203, 82–86. [CrossRef]
4. Kim, W.-T.; Hwang, T.-H.; Choi, W.-Y. Composite photoelectrode with TiO2 nanofibers and nanoparticles in dye-sensitized solar
cells. Sci. Adv. Mater. 2018, 10, 210–214. [CrossRef]
5. Hwang, T.-H.; Kim, W.-T.; Choi, W.-Y. Mixed dimensionality with a TiO2 nanostructure and carbon nanotubes for the photoelec-
trode in dye-sensitized solar cells. J. Nanosci. Nanotechnol. 2017, 17, 4812–4816. [CrossRef]
6. Jeon, N.J.; Noh, J.H.; Yang, W.S.; Kim, Y.C.; Ryu, S.; Seo, J.; Seok, S.I. Compositional engineering of perovskite materials for
high-performance solar cells. Nature 2015, 517, 476–480. [CrossRef]
7. Mor, G.K.; Varghese, O.K.; Paulose, M.; Shankar, K.; Grimes, C.A. A review on highly ordered, vertically oriented TiO2 nanotube
arrays: Fabrication, material properties, and solar energy applications. Sol. Energy Mater Sol. Cells 2006, 90, 2011–2075. [CrossRef]
8. Grätzel, M. Dye-sensitized solar cells. J. Photochem. Photobiol. C 2003, 4, 145–153. [CrossRef]
9. Kim, W.-T.; Na, K.-H.; Park, D.-C.; Yang, W.-H.; Choi, W.-Y. Photocatalytic Methylene Blue Degradation of Electrospun Ti–Zn
Complex Oxide Nanofibers. Nanomaterials 2020, 10, 1311. [CrossRef]
10. Kim, W.-T.; Kim, I.-H.; Choi, W.-Y. Fabrication of TiO2 nanotube arrays and their application to a gas sensor. J. Nanosci. Nanotechnol.
2015, 15, 8161–8165. [CrossRef]
11. Kim, W.-T.; Na, K.-H.; Lee, J.-K.; Jang, I.; Choi, D.-S.; Choi, W.-Y. Porous TiO2 Nanotube Arrays for Drug Loading and Their
Elution Sensing. J. Nanosci. Nanotechnol. 2019, 19, 1743–1748. [CrossRef]
12. Kim, W.-T.; Choi, W.-Y. Optical interference of TiO2 nanotube arrays for drug elution sensing. Sci. Adv. Mater. 2018, 10, 283–287.
[CrossRef]
13. Kim, W.-T.; Choi, W.-Y. Fabrication of TiO2 photonic crystal by anodic oxidation and their optical sensing properties. Sens.
Actuator A Phys. 2017, 260, 178–184. [CrossRef]
14. Mustafa, K.; Wroblewski, J.; Lopez, B.S.; Wennerberg, A.; Hultenby, K.; Arvidson, K. Determining optimal surface roughness of
TiO2 blasted titanium implant material for attachment, proliferation and differentiation of cells derived from human mandibular
alveolar bone. Clin. Oral Implant. Res. 2001, 12, 515–525. [CrossRef]
15. Bavykin, D.V.; Friedrich, J.M.; Walsh, F.C. Protonated titanates and TiO2 nanostructured materials: Synthesis, properties, and
applications. Adv. Mater. 2006, 18, 2807–2824. [CrossRef]
16. Tang, H.; Prasad, K.; Sanjines, R.; Schmid, P.; Levy, F. Electrical and optical properties of TiO2 anatase thin films. J. Appl. Phys.
1994, 75, 2042–2047. [CrossRef]
17. Kim, W.-T.; Choi, W.-Y. Anodic Growth Behavior of TiO2 Nanotube Arrays with Process Parameter Control. J. Nanomater. 2019,
2019, 1–11. [CrossRef]
18. Lee, C.-G.; Na, K.-H.; Kim, W.-T.; Park, D.-C.; Yang, W.-H.; Choi, W.-Y. TiO2 /ZnO Nanofibers Prepared by Electrospinning and
Their Photocatalytic Degradation of Methylene Blue Compared with TiO2 Nanofibers. Appl. Sci. 2019, 9, 3404. [CrossRef]
19. Lee, C.-G.; Kim, W.-T.; Na, K.-H.; Park, D.-C.; Yang, W.-H.; Choi, W.-Y. Control of Microstructure on TiO2 Nanofibers for
Photocatalytic Application. J. Korean Inst. Electr. Electron. Mater. Eng. 2018, 31, 417–421.
20. Mondal, K. Recent advances in the synthesis of metal oxide nanofibers and their environmental remediation applications.
Inventions 2017, 2, 9. [CrossRef]
21. Caratão, B.; Carneiro, E.; Sá, P.; Almeida, B.; Carvalho, S. Properties of electrospun TiO2 nanofibers. J. Nanotechnol. 2014, 2014, 1–5.
[CrossRef]
22. Ji, B.C.; Bae, S.S.; Rabbani, M.M.; Yeum, J.H. Photocatalytic Activity of Electrospun PAN/TiO2 Nanofibers in Dye Photodecompo-
sition. Text. Color. Finish. 2013, 25, 94–101. [CrossRef]
23. Li, D.; Xia, Y. Fabrication of titania nanofibers by electrospinning. Nano Lett. 2003, 3, 555–560. [CrossRef]
24. Cai, Z.; Song, J.; Li, J.; Zhao, F.; Luo, X.; Tang, X. Synthesis and characterization of zinc titanate fibers by sol-electrospinning
method. J. Sol. Gel Sci. Technol. 2012, 61, 49–55. [CrossRef]
25. Yin, H.; Wada, Y.; Kitamura, T.; Kambe, S.; Murasawa, S.; Mori, H.; Sakata, T.; Yanagida, S. Hydrothermal synthesis of nanosized
anatase and rutile TiO2 using amorphous phase TiO2 . J. Mater. Chem. A 2001, 11, 1694–1703. [CrossRef]
26. Bhardwaj, N.; Kundu, S.C. Electrospinning: A fascinating fiber fabrication technique. Biotechnol. Adv. 2010, 28, 325–347.
[CrossRef]
27. Bognitzki, M.; Czado, W.; Frese, T.; Schaper, A.; Hellwig, M.; Steinhart, M.; Greiner, A.; Wendorff, J.H. Nanostructured fibers via
electrospinning. Adv. Mater. 2001, 13, 70–72. [CrossRef]
28. Spivak, A.; Dzenis, Y.; Reneker, D. Model of steady state jet in the electrospinning process. Mech. Res. Commun. 2000, 27, 37–42.
[CrossRef]
29. Choi, S.K.; Kim, S.; Lim, S.K.; Park, H. Photocatalytic comparison of TiO2 nanoparticles and electrospun TiO2 nanofibers: Effects
of mesoporosity and interparticle charge transfer. J. Phys. Chem. C 2010, 114, 16475–16480. [CrossRef]
Nanomaterials 2021, 11, 1616 15 of 15

30. Doh, S.J.; Kim, C.; Lee, S.G.; Lee, S.J.; Kim, H. Development of photocatalytic TiO2 nanofibers by electrospinning and its
application to degradation of dye pollutants. J. Hazard. Mater. 2008, 154, 118–127. [CrossRef]
31. Siwińska-Stefańska, K.; Kubiak, A.; Piasecki, A.; Goscianska, J.; Nowaczyk, G.; Jurga, S.; Jesionowski, T. TiO2 -ZnO binary oxide
systems: Comprehensive characterization and tests of photocatalytic activity. Materials 2018, 11, 841. [CrossRef] [PubMed]
32. Nair, A.S.; Jose, R.; Shengyuan, Y.; Ramakrishna, S. A simple recipe for an efficient TiO2 nanofiber-based dye-sensitized solar cell.
J. Colloid Interface Sci. 2011, 353, 39–45. [CrossRef] [PubMed]
33. Mustafa, M.N.; Shafie, S.; Wahid, M.H.; Sulaiman, Y. Light scattering effect of polyvinyl-alcohol/titanium dioxide nanofibers in
the dye-sensitized solar cell. Sci. Rep. 2019, 9, 1–8. [CrossRef]
34. Moon, J.; Park, J.-A.; Lee, S.-J.; Zyung, T.; Kim, I.-D. Pd-doped TiO2 nanofiber networks for gas sensor applications. Sens. Actuators
B Chem. 2010, 149, 301–305. [CrossRef]
35. Nikfarjam, A.; Hosseini, S.; Salehifar, N. Fabrication of a highly sensitive single aligned TiO2 and gold nanoparticle embedded
TiO2 nano-fiber gas sensor. ACS Appl. Mater. Interfaces 2017, 9, 15662–15671. [CrossRef]
36. Du, P.; Song, L.; Xiong, J.; Xi, Z.; Chen, J.; Gao, L.; Wang, N. High-Efficiency Photocatalytic Degradation of Methylene Blue Using
Electrospun ZnO Nanofibers as Catalyst. J. Nanosci. Nanotechnol. 2011, 11, 7723–7728. [CrossRef] [PubMed]
37. Blachowicz, T.; Ehrmann, A. Recent developments in electrospun ZnO nanofibers: A short review. J. Eng. Fiber. Fabr. 2020, 15, 1–6.
[CrossRef]
38. Singh, P.; Mondal, K.; Sharma, A. Reusable electrospun mesoporous ZnO nanofiber mats for photocatalytic degradation of
polycyclic aromatic hydrocarbon dyes in wastewater. J. Colloid Interf. Sci. 2013, 394, 208–215. [CrossRef]
39. Taylor, G.I. Electrically driven jets. Proc. R. Soc. A 1969, 313, 453–475.
40. Luo, C.; Edirisinghe, M. Core-liquid-induced transition from coaxial electrospray to electrospinning of low-viscosity poly
(lactide-co-glycolide) sheath solution. Macromolecules 2014, 47, 7930–7938. [CrossRef]
41. Basu, S.; Gogoi, N.; Sharma, S.; Jassal, M.; Agrawal, A.K. Role of elasticity in control of diameter of electrospun PAN nanofibers.
Fibers Polym. 2013, 14, 950–956. [CrossRef]
42. Shenoy, S.L.; Bates, W.D.; Frisch, H.L.; Wnek, G.E. Role of chain entanglements on fiber formation during electrospinning of
polymer solutions: Good solvent, non-specific polymer–polymer interaction limit. Polymer 2005, 46, 3372–3384. [CrossRef]
43. Song, Z.; Chiang, S.W.; Chu, X.; Du, H.; Li, J.; Gan, L.; Xu, C.; Yao, Y.; He, Y.; Li, B. Effects of solvent on structures and properties
of electrospun poly (ethylene oxide) nanofibers. J. Appl. Polym. Sci. 2018, 135, 45787. [CrossRef]
44. Vongsetskul, T.; Chantarodsakun, T.; Wongsomboon, P.; Rangkupan, R.; Tangboriboonrat, P. Effect of solvent and processing
parameters on electrospun polyvinylpyrrolidone ultra-fine fibers. Chiang Mai J. Sci. 2015, 42, 436–442.
45. Trejo-Tzab, R.; Caballero-Espada, L.; Quintana, P.; Ávila-Ortega, A.; Medina-Esquivel, R. Controlled phase changes of titania
using nitrogen plasma. Nanoscale Res. Lett. 2017, 12, 1–8. [CrossRef] [PubMed]
46. Ansari, M.A.; Albetran, H.M.; Alheshibri, M.H.; Timoumi, A.; Algarou, N.A.; Akhtar, S.; Slimani, Y.; Almessiere, M.A.; Alahmari,
F.S.; Baykal, A. Synthesis of Electrospun TiO2 Nanofibers and Characterization of Their Antibacterial and Antibiofilm Potential
against Gram-Positive and Gram-Negative Bacteria. Antibiotics 2020, 9, 572. [CrossRef]
47. Rioux, R.; Song, H.; Grass, M.; Habas, S.; Niesz, K.; Hoefelmeyer, J.; Yang, P.; Somorjai, G. Monodisperse platinum nanoparticles of
well-defined shape: Synthesis, characterization, catalytic properties and future prospects. Top. Catal. 2006, 39, 167–174. [CrossRef]
48. Kumar, A.; Jose, R.; Fujihara, K.; Wang, J.; Ramakrishna, S. Structural and optical properties of electrospun TiO2 nanofibers. Chem.
Mater. 2007, 19, 6536–6542. [CrossRef]
49. Lee, S.-H.; Tekmen, C.; Sigmund, W.M.J.M.S. Three-point bending of electrospun TiO2 nanofibers. Mater. Sci. Eng. A 2005, 398,
77–81. [CrossRef]
50. Li, H.; Zhang, W.; Li, B.; Pan, W. Diameter-dependent photocatalytic activity of electrospun TiO2 nanofiber. J. Am. Ceram. Soc.
2010, 93, 2503–2506. [CrossRef]
51. Ahmadpoor, P.; Nateri, A.S.; Motaghitalab, V. The optical properties of PVA/TiO2 composite nanofibers. J. Appl. Polym. Sci. 2013,
130, 78–85. [CrossRef]