Imp Polymer Test

U. SASIKALA* et al.
ISSN: 22503676
[IJESAT] INTERNATIONAL JOURNAL OF ENGINEERING SCIENCE & ADVANCED TECHNOLOGY Volume-2, Issue-3, 722 730

IJESAT | May-Jun 2012
Available online @ http://www.ijesat.org 722
STRUCTURAL, ELECTRICAL AND PARAMETRIC STUDIES OF A PEO
BASED POLYMER ELECTROLYTE FOR BATTERY APPLICATIONS

U. Sasikala
*
, P. Naveen Kumar, V.V.R.N.Rao and A. K. Sharma

Department of Physics, S.V.University, Andhra Pradesh, India, sasi2483@gmail.com

Abstract
Ion conducting polymer electrolyte films based on Polyethylene oxide (PEO) complexed with sodium fluoride (NaF) have been
prepared by solution cast technique for solid state battery applications. Miscibility studies were performed using X-ray diffraction
(XRD) and Fourier Transform Infrared analysis (FTIR) measurements. Frequency dependent conductivity (
ac
) values were obtained
from complex impedance (Cole-Cole) plots. It was observed that the magnitude of conductivity increased both with the increase in the
salt concentration and the temperature. The activation energy values showed a decreasing trend with increasing ionic conductivity.
Optical constants like absorption edge, direct band gap and indirect band gap were investigated in pure and doped PEO films from
their UV-VIS absorption spectra in the 200-600 nm wavelength region. It was observed that these optical constants shifted to lower
energies on doping with NaF salt. The charge transport of these electrolytes is mainly due to ions which were confirmed by the
transference number experiment. Using this electrolyte, cells were fabricated and their discharge profiles were studied under constant
load. Several cell parameters associated with the cells were evaluated and compared with earlier reports.

Index Terms: xrd studies, frequency dependant conductivity, transference numbers, discharge profiles
--------------------------------------------------------------------- *** ------------------------------------------------------------------------
1. INTRODUCTION
The development of polymer systems with high ionic
conductivity is one of the main objectives in polymer
research. This is because of their potential applications as
electrolytes in solid-state batteries, fuel cells, electrochemical
display devices/smart windows, photo electrochemical cells
etc. [1-3], due to their high conductivity, high energy density,
wide electrochemical stability and easy processability. The
main advantages of polymer electrolytes are their mechanical
properties, ease of fabrication of thin films of desirable sizes
and their ability to form proper electrode/electrolyte contact
in electrochemical devices. Polyethylene oxide (PEO), in
particular, is an exceptional polymer, which dissolves high
concentrations of a wide variety of salts [4]. The oxygen
atom in PEO is the backbone to coordinate with the metal
cations and facilitate ion-pair separation, which can then
favour electrical conduction through ion transport. Most of
the studies in this field are reported on PEO-based polymer
electrolytes using alkali salts [5, 6]. Sodium-ion conducting
polymer electrolytes have been investigated [7, 8] based on
PEO, polypropylene oxide (PPO) or polybismethoxy ethoxy
phosphazene (MEEP) complexed with NaI, NaClO
4
or
NaCF
3
SO
3
. Some silver-ion conducting polymer complexes
with PEO have also been examined [9, 10]. Other studies
have been investigated on PEO-based electrolytes using
divalent cationic salts as dopants [11, 12]. The effect of the
addition of -Al
2
O
3
has been investigated in PEO+LiClO
4

[13] and PEO+NaSCN [14] systems. Reports on a composite
polymer electrolyte (PEO+NH
4
I+Al
2
O
3
) are also available
[15].

The present work is concerned with solid-state
electrochemical cells which are based on (PEO+NaF)
electrolyte films. Several experimental techniques such as
optical, electrical, XRD, FTIR and transport number
measurements were performed to characterize these polymer
electrolytes. Based on these electrolytes, electrochemical
cells were fabricated with anode/polymer electrolyte/cathode
configuration. The discharge characteristics of the cell were
studied for a load of 100 k.

2. EXPERIMENTAL
Films (thickness ~ 150 m) of pure PEO (molecular weight
1X 10
5
) and various compositions of complexed films of
PEO with NaF salt were prepared with weight ratios (90:10),
(80:20) and (70:30) by a solution-cast technique using
methanol (water-free) as solvent. The solutions were stirred
for 10-12 h, and then poured into polypropylene dishes and
allowed to evaporate slowly at room temperature. The final
product was vacuum-dried thoroughly at 10
-3
torr. The X-ray
diffraction studies of these films were performed by means of
a SEIFERT X-ray diffractometer system with Ni-filtered Cu
U. SASIKALA* et al. ISSN: 2250
3676
[IJESAT] INTERNATIONAL JOURNAL OF ENGINEERING SCIENCE & ADVANCED TECHNOLOGY Volume-2, Issue-3, 722
730

Available online @ http://www.ijesat.org
723
k

radiation. The IR spectra were recorded with the help of
Perkin Elmer FTIR spectrophotometer in the range 4000 -
400 cm
-1
. The AC conductivity was measured using PSM
1700 Impedance Analyzer in the frequency range 1 Hz 1
MHz and in the temperature range 303363 K. Optical
absorption spectra were recorded at room temperature in the
wavelength range 200-600 nm using Shimadzu UV-VIS-NIR
(Model UV-3100) spectrophotometer from which the optical
constants such as band edge, optical band gap (both direct
and indirect) were determined. The total ionic transport
number (t
ion
) was evaluated by means of Wagners
polarization technique [16]. In this technique, freshly
prepared polymer electrolyte films were polarized in the
configuration Na/polymer electrolyte/C under a DC bias. The
resulting current was monitored as a function of time.
Electrochemical cells were fabricated with the configuration
Na/ PEO+NaF/ (I
2
+C+electrolyte). The discharge
characteristics were monitored under a constant load of 100
k.

3. RESULTS AND DISCUSSION
3.1 X-ray diffraction studies
In order to investigate the complexation of sodium fluoride
salt with the polymer electrolyte, XRD studies were
performed. Fig. 1 shows the comparative profiles of the XRD
patterns of Pure PEO film, NaF salt and the complexed
(PEO+NaF) films with different wt% ratios (90:10), (80:20)
and (70:30).
A comparison of the diffraction spectra of complexed PEO
with that of pure PEO and NaF reveals the following
differences.

- The diffraction peaks observed for 2 values at 19.1
o

and 23.3
o
were found to be less intense in
complexed PEO films compared to the pure PEO
film. This indicated that the addition of NaF salt
caused a decrease in the degree of crystallinity of the
polymer PEO. This could be due to the disruption of
the semi-crystalline structure of the film by NaF salt.
Hodge et al [17] established a correlation between
the intensity of the peak and the degree of
crystallinity.
- Peaks corresponding to the polymer PEO were also
present in the complexed PEO films. This showed
the simultaneous presence of both crystalline
complexed and uncomplexed PEO.

Fig-1: X-ray diffraction spectra of (a) pure PEO (b)
PEO+NaF (90:10) (c) PEO+NaF (80:20) (d) PEO+NaF
(70:30) (e) NaF salt

- No peaks corresponding to NaF were observed in
complexed PEO, indicating the absence of excess
salt (uncomplexed) in the complexed polymer films.
The peaks exhibited a decrease in intensity with broadening
at higher concentrations of NaF salt in the polymer. This
indicated a decrease in the crystalline phase and a dominant
presence of the amorphous phase. This amorphous nature
resulted in greater ionic diffusivity with high ionic
conductivity, as amorphous polymers have flexible backbone
[18].

3.2 IR studies
The IR spectra of pure PEO, NaF and NaF complexed with
PEO are shown in Fig. 2. The following differences in the
spectral features have been observed on comparing the
spectra of complexed PEO with pure PEO and NaF.
- The strong broad absorption band appearing
between 2962 and 2823 cm
-1
in pure PEO
corresponds to symmetric and asymmetric C-H
stretching modes of CH
2
group [19]. The width
of this band in PEO was found to decrease with
an increase of dopant concentration.
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- In addition to this, CH
2
wagging mode exhibited
at around 1360 cm
-1
in pure PEO is shifted to
1349, 1342 and 1334 cm
-1
in 10, 20 and 30 wt%
NaF salt complexed films, respectively. This
decrease in the wave number results in the
increase in band length, and hence
complexation takes place [20].
- The width of the C-O stretching band observed
around 1100 cm
-1
in PEO also showed a
decrease with an increase of NaF in the polymer
[21].
- New peaks around 2360.7, 1778.4 and 1640.2
cm
-1
are present in the IR pattern for complexed
PEO.
- The appearance of new peaks along with
changes in the existing peaks and/or their
disappearance in the IR spectra directly indicate
the complexation of NaF with PEO.
If the cations of NaF get coordinated with etherial oxygen of
PEO, the spectral changes are expected to be in the COC
stretching and deformation ranges. The decrease in the width
of 1100 cm
-1
band which is assigned to COC symmetrical and
asymmetrical stretching suggests the coordination
complexation of the salt with PEO [21].

Fig-2: IR spectra of (a) pure PEO (b) PEO+NaF (90:10),
(c) PEO+NaF (80:20), (d) PEO+NaF (70:30), (e) NaF salt
3.3 AC impedance studies
Complex impedance is given by
Z = Z' Z" (1)
Z =
C
j
C
D
e e

(2)
Where Z' is the real part of impedance; Z
"
, the imaginary part
of impedance; D, the dissipation factor (or) loss tangent; ,
the angular frequency; and C, the capacitance of the film.

Typical impedance plots (Z' vs Z
"
) for PEO and (PEO+NaF)
composite electrolytes at room temperature are shown in
Fig.3, which showed a normal impedance behaviour such as a
depressed semicircular portion followed by a spike (residual
tail). In the complex impedance representation, the low
frequency response appears as an inclined spike and such a
spike (tail-like) is characteristic of a blocking double-layer
capacitance. The high frequency semicircle corresponds to
the bulk response of the films. These results suggest that the
migration of ions may occur through the volume of matrix
polymer, which can be represented by a resistor. The
immobile polymer chains, on the other hand, become
polarized in the alternating field, and can therefore be
represented by a capacitor. The ionic migration and bulk
polarization are physically in parallel, and therefore, the
portion of the semicircle can be observed at high frequencies
[22].

Fig-3: Impedance plots (Cole-Cole plots) of pure and NaF
complexed PEO films at 303K

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Fig-4: Composition vs conductivity plots of PEO+NaF
polymer electrolyte system at different temperatures

The ionic conductivity of PEO and (PEO+NaF) polymer
electrolytes is calculated from the relation
A R I
b
= o (3)
where I, the thickness of the film, A, the area of the film and
R
b,
the bulk resistance of the material which is obtained from
the intercept on the real axis at the high frequency end of the
Nyquist plot of complex impedance [23].
The variation of conductivity (), as a function of NaF salt
concentration in PEO is shown in Fig. 4 in the temperature
range of 303 363 K while the conductivity data at room
temperature is presented in Table 1. The data reveals that the
conductivity of pure PEO is about 3.24 X 10
-8
Scm
-1
at room
temperature and increases to 1.53 X 10
-7
Scm
-1
for 10 wt%
NaF. The increase in conductivity becomes flatter on further
addition of NaF to the polymer. The increase in conductivity
at lower dopant concentrations of NaF is attributed to the
formation of charge transfer complexes or decrease in the
crystallanity [24], while the slow increase at higher dopant
concentrations is due to the formation of ionic aggregates.
These ionic aggregates impede the conduction process and
decrease the conductivity.
The variation of conductivity as a function of temperature for
pure and different concentrations of NaF salt in PEO is
shown in Fig. 5 over a temperature range 303 363 K. In the
temperature range of study, the conductivity increased with
temperature and followed Arrhenius behavior throughout the
three regions (regions I, II and III) having different activation
energies. While regions I and III might be due to intrachain
and interchain segmental motions, region II may be due to the
transition of the polymer from the crystalline to amorphous
phase [25, 26].
In polymer electrolytes, change of conductivity with
temperature is due to the segmental motion, which results in
an increase in the free volume of the system. This increase in
free volume would facilitate the motion of ionic charge [27].
Similar behaviour was observed in other films also [24, 25,
28].

Fig-5: Temperature-dependant conductivity of: (a) pure
PEO, (b) PEO+NaF (90:10), (c) PEO+NaF (80:20) and (d)
PEO+NaF (70:30)

As per Arrhenius relation the dependence of conductivity has
the form
) exp(
0
kT E
a
=o o (4)
where
0
is the pre-exponential factor, E
a
, the activation
energy and k is the Boltzmann constant.
The activation energies were calculated from the slope of
these plots and the values are shown in Table 1. These values
are found to decrease with increasing concentration of NaF.
This may be due to the fact that the addition of small amounts
of dopant forms charge transfer complexes in the host lattice
[29]. These charge transfer complexes increase the electrical
conductivity by providing additional charges in the lattice,
resulting in a decrease of activation energy.

3.4 Optical absorption studies
Optical absorption studies on pure and doped films were
carried out to determine the optical constants such as optical
band gap (E
g
) and the position of the fundamental band edge.
The absorption coefficient was determined from the spectra
using the formula:
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726
d A = o (5)
Where A is the absorbance and d is the thickness of the
film.
The position of the absorption edge was estimated by
extrapolating the linear portions of the vs h plots (Fig. 6)
to zero absorption value. For pure PEO film, the absorption
edge lies at 5.00 eV, while for 10, 20 and 30 wt% NaF doped
PEO polymer films the absorption edge lies at 4.91 eV, 4.88
eV and 4.85 eV respectively.

Fig-6: o vs. hv of (a) pure PEO, (b) PEO+NaF (90:10), (c)
PEO+NaF (80:20), (d) PEO+NaF (70:30)

When a direct band gap exists, the absorption coefficient has
the following dependence on the energy of the incident
photon [30]

2 1
) (
g
E h C h = v v o
(6)
where E
g
is the band gap, C is a constant dependent on
specimen structure, is the frequency of incident light and
h is the Plancks constant.
The direct band gaps were evaluated from (h)
2
vs h plots
(Fig. 7) and the allowed direct transition energies were
determined by extrapolating the linear portions of the curves
to zero absorption. For pure PEO film the direct band gap lies
at 5.14 eV, while for 10, 20 and 30 wt% NaF doped PEO
films, it lies at 5.01 eV, 4.95 eV and 4.92 eV respectively.
For indirect transition which required photon assistance, the
absorption coefficient has the following dependence on the
photon energy [30]

2 2
) ( ) (
p g p g
E E h B E E h A h + + = v v v o
(7)

Where E
p
is the energy of the photon associated with
transition and A and B are constants depending on the
band structures.

Fig-7: (ohv)
2
vs. hv of (a) pure PEO, (b) PEO+NaF
(90:10), (c) PEO+NaF (80:20), (d) PEO+NaF (70:30)

Fig-8: (ohv)
1/2
vs. hv of (a) pure PEO, (b) PEO+NaF
(90:10), (c) PEO+NaF (80:20), (d) PEO+NaF (70:30)
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Table-1: Conductivity, activation energies and transference numbers of PEO+NaF electrolyte systems

Polymer
electrolyt
e
Conductivity
at 303K (S
cm
-1
)
Activation energy (eV) Transference Number
Region I Region II Region III t
ion
t
ele

Pure PEO 3.24 X 10
-8
0.56 1.71 0.53 - -
PEO+NaF
(90:10)
1.53 X 10
-7
0.49 1.46 0.44 0.89 0.11
PEO+NaF
(80:20)
2.65 X 10
-7
0.40 1.40 0.38 0.90 0.10
PEO+NaF
(70:30)
4.73 X 10
-7
0.32 1.36 0.30 0.91 0.09

Table-2: Absorption Edge and Optical band gap values of Pure PEO and (PEO+NaF) Polymer system

Polymer electrolyte
Absorption
edge (eV)
Direct
band gap
(eV)
Indirect
band gap
(eV)
Pure PEO 5.00 5.14 5.10
PEO+NaF (90:10) 4.91 5.01 4.94
PEO+NaF (80:20) 4.88 4.95 4.89
PEO+NaF (70:30) 4.85 4.92 4.81

The indirect band gaps were obtained from the plots of (h)
1/2
vs h plots as shown in the Fig. 8. For pure PEO films, the
indirect band gap lies at 5.10 eV while for 10, 20 and 30 wt%
NaF doped PEO films, it lies at 4.94 eV, 4.89 eV and 4.81 eV
respectively.

The values of absorption edge, direct band gap and indirect
band gap are shown in Table 2. It is clear from the Table 2 that
the band edge, direct band gap and indirect band gap values
showed a decrease with increase in NaF content. NaF is
responsible for the formation of defects in the films. These
defects produce the localized states in the optical band gap.
This may be responsible for the decrease of energy band gap
when NaF content is increased in the polymer matrix [31]. In
other words, the decrease in the optical gap results in an
increase in the degree of disorder in the films. These results
are in agreement with those obtained from XRD and
conductivity studies in the present work.

3.5 Transference number
Electronic and ionic transference number measurements play
an important role in explaining the conductivity of the
polymer electrolyte system. The transference numbers
corresponding to ionic (t
ion
) and electronic (t
ele
) transport have
been evaluated in the (PEO+NaF) electrolyte system using
Wagners polarization technique [16]. In this technique dc
current was monitored as a function of time on application of
fixed dc voltage across the Na/polymer electrolyte/C. After
polarization of the cell with 1.5 V dc, the current versus time
plots were obtained and shown in Fig. 9.

Fig-9: Current vs. time plots of (PEO + NaF) polymer
electrolytes


The transference numbers (t
ion
and

t
ele
) are calculated from the
polarization current versus time plots using the equations:
i f ion
I I t / 1 = (8)
ion ele
t t =1 (9)

where I
i

is the initial current, and I
f
is the final residual
current.
The resulting data is given in Table 1. For all the compositions
of (PEO+NaF) electrolyte system, the values of ionic
transference numbers are in the range 0.89 - 0.91. This
suggests that the charge transport in these polymer electrolyte
films is predominantly due to ions; only a negligible
contribution comes from electrons [30].

3.6 Discharge profiles
Solid state electrochemical cells were fabricated with the
configuration Na(anode)/polymer electrolyte/(I
2
+ C +
electrolyte)(cathode) using (PEO+NaF) polymer electrolyte
films. Sodium metal was used as the negative electrode, and a
mix of iodine (I
2
), graphite (C) and electrolyte in the ratio
5:5:1 as the positive electrode.

Fig-10: Discharge characteristics of (PEO+NaF)
electrochemical cell at a constant load of 100 kO

Cell parameters
(PEO+NaF)
(90:10)
(PEO+NaF
) (80:20)
(PEO+Na
F) (70:30)
Open circuit voltage
(V)
2.31 2.46 2.52
Short circuit current
(mA)
1.15 1.29 1.35
Area of the cell (cm
2
) 1.33 1.33 1.33
Weight of the cell (g) 1.82 1.83 1.83
Time for plateau
region (h)
75 92 101
Power density (W/kg) 1.46 1.73 1.86
Energy density
(Wh/kg)
109 159 188
Current density
(mA/cm
2
)
0.86 0.97 1.02

Table-3: Cell parameters of
Na/(PEO+NaF)/(I
2
+C+Electrolyte) polymer electrolytes

The discharge characteristics of
Na / (PEO+NaF)(90:10) / (I
2
+C+electrolyte), Na /
(PEO+NaF)(80:20) / (I
2
+C+electrolyte) and Na /
(PEO+NaF)(70:30) / (I
2
+C+electrolyte) cells at ambient
temperature for constant load of 100 k are presented in Fig.
10. The sharp initial decrease in voltage may be due to the
polarization and/or the formation of thin layer sodium at
electrode-electrode interface.

The cell parameters were calculated and are shown in the
Table 3. From the data, it is clear that the short circuit current
(SCC), open circuit voltage (OCV) and discharge time for the
plateau region were found to be greater in (PEO+NaF; 70:30)
cell comparable to the other complexed films. This may be
due to the high ionic conductivity and higher degree of
amorphosity of this system when compared to other systems.
The cell parameters of the present electrolyte system are

comparable with the earlier work reported on different
polymer electrolyte systems [32, 33]. This supports the
practical application of the present electrolyte in solid-state
battery applications.

4. CONCLUSION
XRD patterns of the (PEO+NaF) showed the decrease of
intensity of peaks corresponding to pure PEO with the
increase of salt wt% ratio suggesting a decrease in the
crystallinity of the complex. The complexation of the NaF salt
with PEO polymer was confirmed by FTIR studies.

The conductivity was found to increase with increase of
dopant concentration and temperature in pure PEO as well as
in all compositions of (PEO+NaF) polymer electrolytes.
Optical absorption edge and optical band gaps (both direct and
indirect) showed a decreasing trend with increased
concentration of the dopant.

The ionic transport number data in the (PEO+NaF) polymer
electrolyte films indicate that the conduction is due to ions
rather than electrons. Using these films, electrochemical cells
were fabricated and the parameters of the cells are compared
with those reported by earlier workers. Thus, (PEO+NaF)
electrolytes are found to be worthy candidate for solid-state
batteries.

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