The Role of Glycerol in Modulating Ionic Transport and Electrochemical Performance of PEO:NaCl Solid Polymer Electrolytes

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University of Sulaimani

University of Raparin

Koya University, Kurdistan Region – F.R

University of Sulaimani

Soran University

PEO, NaCl, Polymer electrolytes, plasticizer, Glycerol

January 8th, 2025

[https://doi.org/10.21203/rs.3.rs-5763604/v1](https://doi.org/10.21203/rs.3.rs-5763604/v1)

  This work is licensed under a Creative Commons Attribution 4.0 International License.
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No competing interests reported.

### The Role of Glycerol in Modulating Ionic Transport and Electrochemical Performance of PEO:NaCl Solid Polymer Electrolytes

_Shujahadeen Bakr Aziz_ _1,2_ _, Hazhar Hamad Rasul_ _3,_ _*_ _, Safar Saeed Mohammed_ _3_ _, Abubakr Wsu_

_Muhammed_ _3_ _, Peshawa H. Mahmood_ _4_ _,_ _Sleman Yousif Omar_ _5_ _, Dlshad Aziz Hamid_ _4_ _, Ibrahim_

_Luqman Salih_ _4,6_ _, Karukh Ali Babakr_ _4,7_ _, Ibrahim Nazem Qader_ _3,7_ _, Pshdar Ahmed Ibrahim_ _3_ _,_

_Rebaz Anwar Omer_ _8_ _, Ari Ahmed Abdul Rahman_ _9_ _, Samir Mustafa Hamad_ _10_ _, Peyman Aspoukeh_ _10_ _,_

_Sarbast Mamnd Hussein_ _10_

_1_ _Research and Development Center, University of Sulaimani, Qlyasan Street, Kurdistan Regional Government, Sulaymaniyah,_
_46001, Iraq_
_2Department of Physics, College of Science, Charmo University, 46023, Chamchamal, Sulaymaniyah, Iraq_
_3_ _Department of Physics, College of Science, University of Raparin, Rania, 46012, Sulaymaniyah, Iraq_
_4_ _Chemistry Department, College of Science, University of Raparin, Rania, 46012, Sulaymaniyah, Iraq_
_5_ _Department of Biology, College of Science, University of Raparin, Rania, 46012, Sulaymaniyah, Iraq_
_6_ _Department of Pharmacy, Raparin Technical and Vocational Institute, Rania, 46012, Sulaymaniyah, Kurdistan Region, Iraq_
_7Department of Pharmacy, College of Pharmacy, Knowledge University, Erbil 44001, Iraq_
_8_ _Department of Chemistry, Faculty of Science & Health, Koya University, Koya KOY45, Kurdistan Region – F.R., Iraq_
_9Department of Physics, College of Education, University of Sulaimani, Qlyasan Street, Kurdistan Regional Government,_
_Sulaymaniyah, 46001, Iraq_
_10_ _Soran Research Center, Soran University, Soran, 44008, Iraq_

_*Corresponding Author: H. H. Rasul (E-mail:_ _[hazharhrm@uor.edu.krd](mailto:hazharhrm@uor.edu.krd)_ _)_

Abstract

Solid polymer electrolytes (SPEs) are promising alternatives to liquid electrolytes, offering

stability and versatility. However, low ionic conductivity remains a challenge, which can be

addressed through strategies such as salt incorporation and plasticizer optimization. This study

aims to enhance PEO-NaCl-based polymer electrolyte films by adding glycerol to modify

crystallinity and improve electrical properties. Characterization included Fourier-transform

infrared spectroscopy (FTIR), X-ray diffraction (XRD), and electrochemical impedance

spectroscopy (EIS) to analyze structural, spectroscopic, and electrochemical properties as a

function of plasticizer content. The study demonstrated significant enhancements in the

electrochemical and dielectric properties of PEO-NaCl polymer electrolytes with increasing

glycerol content. Electrical Impedance Spectroscopy (EIS) revealed a marked improvement in

DC conductivity, increasing from 1.38 × 10 -8 S/cm for the glycerol-free sample to 1.74 × 10 -4

S/cm at 32% glycerol concentration, attributed to reduced bulk resistance and enhanced ion

mobility. Glycerol also improves the dielectric properties of PEO-NaCl electrolytes by

increasing polarizability, enhancing ion motion, and reducing ion aggregation, which leads to

better ionic conductivity and energy dissipation. Additionally, the relaxation dynamics

improved, as evidenced by sharper and higher dielectric loss tangent peaks (tanδ) with glycerol

addition. The findings confirm that glycerol effectively reduces polymer rigidity, boosts ionic

mobility, and improves conductivity, positioning it as a promising plasticizer for solid-state

electrolytes.

Keywords : PEO; NaCl; Polymer electrolytes; plasticizer; Glycerol

1. Introduction

Electrolytes are essential in facilitating ionic mobility between electrodes, which is vital for the

functioning of electrochemical devices. However, liquid electrolytes have several drawbacks,

including leakage, high flammability, and chemical instability. Consequently, there is a growing

trend to replace them with polymers [1]. Solid polymer electrolytes (SPEs) offer several

advantages, including excellent electrochemical stability, versatility, high specific energy, and

ease of fabrication into thin films [2]. The SPEs are suitable for a range of solid-state

electrochemical devices, such as supercapacitors, batteries, fuel cells, and chemical sensors.

Nevertheless, one major challenge with SPEs is their low electrical conductivity, which requires

improvement for optimal performance [3, 4]. Dry polymer electrolytes, also referred to as

solvent-free electrolytes, allow for the mobility of both positively charged ions (cations) and

negatively charged ions (anions), as they are loosely bound.

Polyethylene oxide (PEO)-based polymer electrolytes remain among the most widely studied

polymer ion conductors due to PEO's beneficial structure that supports fast ion transport. The

main requirement for high conductivity appears to be the ability of the polymer's coordination

groups to readily dissolve cations. Polymers containing Lewis bases (usually ether oxygens)

can act as coordinating cations, thereby promoting the dissolution of salts. Due to the chain

entanglement of the polymer host, these polymer salt complexes exhibit mechanical properties

that are similar in most respects to those of real solids. For metal ions, the microscopic

environment remains liquid, and the ionic conductivity is "coupled" with the local segmental

motion of the polymer [5]. The relatively high crystallinity of PEO-based electrolytes at

ambient temperature leads to poor ionic conductivity. Several strategies have been developed

to enhance the conductivity of electrolytes, including salt incorporation, and the use of

plasticizers. For example, the addition of ammonium salts to a chitosan-dextran blend has been

shown to significantly improve DC ionic conductivity due to the increased concentration of

mobile ions [6, 7]. The dissociation of salts within the polymer matrix is critical; as the salt

concentration increases, the number of free ions available for conduction also increases, leading

to enhanced conductivity [8, 9]. However, excessive salt can lead to phase separation or

crystallization, which can negatively impact conductivity.

Plasticizers, such as glycerol and succinonitrile, play a crucial role in modifying the properties

of polymer electrolytes. For instance, Aziz et al. demonstrated that the addition of glycerol to

chitosan-dextran polymer electrolytes significantly suppressed crystallinity, allowing for

enhanced ionic conductivity due to increased ion dissociation and mobility [10]. Similarly, the

study by Sadiq et al. highlighted that incorporating plasticizers into polyvinyl alcohol (PVA)

and chitosan blends resulted in a substantial increase in ionic conductivity, approaching that of

gel-based electrolytes [11]. The plasticization effect is attributed to the disruption of hydrogen

bonding between polymer chains, which allows for greater segmental motion and,

consequently, improved ion transport [12].

While the addition of plasticizers generally enhances the ionic conductivity of polymer

electrolytes, it is essential to optimize their concentration to achieve the best performance.

Excessive plasticization can lead to a reduction in mechanical strength and stability of the

polymer matrix, which may compromise the overall performance of the electrochemical

device[10]. For instance, Aziz et al. emphasized that finding the right balance in plasticizer

content is crucial, as too much plasticizer can result in a decrease in the structural integrity of

the polymer electrolyte, leading to potential leakage or failure in practical applications [13].

Research has shown that the optimal concentration of plasticizers varies depending on the

specific polymer and salt used. Dannoun et al. stated that incorporating 42 wt% glycerol into a

chitosan-based electrolyte significantly improved conductivity, but further increases in glycerol

content led to diminishing returns in performance [14]. This highlights the importance of

conducting systematic studies to determine the optimal plasticizer concentration for each

specific polymer electrolyte system.

In this study, a 9% NaCl salt solution was dissolved in PEO, and glycerol was added to modify

the polymer's crystallinity and improve its electrical properties. We conducted both

electrochemical and non-electrochemical analyses, including crystal structure analysis via X
ray diffraction (XRD) and spectroscopic analysis using Fourier-transform infrared spectroscopy

(FTIR), on the modified polymers. Electrochemical impedance spectroscopy (EIS) was

employed to investigate the electrical phenomena associated with the chemical reactions of the

polymer films as different amounts of plasticizer were introduced.

2. Experimental Procedure

The poly(ethylene oxide) (PEO) employed in this study, featuring a molecular weight of

2,000,000 and the chemical formula (-CH₂CH₂O-)ₙ, was obtained from Sigma-Aldrich. A

weight of 5 g of PEO powder was dissolved in 500 mL of acetonitrile and 0.495 g of a 9% NaCl

solution. The resulting solution was divided into five small beakers containing glycerol

concentrations of 0%, 8%, 16%, 24%, and 32%. After adding each mixture, it was stirred for

one hour and then left exposed to air at room temperature overnight to allow any bubbles formed

during mixing to rise. A magnetic stirrer set to medium rotation was used to ensure that the PEO

and salts were fully dissolved in the solution. Volumes of 60 mL and 40 mL of the solution were

transferred to petri dishes. After casting, the dishes were placed at room temperature to allow

the solvent to evaporate. Consequently, thick and thin polymer films were formed after one

week. The materials used for the polymer films are listed in Table 1. Scheme 1 illustrates the

synthesis of the PEO:NaCl polymer electrolyte films.

Table 1. The amount of PEO, NaCl, and glycerol in polymer films

Sample code PEO NaCl Glycerol
(gram) (%) (gram) (%) (gram)
PNCG-0 1 9% 0.099 0% 0
PNCG-8 1 9% 0.099 8% 0.0956
PNCG-16 1 9% 0.099 16% 0.2093
PNCG-24 1 9% 0.099 24% 0.3470
PNCG-32 1 9% 0.099 32% 0.5171

Scheme 1. Schematic Procedure for Preparing PEO:NaCl Solid Polymer Electrolytes

3. Results and Discussions

3.1. Electrical Impedance Spectroscopy

Electrical Impedance Spectroscopy (EIS) is a crucial technique for analyzing the impedance

characteristics of materials across a range of frequencies. It provides valuable insights into

charge transfer, ion mobility, and dielectric behavior, making it useful in fields such as energy

storage, corrosion science, and biomaterials. EIS operates by applying an alternating current

(AC) signal to a system and measuring its voltage response, which yields impedance with real

and imaginary components [15, 16]. These components are analyzed using a Nyquist plot and

modeled with equivalent circuits. Recent advancements in EIS focus on enhancing sensitivity,

data analysis, and integration with machine learning for more accurate modeling. Portable EIS

devices are also being developed for field applications [17-19]. EIS is a powerful tool for

characterizing materials like polymer electrolytes, and when combined with techniques such as

FTIR and XRD, it enables researchers to gain a comprehensive understanding of material

properties, thereby supporting advancements in sustainable energy storage technologies.

The corresponding circuit, shown as an inset in Figure 1, is created by connecting the constant

phase element (CPE1) and bulk resistance ( _Rb_ ) in parallel. Together, these components form the

semicircle portion of the Nyquist plot. Additionally, an extra constant phase element (CPE2) is

connected in series with both CPE1 and _Rb_, resulting in the spike portion of the plot. The

mathematical basis for the impedance of the CPEs ( _Z_ CPE) is given by the following equation

[20]:

(1)
1 1
?CPE = [ ~~???~~ ~~?~~ cos(?) −? ~~???~~ ~~?~~ sin(?)]

??/2), representing the phase angle, ?? corresponds to the capacitance of the

?CPE = [ ~~???~~ ~~?~~ cos(?) −? ~~???~~ ~~?~~ sin(?)]

where (? =??/2), representing the phase angle, ?? corresponds to the capacitance of the

constant phase element (CPE), and ? is the angular frequency, calculated using the formula

where (? =??/2), representing the phase angle, ?? corresponds to the capacitance of the

constant phase element (CPE), and ? is the angular frequency, calculated using the formula

?=2??. The parameter ? indicates the degree of deviation of the plot from the imaginary axis.

constant phase element (CPE), and ? is the angular frequency, calculated using the formula

?=2??. The parameter ? indicates the degree of deviation of the plot from the imaginary axis.

The imaginary component of the measured impedance (??) is plotted on the y-axis, while the

?=2??. The parameter ? indicates the degree of deviation of the plot from the imaginary axis.

The imaginary component of the measured impedance (??) is plotted on the y-axis, while the

real component (??) is plotted on the x-axis. For plots containing only a semicircle, as observed

The imaginary component of the measured impedance (??) is plotted on the y-axis, while the

real component (??) is plotted on the x-axis. For plots containing only a semicircle, as observed

in PNCG-0, ?? and ?? can be determined using Equations (2) and (3) [21]:

real component (??

in PNCG-0, ?? and ?? can be determined using Equations (2) and (3) [21]:

?? + ??2
?? =

~~1 + ???1(2?~~ ~~?1~~

(2)

?? + ??2?1 ??1cos (?1)

~~1 + ???1(2?~~ ~~?1~~ ~~cos(?1) + ???1?~~ ~~2?1~~ ~~)~~

??2?1 ??1sin (?1)

??2
?? =

~~1 + ???1(2?~~

(3)

??2?1 ??1sin (?1)

~~1 + ???1(2?~~ ~~?1~~ ~~cos(?1) + ???1?~~ ~~2?1~~ ~~)~~

represents the extent to which the semicircle deviates from the vertical axis.

~~1 + ???1(2?~~ ~~?1~~ ~~cos(?1) + ???1?~~ ~~2?1~~ ~~)~~

Furthermore, the plots for PNCG-8, PNCG-16, PNCG-24, and PNCG-32 exhibit both a

Here, ?1 represents the extent to which the semicircle deviates from the vertical axis.

Furthermore, the plots for PNCG-8, PNCG-16, PNCG-24, and PNCG-32 exhibit both a

semicircular region and a spike. The values of ?? and ?? were determined as follows [22]:

Furthermore, the plots for PNCG-8, PNCG-16, PNCG-24, and PNCG-32 exhibit both a

(4)

?? + ??2?1 ??1cos (?1) 1

~~1 + ???1(2?~~ ~~?1~~ ~~cos(?1) + ???1?~~ ~~2?1~~ ~~)~~ + ~~?2?~~ ~~?2~~ cos (?2)

??2?1 ??1sin (?1) 1

?? + ??2
?? = ~~1 + ???1(2?~~ ~~?1~~

(5)

??2?1 ??1sin (?1) 1

~~1 + ???1(2?~~ ~~?1~~ ~~cos(?1) + ???1?~~ ~~2?1~~ ~~)~~ + ~~?2?~~ ~~?2~~ sin (?2)

represents the degree of deviation of the spike from the horizontal axis. ?1 corresponds

??2
?? = ~~1 + ???1(2?~~

~~1 + ???1(2?~~ ~~?1~~ ~~cos(?1) + ???1?~~ ~~2?1~~ ~~)~~ + ~~?2?~~ ~~?2~~ sin (?2)

here, ?2 represents the degree of deviation of the spike from the horizontal axis. ?1 corresponds

to the capacitance observed at high frequencies, whereas ?2 refers to the capacitance measured

here, ?2 represents the degree of deviation of the spike from the horizontal axis. ?1 corresponds

at low frequencies.

to the capacitance observed at high frequencies, whereas ?2 refers to the capacitance measured

at low frequencies.

Table 2 summarizes the results obtained from the Electrical Impedance Spectroscopy (EIS)

analysis. The DC conductivity (???) is calculated using Eq. (6), which depends on the bulk

resistance ( ??), film thickness ( _t_ ), and electrode area (?) [21]:

Table 2 summarizes the results obtained from the Electrical Impedance Spectroscopy (EIS)

analysis. The DC conductivity (???

resistance ( ??), film thickness ( _t_ ), and electrode area (?) [21]:

?

_t_ ), and electrode area (?) [21]:

(6)
?
??? =
~~???~~

??? values rise while ??

~~???~~

decreases. This can be attributed to the higher ion concentration in the electrolytes, which boosts

It has been observed that as glycerol concentration increases, the ??? values rise while ??

decreases. This can be attributed to the higher ion concentration in the electrolytes, which boosts

electrode polarization and, as a result, increases capacitance at low frequencies. This also

enhances ionic conductivity by facilitating greater ion mobility and dissociation. These findings

suggest that glycerol molecules interact attractively with the polymer chain segments, leading

to a reduction in cohesive forces [23]. Additionally, glycerol can improve the electrical

characteristics of the polymer electrolyte and expand its application areas. As a plasticizer,

glycerol breaks the bonds in the polymer, increasing the mobility of cations and anions within

the polymer electrolyte. This is significant because the electrical conductivity value is directly

proportional to the mobility of the electrical carriers [24].

300

200

100

(a) PNCG-0 Experimental
Fitting

0
0 50 100 150 200 250 300

_Z'_ ( k W )

18
(b) PNCG-8

Experimental
Fitting

3.5
(c) PNCG-16

3.0

2.5

2.0

1.5

1.0

0.5

Experimental
Fitting

0
0 2 4 6 8 10 12 14 16 18

_Z'_ ( k W )

0.0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5

_Z'_ ( k W )

2.0
(d) PNCG-24

1.6

1.2

0.8

0.4

Experimental
Fitting

1.2
(e) PNCG-32

1.0

0.8

0.6

0.4

0.2

Experimental
Fitting

0.0

0.0 0.4 0.8 1.2 1.6 2.0

_Z'_ ( k W )

0.0
0.0 0.2 0.4 0.6 0.8 1.0 1.2

_Z'_ ( k W )

Figure 1. Impedance plot for MC:NaF samples with different ratios of glycerol

Table 2. The calculated EIS parameters after fitting the experimental data of PEO-NaCl

polymer electrolyte samples.

Ф1

Ф2

CPE1

CPE2

Rb

(Ω)

(S/cm)

~~???~~

Sample Codes

(µm)

_t_

(µm) (Rad) (Rad) (F -1 ) (F -1 ) (Ω) (S/cm)

PNCG-0 135 1.19 - - 1,590,400

PNCG-8 250 1.19 0.58 10,282

~~1.87 × 10~~ ~~−8~~ ~~1.38 × 10~~ ~~−8~~

4.11 × 10 −9 7.29 × 10 −6 3.94 × 10 −6

(Rad)

(F -1 )

PNCG-0 135 1.19 - - 1,590,400

PNCG-8 250 1.19 0.58 10,282

~~1.87 × 10~~ ~~−8~~ ~~1.38 × 10~~ ~~−8~~

PNCG-16 279 1.10 0.91 1,840

4.11 × 10 −9 7.29 × 10 −6 3.94 × 10 −6

2.87 × 10 −8 8.95 × 10 −6 2.46 × 10 −5

PNCG-8 250 1.19 0.58 10,282

PNCG-16 279 1.10 0.91 1,840

4.11 × 10 −9 7.29 × 10 −6 3.94 × 10 −6

PNCG-24 215 1.09 0.99 390

2.87 × 10 −8 8.95 × 10 −6 2.46 × 10 −5

5.81 × 10 −8 8.17 × 10 −6 8.94 × 10 −5

PNCG-16 279 1.10 0.91 1,840

PNCG-24 215 1.09 0.99 390

2.87 × 10 −8 8.95 × 10 −6 2.46 × 10 −5

PNCG-32 315 1.10 1.02 294

5.81 × 10 −8 8.17 × 10 −6 8.94 × 10 −5

4.75 × 10 −8 1.20 × 10 −5 1.74 × 10 −4

PNCG-24 215 1.09 0.99 390

PNCG-32 315 1.10 1.02 294

5.81 × 10 −8 8.17 × 10 −6 8.94 × 10 −5

4.75 × 10 −8 1.20 × 10 −5 1.74 × 10 −4

Relaxation time ( ~~?~~ ) represents the time required for ions or electrons to return to equilibrium

PNCG-32 315 1.10 1.02 294
4.75 × 10 −8 1.20 × 10 −5 1.74 × 10

after being perturbed by an external force, such as an electric field [18, 19].

Relaxation time ( ~~?~~ ) represents the time required for ions or electrons to return to equilibrium

after being perturbed by an external force, such as an electric field [18, 19].

1 1

~~2~~ ~~?????~~

?

?= 1

~~2~~

(7)

~~2~~ ~~?????~~

where maximum frequency ???? (in Hz) is the frequency of the relaxation peak. The diffusivity

(?) of ions in polymer electrolytes calculated by follow equation

where maximum frequency ????

(?) of ions in polymer electrolytes calculated by follow equation

?= 1 ? ????. ? 2

1 ? ????. ? 2

~~16~~ ~~(tan ????)~~

?= 1

~~16~~

(8)

? ????. ? 2

~~(tan ????)~~ ~~3~~

(tan ????) is the maximum tangent loss and ????is the

~~16~~ ~~(tan ????)~~ ~~3~~

frequency corresponding to maximum tangent loss. According to the Einstein equation, the

where ( _t_ ) is the sample thickness, (tan ????) is the maximum tangent loss and ????is the

frequency corresponding to maximum tangent loss. According to the Einstein equation, the

can be expressed through a relationship that incorporates temperature, DC conductivity, and

number of charge carriers (?) in electrochemical systems, particularly in polymer electrolytes,

frequency corresponding to maximum tangent loss. According to the Einstein equation, the

can be expressed through a relationship that incorporates temperature, DC conductivity, and

?= σ????

~~?. ?~~ ~~2~~

diffusivity, providing a comprehensive understanding of ion transport behavior.

(9)

????

represents the electric charge (1.6×10 ~~?. ?~~ ~~2~~ × ? -19 C), T is the ambient temperature

where _q_ represents the electric charge (1.6×10 -19 C), T is the ambient temperature

(approximately 300. K in this study), and kB denotes the Boltzmann constant (1.381×10 -23 J/K).

The DC conductivity ( _σdc_ ) is a measure of the mobility ( _μ_ ) of ions, which depends on the ion's

charge ( _q_ ) and the concentration of charge carriers ( _N_ ).

?= 1

~~?~~

1

~~?~~

σ??

~~?~~

(10)

??

~~?~~

The conductivity of a material is fundamentally influenced by the mobility of charge carriers,

with higher mobility generally correlating to increased conductivity. However, this relationship

is also contingent on the concentration of charge carriers within the material. Table 3 outlines

the ion transport parameters calculated using equations (7–10). The incorporation of 32 wt.%

glycerol into the polymer electrolyte substantially reduced the relaxation time, which in turn

enhanced ion diffusivity and mobility. These improvements in ion transport parameters

mobility, diffusivity, and charge carrier concentration are critical for boosting the performance

of energy storage devices like batteries and supercapacitors. The role of plasticizers, such as

glycerol, is pivotal in optimizing the physicochemical properties of polymer electrolytes for

efficient ion transport. Enhancements in these properties directly contribute to better energy

storage performance, as demonstrated by studies on glycerolized polymer electrolytes. For

instance, Aziz et al. and Adam et al. reported that glycerolized polymer electrolytes exhibited

high specific capacitance and energy density over prolonged cycles, emphasizing glycerol's

potential as an effective plasticizer in high-performance solid-state electrolytes [25].

Furthermore, Adam et al. (2023) observed that the addition of glycerol in potassium-ion
conducting solid biopolymer electrolytes increased ion mobility and facilitated the dissociation

of ion aggregates, resulting in higher ion concentration and improved mobility [7]. Glycerol, as

a plasticizer, plays a crucial role in enhancing the ion transport properties of polymer

electrolytes. By increasing ion mobility, diffusivity, and number density while simultaneously

reducing relaxation time, glycerol contributes significantly to the efficiency and durability of

energy storage devices. These advancements underscore the importance of designing polymer

electrolytes with optimized compositions to meet the demands of next-generation energy

storage technologies

Table 3 . Ion transport properties, including mobility, relaxation time, diffusivity, and charge

carrier density.

_N_

Sample Codes

(µs)

~~?~~

_D_

(µs) (cm 2 /s) (cm -3 ) (cm 2 V -1 s -1 )

PNCG- 0 1591.5494

PNCG- 8 140.6273

1.40 ~~× 10~~ ~~−2~~ 1.59 ~~× 10~~ ~~11~~ 5.43 ~~× 10~~ ~~−1~~

1.00× 10 −3 6.35× 10 14 3.87× 10 −2

(cm -3 )

(cm 2 V -1 s -1 )

V -1

~~?~~

(cm 2 /s)

PNCG- 0 1591.5494

PNCG- 8 140.6273

1.40 ~~× 10~~ ~~−2~~ 1.59 ~~× 10~~ ~~11~~ 5.43 ~~× 10~~ ~~−1~~

PNCG- 16 27.440886

1.00× 10 −3 6.35× 10 14 3.87× 10 −2

3.16× 10 −3 1.26× 10 15 1.22× 10 −1

PNCG- 8 140.6273

PNCG- 16 27.440886

1.00× 10 −3 6.35× 10 14 3.87× 10 −2

PNCG- 24 6.212161

3.16× 10 −3 1.26× 10 15 1.22× 10 −1

1.05× 10 −2 1.37× 10 15 4.06× 10 −1

PNCG- 16 27.440886

PNCG- 24 6.212161

3.16× 10 −3 1.26× 10 15 1.22× 10 −1

PNCG- 32 5.095926

1.05× 10 −2 1.37× 10 15 4.06× 10 −1

9.62 × 10 −3 2.94× 10 15 3.72 × 10 −1

PNCG- 24 6.212161

PNCG- 32 5.095926

1.05× 10 −2 1.37× 10 15 4.06× 10 −1

9.62 × 10 −3 2.94× 10 15 3.72 × 10 −1

3.2. Dielectric Properties

The dielectric constant ( 3.2. Dielectric Properties ?r) and dielectric loss (?i) describe the ability of materials to store and

dissipate electrical energy [26-28]. The ?r represents the polarization response to an applied

The dielectric constant (?r) and dielectric loss (?i) describe the ability of materials to store and

dissipate electrical energy [26-28]. The ?r represents the polarization response to an applied

electric field, while ?i indicates the energy dissipated as heat due to ionic motion [29, 30]. The

dissipate electrical energy [26-28]. The ?r represents the polarization response to an applied

electric field, while ?i indicates the energy dissipated as heat due to ionic motion [29, 30]. The

values of ?r and ?i were determined at different frequencies using the following equations [31]:

electric field, while ?i indicates the energy dissipated as heat due to ionic motion [29, 30]. The

values of ?r and ?i were determined at different frequencies using the following equations [31]:

? ??

? ??
ε? =
~~????(??2~~

? ??
ε? =

(11)

?

~~2 + ??2)~~

(12)

?

ε? =
~~????(??2~~

? ??
ε? =
~~????(??2~~

~~2)~~

(12)

?

~~2 + ??2)~~

8.85 × 10 −12 F/m).

ε? =
~~????(??2 + ??2)~~

where ?? is the permittivity of free space (8.85 × 10 −12 F/m).

Figure 2 (a) and (b) display the amounts of ?r and ?i

where ?? is the permittivity of free space (8.85 × 10 −12 F/m).

Figure 2 (a) and (b) display the amounts of ?r and ?i, respectively, at different frequencies for

all samples. At low frequencies, both ?r and ?i exhibit higher values due to efficient ionic and

Figure 2 (a) and (b) display the amounts of ?r and ?i, respectively, at different frequencies for

dipolar polarization, as ions have enough time to orient themselves with the applied electric

all samples. At low frequencies, both ?r and ?i exhibit higher values due to efficient ionic and

dipolar polarization, as ions have enough time to orient themselves with the applied electric

field [32]. However, as the frequency increases, these values decline sharply because the rapid

oscillations of the field inhibit ionic and dipole responses. The convergence of dielectric

constant values across glycerol concentrations at high frequencies highlights the diminishing

role of ionic mobility under fast field reversals, emphasizing the system's relaxation dynamics

[33].

Additionally, Figure 2 indicates that the glycerol additive, as a plasticizer, significantly

enhances the dielectric properties. The hydroxyl groups in glycerol interact with ions from the

polymer and salt, enhancing polarizability and promoting dipole alignment with the electric

field. This interaction results in improved ionic conductivity and increased energy dissipation

capacity [34]. This is achieved by enhancing ion motion within the polymer, which reduces ion

aggregation and allows a greater number of free ions to participate in charge transport [32].

The high ionic mobility, particularly at low frequencies, leads to greater dielectric loss due to

the dissipation of energy during ionic migration. However, dielectric loss decreases because the

ions are unable to keep up with the field oscillations at higher frequencies [35]. The

improvement in ionic conductivity underscores glycerol's significance in enhancing the

electrochemical performance of polymer electrolytes.

100000

(a) PNCG-0

90000 PNCG-8

PNCG-16

80000

PNCG-24

70000 PNCG-32

90000

(a)

80000

70000

60000

50000

40000

30000

20000

10000

2 3 4 5 6

log ( _f_ /Hz)

90000 (b) PNCG-0
PNCG-8

80000 PNCG-16

PNCG-24

70000

PNCG-32

(b)

80000

70000

60000

50000

40000

30000

20000

10000

2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5

log ( _f_ /Hz)

Figure 2. Frequency-dependent dielectric properties of the PEO:NaCl system with varying

glycerol ratios: ( a ) real dielectric constant and ( b ) dielectric loss (imaginary component)

The ratio of the imaginary component (glycerol ratios: ( a ) real dielectric constant and (??) to the real component ( b ) dielectric loss (imaginary component) ??) defines a parameter known

as the dielectric loss tangent (tan ?) [36], also referred to as the dissipation factor. It can be

The ratio of the imaginary component (??) to the real component (??) defines a parameter known

determined using the following expression [37]:

as the dielectric loss tangent (tan ?) [36], also referred to as the dissipation factor. It can be

determined using the following expression [37]:

tan ?= ε?

~~ε?~~

ε?

~~ε?~~

(13)

NaCl polymer electrolytes with different glycerol concentrations (8–32%). The sample without

Figure 3 reveals that the dielectric loss tangent (tan?) varies as a function of frequency for PEO

NaCl polymer electrolytes with different glycerol concentrations (8–32%). The sample without

energy dissipation. Distinct peaks emerge at specific frequencies, which shift toward higher

glycerol (PNCG-0) exhibits lower tan? values, indicating limited ionic mobility and minimal

NaCl polymer electrolytes with different glycerol concentrations (8–32%). The sample without

energy dissipation. Distinct peaks emerge at specific frequencies, which shift toward higher

frequencies with increasing glycerol content. This shift reflects reduced relaxation times due to

enhanced polymer chain mobility [38]. The incorporation of glycerol produces sharper and

more pronounced peaks, signifying improved relaxation dynamics. At the highest glycerol

concentration (PNCG-32), the peaks display increased intensity along with a frequency shift,

indicating further enhancement of energy dissipation and ionic mobility. These results

demonstrate that glycerol effectively enhances dielectric properties and ionic mobility by

reducing polymer rigidity [39].

PNCG-0
PNCG-8
PNCG-16
PNCG-24
PNCG-32

0
2 3 4 5 6

log ( _f /_ Hz)

Figure 3. The dielectric loss tangent vs. frequency for PEO:NaCl system

The electrical modulus is a useful parameter for analyzing relaxation dynamics and ionic

conduction in polymer electrolyte systems. It consists of two components: the real part (??)

and the imaginary part (??), which can be calculated using the following expressions [20]:

The electrical modulus is a useful parameter for analyzing relaxation dynamics and ionic

conduction in polymer electrolyte systems. It consists of two components: the real part (

and the imaginary part (??), which can be calculated using the following expressions [20]:

(14)
ε?
?? = [ ~~(ε?~~ ~~2~~ ~~+ ε?~~ ~~2~~ ~~)~~ ]

(15)
ε?

Figure 4 illustrates the frequency dependence of the real (?? = [ ~~(ε?~~ ~~2~~ ~~+ ε?~~ ~~2~~ ~~)~~ ] _Mr_ ) and imaginary ( _Mi_ ) components

of the electrical modulus for the polymer electrolyte system:

(a) As shown in Figure 4a, _Mr_ remains close to zero at lower frequencies, indicating the

dominance of electrode polarization effects in this range. This behavior is associated with the

material's high capacitance, which obscures relaxation processes [40]. As the frequency

increases, _Mr_ steadily rises, signifying the reduction of electrode effects and the increasing

prominence of the material's intrinsic relaxation dynamics.

(b) Figure 4b displays the imaginary component _Mi_, which exhibits a distinct peak at higher

frequencies. This peak corresponds to the conductivity relaxation process, involving ionic

mobility and polymer matrix reorganization [41]. The relaxation frequency ( _fmax_ ), associated

with the peak, is inversely proportional to the relaxation time, as described by Equation (7) [42].

The height and width of the _Mi_ peak provide insights into the degree of ionic interaction and

the structural heterogeneity of the material [43].

The results reveal that the addition of a plasticizer to the polymer electrolyte system causes the

_Mi_ peak to shift dramatically toward higher frequencies. This shift becomes more pronounced

with increasing plasticizer content, indicating enhanced ionic mobility and reduced relaxation

times in the system.

0.40
PNCG-0
PNCG-8

0.35

PNCG-16
PNCG-24

0.30

PNCG-32

(a)

0.35

0.30

0.25

0.20

0.15

0.10

0.05

0.00

1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5

log ( _f_ /Hz)

PNCG-0
0.10 PNCG-8
PNCG-16
PNCG-24

0.08

PNCG-32

0.06

0.04

0.02

0.00

(b)

1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5

log ( _f_ /Hz)

Figure 4. Electrical modulus components of PEO:NaCl polymer electrolytes with varying

glycerol concentrations: ( a ) real part (??) and ( b ) imaginary part (??)

Figure 4. Electrical modulus components of PEO:NaCl polymer electrolytes with varying

3.3. FTIR Spectroscopy

FTIR (Fourier-transform infrared) spectrum showing transmittance (%) as a function of

wavenumber (cm⁻¹) for five samples, labeled S1 to S5. FTIR spectra are frequently utilized to

detect functional groups in a substance by studying absorption bands that represent the

vibrations of molecules. Figure 5 illustrates the FTIR spectra of PEO-NaCl with various

percentages of glycerol added. The peaks in S2, S3, S4, and S5 that appear around 3300-3500

cm⁻¹ are often attributed to O-H stretching vibrations, indicating the presence of hydroxyl

groups in alcohols [44]. The broad intensity of PEO-NaCl at 3356 cm⁻¹ increases from 0% to

32% with glycerol addition, due to the O-H group in the glycerol structure [20]. Peaks around

2880 cm⁻¹ may signify C-H stretching vibrations [45], while the weak absorption band around

2361 cm⁻¹ indicates the presence of complex salt [46]. The peak around 1461 cm⁻¹ corresponds

to CH₂ bending vibrations in the glycerol molecule [47]. The sharp and strong peak around

1096 cm⁻¹ indicates C-O stretching vibrations [48]. This peak is common in compounds

containing alcohols, such as glycerol, and arises from stretching vibrations of the C-O bond in

the hydroxyl groups. The peak around 530 cm⁻¹ in an FTIR spectrum is often associated with

lattice and bending vibrations [48]. The observed peak could be related to glycerol or the

polymeric system and the interaction between glycerol and salt [49]. Glycerol can enhance

polymer mobility by forming hydrogen bonds with PEO and NaCl [50]. These findings

generally suggest that glycerol increases hydrogen bonding, enhances polymer chain flexibility,

and alters the structural patterns of the PEO-NaCl systems [51]. This structural change is

essential for applications that require increased flexibility and conductivity of ions.

C-H Bending C-O Stretching

530

O-H Stretching

3356

C-H Stretching Peak Complex Salt

2880 2361 1461 1343 1096 951 839

4000 3500 3000 2500 2000 1500 1000 500

Wavenumber (cm-1)

Figure 5. The FTIR spectra of the PEO-NaCl with different glycerol additives

Figure 6 reveals the schematic illustrates the polymer-salt complex formation involving sodium

cations (Na⁺) and Chloride (Cl⁻) with PEO polymer. The interaction occurs as Na⁺ coordinates

with the hydroxyl groups present on the PEO polymer backbone, forming ionic crosslinks that

enhance the structural stability of the polymer network. Simultaneously, Cl⁻ interacts through

electrostatic forces with the positively charged regions of the PEO-salt system, further

stabilizing the complex. The illustration highlights the spatial arrangement and binding

mechanism within the PEO-salt complex.

Figure 6. Polymer-Salt Complex Formation of cations (Na + ) and anions (Cl − ) with PEO

3.4. XRD Study

X-ray diffraction (XRD) is a powerful technique for investigating the structural composition of

polymer electrolytes. By analyzing the diffraction peaks, researchers can gain valuable insights

into the relationship between crystalline structures and their corresponding diffraction patterns

[52]. The XRD analysis of the PEO-NaCl–glycerol complex provides detailed information on

the crystalline structure and phase properties of the system. The incorporation of salts, such as

NaCl, and plasticizing agents, like glycerol, induces significant changes in the crystalline

structure of PEO, which is inherently semicrystalline [53].

Figure 7 presents the XRD patterns of PEO-NaCl complexes with varying glycerol

concentrations. The semicrystalline PEO exhibits two distinct diffraction peaks at 18.37° and

22.24°, characteristic of its crystalline phase. Additional peaks at 30.71° and 44.61° correspond

to undissolved NaCl, indicating incomplete salt dissolution in the polymer matrix [4].

At lower glycerol concentrations (0–8%), the XRD patterns exhibit sharp and distinct peaks,

indicating higher crystallinity. At these levels, glycerol has a minimal impact on the crystalline

structure of PEO [24]. With the incorporation of 16% glycerol, the observed peak intensities

decrease, suggesting a reduction in crystallinity. However, as the glycerol concentration

increases to 24%, two distinct peaks reappear with enhanced intensity, signifying a further

reduction in crystallinity and an increase in the amorphous nature of the material [20]. At the

highest glycerol concentration (32%), the peaks become broader and less defined, indicating a

significant decrease in crystallinity. This behavior is attributed to glycerol acting as a

plasticizer, disrupting the crystalline regions of PEO and promoting amorphous characteristics

[21].

The crystallinity of the samples varies substantially, ranging from 84.95% (PNCG-0, the pure

sample) to 34.57%. The pure sample exhibits the highest crystallinity and a more organized

structure, which contributes to enhanced mechanical strength but limits flexibility due to rigid

molecular packing. Glycerol, as a plasticizer, increases polymer chain flexibility by reducing

crystalline domains and creating channels that facilitate ion transport. This increased flexibility

and additional free volume improve ionic mobility [11].

Adjusting the glycerol concentration provides a means to optimize the polymer's structure and

ionic conductivity for electrolyte applications. Electrochemical impedance spectroscopy (EIS)

results further support this, showing that higher glycerol concentrations reduce bulk resistance

from XRD and EIS clearly demonstrate how structural changes in the polymer (as revealed by

(??), thereby enhancing ionic conductivity, as described by Eq. (6). The complementary insights

results further support this, showing that higher glycerol concentrations reduce bulk resistance

from XRD and EIS clearly demonstrate how structural changes in the polymer (as revealed by

XRD) directly influence its electrical performance (as evidenced by EIS) in the PNCG system.

The degree of crystallinity ( _Xc_ ) was calculated using Equation (16) [54]:

? _X_ ? _c_
?? =
~~??~~ ~~+ ??~~

(16)
× 100 _Aa_ represents the area of the amorphous

where _Ac_ represents the area of the crystalline region, _Aa_ represents the area of the amorphous

region, and _Xc_ indicates the percentage of crystallinity. Figure 8 illustrates the crystallinity of

the polymer/salt system before and after the incorporation of the plasticizer. The addition of

glycerol generally reduced the crystallinity of the system, enhancing the dissociation of salt into

cations and anions. This dissociation subsequently increased the concentration of charge

carriers in the solid polymer electrolyte (SPE).

·

PNCG-32

PNCG-24

PNCG-16

PNCG-8

PNCG-0

· PEO ¨ NaCl salt

¨
¨
¨

10 15 20 25 30 35 40 45 50 55 60 65 70

2 Theta (Degree)

Figure 7. The XRD patterns of different glycerol of additives for the PEO-NaCl system

100

0
PNCG-0 PNCG-8 PNCG-16 PNCG-24 PNCG-32

Sample Codes

Figure 8 . The degree of crystallinity was determined from the XRD pattern

4. Conclusion

This study demonstrates the potential of glycerol as a plasticizer for improving the

electrochemical performance of PEO-NaCl-based polymer electrolytes. The addition of

glycerol significantly reduced the crystallinity of PEO, enhancing ion mobility and

conductivity. The EIS measurements revealed that the highest ionic conductivity, 1.74 × 10 -4

S/cm, was achieved at a 32% glycerol concentration, i.e., the conductivity increased by

approximately 12,609 times from the glycerol-free sample to the sample with 32% glycerol.

This enhancement is attributed to improved ion dissociation and mobility due to reduced

polymer rigidity and better interaction between the polymer chains and the salt ions. Dielectric

property analysis confirmed that glycerol increases polarizability by promoting dipole

alignment and reducing ion aggregation, leading to greater energy dissipation and improved

charge transport. The sharp dielectric loss peaks at higher frequencies with increasing glycerol

content indicate enhanced relaxation dynamics and reduced polymer matrix rigidity. The results

underscore the importance of optimizing glycerol concentration to balance ionic conductivity

and mechanical stability. Excessive plasticizer content may compromise structural integrity, but

within the optimal range, glycerol demonstrates substantial improvements in conductivity and

dielectric properties. These findings suggest that PEO-NaCl-glycerol-based polymer

electrolytes are promising candidates for applications in solid-state electrochemical devices,

such as batteries, fuel cells, and supercapacitors, providing an efficient, stable, and cost

effective alternative to conventional liquid electrolytes. Future work should explore the long
term stability and scalability of these materials.

Availability of data and materials

The data that support the findings of this study are available from the corresponding author

upon reasonable request.

Conflict of Interest

There are no financial and non-financial competing interests.

Funding

The authors declare that they have no conflict of interest.

Author contributions:

S. B. Aziz : Supervision, Project administration, Conceptualization, Review.

I. N. Qader and S. Y. Omar visualization.

P. A. Ibrahim synthesis polymer films.

D. S. Muhammad, P. Aspoukeh, S. M. Hamad, and S. M. Hussein performed the

characterizations.

K. A. Babakr, R. A. Omer, I. L. Salih, H. Hamad Rasul, S. S. Mohammed, D. A. Hamid,

P. H. Mahmood, and A. W. Muhammed data analysis and writing.

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