Cogent Engineering

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Preparation of porous graphene-like material from

coconut shell charcoals for supercapacitors

Fahmi Fahmi, Nur Anggita Ayu Dewayanti, Widiyastuti Widiyastuti & Heru
Setyawan |

To cite this article: Fahmi Fahmi, Nur Anggita Ayu Dewayanti, Widiyastuti Widiyastuti & Heru
Setyawan | (2020) Preparation of porous graphene-like material from coconut shell charcoals
for supercapacitors, Cogent Engineering, 7:1, 1748962, DOI: 10.1080/23311916.2020.1748962

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Cyclic voltammogram of (a)
CSC, (b) AC-H, (c) H-AC, and (d)
AC-H-R in 1 M Na2S2O3 at
a scan rate of 50 mV/s.

CHEMICAL ENGINEERING | RESEARCH ARTICLE

Preparation of porous graphene-like material

from coconut shell charcoals for
supercapacitors
Fahmi Fahmi, Nur Anggita Ayu Dewayanti, Widiyastuti Widiyastuti and Heru Setyawan

Cogent Engineering (2020), 7: 1748962

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CHEMICAL ENGINEERING | RESEARCH ARTICLE

Preparation of porous graphene-like material
from coconut shell charcoals for supercapacitors
Fahmi Fahmi1, Nur Anggita Ayu Dewayanti1, Widiyastuti Widiyastuti1 and Heru Setyawan1*

Received: 26 December 2019 Abstract: High-surface area carbon with porous structure can provide a large electrical-
Accepted: 23 March 2020
double layer as energy storage in supercapacitors. Herein, porous graphene-like materials
*Corresponding author: Heru with high-surface area were prepared from renewable coconut shell charcoal via KOH
Setyawan, Department of Chemical
Engineering, Faculty of Industrial activation followed by oxidation in a harsh environment using a modified-Hummer
Technology, Sepuluh Nopember
Institute of Technology, Kampus ITS
method. Using the method, the surface area of the treated coconut shell charcoal
Sukolilo, Surabaya 60111, Indonesia. increased significantly from about 189.97 m2/g to 642.45 m2/g with a pore diameter of
E-mail: [email protected]
approximately 5 nm. As expected, the increase in surface area increased the capacitance
Reviewing editor: significantly, by up to 46-fold, from 3.22 to 148.20 F/g. These results demonstrated that
Harvey Arellano-Garcia,
Brandenburgische Technische the low cost renewable porous graphene-like material prepared from coconut shell
Universitat Cottbus-Senftenberg,
GERMANY charcoals is promising for use as electrode material for supercapacitor.
Additional information is available at Subjects: Materials Science; Nanoscience & Nanotechnology; Chemical Engineering
the end of the article
Keywords: coconut shell; hard carbon; supercapacitor; graphene-like; renewable biomass

1. Introduction
Supercapacitors have attracted considerable attention due to their high-power density, long cycle life, and fast
charging time that make them the promising power source in electronic equipment and hybrid electrical
vehicles. The energy storage in supercapacitors can be in the form of electrical double-layer capacitors (EDLCs)
or fast and reversible Faradaic reactions (pseudocapacitors). Carbon materials have been recommended as
the most promising candidates for supercapacitors (Sun et al., 2013), and in the case of EDLCs, activated
carbon has been the most widely used as the electrode material (Ghosh et al., 2019) (Zhao et al., 2011).
Activated carbon is low cost because it can be prepared easily from abundantly available and low cost

ABOUT THE AUTHOR PUBLIC INTEREST STATEMENT

The research interest in our laboratory range from We have devised a cheap method to convert
the preparation of advanced functional materials coconut shell charcoals into highly porous gra-
for energy, environment and biomedical, especially, phene-like materials. Graphene is a single, thin
from natural resources and solid waste using var- layer of graphite, the material used in pencil lead,
ious methods such as electrochemical, electrospin- that could be the future of technology. It is
ning, and electro spray. Examples of advanced because graphene has unique properties such as
functional materials we are developing including flexible, transparent, highly conductive, and so on.
electrocatalyst for oxygen reduction reaction, cata- Graphene or graphene-like can be used as the
lyst for esterification, high capacity liquid absor- electrode materials for energy storage and con-
bents, etc. This paper is part of our project on version devices such as Li-ion battery and super-
developing carbon-based electrode materials from capacitors. The fast-growing market of the small
renewable biomass resources including coconut portable electronics and hybrid electrical devices
shells, coir fibers, bagasse, etc. highly demand supply of storage system of elec-
trochemical energy. Graphene-like materials
derived from coconut shell charcoals could be an
alternative to fulfill the demand supply, providing
the abundantly available cheap waste renewable
biomass resources and cheap method.

© 2020 The Author(s). This open access article is distributed under a Creative Commons
Attribution (CC-BY) 4.0 license.

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renewable natural resources such as biowastes, sawdust, coconut shell, bamboo, etc. A wide variety of
renewable natural resources have been used to prepare carbon-based electrodes for supercapacitors including
ginkgo leaves (Zhu et al., 2018), Rose (Zhao et al., 2018), wheat straw (Gou et al., 2020), and bamboo (Yang
et al., 2014). The capacitance or storage performance of activated carbon-based supercapacitors is greatly
dependent on the specific surface area of the active material and the charge accumulates at the electrode/
electrolyte interface (Przygocki et al., 2018). The poor conductivity and a huge amount of micropores in
activated carbons hinder the ion and electron transport, which in turn, deteriorate significantly the capacitance
performance at high rates (Sun et al., 2013). To overcome the poor electrical conductivity of activated carbon,
the activated carbon is generally graphitized. However, graphitization leads to reduce the specific surface area.
Recently, hard carbons, a type of disordered carbon material and non-graphitizable, have gained much
attention for use as electrode materials for EDLCs (Ghosh et al., 2019). Hard carbons can be produced by
carbonization of various biomasses such as cellulose, coconut shell, charcoal, etc. Coconut shells, consisting
mainly of cellulose fibers, are biomass waste which is abundantly available in Indonesia and widely distributed
in the earth. They are typically used as raw material to produce charcoal by carbonization in a limited-oxygen
environment for use as either domestic or industrial uses. Coconut shell charcoal is hard carbon and because of
that it can be a potential candidate for conversion into electrode material used in supercapacitors.

In the present work, a modified-Hummer method with either pretreatment or post-treatment

was used to prepare graphene-like material from coconut shell charcoal for use as electrode
material in supercapacitor. The treatment was aimed to increase the surface area of the carbon
material to enhance the capacitance capacity. The effect of the order of pretreatment and post-
treatment on the properties of treated carbon and its capacitance was investigated.

2. Experimental

2.1. Materials
The coconut shell charcoal (CSC) were obtained from local market in Surabaya, Indonesia. The
proximate composition analysis of the CSC is shown in Table 1. All chemicals used to prepare the
graphene from the CSC were reagent grade and used without further purification. The sulfuric acid
(H2SO4; 98.0%) and hydrogen peroxide (H2O2; 30%) were supplied by Merck. The sodium nitrate
(NaNO3; 99.5%) was purchased from SAP Chemical. The potassium permanganate (KMnO4; 99.5%)
and potassium hydroxide (KOH; 99.5%) were purchased from UNI-Chem, Indonesia.

2.2. Synthesis
Prior to use, CSC was ground and sieved to a particle size of approximately 125 μm. The CSC
particles were mixed with KOH solids and ground in an agate mortar. The weight ratio of CSC:KOH
was 1:4. The CSC-KOH mixture was placed in a ceramic boat and introduced into an alumina tube
of tubular furnace. Nitrogen (UHP) gas was flowing during the thermal treatment, which was
carried out successively at 400°C for 1 h and 800°C for 3 h. The heater was turned off, and the
sample was cooled naturally to room temperature, washed with successively 20 wt.% H2SO4 and
deionized water, and dried in an oven at 80°C for 12 h. The dried sample, hereafter will be referred
to as activated carbon (AC), was used as raw materials to produce graphene-like material.

2Graphene-like material was prepared using a modified Hummers approach (Vieira et al., 2016). Two
grams of AC and 2 g of NaNO3 were put into 92 mL of 98.0% H2SO4 in a beaker glass placed in an ice bath
and stirred by a magnetic stirrer. After 30 min, 10 g of KMnO4 was added and the temperature was

Table 1. Proximate analysis of CSC

Parameters Composition (wt.%)
Moisture 7.55
Volatile matter 2.82
Ash 1.32
Fixed carbon 88.31

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increased to 40°C by putting the mixture in a water bath. After 40 min, 100 mL deionized water was added
slowly (in an ice bath) to avoid a rapid temperature raise and it was allowed in the ice bath (~5°C) for 3 h.
Then, it was heated to 35°C and kept at this temperature for 15 min. After that, 100 mL of demineralized
water was added slowly, and the mixture was cooled down to ~5°C and kept at this temperature for
15 min. Fifteen milliliters of H2O2 was added slowly until no bubble could be observed anymore. The solids
were separated from the mixture by a centrifuge, washed subsequently with HCl solution and deionized
water and dried in an oven at 80°C. The sample was denoted as AC-H. For reference, CSC was directly
treated with the same procedure as above and the sample was labeled as CSC-H.

To enhance further the surface properties, the AC-H was reduced by citric acid at high temperature
using the procedure described as follows. The GO in the amount of 5 mg were dispersed in 20 mL of
deionized water and its pH was adjusted to 9 by adding 1 M NH4OH aqueous solution. Then, 4 g of citric
acid as reducing agent for the AC-H was added to the mixture. The mixture was heated in a tubular
furnace at 950°C under flowing nitrogen gas for 120 min. After the heater was turned off, the solid sample
cooled naturally to room temperature. The sample was denoted as AC-H-R.

2.3. Characterization
Crystal structures of graphene were identified by X-ray diffraction (XRD; PANalytical X’Pert Pro, The
Netherlands) using Cu Kα radiations (λ = 1.54 Å). Infrared and Raman spectra were recorded using,
respectively, a Fourier Transform Infrared (FTIR) spectrophotometer (IRTracer-100, Shimadzu, Japan)
and a Raman Spectroscopy (XploraPlus, Olympus, Japan). The specific surface area was measured by
multi-point nitrogen adsorption at its boiling point (Nova 1200, Quantachrome, US). The samples were
degassed at 300°C under flowing nitrogen for 3 h prior to the measurements. The specific surface area was
calculated by Brunauer–Emmet–Teller (BET) method. The pore volume was taken at the relative pressure
approaching unity. The pore size was estimated by Barrett-Joyner-Halenda (BJH) method.

2.4. Electrochemical characterization

The electrochemical properties of the as-prepared graphene were tested as the electrode in
supercapacitor by cyclic voltammetry (CV) using a conventional three-electrode system in a 1 M
Na2S2O3 aqueous solution on a potensiostat/galvanostat instrument (Autolab PGSTAT 302 N,
Metrohm). Platinum foil and Ag/AgCl 3 M KCl (0.21 V vs. SHE) were used as, respectively, the
counter and reference electrodes. The working electrode was prepared by mixing the as-prepared
graphene with poly(vinylidene difluoride) (PVdF; Sigma-Aldrich) binder with a weight ratio of 10:1
using N-methylpyrrolidone (NMP; Sigma-Aldrich) solvent to form a paste. The paste was casted to
a nickel foam and dried in an oven at 60°C. The CV measurement was carried out by scanning the
potential between –1.0 and 0 V (vs. Ag/AgCl) at a scan rate of 50 mV/s.

3. Results and discussion

3.1. Particle characteristics

Figure 1 shows the XRD pattern of activated carbon obtained from coconut shell charcoal using the KOH
activation as described above. The diffraction pattern shows two peaks at around 22.5° and 43° corre-
sponding to disordered graphitic 002 and 100/101 planes, respectively (Pradhan & Sandle, 1999). This
pattern differs from that of the coconut shell charcoal that has only one broadening peak at around 24°,
indicating a non-crystalline carbon. The peaks appear in the diffraction pattern of activated carbon denote
the interlayer spacing/the stacking high (Lc) and the microcrystallite diameter/the lateral size (La) (Girgis
et al., 2007). Moreover, the disorder in carbon structure is probably caused by the random displacement
between adjacent layers and local stacking faults produced during the pre-treatment process including
grinding and thermal treatments (Babu & Seehra, 1996). Since grinding might have an effect on the
disorder of carbon structure, the effect of particle size, i.e., grinding, was investigated.

A well-known Hummer method is the most common methods to prepare graphene by exfoliation of
graphite. Since the structure of carbon in the activated carbon was disordered graphitic, a harsh oxidation
using the modified-Hummer method might be used to treat the activated carbon to have properties like

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Figure 1. XRD pattern of acti-

vated carbon obtained from
coconut shell charcoal (AC).

Figure 2. XRD pattern of the

activated carbon samples of
different sizes treated with the
modified-Hummer method.

graphene. Figure 2 shows the effect of particle size on the XRD patterns of AC treated with the modified-
Hummer method (AC-H). As expected, the diffraction peaks appeared in the original activated carbon still
exist after it was treated with the modified-Hummer method. The diffraction peak broadened when the
initial particle size decreased (from 35 to 200 mesh). As mentioned above, grinding may influence the
disorder structure of carbon. The smaller the size was, the more intense the grinding was. As a result, the
carbon structure became more disorder as shown by the broader diffraction peaks, and in the case of 200
mesh the peak at 43° nearly disappears. The broader peak at 24° indicates the structure similar to the
stacked structure of graphite oxide (Toh et al., 2014).

Figure 3 shows the XRD patterns of the activated carbon treated with only the modified-Hummer
method (AC-H) and the modified-Hummer method plus reduction using citric acid (AC-H-R). As
discussed above, the XRD pattern of AC-H shows a broad peak at around 24° indicating the material
has a stacked structure of graphite oxide. On the other hand, the peak was slightly shifted to 23.3°
when the material was reduced with citric acid (AC-H-R), and the peak at 43° completely disappeared.
The diffraction pattern is similar to that of the reduced graphene oxide (rGO) (De Silva et al., 2017).
Thus, it seems that rGO can be prepared from activated carbon by subsequently treated it with the
modified-Hummer method and citric acid reduction at high temperature.

Figure 4 presents the Raman spectra of the activated carbon treated with: (a) the modified-Hummer
method (AC-H) and (b) the modified-Hummer method plus reduction using citric acid (AC-H-R). There are
three peaks in the Raman spectra of the two samples which are at around 1362 cm–1 (D band), 1569 cm–1

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Figure 3. XRD patterns of acti-

vated carbon treated with the
modified-Hummer method (AC-
H) and the modified-Hummer
method plus reduction using
citric acid (AC-H-R).

Figure 4. Raman spectrum of

samples: (a) AC-H and (b) AC-
H-R.

(G band), and 2743 cm–1 (2D band). The peaks can be attributed to graphitic structure of RGO (Sun et al.,
2013). The D-band indicates the presence of defects in the graphitic materials due to bond-angle
disorder, bond-length disorder, vacancies edge defects, etc. On the other hand, G-band is related to
the stretching motion of the pairs of carbon sp2 atoms while the broad peak in 2D-band indicates the
number of layers formed (Dubale et al., 2014). The intensity of the D band is smaller after reduction that
may be due to the breaking of the stacking order due to the reduction reaction (Khrisnamoorthy et al.,
2013). Based on Broad peak in 2D-band, it shows that AC-H has more than one layer (Shui et al., 2015).

Table 2 presents the porosity properties of various carbon samples based on coconut shell charcoal.
It can be seen that the surface area tends to increase after each tretment. The increase in surface area
after the treatment may also confirm the formation of multi-layer. The surface area of coconut shell
charcoal was 189.97 m2/g. It increased to 496.03 m2/g after being successively activated with KOH and
oxidized with the modified-Hummer method (AC-H). The surface area increased further 642.50 m2/g
after it was reduced with citric acid (AC-H-R). The pore volume had the same tendency as the surface
area while the pore diameter was relatively unchanged after each treatment.

Figure 5 shows the FTIR spectra of coconut shell charcoal (CSC) and the coconut charcoal treated by
different treatments. The spectrum of CSC had a peak at 873 and 1615 cm–1 corresponding to C=C
bond (aromatic group) (Zeng et al., 2011). The C=C bond was broken after the charcoal was activated
with KOH (AC) and further with the modified-Hummer method (AC-H) and citric acid reduction (AC-
H-R) as indicated by the disappearance of the band after the treatment. For all samples treated with
only the modified-Hummer method or further with citric acid reduction, there are peaks at 2890, 1049
and 830 cm–1 that can be attributed to, respectively, C-H groups, C-O groups, and C-N groups (Tang
et al., 2012). All functional groups are the typical groups encountered in GO or rGO. Thus, it can be
assumed that graphene-like material had been successfully prepared from coconut shell charcoal by
first activation and followed by the modified-Hummer method plus citric acid reduction.

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Table 2. The porosity properties of various carbon samples

Sample Surface area Pore volume Pore diameter
(m2/g) (cm3/g) (nm)
CSC 189.97 0.098 4.159
AC 1341.99 0.856 3.394
AC-H 496.03 0.998 4.322
AC-H-R 642.50 1.022 3.406

Figure 5. FTIR spectra of var-

ious carbons: (a) AC, (b) AC-H),
(c) coconut shell charcoal (CSC),
(d) H-AC, and (e) AC-H-R.

3.2. Capacitance properties

Figure 6 shows the CVs for CSC, AC-H, H-AC, and AC-H-R in 1 M Na2S2O3 at a scan rate of 50 mV/s. An
ideal double-layer capacitance of an electrode should exhibit a rectangular shape of CV. However,
instead of a typical rectangular shape, a deviation, but still close to, a rectangular shape was observed.
The CV enclosed area of CSC is very small, indicating the material is not suitable for use as super-
capacitor. On the other hand, the CV enclosed area of AC-H is much larger than that of CSC and it
increases further for AC-H-R, indicating that it has a much higher capacitance. It appears that
graphene-like sample (AC-H-R) is suitable as an electrode material for supercapacitor.

The specific capacitance values were calculated from the CVs using the equation

2òIdV
C¼ (1)
msR

where I is the cathodic current, V is the applied potential, m is the electrode mass, s is the scan rate and
R is the scan range of applied potential. The specific capacitance values of CSC, AC-H, H-AC and AC-
H-R calculated from Figure 6 using Equation (1) were 3.22, 49.38, 86.32, and 148.20 F/g, respectively.
The specific capacitance could be improved from 3.22 F/g to 49.38 and 86.32 F/g by activating the CSC
followed with oxidizing using the modified-Hummer method (AC-H) and oxidizing using the modified-
Hummer method followed by calcination (H-AC). The specific capacitance could be enhanced further
from 86.32 to 148.20 F/g by reducing AC-H with citric acid (AC-H-R). The specific capacitance of carbon-
based electrodes derived from natural resources reported in the published literature is typically in the
range from 100 to 479 F/g (Ghosh et al., 2019). The high specific capacitance indicates that AC-
H-R sample prepared from coconut shell charcoal using successively treatments of activation, oxida-
tion, and reduction is a promising material for supercapacitor.

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Figure 6. Cyclic voltammogram

of (a) CSC, (b) AC-H, (c) H-AC,
and (d) AC-H-R in 1 M Na2S2O3
at a scan rate of 50 mV/s.

4. Conclusion
It has been demonstrated that porous graphene-like materials with high-surface area can be prepared from
renewable coconut shell charcoal via KOH activation followed by oxidation in a harsh environment using a modified-
Hummer method. The surface area of the treated coconut shell charcoal increased significantly from about
189.97 m2/g to 642.45 m2/g with a pore diameter of approximately 5 nm. The increase in surface area leads to an
increase in the capacitance of this material in 1 M Na2S2O3 significantly from 3.22 F/g for coconut shell charcoal to
148.20 F/g for graphene-like material. These results demonstrated that the low cost renewable porous graphene-like
material prepared from coconut shell charcoals is promising for use as electrode material for supercapacitor.

Acknowledgements Fahmi Fahmi, Nur Anggita Ayu Dewayanti, Widiyastuti

This work was supported by the Ministry of Research, Technology Widiyastuti & Heru Setyawan, Cogent Engineering (2020),
and Higher Education of Indonesia through PMDSU research 7: 1748962.
grant (No. 01/E/KPT/2018) and a World Class Research grant
(No. 713/PKS/ITS/2019). One of the authors (F. F.) would like to References
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