Improved Electrical Conductivity of Polyvinyl Alcohol ... · MWCNTs may be interconnected, ......

International Journal of Engineering & Technology IJET-IJENS Vol: 11 No: 06 15

110506-9494 IJET-IJENS @ December 2011 IJENS I J E N S

Abstract-- This paper reports the synthesis and characterisation

of nanofibre composites consisting of polyvinyl alcohol (PVA),

multiwalled carbon nanotubes (MWCNTs) and manganese

dioxide (MnO2) synthesised using the electrospinning process.

The transmission electron microscopy (TEM) images show the

presence of MWCNT-MnO2 nanocomposites inside the PVA

nanofibre, whereas the field emission scanning electron

microscopy (FESEM) data revealed the cross linking network of

the nanofibre composite obtained from the electrospinning

process. The sizes of the pores of the nanofibre composite are

smaller compared to those in the neat PVA nanofibre. The

Fourier transform infrared spectroscopy (FTIR) analysis showed

the addition of MWCNT-MnO2 nanocomposite into PVA created

interaction within the composite structure. The PVA/MWCNT-

MnO2 nanofibre composites showed an enhanced electrical

conductivity of 6.99×10-6 Scm-1compared to 5.26316 ×10-6 Scm-1

for PVA/MWCNT without MnO2 and 1.25 ×10-15 Scm-1 for neat

PVA.

Index Term-- nanofibre composite; electrospinning; electrical

conductivity

I. INTRODUCTION

Electrospinning is a preferable method for producing fibres

from molten polymers or polymer solutions [1-3].

Electrospinning is a fast and simple process driven by

electrical forces. This technique not only produces nanofibre

from polymers, but can also be used to synthesis fibres by

combining different materials. Due to great improvements in

material characteristics, the combination of different materials

as binary or ternary composites has been widely explored by

many researchers [4-7].Since their discovery by Iijima [8],

carbon nanotubes (CNTs) have received much attention. The

introduction of CNTs into polymers can lead to improved

mechanical properties, electrical and thermal conductivities.

To functionalise and improve the physical properties of the

fibres, several researchers have investigated the fabrication of

electrospun composite nanofibre incorporated with CNTs [9-

13].Sung et al. [14] functionalised multiwalled CNTs

(MWCNTs) by modulating the interfacial interaction with the

polymer matrix, which enhanced the physical properties of the

composite. Dror et al.[15] described how the use of MWCNTs

in polymer composites via electrospinning has generated

remarkable interest in the field of electronics applications. The

MWCNTs within polymeric solutions align and are dispersed

along the fibre axis during the spinning process. The

alignment of MWCNTs within the nanofibre indicates that the

MWCNTs may be interconnected, thereby forming networks

that contribute to good electron mobilisation.Polyvinyl alcohol

(PVA) polymers have especially been given a great deal of

attention. These polymers are useful in broad applications due

to their excellent chemical resistance, physical properties, and

biodegradability[16]. The binding characteristics of PVA offer

excellent adhesion to porous and water-absorbent surfaces. To

further improve the electrical properties of PVA, many

researchers have reported the synthesis of PVA/CNT

nanocomposites [17-20].The presence of CNTs inside the

composite allows for electron conduction into the polymer

structure. Although several studies have been done on

PVA/CNT nanocomposites, the electron conduction and

stability of nanofibre composites can still be further improved.

The introduction of foreign materials into the inner cavity of

MWCNT composites can lead to interesting properties[21].

Razak et al. [22] showed that using manganese dioxides

together with polyaniline and CNTs to form nanocomposites

improves the electron conductivity. To the best of our

knowledge, the use of MnO2-filled MWCNTs to generate

nanofibre composites has not yet been investigated. Thus, the

aim of this study was to develop nanofibre composites

consisting of manganese oxide (MnO2), MWCNTs and PVA

using the electrospinning process to improve electron

interactions for better electrical conductivity performances.

II. MATERIALS AND METHODS

A. Materials and Experimental

The MWCNTs used in this study were obtained from the

Chinese Academy of Science, China. The average outer and

inner diameters of the MWCNTs were 40 and 20 nm,

respectively. Manganese (II) nitrate tetra hydrate was supplied

Improved Electrical Conductivity of Polyvinyl

Alcohol/ Multiwalled Carbon Nanotube

Nanofibre Composite Films with MnO2 as Filler

Synthesised using the Electrospinning Process

Mohd Faiz Muaz Ahmad Zamri, Sharif Hussein Sharif Zein*, Ahmad Zuhari Abdullah and Nor Irwin

Basir School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia,

14300 Nibong Tebal, Penang, Malaysia



by Fisher Scientific. These carbon nanotubes were immersed

for four hour in a solution of manganese nitrate. The mixture

was stirred to enable better incorporation into the cavity of the

carbon nanotubes. After mixing, the carbon nanotubes were

separated from solution and dried. The ratio of MWCNT to

Mn(NO3)2.6H2O used was 30: 70 . A complete description of

the purification and filling of MWCNTs with manganese

nitrate has been explained in detail elsewhere [23]. The dried

MWCNT-MnO2 was dispersed using an ultrasonic processor

(USG-150) and subsequently added to a PVA solution. The

PVA used in this study was provided by Sigma Aldrich was

87% to 90% hydrolysed and had an average molecular weight

30000 to 70000 g/mol. The method for preparation of the PVA

nanofibres was adapted from Koski et al. [24]. Five 10 mL

samples of the PVA electrospun solution were prepared using

distilled water as the solvent. Different amounts of MWCNT-

MnO2 (1, 3 and 5 wt %) and MWCNT (1%) were added into

four different PVA electrospun solutions (ratio of PVA:

MWCNT-MnO2, 100: 1) and stirred at 80°C until a

homogenous electrospun solution was obtained. The prepared

electrospun solution was poured into a syringe pump to

proceed with the electrospinning process.

B. Electrospinning Setup

The electrospinning unit setup consisted of a high-voltage

power supply, a syringe pump and a sample collector, as

shown in Figure 1. The syringe was held vertically using a

stainless steel needle. The needle (0.8 mm inner diameter) was

electrically connected to a positive high-voltage power supply

purchased from the Mechanics Electronics Computer

Corporation (MECC) Co., Ltd (Japan).The electrospinning

process was carried out in a closed environment inside a

transparent box at a room temperature and with an applied

voltage of 16 kV. The electrospun nanofibre were collected on

a copper plate covered with aluminium foil. The needle to the

collector distance was 100 mm and the solution flow rate was

maintained at 3 ml/hr using a digitally controlled syringe

pump (model number: KDS 100) purchased from KD

Scientific Inc. (United States of America).

Fig. 1. Schematic diagram of the electrospinning setup

C. Characterisation method

Field emission scanning electron microscopy (FESEM)

images were obtained using a LEO Supra 50 VP system.

Transmission electron microscopy images were obtained using

a Philips TEM CM 12 microscope and Fourier transform

infrared (FTIR) spectra were acquired using a model 2000

Perkin Elmer spectrometer with a resolution of 0.4 cm-1

. The

KBr disks of each sample were prepared in a 9:1 ratio of KBr

to the sample. Each sample was hydraulically pressed with

gradual pressure. The samples were then placed in the

spectrometer beam. The end products from the experiment

were analyzed using TEM (Philip TEM). The instrument was

run at 80 kV for extracting electrons and was equipped with

Soft Imaging System (SIS), model 3.0. Preparation for TEM

characterization involved the dispersion of some particles

from each sample in ethanol, followed by placing a few drops

on a coated copper grid. For scanning electron microscopy

(SEM), samples in finely ground powder forms were spread

evenly on top of an aluminium sample stub stacked with

double-sided tape. The samples were then placed into the

specimen chamber under pressure (5 atm) (A Leo Supra 50

VP Fuel Emission). A Philip XL 40 scanning electron

microscope was used to determine the morphology of the

samples, which were bombarded using an electron beam at 25

kV. The image was recorded with a Philips Graphic Video

recorder, model GP-850

D. Electrical Conductivity Measurements

The electrical conductivity of the nanofibre composites

was measured based on direct current conductivity (σdc

) with

equation (1) [25]. The galvano electrochemical impedance

spectroscopy technique (GEIS) produced by Biologic Science

Instrument Co. Ltd. was used to measure the resistance of the

sample. Direct current conductivity was calculated with the

resistance value (R). The nanofibre composite was stripped

from the aluminium foil and cut into 1 cm × 1 cm pieces for

use in the electrodes. The electrodes were immersed in 6 M

potassium hydroxide solution (electrolyte) and the

measurements were performed over the frequency range of

100 kHz to 0.1 Hz at 1 V. Figure 2 shows the circuit model

(also known as the Randles cell circuit) that been used to

obtain the resistance values from the system. In this circuit,

each components are representing happened in the

electrochemical cell system [26].

Fig. 2. Randles cell circuit



Rs is the resistance of the potassium hydroxide electrolyte

solution, Rct is the resistance of the charge transferred, Cdl is

the capacitance and W is the Warburg coefficient of the circuit

system. The direct conductivity of each sample was calculated

using equation (1). In order to calculate dc conductivity (σ dc),

the resistance (Rct) is obtained from the impedance analysis

tools (Zfit) in GEIS which calculate the value of the resistance

(R) automatically. The thickness (d) and surface area (A) of

each sample were 0.01 cm and 1 cm2, respectively.

σdc

=

(1)

III. RESULT AND DISCUSSION

A. Morphology of PVA nanofibre and PVA/MWCNT

MnO2 nanofibre composites

Figure 3(a) shows the TEM image of an open tip

MWCNT obtained after treatment of the raw MWCNTs using

the wet chemical process. As shown in Figure 3(b), the TEM

image showed that the MWCNT was successfully filled with

MnO2. The dark contrast colour inside the MWCNTs

suggested efficient and homogenous filling of MnO2 inside the

MWCNT cavity. In addition, the smooth surface of the outer

walls did not show any crystallised MnO2, confirming well-

filled MWCNTs [22]. The TEM image in Figure 3(c) shows

the presence of MWCNT-MnO2 nanocomposites inside the

PVA nanofibre. We believe that the MWCNT-MnO2

nanocomposites scattered inside the PVA nanofibre, thus and

forming PVA/MWCNT-MnO2 nanofibre composites with

multilayer structures.

Fig. 3.TEM images of (a) an open tip of a MWCNT, (b) a MWCNT-

MnO2 nanocomposite and (c) a PVA/MWCNT-MnO2 (3%) nanofibre

composites

Figures 4 and 5 show the SEM images of the PVA

nanofibre and nanofibre composites obtained from the

electrospinning process.

Fig. 4. SEM images showing PVA nanofibre at different magnifications:

(a) 100x (b) 1000x and (c) 10000x



Figure 4 contains the images of the PVA nanofibre at different

magnifications of (a) 100x, (b) 1000x and (c) 10000x. This

observation proved that a homogenous cross linking structure

has been obtained with the average pores diameter of 323 ±

0.3 nm as shown in Figure 6 (a).Figure 5(a) shows an

overview of the PVA/MWCNT-MnO2 nanofibre composite.

The surface of the composite was mostly homogenous,

although several rounded lumps projected from the surface.

The morphology image in Figure 5(b) indicated that the beads

had rough surfaces.

Fig. 5. SEM images showing nanofibre composites of PVA/MWCNT-MnO2

at different magnifications: (a) 100x, (b) 2000x and (c) 10000x

The beads were formed when the solutions were not

completely solidified on the collector. Beads have also been

observed with reduced distance and increased field strength

between the needle tip and collector[27].The presence of

beads proved that MWCNT-MnO2 scattered inside the PVA

nanofibres, as shown in Figure 3(c). The SEM image in Figure

5(c) shows the homogenous area of the nanofibre composite at

high magnification. The area was surrounded with a smooth

and beadless nanofibre composite. The pores diameter

distribution of the high magnification area is shown in Figure

6(b). The average diameter of the pore size was recorded to be

280 ±0.07 nm. The cross linking orientation suggested a good

distribution of the composite film pores. In addition, the fibres

diameter and pore size diameter of the PVA/MWCNT-MnO2

nanofibre composite were smaller than that of PVA nanofibre,

as shown in Figure 6(a).The fibres diameter range decreased

from the range of 71.4 - 214 nm down to 71.4 – 143 nm after

MWCNT-MnO2 was added to the neat PVA nanofibre. The

decrease in fibres diameter size may be due to the increased

conductivity. As the conductivity of the electrospun solution

increased, more charges would have been produced during the

electrsopinning process. The increase in charge will reduce the

critical voltage of the solution and produce fibres with small

diameters.

Fig. 6. Percent distribution of the pore diameter of the (a) PVA nanofibre (b)

PVA / (3%) MWCNT-MnO2 nanofibre composites

B. Structural analysis

The FTIR spectra of the PVA nanofibre and the

PVA/MWCNT and 1, 3 and 5% of PVA/MWCNT-MnO2

nanofibre composites are shown in Figure 7 (a), (b), (c), (d)



and (e), respectively. Based on the FTIR wave range

reference[28], we determined that the spectra in Figure 7 (a-e)

shows a broad O–H stretching band for a hydrogen-bonded

alcohol at 3412 cm−1

and banding of CH2 groups from 2922

cm-1

to 2845 cm-1

. In Figure 7(a), we attributed the band at

1429cm-1

to (C–O-H) bending while the band at 1082 cm-1

in

Figure 6(c) is due to C-O stretching of the PVA. We also

compared pure PVA and PVA/MWCNT-MnO2

nanocomposites with different amounts of MWCNT-MnO2.

The FTIR spectra of the nanofibre films suggested the MnO2

has served as a conducting bridge to link PVA and improve

the electron interaction of the nanofibre composites. We

observed clear differences between the FTIR spectra of pure

PVA nanofibre (7(a)) with the PVA/MWCNT-MnO2

nanofibre composites (7(c), 7(d) and 7(e)).With increasing

amounts of MWCNT-MnO2, the band at 798 and 881 cm−1

gradually weakened. The band at 798 cm−1

was attributed to

the out-of-plane vibration of the O–H group, which is broad in

common alcohols [29]. As shown in Figure 7 (c-e), the content

of MWCNT-MnO2 increased and the band at 1084.29 cm−1

decreased in intensity. These results suggest an interaction

between MWCNT-MnO2 and the polymer matrix with the O–

H group.

Fig. 7. FTIR spectra of (a) a PVA nanofibre, (b) a PVA/ (1%) MWCNT

nanofibre, (c) a PVA/ (1%) MWCNT-MnO2 nanofibre, (d) PVA/ (3%)

MWCNT-MnO2 nanofibre and (e) PVA/ (5%) of MWCNT-MnO2 nanofibre

C. Electrical conductivity measurement

The direct conductivity of each sample was calculated with the

resistance value in equation (1). The electrical conductivities

of PVA/MWCNT-MnO2 nanofibre composites with different

wt% of MWCNT-MnO2 are shown in Figure 8. The

conductivity of the neat PVA nanofibre was 1.25 ×10-15

.The

MWCNT-MnO2 affected the nanofibre composites. The

conductivity increased with increasing amounts of MWCNT-

MnO2 incorporated into PVA. The conductivities of the

nanofibre composite at 1, 3, and 5 wt% were 5.698×10-6

,

6.689×10-6

and 6.99×10-6

Scm-1

, respectively. The increase in

conductivity was more pronounced at 1% MWCNT-MnO2.

Above 1% MWCNT-MnO2, the conductivity of the nanofibre

composites increased up to 6.99×10-6

Scm-1

at 5 wt%. Below 1

wt% of MWCNT-MnO2, the conductivity was dominated by

the PVA component. The conductivity of PVA/ MWCNT-

MnO2, compared with neat PVA, was enhanced because the

MWCNT-MnO2 served as a conducting bridge to link PVA

and improve the conductivity of the nanofibre composites.

Fig. 8. Electrochemical impedance spectroscopy of (a) PVA/MWCNT-MnO2

(5%), (b) PVA/MWCNT-MnO2 (3%), (c) PVA/MWCNT-MnO2 (1%), (d)

PVA/MWCNT and (e) PVA nanofibre.

Fig. 9. Electrical conductivity of (a) PVA/MWCNT, (b) PVA/MWCNT-

MnO2 (1%), (c) PVA/MWCNT-MnO2 (3%) and (d) PVA/MWCNT-MnO2

(5%).

IV. SCOPE AND LIMITATION

The scope of this work is to improve the electrical

conductivity of PVA/MWCNT nanofibre composite films

with MnO2 as filler synthesised using the electrospinning

process. The range of frequency studied was from 100 kHz to

0.1 Hz at 1 V of amplitude. As PVA is a non conducting

polymer, the main limitation of this study is to produce high

electrical conductivity material for electronic application. It is

believed the type of material produce from this work is able to

be used only in semi conductor applications.

4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600.0

cm-1

%T

(a)

(b)

(c)

(d)

(e)

2922.11 1735.88

1429.46

3412.73

881.23

798.84

3412.73

2845.99

1084.293412.73

2845.99

1655.02

2845.99

1384.51

3412.732845.99



V. CONCLUSIONS

The electrical conductivity and morphology of MWCNT-

MnO2 within PVA nanofibre were investigated in this work.

We observed that a multilayer structure of PVA and

MWCNT-MnO2 scattered inside the beads of the PVA

nanofibre. The surface morphology showed the rough surfaces

of the beads, which formed when the solutions were not fully

solidified on the collector. FTIR analysis of the nanofibre

composites revealed that the addition of the MWCNT-MnO2

nanocomposite into PVA created an interaction within the

composite structure. The FTIR spectra also suggested that

increasing MWCNT-MnO2 content in the PVA fibres could

enhance interactions within the composite. Electrical

conductivity of the nanofibre composites obtained by the

GEIS technique proved the electron interaction of PVA with

the MWCNT-MnO2. The electrical conductivity increased

gradually as the amount of MWCNT MnO2 increased.

Although the electrical conductivity was low (10-6

Scm-1

), it

could be further enhanced by improving the alignment of the

MWCNT-MnO2 nanocomposite inside the PVA nanofibre. We

believe that the occurrence of the beads contributed to the

poor mobility of electrons within the networks.The MWCNTs

scattered within the nanofibre, indicating the disorder of the

formed networks. In future work, we will aim to improve the

nanocomposite alignment within the nanofibre. We

recommend removing the beads from the network structure to

improve the electron mobility and conductivity. In comparison

with other research work, the value of electrical conductivity

for PVA/MWCNT nanofiber was lower compared to

PVA/MWCNT nanocomposite developed by Zhang et. al

(2009) [30]. This may be due to the different method of

preparation for the electrode material. Furthermore the

arrangement of electrochemical cell, and the type electrolyte

that been used was not the same. To further improve the

electrical conductivity performance, the following suggestion

is recommended:

1. Introducing conducting polymer nanofiber such as

poly(ethylenedioxytiophene) (PEDOT), polypyrrole (PPy) and

polyanile (PANI), which have high surface area, porosity, and

good electrical conductivity to be electrospun into nanofibers

with MWCNT-MnO2.The conducting polymer nanofibers

based electrochemical capacitors are expected to have high

electrical conductivity and power density.

2. Introducing electrical measurement of nanofiber composite

that prepared at different electrospun solution temperatures as

to evaluate and optimize the effect of electrospun solution

temperature to pores size formation for nanofibers. The large

pore size, short pore length and straight forward connectivity

will facilitate ion diffusion with a high speed that contributes

to charge propagation of electrical conductivity. Phase

separation due fast solvent evaporation of volatile solvent

causes original polymer solution to separate into two phases

(polymer rich and solvent rich phases). Once fiber solidifies,

the polymer rich phase forms the fiber matrix while solvent

rich gives rise to the pores

3. Introducing different functional group of MWCNTs and

different types of MWCNTs inner and outer diameter together

with PVA nanofiber composite, for better understanding of the

functional group of MWCNTs and filling metal oxides

particles inside MWCNTs respectively.

ACKNOWLEDGMENT

The financial support provided by RU USM grant is gratefully

acknowledged.

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