Fullerenes, Nanotubes and Carbon Nanostructures

ISSN: 1536-383X (Print) 1536-4046 (Online) Journal homepage: https://www.tandfonline.com/loi/lfnn20

Rambutan peel based hard carbons as anode

materials for sodium ion battery

Arenst Andreas Arie, Hans Kristianto, Henky Muljana & Lorenzo Stievano

To cite this article: Arenst Andreas Arie, Hans Kristianto, Henky Muljana & Lorenzo Stievano
(2019): Rambutan peel based hard carbons as anode materials for sodium ion battery, Fullerenes,
Nanotubes and Carbon Nanostructures, DOI: 10.1080/1536383X.2019.1671372

To link to this article: https://doi.org/10.1080/1536383X.2019.1671372

Published online: 01 Oct 2019.

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FULLERENES, NANOTUBES AND CARBON NANOSTRUCTURES
https://doi.org/10.1080/1536383X.2019.1671372

Rambutan peel based hard carbons as anode materials for sodium ion battery
Arenst Andreas Ariea, Hans Kristiantoa, Henky Muljanaa, and Lorenzo Stievanob
a
Department of Chemical Engineering, Faculty of Industrial Technology, Parahyangan Catholic University, Bandung, Indonesia; bInstitut
Charles Gerhardt Montpellier, Univ. Montpellier, CNRS, Montpellier, France

ABSTRACT ARTICLE HISTORY

Sodium (Na) ion battery (NIBs) are considered as one of the most prospective battery system to Received 23 July 2019
substitute lithium ion batteries (LIBs) especially for stationary applications. In this study, rambutan Accepted 19 September 2019
peels were selected as carbon precursors to prepare hard carbons as anode materials for NIBs.
KEYWORDS
Hard carbons were prepared by applying hydrothermal carbonization and then continued by the
Hard carbons; anodes;
pyrolysis treatment at different temperatures (800, 1000 and 1200
C). The electrochemical studies sodium battery; pyrolysis
were carried out by cyclic voltammetry (CV) and galvanostatic charge discharge (GCD). The
obtained hard carbons at pyrolysis temperature of 1000 exhibited the best electrochemical per-
formance. It showed the highest reversible capacity of 225 mAh g1 (0.1 C-rate, 1 C ¼ 300 mA g1)
after 100 cycles if tested as the anode materials for NIBs. It is attributed to the disordered carbon
structure, low degree of graphitization, large interlayer spacing and flake-like morphology of car-
bon sample which can provide more space for sodium storage and facilitate sodium ion transfer.

1. Introduction
Since their invention by Sony in 1991, lithium ion batteries
(LIBs) have been used in various applications in portable
electronics and electric vehicles because of the high energy
density, long and stable cycle profiles [1–5]. However, the
unbalanced geographical distribution of Li in this world and
the extreme needs of Li in many future applications would
certainly make an insufficiency of Li resources, and finally it
will cause a high cost for using Li in battery systems. On the
contrary, sodium (Na), which is highly abundant and widely
spread all around the world, has similar electrochemical prop-
erties even though further research is required before the
practical implementation of sodium ion batteries (NIBs)
[6–8]. One of the challenges is to find suitable anode materi-
als since graphite cannot be used in NIBs due to the larger
size of sodium ion compared to the lithium ions [9–12].
The most common anode materials for NIBs can be cate-
gorized as carbon based materials [13], alloys [14–16], metal
oxide [17, 18], organic compounds [19, 20], sulfide [21–23]
and phosphorus based materials [24, 25]. The main problem
with the alloy materials is the huge volume expansion caus-
ing enormous capacity reduction during cycling tests [26].
While the organic compounds show some shortcomings
such as low Coulombic efficiency and low electrical con-
ductivity although they have high capacity as anodes in
NIBs [26]. Finally, the metal oxide, sulfide and phosphorus
based materials also have huge volume expansion problems
similar to the alloy materials which can limit their applica-
tion as anodes for NIBs. On the other hand, hard carbons
are the most suitable carbon materials for the storage of
sodium ions due to the large interlayer distance and irregu-
lar carbon structures [27].
As anodes in NIBs, hard carbons can be prepared from
various biomass resources such as spent tea leaves [28], apri-
cot shells [29], sugarcane bagasse [30], waste cigarette butts
[31], peanut shells [32], cucumber stem [33], lotus seedpod
[34], rice husk [35], chrysanthemum [36], waste tea bag
powder [37], caltrop shell [38], typha [39], snake-skin fruit
peel [40], date palm [41], reed straw [42], waste pomegran-
ate peel [43] and many others. The electrochemical proper-
ties of the biomass based hard carbons are highly affected
by the synthesis routes and the properties of biomass car-
bon precursors.
Rambutan (Nephelium lappaceum L.) is a very popular
tropical fruit originated from the southeast Asian countries
such as Indonesia, Malaysia and Thailand [44]. The average
production of rambutan fruit in Indonesia is between
700.000 and 800.000 ton per year. Commonly, after the
edible part of rambutan is consumed, a large amount of
rambutan peel is discarded as rubbish to landfill and there
is no practical application of it which can cause a serious
environmental problem [45]. Further research on the appli-
cation of rambutan peel for the production of carbon mate-
rials would become an interesting solution since it is a
cheap carbon precursor as well as an effort to reduce the
amount of biomass waste. Until now, there are no applica-
tions related to the use of rambutan peel based hard carbon
as anode material in sodium ion battery.

CONTACT Arenst Andreas Arie arenst@unpar.ac.id Department of Chemical Engineering, Faculty of Industrial Technology, Parahyangan Catholic
University, Ciumbuleuit 94, Bandung, 40141, Indonesia.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/lfnn.
ß 2019 Taylor & Francis Group, LLC
2 A. A. ARIE ET AL.
In this work, we prepared the hard carbon originated
from rambutan peel with two-step process. Initially, rambu-
tan peels were treated using hydrothermal treatment to pro-
duce hydrochar. After that, the hydrochar was subject to the
pyrolysis carbonization. The obtained hard carbon products
were then all tested as anode materials for sodium ion bat-
tery using half-cell configurations. This study can provide a
way to transform the morphology and adjust the structure
of hard carbon de- rived from biomass. Meanwhile, it can
also be widely applied to other biomass waste materials to
improve their electrochemical performance.
2. Experimental
2.1. Preparation of hard carbons
Rambutan peel used as carbon precursor in the experiments
was obtained from the local market in Cimahi, Indonesia.
The peel was washed with deionized water and dried in an
oven at 110
C for 24 h to reduce the moisture content.
After drying, the sample was then crushed and sieved to
have powders with uniform particle size distribution. The
powders were then treated using hydrothermal process at a
low temperature and then followed by a pyrolysis carboniza-
tion process. For the hydrothermal treatment, 2 g of rambu-
tan peel powders was mixed with 1 M NaOH solution with
a volume of 60 mL. The mixture was then stored in 100 mL
Teflon-lined stainless steel autoclave and heated at 200
C
for 20 h in an electric oven. This hydrothermal treatment is
used to remove lignin and hemicellulose contained in the
rambutan peel. After cooled down to the room temperature,
the suspension was treated by filtration and then washed
with distilled water and ethanol several times until the pH
value of the solution is around 7. Then, the hydrochar sam-
ples were subjected to pyrolysis carbonization at various
temperatures (800, 1000 and 1200
C) with heating rate of
5
C min1 for 2 h under N2 atmosphere in a tubular fur-
nace, and the obtained carbon products were denoted as
RPHC-800, RPHC-1000 and RPHC-1200 with 800, 1000 and
1200 indicate the pyrolysis temperatures.
2.2. Characterization of hard carbons
The surface physical properties of RPHC samples were
recorded with an automated gas sorption apparatus
(Micromeritics, USA) using N2 gas as adsorbate at 77 K. All
the samples were outgassed at 250
C for 4 h under vacuum
before the gas sorption measurement. The Brunauer-
Emmett-Teller (BET) equation and t-plot method were used
to determine the specific surface area and micropore surface
area, respectively. Pore size distributions were calculated by
the adsorption branch of the isotherms using density func-
tional theory (DFT) for micropores and the Barrett-Joyner-
Halenda (BJH) model for mesopores. The total pore volume
(Vtotal) was estimated from the amount adsorbed at a rela-
tive pressure (P/P0) of 0.99. The micropore volume (Vmicro)
was computed using the t-plot method. The surface morph-
ology of RPAC was observed using field emission scanning
electron microscopy (FE-SEM-Hitachi). XRD analysis was
conducted with a Bruker diffractometer which used Cu Ka
radiation (k ¼ 0.154 nm) as the X-ray source. The interlayer
d-spacing of the RPHC samples were calculated by using
Bragg’s equation:
k
d¼ (1)
sinh
Raman spectra were collected by using Thermo Nicolet
Almega XR Raman Microscope with alaser excitation wave-
length of 532 nm.
2.3. Electrochemical characterization of RPHC
The electrochemical characterization of RPHC samples was
studied using coin cells. The working electrode was prepared
by mixing RPHC powder, Super-P conducting carbon car-
boxy methyl cellulose (CMC) binder at a weight ratio of
8:1:1, coated on a copper foil collector and then dried in the
vacuum oven overnight. Distilled water was used as the dis-
persant for the mixture. The typical mass loading of the
electrodes was about 1.2 mg cm2. The fabricated/working
electrode, polyethylene separator, and Na metal counter
electrode were assembled into a 2032-type button cell filled
with electrolyte (1 M NaPF6 in a polyethylene carbonate
(PC), in an Ar-filled glovebox. Cyclic voltammetry (CV) was
carried out using a Biologic instrument at a scan rate of
0.1 mV s1. The galvanostatic charge-discharge (GCD)
measurements were performed using the same battery meas-
urement systems at various current densities over a voltage
range from 0.01 to 2.0 V vs Na/Naþ. All electrochemical
tests were conducted at room temperature.
3. Results and discussion
The morphology of RPHC samples was observed by scan-
ning electron microscope (Figure 1). Figure 1a shows the
morphology of carbon samples obtained after the hydrother-
mal pretreatment where it can be observed agglomerated
carbon spheres. Hydrothermal process is a low degree of
carbonization process with simple operation, low cost since
it use aqueous solvent and various type of reactant [46, 47].
As we used the pyrolysis carbonization to treat hydrochar
samples at different temperatures, the morphological change
from carbon sphere into the hard carbons can be observed,
as seen in Figure 1b–d. The carbon samples have flake-like
with smooth surface and connected porous structure. It was
followed from the cross-linking and merging of the agglom-
erated carbon spheres As the pyrolysis temperature
increased from 800 to 1200
C, the cross-linking of carbon
spheres can take place faster. This type of flake-like morph-
ology can contribute to the better sodium ion and electron
transfer [48].
Figure 2 shows the XRD results of hard carbons prepared
by pyrolysis process with hydrothermal treatment. As seen,
all XRD patterns showed two broad peaks located at about
24 and 43
, which were assigned to the (002) and (100)
plane of the amorphous carbon materials, respectively. In

Figure 1. SEM images of (a) hydro-char, (b) RPHC-800 (c) RPHC-1000 and (d) RPHC-1200.
Figure 2. XRD patterns of rambutan peel based hard carbons prepared at dif-
ferent pyrolysis temperature.
addition, we can see that the XRD patterns of RPHC sam-
ples have no sharp characteristic peaks, showing that all of
them belong to hard carbons with disordered structures.
Using the positions of (002) peaks of all carbon samples
(RPHC-800, RPHC-1000 and RPHCHC-1200) and Bragg
equation, the interlayer spacing can be estimated. The esti-
mated values of interlayer spacing for RPHC-800, RPHC-
1000 and RPHC-1000 are 0.387, 0.383 and 0.381 nm,
respectively. These estimated values were larger than that of
graphite interlayer spacing value (0.335 nm). So, the larger
interlayer spacing can be expected to facilitate the insertion/
extraction of sodium ions, and finally it can improve the
specific capacity of the RPHC samples.
Figure 3 displays the Raman spectra of RPHC. The two
dominant peaks located at around 1349 and 1580 cm1 refer
FULLERENES, NANOTUBES AND CARBON NANOSTRUCTURES 3
Figure 3. Raman spectra of rambutan peel based hard carbons prepared at dif-
ferent pyrolysis temperature.
to the presence of disorder and graphite-like structures of
carbon materials [49], respectively. The D peak represents
the disordered structures due to the defects in the structure
and disorder-induced features of carbon, while the G band
can be attributed to the vibration of sp2 hybridized carbon.
The ID/IG intensity ratio is usually used to estimate the dis-
order degree of carbon structures. The ID/IG intensity ratio
of RPHC-800, RPHC-1000 and RPHC-1200 was determined
as 0.92, 0.85 and 0.81. As the pyrolysis temperature is
increasing from 800 to 1200 ˚C, the ID/IG ratio of carbon
samples is decreasing, indicating that the degree of structural
ordering of RPHC is increased.
The N2 adsorption-desorption isotherms of RPHC sam-
ples are measured to estimate the BET surface area and the
pore structure. We can see in Figure 4a, the isotherms of
4 A. A. ARIE ET AL.
Figure 4. (a) Nitrogen adsorption desorption isotherms and (b) pore size distribution of RPHC prepared at different pyrolysis temperature.
Table 1. Physical parameters of rambutan peel based hard carbons.
Sample d002 (nm) ID/IG SBET (m2g-1) VT (cm3g-1)
RPHC-800 0.387 0.92 198 0.12
RPHC-1000 0.383 0.85 282 0.22
RPHC-1200 0.381 0.81 254 0.17
d002: interlayer spacing, ID/IG: intensity ratio between disordered and graphite
like structures, SBET: specific surface area. VT: total pore volume. DA: average
pore size diameter.
the three samples of RPHC are classified as type I/IV of
IUPAC classification. It can be seen that the BET surface area
is affected by the pyrolysis temperature, as shown in Table 1.
On the other hand, as displayed in Figure 4b, the pore size
distributions of the RPHC sample are also dependent on the
pyrolysis temperature. The pore distribution range become
broader and the pore volume increased gradually as the pyr-
olysis temperature is increased from 800 to 1200
C. The
RPHC-1000 sample possess the highest BET surface area of
282 m2 g1 and the largest pore volume 0.22 m3 g1, which
can contribute to the higher sodium ion adsorption capability
due to the higher surface of RPHC-1000 sample.
The electrochemical characteristics of RPHC electrodes
were studied using half cells with sodium metal foil as the
counter/reference electrode. Cyclic voltammetry (CV) pro-
files of three RPHC electrodes are similar in shape in the
voltage range between 0.001 and 2 V vs Na/Naþ as shown in
Figure 5a–c. In the first cycle, two small cathodic peaks can
be detected at approximately 0.25 V and 0.7 V, which can be
referred to the solid electrolyte interface (SEI) later forma-
tion and the side reaction of the electrolyte on the surfaces
of RPHC. It causes a low coulombic efficiency or a high
irreversible capacity of RPHC electrodes at the first cycle.
These two cathodic peaks are not found in the next cycles,
showing that the reactions related to the SEI layer formation
and side reaction with the electrolyte only took place in the
first cycle. In the next cycles, the CV profiles are almost
overlapping among others, suggesting a good cycle revers-
ibility. Furthermore, a couple of anodic peaks at low poten-
tial range was found for all RPHC electrodes, which could
be related to sodium ion insertion or extraction into the car-
bon surfaces. Especially for RPHC-1000 electrodes, it can be
observed that RPHC-1000 is capable of storing more sodium
DA (nm) ions than other electrodes due to the highest current
2.35 peak intensity.
2.21 Figure 6a–c show galvanostatic charge-discharge (GCD)
2.25
profiles of the RPHC-800, RPHC-1000 and RPHC-1200 elec-
trodes, respectively at 0.1 C (1 C ¼ 300 mAg1) between 0.01
and 2.0 V vs Na/Naþ. At the first cycle, RPHC-800 shows
charge/discharge capacities of 169/326 mAh g1with an ini-
tial coulombic efficiency (CE) of 51.8%, RPHC-1000 has
208/378 mAh g1with an initial CE of 55% and finally
RPHC-1200 delivers 192/359 giving an inital CE of 53%. It
seemed that RPHC-1000 demonstrated the highest capacity
and coulombic efficiency in the first cycle. It was attributed
to the disordered carbon structure, high surface area and
large pore volume in comparison with other RPHC samples,
as confirmed by the CV results.
Figure 7a–c show the cycle performance of the RPHC elec-
trodes until 100 cycles at 0.1 C. As seen, RPHC-1000 electrode
showed the most superior cycle performance among others in
terms of higher initial specific capacity, higher initial coulombic
efficiency and its specific discharge capacity of 225 mAh g1 at
the end of 100 cycles, corresponding to the capacity retention
of 59.5% with respect to the first cycle. Meanwhile, the other
hard carbon samples show more inferior cycle performance.
For the RPHC-800, its discharge capacity is about 140 mAh
g1 corresponding to the capacity retention of 43% with
respect to the first cycle. Finally, RPHC-1200 showed a specific
discharge capacity of 180 mAh g1, implying a capacity reten-
tion of 50% with respect to the first cycle.
The brief comparison of cycle performance of all RPHC
samples is shown in Figure 8a. The rate capability of RPHC
electrodes is also studied in further by varying C-rate from
0.1 C to 2 C. The RPHC-1000 electrode showed the best rate
capability performance in comparison with others. As showed
in Figure 8b, at 0.1, 0.2, 0.5, 1 and 2 C-rate, the average spe-
cific discharge capacities of RPHC-1000 are about 240, 208,
188, 172 and 155 mAh g1, respectively. When the current
density returned to 100 mAg1 at the end of 50th cycle, the
specific discharge capacity of RPHC-1000 could be returned
to 234 mA g1. In contrary, the RPHC-800 and RPHC-1200
 FULLERENES, NANOTUBES AND CARBON NANOSTRUCTURES 5

Figure 5. Cyclic voltammetry profiles of (a)RPHC-800, (b) RPHC-1000 and (c) RPHC-1200 at a scan rate of 0.1 mVs1.

Figure 6. Galvanostatic charge-discharge profiles of (a) RPHC-800, (b) RPHC-1000 and (c) RPHC-1200 at 0.1 C between 0.01 – 2.0 V vs Na/Naþ.
6 A. A. ARIE ET AL.

Figure 7. Cycle performance of (a) RPHC-800, (b) RPHC-1000 and (c) RPHC-1200 at 0.1 C, under cutoff voltages: 0.01 -2.0 V.

Figure 8. (a) Comparison of cycle performance (0.1 C rate) and (b) Rate Capability of RPHC samples.

samples showed more inferior performances in which their
average discharge capacities at varying current density were
smaller than that of RPHC-1000.
4. Conclusions
In summary, we have successfully prepared low-cost hard
carbon materials using rambutan peel (RPHC) as biomass
resource by a hydrothermal pretreatment and pyrolysis
carbonization at different pyrolysis temperature (800, 1000
and 1200
C). After pyrolysis carbonization, the interlayer
spacing for all RPHC samples is higher than that of graphite
and also the morphology of RPHC samples is changed to
flake-shaped. Due to the morphology, more disordered car-
bon structure, large surface area, suitable interlayer spacing,
the rambutan peel hard carbons prepared at 1000
C per-
forms the best electrochemical performance as anodes for
sodium ion battery with reversible capacity of about 225
mAh g1 at 0.1 C-rate after 100 cycles.

Conflict of interest
The authors declare that they have no conflict of interest.
Funding
This study was supported by the Directorate General of Research and
Development Strengthening, Ministry of Research, Technology and
Higher Education of Republic Indonesia (KEMENRISTEKDIKTI)
through The Scheme for Academic Mobility and Exchange(SAME)
Program 2019, Hibah Penelitian Dasar (Contract No: III/LPPM/2019-
03/85-P and Program Hubert Curien (PHC) Nusantara (Cooperation
program between Campus France and KEMENRISTEKDIKTI) in 2019.
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