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Frequency and temperature-dependent impedance spectroscopy of PVA/PEG

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Original Article

High Performance Polymers

1–9
Frequency and temperature-dependent ª The Author(s) 2018
Reprints and permission:

impedance spectroscopy of PVA/PEG sagepub.co.uk/journalsPermissions.nav

DOI: 10.1177/0954008318774837
journals.sagepub.com/home/hip
polymer blend film

Rakhi Nangia, Neeraj K Shukla and Ambika Sharma

Abstract
In this work, polymer blend films based on polyvinyl alcohol (PVA)/poly(ethylene glycol) (PEG) were prepared by solution
casting technique. X-ray diffraction (XRD) analysis was performed to investigate the structural details of the polymer blend.
XRD pattern confirms the polycrystalline nature of the films. Sandwich structures of the type Ag-PVA/PEG-Ag were formed
to study the dielectric and conduction properties in the frequency range 300 Hz–3 MHz and at different temperatures
varying from 298 K to 420 K. Experimental results show that both dielectric constant ("0 ) and dielectric loss ("00 ) values were
strong functions of frequency and temperature. The AC conductivity (AC) was found to obey the power law A!s and
correlated barrier hopping as the conduction mechanism. The imaginary part of electric modulus shows peak shifting
corresponding to relaxation mechanisms. Electric modulus study was also found to support the dielectric permittivity data.

Keywords
Polyvinyl alcohol, dielectric loss, AC conductivity, electric modulus, dielectric relaxation

Introduction importance, impedance spectroscopy has been widely stud-

ied to find the frequency- and temperature-dependent elec-
The path to the development of all organic flexible electronic
trical properties and relaxation process of the material. In a
devices requires the definition of an organic gate insulator.
dielectric material, there may be two types of polarization,
The structure of dielectric strongly influences a device beha-
one because of hopping of localized charges from one site
viour. A large number of polymers such as polyvinylpyrroli-
to neighbouring sites called hopping polarization, and sec-
done (PVP), polymethyl methacrylate (PMMA) and
ond interfacial polarization due to mobile charged particles
polyvinyl alcohol (PVA) and polymer blends such as poly-
under the influence of an applied field.1
ethylenedioxythiophene: poly-styrenesulfonate-polyvinyl
Many articles have been reported on PEG/PVA blend
alcohol (PEDOT: (PSS)-PVA), PVP-PVA, polypyrrole-
including ionic impurities. Some of these systems are
poly(ethylene glycol) (PPy-PEG) and polymer electrolytes
fPVA-PEG:NaClO4g,4 fPVA-PEG:Mg(NO3)2g,7 fPVA-
have been tested as dielectric layers by researchers.1–5 Blend-
PEG:NH4SCNg8 and fPVA-PEO:AgNO3g,9 wherein the
ing implies mixing of two or more polymers physically and
effect of filler in the polymer blend on conductivity has
allows the creation of new material with specific properties
been studied. The researchers have discussed different
depending upon the composition.3 Blending is known to be
explanations on the improvement in conductivity with the
one of the most effective methods to improve the conductivity
incorporation of salt such as formation of charge transfer
and often results in better properties than the individual
complexes, decrease in the degree of crystallinity and
polymers.4
build-up of charge carriers and so on. Abd Alla et al. have
The dielectric and electrical properties of the materials
are important for its applications in devices like superca-
pacitors, field effect transistors and other components.5,6 School of Engineering and Technology, The NorthCap University,
Interesting electronic properties and easy processability Gurgaon, Haryana, India
of blended polymer suggest their use in organic devices
Corresponding author:
such as organic light emitting diodes (OLED), organic field Rakhi Nangia, School of Engineering and Technology, The NorthCap
effect transistors (OFET), solar cells, supercapacitors and University, Sec23A, Gurgaon, Haryana 122017, India.
so on. On the other hand, because of technological Email: mmrakhi@gmail.com
2 High Performance Polymers XX(X)
studied the effect of gamma radiation on the structural
properties of PVA-PEG blend and reported an increase in
the tensile mechanical properties of PVA with the addition
of PEG.10 All the above-mentioned studies have taken PEG
and PVA in equal concentration with ionic impurities in
blend structure, whereas in the present study, we have taken
pure blend structure of PEG-PVA with 20 wt% PEG in
PVA, and the dielectric studies of the prepared blend have
been compared with pure PVA which has not been reported
so far.
PVA was selected due to its high dielectric strength and
good charge storage capacity. Moreover, PVA shows
excellent film-forming properties, which leads to its appli-
cations in various devices.11–13 Simultaneously, PEG is a
water-soluble, flexible and low toxicity polymer that can be
used in many industrial, biomedical and biotechnological
applications due to its excellent physical and chemical
properties.14–16 PEG has also been applied as the gate insu-
lator in an electric double-layer transistor to induce super-
conductivity in an insulator. In view of the above, an
attempt has been made to develop a PEG-PVA blend and
to study its electrical and dielectric properties in the defined
frequency and temperature ranges using impedance
spectroscopy.
Experimental details
Materials and film preparation
Films of pure PVA and blend of PEG in PVA were pre-
pared by solution cast technique using deionized water as a
solvent. A 5 w/w% of aqueous PVA solution was prepared
by adding 5-g of PVA (Sigma Aldrich [St. Louis, MO,
USA], polymerization degree 1700–1800, hydrolysis
degree 98–99 mol%) in 95 ml of deionized water. The PVA
solution was heated and stirred at 90 C for 3–4 h. PEG
solutions were prepared by adding 0.25-g of PEG (Mn ¼
18,500, Aldrich Chemical Co., Inc., Milwaukee, Wiscon-
sin, USA) in 4.75 ml of deionized water. PEG dissolves in
water at a temperature lower than the room temperature.16
Therefore, the PEG solution was kept under water to bring
it at a temperature lower than the room temperature to
completely dissolve the polymer, while the PVA solution
was kept at room temperature before both the solutions
were mixed. Blends of 20 wt% PEG in PVA were prepared
by adding 5 ml of PEG solution to 20 ml of PVA solution.
The mixed PEG-PVA solution was slowly agitated and out
of 25 ml, 5 ml of solution was casted into glass Petri dish at
45 C and was kept in hot air oven for 24 h. Pure PVA film
was also casted in the same manner. The synthesized films
were peeled off from the dishes and kept in ziplock pouches
in a silica gel desiccator till further use. The thickness of the
obtained films was measured by micrometre and found to
be of nearly 100 mm. However, the appearance of the two
films is quite different. Pure PVA film was completely
Figure 1. XRD pattern of pure PVA and 20 wt% PEG-PVA blend
films. XRD: X-ray diffraction; PVA: polyvinyl alcohol; PEG: poly
(ethylene glycol).
transparent and colourless, while PEG-PVA blend film was
opaque and somewhat white in colour.
XRD and impedance spectroscopy
The nature of these polymer blend films was investigated
with X-ray diffraction (XRD) technique. PANalytical X
Pert Pro XRD (The Netherlands) with copper K radiation
( ¼ 1.5406 Å) has been used in 2 range from 10 to 90 .
To perform the electrical characterization, the film samples
were cut into rectangular pieces, and electrical contacts
were made on both sides of the film using conductive silver
paste. Sandwich structures of the type Ag-PVA-Ag and Ag-
PVA/PEG-Ag were formed, and the temperature- and
frequency-dependent behaviour is recorded using program-
mable HIOKI 3532-50 LCR Hi Tester (Nagano, Japan),
interfaced with a computer. The measurements were per-
formed in the frequency range 300 Hz–3 MHz at different
temperatures varying from 298 K to 420 K. Logarithmic
frequency readings were used as measurement frequen-
cies.1 A constant amplitude voltage was applied across the
film for maintaining the voltage difference between the two
electrodes.
Results and discussion
Structural characterization
XRD studies. Figure 1 shows the XRD patterns of pure PVA
and 20-wt% PEG-PVA blend films. Figure 1 shows broad
halos at 2 ¼ 19.4 for pure PVA and at 19.4 and 23.5 for
PEG-PVA blend film. These halos are attributed to (111)
and (210) crystal planes, respectively. The broad halos
observed in the XRD pattern and the absence of sharp
peaks indicate the semi-crystalline nature of the samples
and also suggest that the sample contains crystalline as well
as amorphous phases. However, the absence of sharp dif-
fraction peaks in the films indicates dominancy of
Nangia et al.
Table 1. Tabulation of the d-spacing (ds) and crystallite size (D) values for pure PVA and 20 wt% PEG-PVA blend film.
Sample 2 ( ) FWHM (, 2)
Pure PVA 19.48 0.8640
20 wt% PEG-PVA blend film 19.42 0.8266
PVA: polyvinyl alcohol; PEG: poly(ethylene glycol); FWHM: full width at half maximum.
Figure 2. Variation of dielectric constant as a function of frequency at different temperatures for (a) pure PVA and (b) 20 wt% PEG-
PVA blend films. PVA: polyvinyl alcohol; PEG: poly(ethylene glycol).
amorphous phase which may result in greater ionic
conductivity.4
The d-spacing values (ds) (using Bragg’s equation n ¼
2dsSin ) were calculated for both the films using the first-
order reflection. The mean crystallite size was also calcu-
lated using Debye–Scherrer equation as given below and
tabulated in Table 1
K
D¼ ð1Þ
Cos 
where D is the mean crystallite size,  is the X-ray
wavelength,  is the full width at half maximum
(FWHM) of the peak corresponding to plane (111), k
is the so-called shape factor or Scherrer constant which
usually takes a value of about 0.9 and  is the diffrac-
tion angle corresponding to the maximum intensity peak
in XRD pattern. From Table 1, it is observed that crys-
tallite size is higher for PEG-PVA blend film. This may
be attributed to lower FWHM value. The increase in
crystallite size also indicates an increase in the dielec-
tric constant of the sample.17
The polycrystallinity observed in XRD pattern indicates
an increase in the ordering of atoms from short-range order-
ing to long-range ordering.18 This also accounts for the
increased crystallite size in PEG-PVA blend film. Due to
the formation of more ordered structure, dipoles are
oriented on the application of electric field which in turn
increases the capacity of charge storage. This consequently
increases the dielectric constant.
3
Crystallite size (D, Å) d-Spacing (ds, Å)
1.6285 4.5531
1.7021 4.5680
Impedance spectroscopy
Dielectric constant. The complex permittivity (" ) is defined
by its real and imaginary parts as follows
0 00
" ¼ "  j" ð2Þ
0 00
where " is the dielectric constant and " is the dielectric
0
loss. Dielectric constant " is determined by using the
relation
0 dC
" ¼ ð3Þ
"0 A
where C is the parallel capacitance of the film, "0 is the
permittivity of free space ("0 ¼ 8.854  1012 F/m), and d
and A are thickness and area of the sample, respectively.
Figure 2(a) and (b) shows frequency (f) dependence of
dielectric constant in 298–420 K temperature range for
pure PVA and PEG-PVA blend films.
From the figures, it is observed that dielectric constant
increases with increase in temperature. This is due to the
fact that at lower temperatures the dipoles remain freezed.
But as the temperature increases, they orient themselves in
response to the applied electric field which results in higher
polarization and consequently higher dielectric constant
0
values are observed.19 Therefore, high " at higher tempera-
ture is due to oriental polarization. On the other hand,
Figure 2 also shows a decrease in dielectric response with
increase in frequency.
At lower frequencies, dipoles have sufficient time to get
aligned with the electric field and thus results in higher
4 High Performance Polymers XX(X)

Figure 3. Plot of loss tangent ðtanÞ with frequency at different temperatures for (a) pure PVA and (b) 20 wt% PEG-PVA blend film.
PVA: polyvinyl alcohol; PEG: poly(ethylene glycol).

polarization. This leads to an increase in dielectric constant

0
(" Þ. Similar trend was observed by Makled et al. for PVA/
copper iodide (CuI) polymer composite.20 Interfacial polar-
ization occurs up to the frequency limit of 3 kHz. At higher
frequencies, dielectric permittivity decreases due to the
inability of dipoles to align themselves with the rapidly
changing applied field.21
The imaginary part of complex dielectric constant deter-
mines the dielectric loss ("00 ) given by
00 0
" ¼ " tan  ð4Þ
In the above equation, tan is the dielectric parameter
that describes the maximum loss of the system occurring at
a frequency called relaxation frequency. The variation of
tan with frequency has been shown in Figure 3(a) and (b)
Figure 4.  versus T1 for pure PVA and 20 wt% PEG-PVA blend
for pure PVA and 20 wt% PEG-PVA blend film, respec- film. PVA: polyvinyl alcohol; PEG: poly(ethylene glycol).
tively, at different temperatures. From the figure, it is clear
that values of tan are slightly higher at lower frequency for
pure PVA film than for blended polymer. It can also be In the above equation, 1 is the time constant of relaxa-
observed from the figure that as temperature increases, tion at infinite temperature, Et is the activation energy, K is
there is peak shifting towards the higher frequency which the Boltzmann constant and T is the temperature in K. From
may be associated with relaxation time. the plot, it is observed that relaxation time decreases with
Relaxation time () is the inverse of the relaxation fre- increasing temperature. Further, it is observed that at any
quency expressed by the following relation22 temperature, the relaxation time for PEG-PVA blend is
more than that for pure PVA. This may be due to the crys-
1
¼ ð5Þ tallinity of the film which constrains the rotatory motion of
2 fpeak
the dipoles and thus increases the relaxation time.
00
where f peak is the frequency at which tangent loss is The frequency variation of " at different temperatures
maximum. for pure PVA and PEG-PVA films has been shown in
Figure 4 shows the variation of relaxation time  with Figure 5(a) and (b), respectively. From the plots, it is evi-
T1 for pure PVA and 20 wt% PEG-PVA blend film. The dent that both pure PVA and PEG-PVA blend have high
plot obeys the Boltzmann temperature-dependent dielectric dielectric loss at lower frequencies, but as frequency
00
relaxation equation increases, " decreases and attains nearly a constant value
00
  at higher frequency. Change in " with frequency and tem-
Et perature may be attributed to the movement of charged
T ¼ 1 exp ð6Þ
KT carriers and relaxation mechanism of the material.23
Nangia et al. 5

Figure 5. Variation of imaginary part of dielectric constant as a function of frequency at different temperatures for (a) pure PVA and
(b) 20 wt% PEG-PVA blend film. PVA: polyvinyl alcohol; PEG: poly(ethylene glycol).

Figure 6. Nyquist plot of dielectric constant for (a) pure PVA and (b) 20 wt% PEG-PVA blend film. PVA: polyvinyl alcohol;
PEG: poly(ethylene glycol).

Nyquist plots. In order to ascertain the extent to which the
00
loss peaks could be described by Debye process, " has
0
been plotted against " . Figure 6(a) and (b) depicts the
00 0
Nyquist or Cole–Cole plot ð" vs: " Þ for pure PVA and
PEG-PVA blend at different temperatures. The plot shows
part of semicircle or broad ended arc in the defined range
whose centre was found to be depressed somewhat below
the real axis that shows the relaxation behaviour of the
dielectric is not perfectly Debye and there is distribution
of relaxation time as well as polarization mechanism. Sim-
ilar plots have been observed for PVA/PVP blend by Desh-
mukh et al.2 and for PEDOT:PSS/PVA blend by Chen
et al.1 The complex dielectric constant is given by
8 9
< of relaxation time due to losses in the material. For pure
" rs  " r1 =
0 0
0
"r ¼ " r1 þ  ð7Þ
: 1 þ ðj!Þ1 Þ;
0 0
where " r1 and " rs are high- and low-frequency values of
dielectric constant, respectively,  is the relaxation time
and  is the inclination of the semicircle and is a measure
of distribution of relaxation time. Lower value of  indi-
cates fairly narrow distribution of relaxation time. The dis-
tribution of  is reflected in the frequency spread in tan
peaks as illustrated in Figure 3. The semicircle observed in
the high-frequency region is due to parallel combination of
bulk resistance and bulk capacitance.1 From the plot, it can
be observed that as the temperature increases, the diameter
of semicircle or arc decreases for pure PVA as well as for
PEG-PVA blend that may be attributed to the decrease in
bulk capacitance with the increase in temperature. From the
plot of Figure 6(b), it is also observed that at higher tem-
perature (420 K), there is a tail portion in the low-frequency
region for PEG-PVA blend film. This indicates distribution
PVA, no tail portion is visible in the given range even at
higher temperature that shows blend film becomes a little
lossy at higher temperature than that of pure PVA film.
The value of low- and high-frequency limits of dielec-
0 0
tric constant " rs and " r1 , respectively, can be found by
6 High Performance Polymers XX(X)
Figure 7. Plot of ln AC versus ln f for (a) pure PVA and (b) 20 wt% PEG-PVA blend film. PVA: polyvinyl alcohol; PEG: poly(ethylene
glycol).
completing the semicircle or the arc and finding the value
of intercept at the x-axis.
Frequency and temperature-dependent AC conductivity. The
total measured conductivity (t) of the samples has been
calculated from the dielectric loss values according to the
following relation
t ¼ !"0 "00 ð8Þ
According to Jonscher’s law, the total measured conduc-
tivity of the materials can be separated in two terms as
given below19
t ¼ DC þ AC ¼ DC þ 0 f s ð9Þ
In the above equation, DC is the DC conductivity,
which is frequency independent, while the AC conductivity
AC is frequency dependent and follows a power law with
‘s’ as frequency exponent parameter.13 Subtracting DC and
taking natural logarithm on both sides, AC conductivity can
be written as
ln AC ¼ ln 0 þ s ln f ð10Þ
Figures 7(a) and 6(b) show the plot of ln AC versus ln
f for pure PVA and PEG-PVA blend, respectively, at
different temperatures. These plots are fitted to straight
lines and the slope of straight lines gives the value of ‘s’,
while the intercept of straight lines on the y-axis gives
the value of DC conductivity. It is also observed that
conductivity increases with frequency, and this may be
attributed to ionic hopping mechanism.24 The values of
‘s’ were found to vary between 0.12–0.8 for pure PVA
and 0.29–0.94 for PEG-PVA blend. These values have
been plotted against the temperature for blend film and
has been depicted in the inset of Figure 7(b). The value
of s is found to decrease with the increase in temperature
which suggests that both samples obey correlated barrier
hopping (CBH) model. CBH model relates s and T and
can be written as19
6KT
s¼1h  i ð11Þ
!m  KT ln !1 0
where K is the Boltzmann constant (1.3807  1023 J/K)
and !m is the barrier height. !m value can be determined
from the slope of plot s versus temperature and is found to
be 0.11 eV for 20 wt% PEG-PVA blend. It can be observed
that AC conductivity increases with temperature especially
more at lower frequencies as compared to higher frequen-
cies. This may be attributed to the DC conductivity contri-
bution at low frequencies. As the frequency increases, AC
conductivity dominates which is comparatively less
temperature-dependent especially for 20 wt% PEG-PVA
blend film as clear from the plot of Figure 7(b). This shows
that thermal stability is higher for PEG-PVA blend film.
Figure 8(a) shows variation of total conductivity with
frequency at 318 K for pure PVA and 20 wt% PEG-PVA
blend film, and Figure 8(b) shows plot for T at 10 kHz for
both the films. From Figure 8(a), it is observed that the
conductivity of both the films increases with frequency and
the conductivity of the blend film is greater than that of the
pure PVA film, which may be due to the plasticizing effect
of PEG that increases the mobility of polymer chain and
hence the conductivity.25 Similarly, from Figure 8(b) it is
evident that T strongly depends on temperature and fol-
lows Arrhenius equation given by19,26
 
Ec
T ¼ 0 exp ð12Þ
KT
Here 0 is the pre-exponential factor, Ec is the activation
energy and K is the Boltzmann constant. It is also noted that
these plots (Figure 8(b)) have two slopes which indicate
that both samples do not have a single activation energy but
a range of activation energies.
Electric modulus variation with frequency at different
temperatures. Complex electric modulus has also been
Nangia et al. 7

Figure 8. (a) t versus frequency (at 318 K) and (b) ln T versus T1 at 10 kHz for pure PVA and 20 wt% PEG-PVA blend film.
PVA: polyvinyl alcohol; PEG: poly(ethylene glycol).

Figure 9. Plotting of the frequency dispersions of the real part of the electric modulus for (a) pure PVA and (b) 20 wt% PEG-PVA blend
film. PVA: polyvinyl alcohol; PEG: poly(ethylene glycol).

studied to get the bulk response of the films and dielectric zero value in the low-frequency region, whereas as fre-
relaxation mechanism. Dielectric relaxation refers to the quency increases, it shows a step-like transition without
delay in response of a dielectric medium to a changing any peak. This may be attributed to the bulk effect and
stimulus.27,28 indicates the energy storing capability of the material.1
At higher temperatures, dielectric permittivity becomes Very low values of M0 in the low-frequency region corre-
very high due to electrode polarization. For that reason, the spond to negligible electrode polarization. The plot of M00
complex permittivity (" ) data have been transformed into exhibits peak that corresponds to the time constant of the
the complex electric modulus (M  ) according to the rela- circuit model. M00 spectra of pure PVA and PEG-PVA
tion given below28 blend polymer samples show relaxation peaks correspond-
0 00 ing to ionic conduction relaxation, that is, interfacial polar-
1 0 00 " " ization relaxation process. As the temperature increases,
M ¼ ¼ M þ jM ¼ 02 þ j 02 ð13Þ
" " þ "00 2 " þ "00 2 the position of peak shifts towards high-frequency side and
where M0 and M00 are real and imaginary parts of complex this is the reason that peaks are not visible in the given
electric modulus, respectively. frequency range above 358 K for pure PVA film. However,
Figures 9 and 10 show the frequency-dependent varia- for PEG-PVA blend film, peaks are visible for higher tem-
tions of real (M0 ) and imaginary parts (M00 ) of the electric peratures as well. It has also been observed that relaxation
modulus, respectively, at different temperatures for pure curve is broader in case of pure PVA which corresponds to
PVA and PEG-PVA blend films. From the figure, it is deviation from Debye response.19 This also indicates the
observed that as the temperature increases, M0 approaches change in relaxation mechanism for the PEG-PVA blend
8 High Performance Polymers XX(X)
Figure 10. Plotting of the frequency dispersions of the imaginary part of the electric modulus for (a) pure PVA and (b) 20 wt% PEG-
PVA blend film. PVA: polyvinyl alcohol; PEG: poly(ethylene glycol).
film than for pure PVA film. Peak shifting with the increase
in temperature may be due to availability of more thermally
generated charge carriers.
Conclusion
The present article reports the temperature- and frequency-
dependent electrical and dielectric properties of pure PVA
and 20 wt% PEG-PVA film synthesized by solution casting
technique. Pure PVA film was found to be transparent,
while PEG-PVA blend film was opaque. It has been
observed that the addition of PEG into PVA results in
comparatively higher effective permittivity at lower tem-
peratures, but as the temperature increases, effective per-
mittivity approaches comparative values for both samples
under study. CBH has been found to be the main charge
transport mechanism for the two films and conductivity is
found to be higher for PEG-PVA blend film than that of
pure PVA. Different formalisms like complex permittivity
and complex dielectric modulus are obtained to study the
dielectric behaviour of the polymer films. The high dielec-
tric constant and electric modulus behaviour indicates
higher energy storing capability of the material which sug-
gest applications of these films as an interlayer dielectric in
organic electronic devices.
Acknowledgement
The authors thank The NorthCap University Gurgaon (Formerly
ITM University, Gurgaon) for providing necessary research facil-
ities during this research work.
Declaration of Conflicting Interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship and/or publication of this
article.
Funding
The author(s) received no financial support for the research,
authorship and/or publication of this article.
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