Effect of Fabrication and Polyvinylpyrrolidone

on Electrospun Titanium Oxide

Nanofibres Diameter
Zi Sheng Tanga*, Nurmin Bolonga*, Ismail Saada, Ahmad Fauzi Ismailb,
Rosdianah Ramlia, Franklin Tiam Yang Lima
aFaculty

of Engineering, Universiti Malaysia Sabah, Jalan UMS, 88400 Kota Kinabalu, Sabah, Malaysia
bAdvanced Membrane Technology Research Centre, Universiti Teknologi Malaysia, 81310 Skudai, Johor, Malaysia

OUTLINE
Introduction

Methodology
Results and Discussion

Conclusion

Introduction
One-dimensional (1D) nanostructured materials.
How to produce 1D nanostructured materials?

Why titanium oxide (TiO2)?

The study focuses in producing eletrospun titanium oxide (TiO2)

nanofibres. The effects of the fabrication parameters and PVP
content on TiO2 nanofibres diameter are investigated in order
to produce continuous fibres with uniform size.

Methodology

i. Solution Preparation
Alkoxide Precursor (TTiP), carrying polymer (PVP), solvent
(Ethanol) and stabiliser (Acetic acid).
Two steps process:
S1: Dissolve 6.5 wt.% of PVP in 15 ml ethanol and magneticstirred for 2 hours to form transparent and homogeneous
solution
S2: Add 2 ml of TTiP into a mixture containing 4 ml glacial
acetic acid and 6 ml ethanol with a 10 minutes magnetic
stirring to form yellowish homogeneous solution.
Mix S2 with S1 followed by 2 hours stirring and formed
pale yellow solution as spinning solution.

Methodology

ii. Electrospinning
[1] high voltage power supply (Gamma High Voltage, ES30P-5W)
[2] syringe pump (Terumo Terufusion TE-331) with metal needle, Teflon tube
[3] grounded rotating drum collector

Figure 1:
Electrospinning Setup

Methodology

iii. Samples Preparation

The concentration of PVP, applied voltage, flow rate
and tip to collector distance are manipulated in
determining fibres diameter.
Samples with different key factors are prepared as
presented in Table 1 (in the later slide). Rotation speed
of the rotating drum collector was tuned at 105 rpm.
Total of 19 samples were prepared.

Methodology

iv. Fibres Morphology Characterization

The morphology of the fibres is revealed with scanning
electron microscope (SEM).
SEM images were furthered analysed with JMicroVision
v1.2.7 to determine the fibres diameter.
Mean diameter of fibres was determined from 15
random fibres.

Table 1: The samples for each parameters with their

standard deviation
Sample ID

Voltage
(kV)

V10
V15
V20
V25
V30
F0.5
F1.0
F1.5
F2.0
F2.5
D6
D8
D10
D12
D14
P4
P6
P7
P8

10
15
20
25
30
15
15
15
15
15
15
15
15
15
15
18
18
18
18

Parameters
Flow Rate
Distance
(ml/hr)
(cm)
1.0
1.0
1.0
1.0
1.0
0.5
1.0
1.5
2.0
2.5
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0

10
10
10
10
10
10
10
10
10
10
6
8
10
12
14
10
10
10
10

PVP Content
(wt.%)

Standard deviation
of fibre size,
(nm)

6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
6.5
4.0
6.0
7.0
8.0

94
36
130
102
128
120
55
78
66
78
98
98
60
106
79
51
45
73
76

Results
Table 2: The fabrication and PVP content
parameters
and
its
respective
experimental values.
Parameters

Parameter Key Level (#)

Applied
Voltage (kV)

10

15

20

25

30

Flow Rate
(ml/hr)

0.5

1.5

2.5

Tip to Collector
Distance (cm)

10

12

14

PVP Content
(weight %)

8
Figure 2: Relationship of different parameters
on mean diameter of fibres at different levels.

Discussion

i. Effect of Polymer Content

Figure 3: SEM images for varying weightage of PVP: a) 4 wt.%, b) 6 wt.%, c) 7 wt.% and d) 8 wt.%

Increasing in PVP content from 4 to 8 wt.% causes fibres

increase from 11051 to 22576 nm.
Increase in PVP content in the spinning solution causing
elevation to the viscosity of the solution and widen fibres
diameter

Discussion

ii. Effect of Tip to Collector Distance

Figure 4: SEM micrographs at varying tip to collector distance: a) 6 cm, b) 8 cm, c) 10 cm, d) 12 cm and
e) 14 cm

When the tip to collector distance increases from 6 to 14

cm, fibres size decreases from 24298 nm to 17579 nm.
Increase in tip to collector distance can reduce fibres
diameter.

Discussion

iii. Effect of Applied Voltage

Figure 5: SEM images for different applied voltage: a) 10 kV, b) 15 kV, c) 20 kV, d) 25 kV and e) 30 kV

As the applied voltage raises from 10 to 30 kV, the fibres

size decreased slightly from 22094 to 18973 nm.
Diameter of electrospun fibres is reduced by increasing
the applied voltage.
Breakage and discontinuous in fibres as in the red circle
(Fig 5 d and 5e)

Discussion

iv. Effect of Flow Rate

Figure 6: SEM micrographs for different flow rate: a) 0.5 ml/hr, b) 1.0 ml/hr, c) 1.5 ml/hr, d) 2.0 ml/hr and e)
2.5 ml/hr

When the flow rate increases from 0.5 to 2.5 ml/hr, the
fibres size increases gradually from 208103 to 22978
nm. Diameter of electrospun fibres increase with the
increasing flow rate.

Conclusion
An ethanolic solution containing TTiP, PVP and acetic
acid was prepared to produce TiO2 nanofibres via the
developed custom-made electrospinning system.
The significance for the influencing parameters were
observed from high to low order as PVP content > tip to
collector distance > applied voltage > flow rate.
Uniform and unbreakable TiO2 nanofibres as in this work
are: Applied voltage (15 kV), flow rate (1 ml/hr), tip to
collector distance (10 cm) and PVP content (7 wt.%)