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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 Figure 1. XRD pattern of pure PVA and 20 wt% PEG-PVA blend
water-soluble, flexible and low toxicity polymer that can be films. XRD: X-ray diffraction; PVA: polyvinyl alcohol; PEG: poly
used in many industrial, biomedical and biotechnological (ethylene glycol).
applications due to its excellent physical and chemical
properties.14–16 PEG has also been applied as the gate insu- transparent and colourless, while PEG-PVA blend film was
lator in an electric double-layer transistor to induce super- opaque and somewhat white in colour.
conductivity in an insulator. In view of the above, an
attempt has been made to develop a PEG-PVA blend and XRD and impedance spectroscopy
to study its electrical and dielectric properties in the defined
frequency and temperature ranges using impedance The nature of these polymer blend films was investigated
spectroscopy. 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 .
Experimental details To perform the electrical characterization, the film samples
were cut into rectangular pieces, and electrical contacts
Materials and film preparation were made on both sides of the film using conductive silver
Films of pure PVA and blend of PEG in PVA were pre- paste. Sandwich structures of the type Ag-PVA-Ag and Ag-
pared by solution cast technique using deionized water as a PVA/PEG-Ag were formed, and the temperature- and
solvent. A 5 w/w% of aqueous PVA solution was prepared frequency-dependent behaviour is recorded using program-
by adding 5-g of PVA (Sigma Aldrich [St. Louis, MO, mable HIOKI 3532-50 LCR Hi Tester (Nagano, Japan),
USA], polymerization degree 1700–1800, hydrolysis interfaced with a computer. The measurements were per-
degree 98–99 mol%) in 95 ml of deionized water. The PVA formed in the frequency range 300 Hz–3 MHz at different
solution was heated and stirred at 90 C for 3–4 h. PEG temperatures varying from 298 K to 420 K. Logarithmic
solutions were prepared by adding 0.25-g of PEG (Mn ¼ frequency readings were used as measurement frequen-
18,500, Aldrich Chemical Co., Inc., Milwaukee, Wiscon- cies.1 A constant amplitude voltage was applied across the
sin, USA) in 4.75 ml of deionized water. PEG dissolves in film for maintaining the voltage difference between the two
water at a temperature lower than the room temperature.16 electrodes.
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 Results and discussion
was kept at room temperature before both the solutions
were mixed. Blends of 20 wt% PEG in PVA were prepared
Structural characterization
by adding 5 ml of PEG solution to 20 ml of PVA solution. XRD studies. Figure 1 shows the XRD patterns of pure PVA
The mixed PEG-PVA solution was slowly agitated and out and 20-wt% PEG-PVA blend films. Figure 1 shows broad
of 25 ml, 5 ml of solution was casted into glass Petri dish at halos at 2 ¼ 19.4 for pure PVA and at 19.4 and 23.5 for
45 C and was kept in hot air oven for 24 h. Pure PVA film PEG-PVA blend film. These halos are attributed to (111)
was also casted in the same manner. The synthesized films and (210) crystal planes, respectively. The broad halos
were peeled off from the dishes and kept in ziplock pouches observed in the XRD pattern and the absence of sharp
in a silica gel desiccator till further use. The thickness of the peaks indicate the semi-crystalline nature of the samples
obtained films was measured by micrometre and found to and also suggest that the sample contains crystalline as well
be of nearly 100 mm. However, the appearance of the two as amorphous phases. However, the absence of sharp dif-
films is quite different. Pure PVA film was completely fraction peaks in the films indicates dominancy of
Nangia et al. 3

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) Crystallite size (D, Å) d-Spacing (ds, Å)

Pure PVA 19.48 0.8640 1.6285 4.5531

20 wt% PEG-PVA blend film 19.42 0.8266 1.7021 4.5680
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 Impedance spectroscopy

conductivity.4
Dielectric constant. The complex permittivity (" ) is defined
The d-spacing values (ds) (using Bragg’s equation n ¼
by its real and imaginary parts as follows
2dsSin ) were calculated for both the films using the first-
0 00
order reflection. The mean crystallite size was also calcu- " ¼ "  j" ð2Þ
lated using Debye–Scherrer equation as given below and 0 00
where " is the dielectric constant and " is the dielectric
tabulated in Table 1 0
loss. Dielectric constant " is determined by using the
K relation
D¼ ð1Þ
Cos  0 dC
" ¼ ð3Þ
where D is the mean crystallite size,  is the X-ray "0 A
wavelength,  is the full width at half maximum where C is the parallel capacitance of the film, "0 is the
(FWHM) of the peak corresponding to plane (111), k permittivity of free space ("0 ¼ 8.854  1012 F/m), and d
is the so-called shape factor or Scherrer constant which and A are thickness and area of the sample, respectively.
usually takes a value of about 0.9 and  is the diffrac- Figure 2(a) and (b) shows frequency (f) dependence of
tion angle corresponding to the maximum intensity peak dielectric constant in 298–420 K temperature range for
in XRD pattern. From Table 1, it is observed that crys- pure PVA and PEG-PVA blend films.
tallite size is higher for PEG-PVA blend film. This may From the figures, it is observed that dielectric constant
be attributed to lower FWHM value. The increase in increases with increase in temperature. This is due to the
crystallite size also indicates an increase in the dielec- fact that at lower temperatures the dipoles remain freezed.
tric constant of the sample.17 But as the temperature increases, they orient themselves in
The polycrystallinity observed in XRD pattern indicates response to the applied electric field which results in higher
an increase in the ordering of atoms from short-range order- polarization and consequently higher dielectric constant
0
ing to long-range ordering.18 This also accounts for the values are observed.19 Therefore, high " at higher tempera-
increased crystallite size in PEG-PVA blend film. Due to ture is due to oriental polarization. On the other hand,
the formation of more ordered structure, dipoles are Figure 2 also shows a decrease in dielectric response with
oriented on the application of electric field which in turn increase in frequency.
increases the capacity of charge storage. This consequently At lower frequencies, dipoles have sufficient time to get
increases the dielectric constant. 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 and  is the inclination of the semicircle and is a measure
00
loss peaks could be described by Debye process, " has of distribution of relaxation time. Lower value of  indi-
0
been plotted against " . Figure 6(a) and (b) depicts the cates fairly narrow distribution of relaxation time. The dis-
00 0
Nyquist or Cole–Cole plot ð" vs: " Þ for pure PVA and tribution of  is reflected in the frequency spread in tan
PEG-PVA blend at different temperatures. The plot shows peaks as illustrated in Figure 3. The semicircle observed in
part of semicircle or broad ended arc in the defined range the high-frequency region is due to parallel combination of
whose centre was found to be depressed somewhat below bulk resistance and bulk capacitance.1 From the plot, it can
the real axis that shows the relaxation behaviour of the be observed that as the temperature increases, the diameter
dielectric is not perfectly Debye and there is distribution of semicircle or arc decreases for pure PVA as well as for
of relaxation time as well as polarization mechanism. Sim- PEG-PVA blend that may be attributed to the decrease in
ilar plots have been observed for PVA/PVP blend by Desh- bulk capacitance with the increase in temperature. From the
mukh et al.2 and for PEDOT:PSS/PVA blend by Chen plot of Figure 6(b), it is also observed that at higher tem-
et al.1 The complex dielectric constant is given by perature (420 K), there is a tail portion in the low-frequency
region for PEG-PVA blend film. This indicates distribution
8 9
< of relaxation time due to losses in the material. For pure
" rs  " r1 =
0 0
0
"r ¼ " r1 þ  ð7Þ PVA, no tail portion is visible in the given range even at
: 1 þ ðj!Þ1 Þ; higher temperature that shows blend film becomes a little
0 0
lossy at higher temperature than that of pure PVA film.
where " r1 and " rs are high- and low-frequency values of The value of low- and high-frequency limits of dielec-
0 0
dielectric constant, respectively,  is the relaxation time 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

6KT
of intercept at the x-axis. s¼1h  i ð11Þ
!m  KT ln !1 0
Frequency and temperature-dependent AC conductivity. The where K is the Boltzmann constant (1.3807  1023 J/K)
total measured conductivity (t) of the samples has been and !m is the barrier height. !m value can be determined
calculated from the dielectric loss values according to the from the slope of plot s versus temperature and is found to
following relation be 0.11 eV for 20 wt% PEG-PVA blend. It can be observed
t ¼ !"0 "00 ð8Þ that AC conductivity increases with temperature especially
more at lower frequencies as compared to higher frequen-
According to Jonscher’s law, the total measured conduc- cies. This may be attributed to the DC conductivity contri-
tivity of the materials can be separated in two terms as bution at low frequencies. As the frequency increases, AC
given below19 conductivity dominates which is comparatively less
t ¼ DC þ AC ¼ DC þ 0 f s ð9Þ temperature-dependent especially for 20 wt% PEG-PVA
blend film as clear from the plot of Figure 7(b). This shows
In the above equation, DC is the DC conductivity,
that thermal stability is higher for PEG-PVA blend film.
which is frequency independent, while the AC conductivity
Figure 8(a) shows variation of total conductivity with
AC is frequency dependent and follows a power law with
frequency at 318 K for pure PVA and 20 wt% PEG-PVA
‘s’ as frequency exponent parameter.13 Subtracting DC and
blend film, and Figure 8(b) shows plot for T at 10 kHz for
taking natural logarithm on both sides, AC conductivity can
both the films. From Figure 8(a), it is observed that the
be written as
conductivity of both the films increases with frequency and
ln AC ¼ ln 0 þ s ln f ð10Þ the conductivity of the blend film is greater than that of the
Figures 7(a) and 6(b) show the plot of ln AC versus ln pure PVA film, which may be due to the plasticizing effect
f for pure PVA and PEG-PVA blend, respectively, at of PEG that increases the mobility of polymer chain and
different temperatures. These plots are fitted to straight hence the conductivity.25 Similarly, from Figure 8(b) it is
lines and the slope of straight lines gives the value of ‘s’, evident that T strongly depends on temperature and fol-
while the intercept of straight lines on the y-axis gives lows Arrhenius equation given by19,26
the value of DC conductivity. It is also observed that  
Ec
conductivity increases with frequency, and this may be T ¼ 0 exp ð12Þ
KT
attributed to ionic hopping mechanism.24 The values of
‘s’ were found to vary between 0.12–0.8 for pure PVA Here 0 is the pre-exponential factor, Ec is the activation
and 0.29–0.94 for PEG-PVA blend. These values have energy and K is the Boltzmann constant. It is also noted that
been plotted against the temperature for blend film and these plots (Figure 8(b)) have two slopes which indicate
has been depicted in the inset of Figure 7(b). The value that both samples do not have a single activation energy but
of s is found to decrease with the increase in temperature a range of activation energies.
which suggests that both samples obey correlated barrier
hopping (CBH) model. CBH model relates s and T and Electric modulus variation with frequency at different
can be written as19 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 Funding
in temperature may be due to availability of more thermally The author(s) received no financial support for the research,
generated charge carriers. authorship and/or publication of this article.

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