Molekul, Vol. 20. No. 2, July 2025: 258 – 267

Articles

MOLEKUL
eISSN: 2503-0310

https://doi.org/10.20884/1.jm.2025.20.2.11050

N-Doped and Chemically Activated Carbons Derived from Shrimp Shells Waste as Potential
Electrode Materials for Electrochemical Supercapacitors
Siti Khuzaimah1, Muhammad Mujiburohman2*, Agung Sugiharto2, Tri Widayatno2, Ahmad M. Fuadi2
Departement of Chemical Engineering, Fakulty of Industrial Technology, Nahdlatul Ulama Al Ghazali
Cilacap University, Cilacap 53274, Indonesia
2
Departement of Chemical Engineering, Fakulty of Engineering, Muhammadiyah Surakarta University,
Surakarta 57102, Indonesia

1

*Corresponding author email: mmujiburohman@ums.ac.id
Received January 15, 2024; Accepted March 26, 2025; Available online July 20, 2025

ABSTRACT. Supercapacitors are widely recognized as energy storage solutions due to their high-power densities and long
cycle life. Furthermore, there is growing scientific and technological interest in converting biomass waste into carbon
materials for manufacturing supercapacitor electrodes. In addition to their abundance and cost-effectiveness, the appeal of
carbons derived from biomass lies in their tuneable porosity, which enables the rational design of carbon materials to achieve
the desired performance of supercapacitors. This work presents the synthesis of activated carbons from shrimp shells waste
and its application for supercapacitor electrodes, with an activation treatment using phosphoric acid (H3PO4) and nitrogen
doping (N-doped). The activator concentration was varied at 3, 6, and 9 M; while the N-doped ratios were 1:3, 1:5, and
1:7. The characteristics of activated carbon and supercapacitor electrodes was analysed with BET, SEM, CV, and GCD. The
resulting materials exhibited amorphous and predominant microporous structures. Increasing the activation concentration
gave smaller specific surface area, from 17.522 to 9.509 m 2 g−1. The electrochemical properties of these activated carbons
for supercapacitor applications were investigated by cyclic voltammetry, galvanostatic charge–discharge, with KOH
electrolyte. The best activated carbon produced was mesoporous with the highest specific surface of 17.522 m2/g, obtained
at 3 M H3PO4 and a nitrogen doping ratio of 1:3. At the same activator concentration and nitrogen doping ratio (3 M; 1:3),
the highest capacitance was obtained 16.320 Farad, with current charging and discharging stop at 475 seconds and 1235
seconds, respectively. This work showcases the efficient and sustainable utilization of shrimp shells waste as a carbon source
for supercapacitor applications and highlights their value in a circular economy.
Keywords: Activated carbon, Activator H3PO4, Nitrogen doping, Shrimp shell, Supercapacitor

INTRODUCTION
Environmental worries over the continuous use of
non-renewable resources and the growing complexity
of power distribution networks have spurred the urgent
exploitation of sustainable and renewable energy
sources, such as wind and solar energy (Fu et al.,
2023). The energy crisis and growing concerns about
the environmental impact of non-renewable energy
sources have driven recent technological revolutions in
the energy sector (Chaiammart et al., 2024).
Supercapacitors or batteries can be used as energy
storage components in energy storage systems.
Depending on the systems and applications for which
it is designed, each energy storage technology has
unique advantages (Tafete et al., 2024). The
advancement of energy storage equipment and
technology is fuelled by rising energy usage.
Supercapacitors are impressive devices with steady
cycle performance and good charge-discharge
efficiency, but their low energy density remains a

significant problem that requires attention (Zhou &
Yao, 2022). Conventional batteries in the form of dry
cells as used in TV remotes or clocks are only used
once, then become waste and pollute the
environment. To avoid environmental pollution due to
battery waste, rechargeable battery components have
been developed as electrical energy storage devices.
Apart from batteries, electrical energy storage can be
in the form of capacitors.
Waste or by-products from natural resources can
offer an alternative to the electrode material used for
renewable energy storage, thereby addressing the
issues of cost and environmental impact (Boamah et
al., 2023). The development of capacitors continues,
one of which is called a supercapacitor (Sharma &
Bhatti, 2010). Supercapacitors have some advantages
including high capacity, large power density, and fast
charging (González et al., 2016; Park et al., 2013;
Senthil & Lee, 2021). To improve the performance of
supercapacitor, electrochemically double layer

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Siti Khuzaimah, et al.

capacitors (EDLC) or electrical double layer
supercapacitors have been developed which consist of
two layers of electrodes separated by a separator (Liu
et al., 2018; Qu et al., 2015; Raj et al., 2018; Taer et
al., 2013). Electric double-layer capacitance (EDLC) is
the electrostatic storage of charges in pure carbon
materials (Zhou & Yao, 2022). EDLCs are based on
the separation of charge at the electrode–electrolyte
interface while PCs involve reversible Faradaic redox
reactions, similar to those occurring in batteries
(Chaiammart et al., 2024).
Supercapacitor electrode materials are usually
chemicals containing heavy metals such as lead,
mercury, and nickel. However, heavy metals are
expensive and pose a risk of polluting the
environment. The use of electrodes from cheap and
safe materials has been developed. Electrodes and
electrical energy storage in electronic devices can use
activated carbon-based materials (Gao et al., 2017;
Treeweranuwat et al., 2020; Tumimomor &
Palilingan, 2018). Carbon electrode materials have
some unique advantages: (1) resource-rich, (2) no
concern for price, (3) easily manufacturing, (4)
hierarchical porous structure, (5) high thermal and
chemical stability, (6) good electronic conductivity, (7)
wide working temperature range (Lesbayev et al.,
2023). This is reasonable due to the characteristics of
activated carbon in which it has a high specific surface
and good electrical conductivity.
Activated carbon naturally exhibits high surface
area and porosity, which are critical for applications
like energy storage (Zhou & Yao, 2022). While
graphene and carbon nanotubes may offer higher
conductivity and mechanical strength, these
advantages are often unnecessary or marginal in costsensitive applications like supercapacitors, where
activated carbon's properties suffice (Thi et al., 2023).
Activated carbon stands out due to its affordability,
resource abundance, and well-suited properties for
supercapacitor applications. While graphene and
carbon nanotubes may offer superior performance
metrics in specific high-end applications, their high
costs and complex production processes limit their
practicality in cost-sensitive and large-scale
deployments (Fu et al., 2023). This makes activated
carbon a more viable and sustainable choice for most
supercapacitor applications (Boamah et al. 2023).
Activated carbon can be produced from natural
materials such as coconut shells, wood, or fruit peels
(Liu et al., 2016; Rawal et al., 2021; Trinh et al.,
2020). Activated carbon has many pores obtained
from the combustion process of materials having
carbon content of 85-90% with a specified pore
surface area (Elmouwahidi et al., 2017). Activated
carbon can be made according to its purpose after
carbonation and activation processes are conducted,
tailored to the desired characteristics. Besides plant
materials, carbon sources can also be found in animal
materials which are processed through both physical

and chemical activation processes. The carbon
sources from animal materials include shrimp shell
waste, which is not consumed because of its hard
texture (Sun et al., 2014). Shrimp shells contain 4050% calcium carbonate (Gao et al., 2016), so the
carbon content in carbonate has the potential to be
used as activated carbon for energy storage electrode
materials. The presence of calcium carbonate in
shrimp shells can significantly influence the outcomes
of the carbonization process due to its chemical
properties. During carbonization, calcium carbonate
undergoes thermal decomposition, releasing carbon
dioxide (CO₂) and leaving behind calcium oxide
(CaO). The release of CO₂ during decomposition can
create pores within the carbon structure, enhancing its
surface area and porosity. This is particularly useful for
applications like adsorption or catalysis. The release
of CO₂ during decomposition can create pores within
the carbon structure, enhancing its surface area and
porosity. This is particularly useful for applications like
adsorption or catalysis. Residual calcium compounds
in the final product can change the chemical reactivity
of the carbon, affecting its suitability for specific
applications.
Activated carbon having a high specific surface can
improve the performance of EDLC in supercapacitor
devices. The literature demonstrates that because of
their large specific surface area, superior electrical
conductivity,
affordability,
and
environmental
friendliness, activated carbon (AC) materials have
emerged as a potential material for electrostatic
accumulation (EDLC) (Hounkanrin et al., 2023).
(Tong et al., 2016) found that the capacitance of
activated carbon in supercapacitors is influenced by
the activation process, both activation time and
activator concentration. With carbon activated by 9 M
KOH solution and a nitrogen doping ratio of 1:7
(mass of carbon : mass of urea) (Qu et al., 2015)
obtained a supercapacitor capacitance of 25 Farad.
Even though it is not too high, this capacitance meets
the IEC 62391-1:20026 standard, i.e. 0.6-700 Farad.
Recent research indicates that nitrogen doping on
carbon surfaces results in charge delocalization, which
facilitates the binding and transfer of certain molecules
onto carbon (Gao et al., 2019). Such doping also
increases the conductivity of the porous carbon.
Considering the potency of shrimp shells waste, this
work presents the synthesis of activated carbons from
shrimp shells waste using an activator of phosphoric
acid (H3PO4) and nitrogen doping. The effects of
activator concentration and N-doped ratio on the
characteristics of activated carbon and the
electrochemical
properties
of
manufactured
supercapacitors were investigated. The supercapacitor
was made of a stainless-steel collector, and the
electrolyte in the separator was a KOH solution. For
the purpose of characterizing activated carbon and
supercapacitors, Brunauer-Emmet-Teller (BET) test,
Scanning Electron Microscopy (SEM), Cyclic

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Voltammetry (CV), and Galvano charge discharges
(GCD) were used.
EXPERIMENTAL SECTION
The materials used in this research include shrimp
waste, distilled water, H3PO4, KOH, dimethyl sulfoxide
(DMSO), polyvinylidene fluoride (PVDF), technical
grade urea, and ethanol. The tools and analysers used
standard analytic laboratory glass wares, BET, SEM,
CV, and GCD. The experimental work was carried out
through several stages, namely preparation of raw
materials, carbonation of shrimp waste, carbon
activation, manufacture of supercapacitors, as well as
testing the characteristics of activated carbon and
electrochemistry of supercapacitors.
The shrimp waste in the form of shrimp shells and
tails was cleaned with clean water, and then cleaned
using distilled water. The cleaned shrimp waste was
dried in the sun for 3 days. The results were dried in
the oven for 5 hours at 100°C. Then, the dried shrimp
waste was ground using a blender and sieved through
a 150-mesh sieve for 7 hours. A total of 12 g of urea
was dissolved in ion-free water to 100 mL. Dry shrimp
waste from the furnace was weighed as much as 20 g,
to be put into an impregnation flask, refluxed using a
temperature of 70°C, and stirred using a magnetic
stirrer with the addition of urea until a mixture of slurry
was produced. The shrimp waste slurry was put into an
autoclave reactor for carbonation. After impregnation
with urea, the mixture was separated and rinsed using
ethanol.
A total of 10 g of shrimp shell biochar that had
been impregnated with urea was soaked in a
phosphoric acid activator solution (H3PO4) with
concentration variations of 3, 6, and 9 M. Soaking was
carried out for 24 hours to ensure the diffusion process
reached the inside of the charcoal, carbonization,
subsequent activation, and modification of their
surface have a significant impact on the structure and
properties of activated carbon (Lesbayev et al., 2023).
Then, the activated carbon was dried in an oven for
24 hours. The carbon that has been activated was then
washed using distilled water until the pH was neutral.
The washing results were filtered and then the
activated carbon was dried again in the oven for 2
hours.

5 g of activated carbon material was mixed with
PVDF and DMSO, with a ratio of 40% PVDF and 4 mL
DMSO. The gluing technique used the solid-state
reaction or wet mixing method. The solution was
heated and stirred using a hot plate until a gel forms.
The gel was used as a supercapacitor electrode.
The type of capacitor made was an Electrical
Double Layer Capacitor (EDLC) in a symmetrical
shape using two activated carbon electrodes with
dimensions of 2 x 2 cm, and two stainless steel mesh
plates that have been sprinkled with carbon composite
with PVDF and DMSO. The activated carbon electrode
was separated by a separator in the form of a 6 M
KOH solution electrolyte. The EDLC scheme is
illustrated in Figure 1.
Sample Analysis
The characteristic of activated carbon was
measured from the specific surface using the BET test
(Rawal et al., 2021). The electrochemical
characteristics of supercapacitors were determined
from the capacitance and charge-discharge time. The
capacitance and charge-discharge time were
measured by GCD (Kampouris et al., 2015). The GCD
test applied a voltage range of 0.1-1 V. The
capacitance value C (in Farad) was calculated using
the following formula (Lin et al., 2019):
𝐶=

∫ 𝐼𝑑𝐸
2𝛾𝑉𝐸

͌

=|

𝐼𝑐 𝑥𝑙𝑛𝑙𝑛 ∆𝐸 𝑥 𝐴
2𝛾

|

where γ is the scane rate (V/s), ΔE is the potential
windows (Volt), Ic is the current density (A/m2), and A
is the surface area (m2).
RESULTS AND DISCUSSION
Surface Morphology of Activated Carbon
The activated carbon electrodes from shrimp waste
which were activated using H3PO4 solution can be
seen in Figure 2. Meanwhile, the surface morphology
of the activated carbon as influenced by the H3PO4
activator concentration (3, 6, 9 M) is shown
respectively in Figure 3a, 3b, and 3c. The
characterization of activated carbon to determine the
physical properties and surface morphology of
activated carbon used SEM (De et al., 2023; Salawu
et al., 2022).

Figure 1. A schematic supercapacitor of EDLC
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Siti Khuzaimah, et al.

Figure 2. The carbon-based electrode activated with H3PO4 and nitrogen doping

(a)

(b)

(c)
Figure 3. The morphological structure of activated carbon from shrimp waste with activator concentration of 9
M doping ratio 1:7 (a), 6 M doping ratio 1:5 (b), and 3 M doping ratio 1:3 (c).
The results of surface analysis of activated carbon
using SEM (3000 × magnification) show that there are
differences in morphology because of variations in
activator concentration. The role of the activator in the
activation process is to absorb the mineral content in
the material and to prevent the formation of ash on
the carbon (Prayogatama et al., 2022). The content of
oxygen groups in the raw material allows reactions to
occur with acid (H3PO4). H3PO4 is also able to remove
hydrocarbon compounds and to open pores on the
surface of materials. At a concentration of 9 M H3PO4,
the particle size is not uniform and looks like irregular
chunks, with a pore size of around 10 µm. At a
concentration of 6 M H3PO4, it appears that the pores

are more numerous and more uniform with a smaller
pore size, around 5 µm. At a concentration of 3 M
H3PO4, more and smaller pores are visible with a pore
size of around 1.6 µm. It can be concluded that the
lower the concentration of the H3PO4 activator in fact
opens more pores in the carbon. H3PO4 is a weak
acid, thus the ionization process is reversible and
undergoes through 3 stages to form H2PO4-, HPO42-,
and PO43, so that pore formation in carbon occurs
more effectively at low H3PO4 concentrations. The
results of this work are different from those conducted
by (Qu et al., 2015) which used HCl acid as an
activator to activate carbon from shrimp head waste.
HCl is a strong acid, almost completely ionizes into H+

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and Cl- ions and is able to remove CaCO3 from
carbon materials so it has a smaller pore structure with
a pore size of 3.9 nm. Biocarbon derived from
Miscanthus activated KOH thus open channels
remained and surface morphology became rough
when the KOH/BC ratio increased to 5:1, the BC bulk
structure partly collapsed and became interconnected
with the channels inside (You et al., 2018).
The greater the carbon pore volume and the
smaller the carbon pore diameter, the greater the
surface area and adsorbent power of the carbon. The
morphological structure of activated carbon is closely
related to the electrochemical properties of energy
storage devices, where the pores on the carbon
electrode can facilitate the process of ion diffusion into
the micropores on the electrode surface (Taer et al.,
2018), thereby influencing the capacitance value
where the pores become the charge storage (Rawal et
al., 2018). This cluster can prevent the aggregation of
N-doped carbon layers and improve the porosity and
roughness of the N-doped carbon electrode, therefore
increasing its surface area and catalytic activity.
Because of the increased nitrogen content, HC4 has a
hollow structural shape and a greater surface area of
560.72 m2/g (Tafete et al., 2024).
Specific Surface of Activated Carbon
The specific surface was analysed based on the
amount of nitrogen gas absorbed by the activated
carbon, using the BET method. The specific surface of
activated carbon from shrimp waste is shown in Figure
4. At H3PO4 concentrations of 9 M, 6 M, 3 M, and
doping ratios of 1:7, 1:5, 1:3, the specific surfaces are
9.509 m2/g, 11.581 m2/g, and 17.522 m2/g,
respectively. This is consistent with the surface
morphology of activated carbon shown in Figure 3a,
3b, and 3c, that at lower H3PO4 concentrations it
produces more pores with smaller pore diameters. The
pore diameter and pore volume affect the specific
surface and absorption capacity of carbon. In BET
analysis, smaller pore diameters allow more nitrogen
molecules to adsorb to the surface, hence increasing
the specific surface area. Thus, the smaller the pore
diameter, the larger the specific surface.

Capacitance of Activated Carbon Electrode
The ability to store electrical energy by
supercapacitor electrodes is measured from the
capacitance
properties
and
charge-discharge
performance characteristics. A good supercapacitor is
one that meets the International Electrotechnical
Commission (IEC) 62391-1:2006 double layer
supercapacitor standard which is used in electronic
component applications. The capacitance is expressed
in Farad (F) units. The determination of capacitance
used the CV method based on the initial and final
voltage characteristics (Rawal et al., 2021). The
potential that exists in CV measurements consists of the
charging and discharging current density. The
electrodes used in the voltammetry cell consist of 3
electrodes, namely working electrode, reference
electrode, and auxiliary electrode. The reference,
support, and working electrodes are gold disc,
platinum wire and Ag/AgCl, respectively. The
voltammogram curve of the measurement results with
a potential difference of 0-1 V at various activator
concentrations and nitrogen doping ratios can be seen
in Figure 5, 6, and 7.
At a potential difference of 0-1 V and a scan rate
of 0.002 V/s A slow scan rate, such as 0.002 V/s,
allows the system to remain closer to equilibrium
during the measurement. This minimizes distortions
caused by resistive or kinetic limitations, ensuring
more accurate measurement of capacitance. The
highest current is obtained at a concentration of 3 M
with a nitrogen doping ratio of 1:3. The curve
obtained is rhomboid in shape. Referring to the
literature (Zhang et al., 2021) the curve has sharp
edges because the electric current flow is proportional
to the potential difference generated. The shape of the
curve is also influenced by the charge and discharge
currents, where the greater the charge-discharge
current, the wider the shape of the curve (Elmouwahidi
et al., 2017). The capacitance values of activated
carbon electrodes based on the CV test results are
presented in Table 1 and Figure 6. The sample that
has the highest capacitance is the AC-001 sample,
which was activated by 3 M H3PO4 and a nitrogen
doping ratio of 1:3, i.e. 16.3206 Farad.

Figure 4. Specific surface of activated carbon from shrimp waste.
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N-Doped and Chemically Activated Carbons Derived

Siti Khuzaimah, et al.

(a)

(b)

(c)
Figure 5. The voltamogram curve of H3PO4 activator with 1:3 nitrogen doping.
Table 1. The results of the capacitance calculation are based on the voltammogram curve
Sample
AC-001
AC-002
AC-003
AC-004
AC-005
AC-006
AC-007
AC-008
AC-009

Scane Rate/Y
(V/s)
0.002
0.002
0.002
0.002
0.002
0.002
0.002
0.002
0.002

Ec (V)

Ic (A/m2)

A (m2)

Ln (ΔE)

C (Faraday)

0.53808
0.46569
0.43223
0.69820
0.69830
0.69715
0.69868
0.69821
0.69718

26.33
16.90
8.473
3.692
2.632
6.715
5.538
3.757
7.284

0.004
0.004
0.004
0.004
0.004
0.004
0.004
0.004
0.004

0.6197
0.7642
0.8387
0.3592
0.3591
0.3607
0.3585
0.3592
0.3607

16.3206
12.9206
7.10726
1.32651
1.94522
0.42250
1.98604
1.34979
0.62744

Figure 6. The capacitances of activated carbon electrodes at various activator
concentrations and doping ratios
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The 9 M concentration with the nitrogen doping
ratio of 1:7 has a lower capacitance value. The trend
of capacitance is similar to that of specific surfaces in
which the higher the concentration and nitrogen
doping ratio, the lower the capacitance value. The
capacitance is influenced by carbon pores, carbon
specific surface, sample thickness, and material
permittivity. The wider the specific surface of activated
carbon, the more electric charge can be stored, so the
higher the capacitance. The BET test shows that the
specific surface of activated carbon at a concentration
of 3 M and doping ratio of 1:3 is 17.522 m2/g, greater
than at a concentration of 9 M and doping ratio of
1:7, i.e. 9.509 m2/g.
Characteristics of Charge-Discharge
The performance of supercapacitor electrodes
made from shrimp waste activated carbon was
measured from the charging and discharging times
using the GCD method. The supercapacitors are
capable of discharging two voltage points at a
constant current. The potential used was 0-2 V at a
current of 10 mAcm-2. The GCD curves for carbonbased supercapacitors are generally triangularly
symmetric, showing almost linear changes in potential
as a function of time during charging and discharging
(Farma et al., 2013). The generated potential is
plotted against time, producing a linear data trend,
with both positive and negative slopes. The deviations
from linearity can occur due to an increase in voltage
with each additional time, so that the same resistance
can cause a rapid decrease. The performance of
supercapacitors depends on the presence of
electrically charged ions, which fill the pore walls of

the activated carbon electrode by a diffusionadsorption mechanism. The electric charge is released
when used by a desorption-diffusion mechanism. The
potential change profiles during charging and
discharging at various activator concentrations and
nitrogen doping ratios are shown in Figure 7.
The long-term electrode stability is also an
important factor in evaluating carbon materials as
supercapacitor electrodes. The characteristic of
supercapacitor can be indicated from the time
required in charging and discharging. A good
capacitor has a short time in charging but a long time
in discharging. Figure 7 shows the variation of
gravimetric capacitance with time required in a
charge-discharge cycle on a current density of 1 Ag
with a KOH electrolyte on both electrodes. The
activated carbon electrodes activated by 3 M H3PO4
with nitrogen doping ratio of 1:3 show that the current
charging stops at 475 seconds, and the current
discharging ends at 1235 seconds. The results are
significantly different from the concentration of 6 M
with a doping ratio of 1:5 particularly in current
discharging; the charge stops at 380 seconds and
ends with discharging at 665 seconds. This is in line
with the capacitance value where at 3 M and doping
ratio of 1:3 the highest capacitance was obtained.
Meanwhile, the longest charging occurred at a
concentration of 9 M with a nitrogen doping ratio of
1:5 with a charging value of 750 seconds. The
resulting GCD curve does not show a symmetrical
shape due to the higher scanning speed and large
barriers to ion transport in the pores, which will inhibit
the formation of the electric double layer (Yan et al.,
2018).

(a)

(b)

(c )
Figure 7. GCD curve at concentrations of 3, 6, 9 M with a doping ratio of 1:3, 1:5, 1:7
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Siti Khuzaimah, et al.

CONCLUSIONS
Supercapacitors electrodes were prepared from a
renewable, low cost, abundant and
sustainable
natural resource (i.e. waste shrimp shells), with an
activation treatment using N-doping and H3PO4.The
concentration of H3PO4 activator and the addition of
nitrogen doping from urea were known to affect the
characteristics of activated carbon in terms of
morphological surface and specific surface, and the
electrochemical properties of supercapacitor in terms
of capacitance and current charge-discharge cycle.
This effect is likely due to the increased pore formation
and enhanced structural properties that facilitate ion
diffusion. In the range of H3PO4 concentrations and
nitrogen doping ratios studied, the highest specific
surface of activated carbon and supercapacitor
capacitance were obtained at a concentration of 3 M
and a doping ratio of 1:3, i.e. 17.522 m2/g and 16.3
Farad, respectively. In terms of charging and
discharging
time,
the
best
supercapacitor
performance was also obtained at 3 M H3PO4 and a
nitrogen doping ratio of 1:3, i.e. The best performance
was observed with a charging time of 475 seconds
and a discharging time of 1235 seconds.

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ACKNOWLEDGEMENTS
We, the authors, express our gratitude to the
Research Laboratory of the Department of Chemical
Engineering
of
Universitas Muhammadiyah
Surakarta which has facilitated our experimental
works, as well as to Universitas Muhammadiyah
Surakarta which has given the funding in the form of
Magister Research Grant.
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