Journal of Saudi Chemical Society 27 (2023) 101743

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Original article

Investigation on polyvinyl alcohol and sodium alginate blend matrix

with ammonium nitrate conducting electrolytes for electrochemical
applications
R. Jansi a,c, Boligarla Vinay b, M.S. Revathy a,⇑, V. Aruna Janani b, P. Sasikumar d,⇑, Mohamed Abbas e
a
Department of Physics, School of Advanced Sciences, Kalasalingam Academy of Research and Education, Krishnankoil 626126, Virudhunagar, Tamil Nadu, India
b
Department of Chemical Engineering, School of Bio, Chemical and Processing Engineering, Kalasalingam Academy of Research and Education, Krishnankoil 626126, Virudhunagar,
Tamil Nadu, India
c
Multifunctional Materials Laboratory, International Research Centre, Kalasalingam Academy of Research and Education, Krishnankoil 626126, Virudhunagar, Tamil Nadu, India
d
Department of Physics, Saveetha School of Engineering, SIMATS, Thandalam, Chennai 602105, India
e
Electrical Engineering Department, College of Engineering, King Khalid University, Abha 61421, Saudi Arabia

a r t i c l e i n f o a b s t r a c t

Article history: Polyvinyl alcohol (PVA) Sodium alginate (NaAlg) polymer composites were synthesized by solution cast-
Received 23 June 2023 ing technique and doping with ammonium nitrate (NH4NO3). The functionalization structure of the pro-
Revised 13 September 2023 duced electrolytes was investigated using XRD and AC impedance spectroscopy. XRD confirms
Accepted 27 September 2023
amorphous nature. The ionic conductivity of the electrolytes is evaluated using ac impedance measure-
Available online 4 October 2023
ments at temperatures ranging from 303 to 353 K. PVA: NaAlg: NH4NO3 (60:40:15 wt%) blend polymer
electrolyte was observed to have the highest conductivity of 1.05
106 S cm1. The Arrhenius plot
Keywords:
appears to be obeyed by the temperature dependent ionic conductivity and is of non-debye type.
Solution casting
Biopolymer
Activation energy for best conducting electrolyte was 0.2364 eV. The dielectric relaxation of the polymer
Powder-XRD electrolyte has been studied, and the results are described. Relaxation time estimated from loss tangent
AC Impedance analysis also affirms that value is low for highest conducting sample. Results of CV and LSV studies gave a
Ionic conductivity plausible approach for electrochemical application.
Sodium alginate Ó 2023 The Author(s). Published by Elsevier B.V. on behalf of King Saud University. This is an open access
article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction Solid electrolyte(SE) has gained more focus from researchers

High performance batteries are becoming more and more vital
in today’s society as faster, lighter, and significantly less expensive,
portable and new battery packs become essential for daily use.
Currently, huge energy retention systems are needed to effectively
conserve the electrical energy generated from various sources. A
portable power network implies the selection of a material which
is minimal in cost, secure, and ableness of storing greater energy
[1–3].
⇑ Corresponding authors.
E-mail addresses: revz27vijay@gmail.com (M.S. Revathy), sasijanaki123@gmail.
com (P. Sasikumar).
Peer review under responsibility of King Saud University. Production and hosting by
Elsevier
Production and hosting by Elsevier
than liquid electrolyte due to its superior consistency, low weight,
lack of leaking issues, adjustable shape, exceptional protected
functionality, excellent biocompatibility with electrode, and envi-
ronmentally friendly nature. Despite its low electronic conductiv-
ity, the SE has potential uses in electrochemical devices including
power steering, diesel generator, batteries, and super capacitors.
Even then, a revolution in cell manufacturing has been brought
about by conducting polymers electrolyte in the past decades [4,5].
Polymeric electrolytes have several benefits, including excellent
mechanical qualities, simplicity of manufacture of thin films of
suitable sizes, and the ability to create emphasis on technical elec-
trolyte interaction. Numerous strategies were employed to raise
their conductivity to a desirable level for applications. This com-
prises the use of biopolymer, the inclusion of harmless nanoparti-
cles insulating matrix, an addition of plasticizers, the incorporation
of salts with substantial ionic species, as well as the mixing of two
polymers [6–8].
In recent years, researchers have concentrated on the improve-
ment of solid polymer blend electrolytes (SPBE) made with syn-

https://doi.org/10.1016/j.jscs.2023.101743
1319-6103/Ó 2023 The Author(s). Published by Elsevier B.V. on behalf of King Saud University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
R. Jansi, B. Vinay, M.S. Revathy et al.
thetic polymer such as Polyethylene oxide (PEO),polyacrylic acid
(PAA), Polyvinyl pyrrolidone (PVP), Polyvinyl chloride (PVC),Poly-
acrylonitrile (PAN), Polyethylene glycol (PEG), Polymethyl
methacrylate (PMMA), Poly-o-methoxyaniline (POMA), Poly 3-
thiophene acetic acid (PTAA) and Poly 3,4 ethylenedioxythiophene
(PEDOT). However synthetic polymers have several drawbacks
such as being poisonous, more costly, and not environmentally
sustainable [9,10].
The development of proton conducting and ion conducting elec-
trolytes employing PVA as the parent polymer has been the subject
of several research studies. PVA, a synthetic semi-crystalline struc-
tured polymer. The semi-crystalline form of PVA must be con-
verted into amorphous utilising the suitable salts, solvents,
binders, or blending material substrate in order to prepare conduc-
tive polymer solid electrolyte by PVA as the polymeric matrix.
These electrolytes truly relate to PVA/salt combination devoid of
solvent. When the temperature is ambient, the electrolytes show
a certain conductivity 107103 S/cm [11–13].
Alginates, a biopolymer contain sodium and calcium ions also
were used first in a variety of agricultural, textile, medicinal, and
commercial processes. Previously the researchers developed elec-
trolyte through various biopolymer, as blend substrates such as
gelatine, agar, starch, chitosan, Dextran, carboxymethyl cellulose.
Sodium alginate (NaAlg) is a polyelectrolyte with superior proper-
ties; yet, it has manufacturing constraints. Their structural quali-
ties are frequently weak, limiting their applicability [14,15].
Ammonium Nitrate has a high contribution in ionization that can
allow proton conduction across a SPBE lattice and increase ionic
conductivity in a SPBE system. For this study, NH4NO3 was used
as a salt-to-polymer electrolyte to improve ion (H+) conductivity
in the polymer blend electrolytes system.
Table 1
Sample code and designation of the prepared SPBEs.
Sample Composition
(wt.%)
PVA:NaAlg:NH4NO3 60:40:5
PVA:NaAlg:NH4NO3 60:40:10
PVA:NaAlg:NH4NO3 60:40:15
PVA:NaAlg:NH4NO3 60:40:20
Fig. 1. Schematic illustration of the preparation of the PVA/NaAlg and the dopant NH4NO3 polymer blend electrolytes.
Journal of Saudi Chemical Society 27 (2023) 101743
Polymer-biopolymeric blends has been a focus in recent years.
C. Nithya Priya et al. 2023 has reported polyvinyl alcohol and cas-
sava/starch synthesized by solution casting process, exhibited a
conductivity of 1.53
105 S/cm [9]. Ghazali, N. M., et al. 2022
[16] has incorporated bio-polymer blend electrolytes (BBEs) of
PVA/alginate with ammonium nitrate, possessed an amorphous
phase and the conductivity reported was 5.20
104 S cm1,
and Fuzlin, A. F., 2022 et al. has reported 1.29
104 S cm1 for
ammonium iodide [17]. Saadiah et al. 2021 employed car-
boxymethyl cellulose (CMC)/polyvinyl alcohol (PVA)–NH4NO3
blended with PEG(polyethylene glycol) and EC possess
3.92
103 S/cm [18]. Rasali et al. 2019 presented biopolymer
alginate doping with NH4NO3 under solid biopolymer electrolyte
system with an ionic conductivity 5.56
105 S cm1 [19].
T. Sheela et al 2016 reported 1.83
104 S/cm conductivity for
Poly vinyl alcohol (PVA)/sodium alginate (NaAlg) polymer compos-
ites, were developed via includes the implementation and doped
with lithium perchlorate salt [20].
In the field of polymer electrolyte preparation, solution casting
is one of the earliest methods. Although SC is still widely used to
produce thin membranes of high quality, the following conditions
must be met while using the polymer: the polymer must dissolve
in water or another liquid solvent, the solution must reach a spec-
ified viscosity, and the PEs must be homogeneous and easy to
convert.
Owing to the aforementioned merits, current research focus is
on solid blend polymer electrolytes. Polyvinyl alcohol (synthetic
polymer), Sodium alginate (biopolymer) have blended over with
ammonium nitrate salt [21,22]. Therefore, in this study NH4NO3
has been added to PVA/NaAlg to determine the optimal concentra-
tion for generating a highly ion-conductive biopolymer electrolyte.
2. Material and method
Code
2.1. Material
PNN1
PNN2 PVA purchased from otta chemical private Ltd molecular weight
PNN3
(MW) = 44.19 g/mol, NaAlg (MW = 198.11 g/mol) received from
PNN4
Sigma-Aldrich and NH4NO3 MW = 80.043 g/mol (procured from
2
R. Jansi, B. Vinay, M.S. Revathy et al.
Avra Chem Ltd.) were used as materials. The solvent employed in
this formulation was distilled water.
2.2. Synthesis of electrolyte
Different ratio (100:0) (80:20) (60:40) (40:60) (20:80) (0:100)
of PVA:NaAlg to prepared a polymer electrolyte. Using Ac Impe-
dance and XRD we confirmed the optimized blend ratio as
(60:40) was best. Optimized blend polymer was observed to be
PVA(60 wt%) and NaAlg (40 wt%)This was used throughout the
synthesis of electrolytes with different concentrations of NH4NO3
(5,10,15 and 20% respectively) added PVA blend NaAlg. In this elec-
trolyte was prepared by using solution casting method. Table 1
lists the sample code and designation of the prepared SPBEs. PVA
and NH4NO3 salt solution mixture was prepared separately in dis-
tilled water (solvent), at the same time NaAlg stirred separately in
hot distilled water. After 6 h the solutions are mixed. The mixture
was stirred continuously to attain homogeneous. Next stage is to
transfer the mixture into polypropylene dish, and dried at 60 °C
using oven. Film was formed, thereafter the membranes were kept
in a desiccator. The thickness measurement from screw gauge of
the electrolytes were in the range 0.006–0.009 mm.
Fig. 1 illustrates the preparation of prepared polymer composite
electrolytes in detail.
2.3. Characterization techniques
Using an X- ray diffraction made by Bruker (Cu-K radiation
1.540 Å) and a scanning rate of 5° per minute in the range of 10°
to 60°, the amorphous/crystalline phase of the SPE was examined.
Using the ‘‘SHIMADZU IR Tracer 10000 spectrometer, the incorpora-
tion of NH4NO3 in the blend polymer was traced using FTIR trans-
mittance spectra, wave number range 4000 cm1 and 500 cm1 in
order to analyse the complexion between PVA, NaAlg and NH4NO3.
HIOKI 3532-50 LCR HI-TESTER was used to measure the ionic con-
ductivities of the prepared PE over the range of 42 Hz to 106 Hz. CV
on the CH-Instrument Model 6008e was used to examine the elec-
trochemical characteristics of the prepared sample.
3. Result and discussion
3.1. XRD analysis
X-ray diffraction enables to investigate the behaviour of crys-
tallinity PVA/NaAlg/NH4NO3 (PNN) films. The XRD patterns for
PNN1, PNN2, PNN3 and PNN4 are shown in Fig. 2. The PVA/NaAlg
blend has a strong peak around 13.44° and 19.36°, indicating that it
Fig. 2. XRD patterns of PNN system.
3
Journal of Saudi Chemical Society 27 (2023) 101743
has a semi crystalline structure [23–25]. The intensity of these
peaks as well as the hump at 30° were slightly reduced when
ammonium salt is added to the polymer matrix. There are no
appreciable crystalline NH4NO3 peaks in the 5- wt%(PNN1) to
20- wt%(PNN4)NH4NO3 added SPBEs [13,26,27]. This clearly con-
firms that the NH4NO3 salt is fully dissolved to produce a complex
structure of the polymer matrix. The intensity of the peaks was
increased with further doping of ammonium salt in PNN4 (20 wt
%), indicate increased crystallinity, formation of ion aggregation
which reduces solubility, poor complexation, and reforms in poly-
mer chains and it is shown in Table 2. The polymer blend and 15%
NH4NO3 together produced a high amorphous nature compared to
other SPBE film. The degree of crystallinity (vc ) of the electrolytes
was calculated using following Eq. (1),Thus, XRD analysis aids to
identify the optimal concentration of PNN3 for acquiring an
enhanced amorphous phase and this might pave way for the move-
ment of ions [28,29].
Ac
vc ¼
100ð%Þ ð1Þ
Ac þ Aa
where, Ac is an area of the crystalline region and Aa is an area of the
amorphous region.
3.2. FTIR analysis
The FTIR spectroscopy is used to investigate the molecular
interactions between synthesized electrolyte (PVA:NaAlg: NH4-
NO3). Table 3, lists the FTIR spectral assignments of PNN systems
and the spectra is shown in Fig. 3. Vibrational bands of pure PVA,
3293, 2920, 1719, 1419, 1243, and 839 cm1 are ascribed to
OAH (stretching), CAH (stretching), C@O (stretching), CAO
(stretching), CAOAC (stretching) and CAH (Bending) respectively
[29–31]. The vibrational bands of pure NaAlg are 1732, 1528 and
1130 cm1 was due to OAH stretching, symmetric stretching of
CAO group correspondingly [32,33].
Band assignments of PVA blend NaAlg 3319, 2932, 1722,
1244,922, and 841 cm1 are attributed to OAH stretching, CAH
stretching, C@O stretching, CAOAC stretching, (CAC) bending
vibration and CAH Bending [34,20,35]. Furthermore on incorpora-
tion of different wt. %(5 to 20) of NH4NO3the intensity has been
decreased with increase in salt concentration and is due to the
strong interaction between salt and polymer. But in 15 wt% NH4-
NO3added PNN3 system exhibit an increase in the intensity of
the peak comparably high than their counter parts. Further addi-
tion of salt to 20 wt%, intensity was decreased. There is no new
peak and change in peak position in the (NH4NO3) salt-doped
SBPEs and theresult conforms, the molecular interaction and com-
plexation of NH4NO3 in the prepared PNN systems.
3.3. AC impedance spectroscopy
AC impedance-spectroscopy technique is used to analyse the
electrical properties of the synthesized solid polymer-blend elec-
trolytes. Using AC impedance analysis, the electrochemical perfor-
mance of the electrolyte is calculated. It is possible to test the
electrolyte’s AC impedance (Z00 ) (O) change with frequency at room
Table 2
Degree of crystallinity of SPBEs system.
NH4NO3 concentration(wt. %) Crystallinity(%) Amorphous(%)
PVA blend NaAlg 19.1 80.9
PNN1 14.6 85.4
PNN2 15.3 84.7
PNN3 14.7 85.3
PNN4 16.3 83.7
R. Jansi, B. Vinay, M.S. Revathy et al. Journal of Saudi Chemical Society 27 (2023) 101743

Table 3
FTIR assignment of PNN system.

Assignments Wavenumber (cm1)

PVA:NaAlg
Blend 5 wt% 10 wt% 15 wt% 20 wt% NH4NO3
NH4NO3 NH4NO3 NH4NO3
(OAH) Stretching Vibration 3319 3319 3319 3319 3319
(CAH) Stretching Vibration 2932 2932 2932 2932 2932
(C@O)Stretching Vibration 1723 1723 1723 1723 1723
CAOAC stretching Vibration 1244 1244 1244 1244 1244
(CAOAC)Stretching vibration 1091 1089 1089 1086 1086
1029 1029 1029 1024 1024
(CAC) bending Vibration 922 922 922 922 922
(CAH) bending Vibration 839 841 841 841 841

which aids in calculating conductivity (ionic), was estimated from

ZSimpWin software. Table 4 lists the values of bulk resistance and
capacitance PVA/NaAlg/(5, 10, 15, 20) wt. % NH4NO3films [36].
Using the formula, the ionic conductivity of the synthesized SPBEs
with the addition of ionic salt was estimated.
For the PNN3 blend polymer electrolyte, the highest conductiv-
ity was determined to be 1.05
106 S cm1 and 2.46
106 S
cm1at 303 K and 353 K respectively (Table 5). This infers that as
the temperature increases conductivity also increases.

3.3.2. Conduction spectra

Fig. 3. FTIR spectra of polymer blend electrolytes of PNN system.
temperature. Ac conductivity plot, Nyquist plot, or cole–cole plot is
a plot of the actual and real parts of impedance as a frequency-
dependent function. The Nyquist plot is split into two distinct
zones in practice. The bulk impact of the polymer membrane is
first illustrated by the semicircle in the high-frequency region,
which would be represented by a circuit with a parallel connection
of bulk capacitance and resistance (R) of the electrolytes. Further-
more, the tilted spike at shorter wavelengths is caused by the con-
stant potential element (polarization effect) inhibiting double-
layer capacitance at the interfacial region.
3.3.1. Nyquist plots
Fig. 4 shows the Nyquist plot of blend polymer electrolyte
membranes of varying concentrations of salt NH4NO3 at room tem-
perature. Frequency response tests assess the overall ionic conduc-
tivity of the SPBE system. Observations have been made on each
sample. In the low-frequency region of Fig. 4, a semicircle and cor-
responding spike suggest that the sample has an impedance with a
combination of capacitance as well as resistance. Bulk resistance
(Rb) of the samples is given by the intersection of a semicircle on
the x-axis [36]. The sample PNN3 has the lowest bulk resistance,
thereby showing enhanced conductivity at ambient temperature.
The Nyquist curves for the maximum ionic conducting PNN3 at
various temperatures (303, 313, 323, 333, 343, and 353 K) are
shown in Fig. 4(b). The following Eq. (2) was used to calculate
the ionic conductivity (rÞ of the prepared films:
L
r¼ ðS cm1 Þ
ARb
Here L is the film’s thickness, Rb is the bulk impedance, and A is
the film’s area [37,38]. Bulk resistance Rb for the present study,
The conduction spectra of Fig. 5a and b show highly ionic beha-
viour for PNN1, PNN2, PNN3 and PNN4at various temperatures.
Conductance spectra typically have three distinct regions: The
electrode polarization effect’s Maxwell-Wagner polarisation is
responsible for Region I (the low frequency dispersion zone). As
the frequency decreases, conductivity reflects the polymer sys-
tem’s non-debye nature [39]. This may be because there are less
mobile ions due to the interface of charges accumulating at the
electrode or electrolyte. The DC conductivity measurement of SPBE
is provided by Region II (mid-frequency plateau zone). Region III,
also known as the ‘‘dispersion zone of high-frequency,” refers to
the phenomenon of bulk relaxation, in which mobile ions hop as
a result of structural system instability and columbic interaction
between charge carriers [9,30,40].
3.3.3. Temperature dependent ionic conductivity studies (Arrhenius
Plot)
Fig. 6 depicts the electrical impedance of four polymer com-
plexes as a function of temperature. According to Fig. 6, the ionic
conductivities for PNN1, PNN2, PNN3 and PNN4 rises with increas-
ing temperature and is governed by Arrhenius type, a thermally
activated process. The Arrhenius equation is
Ea
r ¼ ro expð Þ ð3Þ
kT
where, Ea is activation energy, K is Boltzmann constant, ro is pre-
exponential factor [37].
All the electrolyte samples’ activation energies have been iden-
tified, and indeed the linear fit’s accuracy is evident in the regres-
sion results that were generated from fitting the plot’s data linearly
and seem to be approximately unity. Table 5 shows the regression
values along with the predicted activation energy values. It has
been demonstrated that the activation energy decreases when
the concentrations of ammonium nitrate increases from 5 to
15 wt%, and subsequently increases for 20 wt% NH4NO3. In con-
ð2Þ ducting polymers, the greater amorphous aspect leads to a higher
free volume and lower activation energy. In order to encourage
inter-chain and intra-chain hopping to boost conductivity, the
hydrocarbon chains acquire faster interior phases as its amorphous
4
R. Jansi, B. Vinay, M.S. Revathy et al. Journal of Saudi Chemical Society 27 (2023) 101743

Fig. 4. (a) Nyquist plots for PNN1, PNN2, PNN3 and PNN4 at room temperature and (b) Nyquist plots of higher ionic conducting PNN3 at various temperatures.

nature increases. Bond rotation creates segmental motion in these

Table 4 faster internal patterns [38,39]. The estimated values of activation
Values of QPE1, QPE2, and Rb for PNN1, PNN2, PNN3 and PNN4. energy is shown in Table 5.
Sample QPE1 (F) QPE2 (F) Rb (O)
PNN1 1.996
109 – 6,858,000 3.3.4. Dielectric spectra analysis
PNN2 1.716
107 2.618
106 56,160 Fig. 7a and b represents the frequency dependence of dielectric
PNN3 1.588
109 1.049
105 10,709
constant e0 for PNN1, PNN2, PNN3, and PNN4 systems at 303 K, and
PNN4 3.359
109 – 5,169,000
higher ionic conducting PNN3 at various temperatures respec-
5
R. Jansi, B. Vinay, M.S. Revathy et al. Journal of Saudi Chemical Society 27 (2023) 101743

tively. It has been observed that values of e0 are high at low fre- the decline in e0 with frequency in the intermediate zone is the
quency. It is due to the presence of space charge effects, which interfacial polarisation effect, which inhibits vibrational modes
are contributed by the accumulation of charge carriers near the from aligning with the field employed. Variation in e0 values in
electrodes [44,45]. The high e0 at low frequency is attributed to many polymeric systems confirms the impact of monomer concen-
space charge effects, which are contributed by the accumulation trations on electrode polarisation. Increased salt concentration
of charge carriers near the electrodes. One reason contributing to makes it much simpler to disperse the ions to achieve the maximal
e0 for PNN3. The dielectric constant at higher frequencies has been
found to be constant. This occurs as a result of the charge carriers’
inability to track the periodic reversal of the electric field. The large
Table 5
Ionic Conductivity via Temperature dependence, Activation energy and its fitted value of e00 is attributed to the motion of free charge carriers within
regression value of PNN1, PNN2, PNN3 and PNN4 films. the material [40,41].
The parameters were estimated using the Eqs. (4) and (5),
S. No. Polymer Ionic conductivityat Activation Regression
electrolytes different temperature energy Ea Value(R) Z
(S/cm) (eV) e0 ¼  i  ð4Þ
xC o Z 2r þ Z 2i
303 K 353 K
1 PNN1 8.53
1010 2.75
107 0.619 0.968
107 106 Zr
2 PNN2 1.16
2.57
0.686 0.976 e00 ¼   ð5Þ
3 PNN3 1.05
106 2.46
106 0.236 0.937 xC o Z 2r þ Z 2i
4 PNN4 1.26
109 2.88
107 0.351 0.982

where ; e0 is the dielectric constant (charge storage)e00 is the dielec-

tric loss (energy loss), x is the angular frequency of applied electric
field, Co is the vacuum capacitance and Z is the complex impedance
[42]. Frequency dependence of dielectric constant PNN3 sample at
different temperature is shown in Fig. 7(b). As frequency increases,
conductivity decreases progressively over time and reaches a pla-
teau in the high-frequency zone after quite a cross-over position.
The increased dielectric constant at high temperatures and in the
lower frequency range is attributed to the polarising action of the
electrodes plus space charge, which is responsible for non-Debye
behaviour.
Dielectric loss is a precise measurement of energy breakdown
that often includes contributions from electrode materials in addi-
tion to charge or dipole polarization Fig. 8a and b represents the
frequency dependence of dielectric loss e00 for PNN1, PNN2,
PNN3, and PNN4 systems at 303 K, and higher ionic conducting
PNN3 at various temperatures respectively.. The figure shows that
dielectric loss is greatest at shorter wavelengths, subsequently
decreases with increasing wavelength, and is becoming saturate
at different frequencies. The polarisation phenomenon at the elec-
trode/electrolyte interaction can be used to assess dielectric loss
with in low-frequency range [43]. There is a complex quantity of
free flow of charges with in system, as well as adequate time for
charges to structure at the functionality before the electric poten-
tial is altered, resulting in a significant perceptible value of dielec-
tric loss [44]. There were no charges build-up at the interaction

Fig. 5. (a) Conductance spectra for PNN1, PNN2, PNN3 and PNN4 at room
temperature. (b) Conductance spectra of higher ionic conductingPNN3 at various
temperatures. Fig. 6. Arrhenius Plot for PNN1, PNN2, PNN3 and PNN4 at various temperatures.

6
R. Jansi, B. Vinay, M.S. Revathy et al.
Fig. 7. (a)Variation of dielectric constant spectra for PNN1, PNN2, PNN3 and PNN4
at room temperature (b) Variation of dielectric constant spectra of higher ionic
conducting PNN3 at various temperatures.
with in high-frequency range. It has been noted that when the
polymeric mixture changes, consequently the dielectric loss peak
for the PNN3 is complex. Dielectric loss has been observed to rise
with temperature because of a shift with in mobility of hydronium
ion, as seen in Fig. 8(b). Although the charge - carrier concentration
at the interface increases with temperature, the ion-pair dissocia-
tion process also increases.
3.3.5. Modulus spectrum analysis
Fig. 9(a) and (c) shows for solid polymer blend samples of PNN1,
PNN2, PNN3, and PNN4 at room temperature and Fig. 9(b) and (d)
for PNN3 sample at different temperature both show the variation
in real modulus (M0 ) and imaginary modulus (M00 ) on frequency.
The electric modulus approach has been applied to differentiate
among electrodes polarisation as well as other interface phenom-
ena. Dielectric depictions are commonly used to characterize bulk
dielectric behaviour while neglecting interface factors. Modulus
spectra is particularly useful for identifying polymers with equal
resistances but differing capacitor values from the spectrum ele-
ments. The electric modulus concept also has the advantage of
eliminating the electrode influence [45,46].
7
Journal of Saudi Chemical Society 27 (2023) 101743
Fig. 8. (a)Variation of a Dielectric loss spectra for PNN1, PNN2, PNN3 and PNN4 at
room temperature (b) Dielectric constant spectra of higher ionic conducting PNN3
at various temperatures.
Fig. 9(a) and (b) show that M0 tends to zero, demonstrating that
the presence of detectable electrode or electrical polarisation at
room temperature in the low frequency zone is caused by the elec-
trode’s high capacitance. PNN3 exhibits a long tail at lower fre-
quency, but PNN4 confirms the humps may be distinguished
under varied conditions. The M0 0 spectrum, as shown in Fig. 9(c)
and (d), has an anomalous spike positioned roughly in the transi-
tion region. In Fig. 9(c) PNN3 sample shows a long tail which an
enlarge hump where as PNN1 has observed a extensive breakdown
polarization [44]. The imaginary spectra of PNN3 at various tem-
perature, shows a similar kind of humps, consequently at 303 K a
non-Debye nature is observed due to bulk phenomena. Initially,
dielectric data can be altered into modulus data and complex mod-
ulus (M) which are expressed as,
Eqs. (6) and (7) are used to determine the M’ and M”,
respectively
e0
M0 ¼ ð6Þ
e þ e}2
02
e00
M00 ¼ ð7Þ
e þ e}2
02
where ; e0 is the dielectric constant and e00 is the dielectric loss.
Using these spectra, the lower-frequency zone with almost zero
values of M0 and M00 represents the space occupied by interfacial
R. Jansi, B. Vinay, M.S. Revathy et al.
polarization, while the abrupt increase in the region of the higher
bandwidth area is connected to the bulk properties of the
electrolyte.
3.3.6. Tangent spectra analysis
Tangent delta, also known as the loss angle or loss tangent, is a
measure of energy dissipation in a substance in the presence of a
force or field.
The loss tangent d is the ratio of the dielectric loss factor e00 (x)
to the dielectric constant e0 (x). The relation is expressed as
e00 ðxÞ
tan d ¼
e 0 ð xÞ
Fig. 10(a) illustrates logarithms of a frequency Vs tan d of sam-
ple (PNN1, PNN 2, PNN 3, PNN 4) at room temperature (303 K). The
graphs show that tan d rises with increasing frequency and later
diminishes. For higher weight percentages of NH4NO3 of PNN sys-
tem, peak of the frequency response is migrated towards higher
frequency region. Therefore, this relaxation peak is shifted towards
higher frequency by the addition of NH4NO3. It is exposed that the
prepared PNN system follow the non-Debye nature. Occurrence of
shifting denotes the lower ion relaxation time due to the increment
of charge carrier density and hence the faster segmental motion in
Fig. 9. (a) Real modulus spectra for PNN1, PNN2, PNN3 and PNN4 at room temperature. (b) Real modulus spectra of higher ionic conducting PNN3 at various temperatures. (c)
Imaginary modulus spectra for PNN1, PNN2, PNN3 and PNN4 at room temperature. (d) Imaginary modulus spectra of higher ionic conducting PNN3 at various temperatures.
Journal of Saudi Chemical Society 27 (2023) 101743
the samples by the addition of NH4NO3 [23,47]. The inverse of the
frequency ratio a greatest elevation of the peak is used to calculate
the relaxation time. PNN3 have a less relaxation time of
7.49
105 s. Fig. 10(b) shows Logarithms of a frequency Vs tan
d of a Sample PNN3 electrolyte at various temperatures. It has been
observed that as temperature rises, the highest portion of tan d
shifts to a high-frequency side, which signify the dielectric relax-
ation of the systems are temperature-dependent that leads to
decreases at high temperatures.
3.4. Transference number measurements
ð8Þ
The transport study is essential for relating the diffusion of ionic
contribution in the electrolyte. One graphite-coated silver elec-
trode (SEG) is employed in Wagner’s DC polarisation technique
to limit the passage of ions in the cell configuration of blocked
SEG||SPE||SE. The polarized cell is given a constant potential of
2 V while it is at room temperature. The initial high current is
attained as a result of ions and electrons being transported [37].
The electrodes stop ions from flowing across the external circuit,
and this ion blockage only allows electronic current to flow. The
electrode polarisation effect causes the current to then rapidly
decrease over time [34,48].
8
R. Jansi, B. Vinay, M.S. Revathy et al.
The distinction in current with a function of time is displayed in
Fig. 11. The transference number of ions (tion) and electron (tele) are
calculated by following relation
Fig. 10. (a) Loss tangent spectra for PNN1, PNN2, PNN3 and PNN4 at room
temperature salt and (b) Loss tangent spectra of higher ionic conducting PNN3 at
various temperatures.
Fig. 11. Transference number analysis for PNN1, PNN2, PNN3 and PNN4 polymer
electrolytes at room temperature.
9
Journal of Saudi Chemical Society 27 (2023) 101743
ðIi  If Þ
tion ¼ ð9Þ
Ii
If
tele ¼ ð10Þ
Ii
where, Ii represents the initial current, If represents the finial
current.
For all composition of polymer blend electrolytes, transference
number is obtained as above 0.9. This is the confirmation of pre-
dominant ion conduction in PNN3 polymer blend electrolytes.
Number of charge carriers (n), diffusion coefficients (D), and mobil-
ity (l) of cation and anion in polymer blend matrix is calculated by,
Nq
molar ratio of salt
n¼ ðcm3 Þ ð11Þ
molar weight of the salt
KT r
D¼ ðcm2 s1 Þ ð12Þ
ne2
r
l¼ ðcm2 =VsÞ ð13Þ
ne
Where,
N- Avogadro’s number (6.023
1023 particles per mole).
q- density of the salt (NH4NO3 = 1.725 g/cm3).
K- Boltzmann constant (1.3806
1023 m2 kg s2 K1).
e- charge of the electron (1.602
1019 C).
The transport parameters of prepared SPEs are listed in Table 6.
The value of both diffusion coefficient (D) and mobility(l) are
increased up to the sample PNN3. The cation value of D and l is
higher value than anion in all the polymer blend electrolytes. From
this, it is concluded that D and l are responsible for the enhance-
ment of ion conductivity in polymer blend electrolytes.
3.5. CV and LSV analysis
Cyclic Voltammetry (CV), a potentiodynamic electrochemical
measurement. Additionally, it is possible to examine the type of
charge storage that occurs at each interface between the anodic
and cathodic areas. ESW(electrochemical stability window) of the
highest ion-conducting electrolyte system PNN3 is shown in
Fig. 12. A CV curve showing oxidation and reduction peaks can
be observed within a potential range of 1 to +1 V and with scan
rates of 100, 75, 50, 10 and 5 mV/sec. This one oxidation and dou-
ble reduction peak point indicates that it can be seen that there are
two reactions that cause the reduction reaction or that there are
impurities. Evidence of redox reaction has proved to have energy
storage behaviour. Table 7 summarizes the area values for each
sample after various sweep rates. Oxidation as well as reduction
peak also increased significantly with the increasing scan rate. As
can be seen from these results, the PNN3 system with proton ions
(ammonium ions) exhibits excellent electrochemical stability and
is electrochemically active [34,49]. The electrochemical stability
window for the solid blend polymer electrolytes was calculated
using linear sweep Voltammetry (LSV). Fig. 13 shows the LSV plot
of the highest conducting sample PNN3. A scan rate of 100 mV s1is
till a high current is noticed at a given potential. No evident current
is seen through the electrode potential from 0 V to 0.55 V. When
the electrode potential reached above 0.55 V, a drastic increase
in the value of the current observed which is linked to the decom-
position of SPBE at the inert electrode interface [50].
R. Jansi, B. Vinay, M.S. Revathy et al. Journal of Saudi Chemical Society 27 (2023) 101743

Table 6
Number of charge carrier concentration, transference numbers, diffusion coefficient, and mobility of PNN system.

Sample Code weight of salt% No. of chargecarriers Transference Number Diffusion Mobility (l) cm2/Vs
(n) co-efficient
cm3 cm2/s
T ion T ele D l
PNN1 0.02 2.064
1020 0.9866 0.0133 6.751
1013 2.581
1011
PNN2 0.05 5.160
1020 0.9918 0.0081 3.675
1011 1.401
1009
PNN3 0.07 7.224
1020 0.9942 0.0057 2.226
1010 8.652
1009
PNN4 0.1 1.238
1021 0.9872 0.0128 1.998
1013 7.632
1012

4. Conclusion

Polymer electrolytes of solid blend polymer samples of PVA,

Fig. 12. Cyclic Voltammetry for the higher ionic conductivity sample of PNN3 at
different scan rates of (100, 75, 50, 10 and 5 mV/sec).
NaAlg, and NH4NO3 were synthesised using the solution casting
process. XRD of PPN3 represents to confirm the greater amorphous
nature due higher concentrations of NH4NO3 salt which results in
an increased ionic diffusivity with high ionic conductivity. The
electric properties of a were investigated using Ac impendence
spectroscopy from the analysis of nyquist plot, conduction spectra,
dielectric permittivity, dielectric loss, and modulus spectra, Using
the governing norms of Arrhenius plot, the activation energy of
the high conductivity sample was determined as 0.24 eV. There-
fore, among all samples of the current study, PNN3 sample con-
cludes a high ionic conductivity of 1.05
106 S/cm at room
temperature while a lower conductivity was found at different
temperatures. The CV investigation of PNN3 SPBE exhibited fara-
daic behaviour. LSV studies indicated that PNN3 SPBEhas 0.55 V.
Based on these studies, the inclusion of ammonium salt in this
reported hybrid polymer blend could be used in energy storage
devices.

Declaration of Competing Interest

Table 7 The authors declare that they have no known competing finan-
Scan rate versus area.
cial interests or personal relationships that could have appeared
Scan Rate (mV/s) Area to influence the work reported in this paper.
5 3.367
105
10 5.922
105 Acknowledgement
50 9.337
105
75 1.229
104
100 1.575
104 R.Jansi thanks Kalasalingam Academy of Research and Educa-
tion for offering University Research Fellowship and the authors
extend their appreciation to the Deanship of Scientific Research
at King Khalid University (KKU) for funding this research through
the Research Group Program Under the Grant Number: (R.G.
P.2/515/44).

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