Indonesia Chimica Acta Andhika, et.al.

ISSN 2085-014X
Vol.8. No. 20, December 2015

ELECTRODEPOSITION OF Cu ON THE SURFACE OF SILICA FREE RICE

HUSK ACTIVATED CARBON WITH ULTRASONIC IRRADIATION

Ryan Andhika1, Muhammad Zakir, Maming

Department of Chemistry, Faculty of Mathematics and Natural Sciences, University of Hasanuddin

Jl. Perintis Kemerdekaan Km. 10 Makassar 90245

Abstrak. Elektrodeposisi logam Cu pada permukaan karbon aktif sekam padi bebas silika dengan
iradiasi ultrasonik yang bertujuan untuk meningkatkan nilai kapasitansi spesifik telah dilakukan.
Karbon aktif sekam padi bebas silika disintesis menggunakan aktivator H3PO4 dan ekstraksi silika
menggunakan KOH. Luas permukaan karbon sekam padi yang diperoleh sebelum dan sesudah
ekstraksi silika serta setelah aktivasi berturut-turut adalah 57,2833 m2/g, 180,5378 m2/g dan
184,6074 m2/g. Analisis menggunakan XRF menunjukkan bahwa logam Cu terdeposisi pada
permukaan karbon aktif sekam padi bebas silika dan berdasarkan pengukuran CV menunjukkan
bahwa elektrodeposisi logam Cu dengan iradiasi ultrasonik dapat meningkatkan nilai kapasitansi
spesifik. Kapasitansi spesifik karbon aktif sekam padi bebas silika sebelum dan sesudah
elektrodeposisi logam Cu dengan iradiasi ultrasonik adalah 657,75 nF/g dan 721,08 nF/g.

Kata kunci: Cu, elektrodeposisi, kapasitansi spesifik, karbon aktif, ultrasonik.

Abstract. Electrodeposition of Cu on the surface of silica free rice husk activated carbon with
ultrasonic irradiation aimed to increase the value of specific capacitance was carried out. Silica free
rice husk activated carbon was synthesized using H3PO4 activator and extraction of silica using
KOH. The surface area of rice husk carbon was obtained before and after the extraction of silica and
after activation were 57.2833 m2/g, 180.5378 m2/g and 184.6074 m2/g, respectively. XRF analysis
showed that Cu depositioned on the surface of silica free rice husk activated carbon and based of
CV measurements showed that electrodeposition of Cu with ultrasonic irradiation can increased the
value of specific capacitance. Specific capacitance of silica free rice husk activated carbon before
and after electrodeposition of Cu with ultrasonic irradiation were 657.75 nF/g and 721.08 nF/g,
respectively.

Key words: Cu, electrodeposition, specific capacitance, activated carbon, ultrasonic.

1
ryanandhika17@gmail.com; rhakakim17@yahoo.com
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Vol.8. No. 20, December 2015
INTRODUCTION
Rapid technological progress
requires more energy supply both for
industry and vehicle propulsion (Suhada,
2001). Energy needs, especially in
Indonesia parallel with increased economic
and population growth it is estimated that
average growth of energy needs amounted
4.7% per annum during 2011-2030. Usage
coal increased considerably around 13.4%
per annum from 2000 until 2011 led to high
production of exhaust gas emissions such as
CO2, SOx and NOx. The limited petroleum
reserves is also one consideration to seek
and develop the utilization of other energy
(Sugiyono et al., 2013). Electrochemical
energy is one alternative energy sources to
consider in dealing with worlds energy
crisis. One of promising the system
conversion and energy storage are
electrochemical capacitors. The material
used for the electrode of the electrochemical
capacitors was an activated carbon because
it had a high internal surface area and good
pore accessibility (Dell and Rand, 2001;
Frackowiak and Beguin, 2001; Ariyanto et
al., 2012).
Manufacture of activated carbon
using various types of biomass wastes was
carried out. One of agricultural waste also
attracted the attention to study was rice
husk. When burned, about 20% from rice
husk turned into ashes. Rice husk ash had
more than 95% the weight of silica (Mahvi
et al., 2004) so that when the extraction of
silica, would create many pores and
increased the surface area of carbon (Wei et
al., 2011). Another way that can be used to
increased the surface area is to utilize
ultrasonic waves (Suslick et al., 1996). The
higher surface area then the higher value of
the capacitance. The high capacitance value
is an indicator of the ability of high energy
accumulation (Zakir et al., 2013). One way
to increased the capacitance value is to
ISSN 2085-014X
utilize pseudocapacitance effect in the
presence of the electroactive species such as
transition metals (Frackowiak and Beguin,
2001).
This research was conducted
electrodeposition of Cu on the surface of
silica free rice husk activated carbon with
ultrasonic irradiation treatment to create a
superior carbon as electrode material
electrochemical capacitors.
RESEARCH METHODS
Material
The materials that were used in this
research are rice husk, commercial activated
carbon, KOH (Merck), technical HCl,
technical H3PO4 85%, CuSO4.5H2O
(Merck), H2SO4 (Merck), Argon gas,
methylene blue, paraffin wax, aquadest,
copper wire, platinum wire, Ag/AgCl
electode, Pt electrode, aluminum foil,
universal pH indicator and Whatman filter
paper number 42.
Apparatus
The equipments were used in this
research are glassware tool that commonly
used in laboratories, furnace (Muffle
furnace type 6000), a water bath (hot plate),
a sieve size of 100 mesh, desiccator, saucer
porcelain, mortar porcelain, vacuum pump,
solder fumes, pipette, oven (type
SPNISOSFD), magnetic stirrer
(CERAMAG Midi), analytical balance
(Shimadzu AW220), Ultrasonic Cleaner
(Elmasonic S40H), FTIR (Shimadzu IR
Prestige21), XRD (Shimadzu XRD-7000),
XRF (ThermoFisherXRF), UV-Vis
(Shimadzu UV-2600) and Cyclic
voltammetry (Potentiostats EA161).
Procedure
1. Preparation and Carbonization
Rice husk were washed with water
and then soaked with technical HCl for 1
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Vol.8. No. 20, December 2015
hour. After that, it washed with aquadest
repeatedly until the pH became neutral, then
dried in an oven at 110 °C for 1 hour. Rice
husk was burn in furnace at 350 °C for 1
hour. After that, the rice husk carbon is
cooled, ground and sieved with a sieve size
of 100 mesh (Zakir et al., 2012; Karyasa,
2014).
2. Extraction of Silica
Sample of rice husk carbon was
added with 2, 4 and 8 M KOH with the ratio
of the mass of carbon/volume of KOH 1:10.
Samples were then heated to boil
accompanied by stirring at the same pace
for 1 hour and then filtered with Whatman
filter paper number 42. The filtrate was
removed and the results of filtration washed
with aquadest, then dried in an oven at 110
°
C for 1 hour. As a comparator, the carbon
was prepared without the addition of KOH.
Furthermore, carbon characterized using
XRF (Agung et al., 2013).
3. Activation
Silica free rice husk carbon was
mixed with the activator solution of H3PO4
21.25% with the ratio of volume of
H3PO4/the mass of carbon 5:1 and left for
1x24 hours. After that, filtered using a
Buchner funnel accompanied by washing
with hot aquadest repeatedly until the pH
became neutral, then dried in an oven at 110
°
C for 1 hour. Furthermore, rice husk
activated carbon was cooled in a desiccator
(Shofa, 2012).
4. Determination of The Surface Area
0.3 gram of activated carbon put into
erlenmeyer, then added 25 mL of methylene
blue 600 ppm solution, then stirred with a
magnetic stirrer for 20 minutes, then
filtered. The filtrate was measured
absorbance at the maximum wavelength of
664.5 nm with a UV-Vis
spectrophotometer. The calibration curve or
ISSN 2085-014X
a standard of methylene blue solution were
made at a concentration of 0.5; 1, 2, 4, 8
and 16 ppm (Ramdja et al., 2008).
5. Electrodeposition of Cu
1 gram of silica free rice husk
activated carbon and commercial activated
carbon (as a comparator) dispersed in 50
mL of CuSO4.5H2O 200 ppm solution.
The mixture was stirred for 1 hour in a state
saturated with argon gas. Activated carbon
functionalised with CuSO4.5H2O and then
irradiated with ultrasonic waves for 6 hours.
After that, filtered, washed with aquadest
and dried at 110 °C for 1 hour. The result of
electrodeposition activated carbon with
copper metals were characterized by XRD
and XRF (Zakir et al., 2013).
6. Manufacture of Carbon Paste
Electrodes
Body electrode was made by
connecting copper and platinum wires using
solder fumes. And then, it was inserted into
the pipette and glued together by parafilm.
Silica free rice husk activated carbon before
and after electrodeposition of Cu mixed
with paraffin wax with the ratio of mass of
carbon/paraffin wax 1:1 and stirred until
homogeneous using a spatula on a petri
dish. After that, the carbon paste electrodes
inserted into the body with pressed using a
spatula in order to solidify (Vytras et al.,
2009; Wachid and Setiarso, 2014).
7. Measurement of Specific Capacitance
Specific capacitance of carbon paste
electrodes measured by CV technique using
Potentiostats EA161 with three electrodes,
namely Pt electrode, Ag/AgCl electrode and
carbon paste electrodes. Tests of electrode
at the rate of scan 100 mV/s using an
electrolyte solution of H2SO4 0.1 M thus
obtained voltammogram voltages and
currents, then the calculated value of
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Vol.8. No. 20, December 2015
specific capacitance (Himmaty and
Endarko, 2013).
RESULTS AND DISCUSSION
Manufacture of Rice Husk Carbon
Preparation of raw material for made
carbon was included washing and drying.
Washing with water aims to remove
impurities such as dust and sand attached to
the hull as well as washing with technical
HCl to lower levels of impurities such as
metal oxides contained in rice husk. Drying
under the sun and in the oven at 110 °C for 1
hour aims to remove moisture contained in
rice husk (Andaka 2008; Mujiyanti et al.,
2010).
Carbonization was a burning process
certain raw materials at a temperature of
about 300-900 °C that cause decomposition
of organic compounds to form methanol,
acetic acid vapors, tar and hydrocarbons.
The release of these volatile elements
causing an open pore structure (Ramdja et
al., 2008; Surest et al., 2008). Rice husk
carbonization process in this research was
done in a furnace at 350 °C for 1 hour. This
temperature is the optimum temperature for
the carbonization of rice husk because a
temperature below 350 °C the
carbonization process has not been perfect,
while temperatures above 350 °C was
already happening ashing. Carbon produced
and then crushed and sieved to 100 mesh
size sieve to produce a homogeneous
carbon sized and smaller particle size and
then the surface area of the carbon becomes
larger.
Extraction of Silica
Analysis of compounds in the
carbon content of rice husk using XRF
showed that the content of silica (SiO2)
amounted to 99.05%. To increase the
surface area of rice husk carbon, extraction
of silica was carried out to obtain more
ISSN 2085-014X
space on the surface of carbon (Wei et al.,
2011). According to the Agung et al. (2013)
the higher the concentration of KOH was
used, the more silica was extracted. The
reaction that occurs in the extraction
process silica with KOH is following:
SiO2 + 2KOH → K2SiO3 + H2O
Activation
Activation was a process for
removed hydrocarbon coating the surface of
the carbon thereby increasing the porosity
of carbon. In this research used chemical
activation because it is more profitable than
the physical activation. Mineral elements
activator entered among the sidelines of a
hexagonal carbon layer and separates the
surface initially covered. Thus, when the
heating was carried out, contaminants were
compounds in the pores to be more easily
dislodged. This causes the active surface
area becomes larger (Koleangan and Wuntu
2008; Ramdja et al., 2008).
One of the properties activators
associated with the quality of activated
carbon was covalently character. Covalent
character associated with covalent
interactions between carbon and carbon
activator to open the pores. Therefore, the
activator used in this research was H3PO4.
The elements that constituting H3PO4 were
covalently bonded polar. Composed of
carbon atoms that are covalently C form flat
hexagonal structure with one atom C at each
corner, it would be better interact with
substances that have covalent character than
the character of ionic substances
(Koleangan and Wuntu, 2008).
Determination of The Surface Area
Determination of the surface area of
the carbon was measured by the ability of
carbon to adsorb methylene blue at a
maximum wavelength of 664.5 nm. The
amount of adsorbed methylene blue was
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Vol.8. No. 20, December 2015

directly proportional to the surface area of the adsorbent.

Table 1. The surface area of the carbon.

Samples Surface area (m2/g)

Siliceous rice husk carbon 57.2833
Silica free rice husk carbon 180.5378
Silica free rice husk activated carbon 184.6074

Table 1 showed the extraction of silica and
activation can increase the surface area of
the carbon. In addition, the use of KOH in
extracting silica was very effective because
it can increase the surface area of the carbon
was three times greater.
Electrodeposition of Cu
Electrodeposition was one method of
attachment of the metal on the surface of a
material that can be used to increase the
value of specific capacitance. An increase in
specific capacitance was done by utilizing
electroactive species such as transition
metals, namely copper (Cu). Cu chosen
because it was not easily oxidized and had a
fairly high reduction potential was 0.340 V
thus the estimated Cu can act as an electron
trap (Rahmawati et al., 2008).
Electrodeposition process in this research
using silica free rice husk activated carbon
and commercial activated carbon as a
comparable mixed with a solution of
CuSO4.5H2O and stirred with a magnetic
stirrer in a state saturated with argon gas,
then treated with ultrasonic irradiation.
XRF analysis results after the
electrodeposition process showed the Cu
metal deposited on the surface of silica free
rice husk activated carbon by 75.98% and
12.24% for commercial activated carbon in
the form of CuO. The concentration of Cu
deposited on the surface of silica free rice
husk activated carbon more than the
commercial activated carbon because the
surface area of silica free rice husk activated
carbon was greater than the commercial
activated carbon which still contains silica.
The reaction is thought to occur
during the electrodeposition process is
following (Kasuma, 2012; Triastuti and
Purwanto, 2012):
Cu2+ (aq) + 2OH- (aq) → Cu(OH)2 (s)
Cu(OH)2 (s) → CuO (s) + H2O (l)

Table 2. The content of the compound Cu(I).

Content of Compound
CuO8TbW2 Cu6Mo5O18
CuO8SmW2 Cu2O2Sr
CuLaO8W2 CuFeO6Pb2Sr2
CuO8W2Y CuO2Sc

XRD analysis results in Table 2 after because there were compounds of copper in
being processed using software Match! the form of copper(I). The reaction was
indicates that during the process of thought to occur are following (Rahmawati
electrodeposition occurs redox reaction et al., 2008):

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Vol.8. No. 20, December 2015
Reduction: 2Cu2+ + 2e- → 2Cu+
Oxidation: H2O → ½O2 + 2H+ + 2e-
Measurement of Specific Capacitance
Capacitance was the ability of a
capacitor to hold the charge of electrons or
electrochemical energy. Specific
capacitance measurements in this research
using a Potentiostats EA161 with three
Figure 1. Voltammogram (a) before and (b) after electrodeposition.
Figure 1a showed the storage
process takes place unstable. This was
because the magnitude of the current
density tends to increase with increasing
potential difference and at the time of the
discharge process, charge out too unstable
(Suwandana and Susanti, 2015) while
Figure 1b showed the storage process tend
to be stable because of the current density is
almost fixed with increasing potential
difference and at the time of discharge, a
charge that came out was almost stable.
Shape of the curve obtained from the
measurement results with the technique of
cyclic voltammetry in Figure 1 showed the
specific capacitance value generated.
Specific capacitance values were influenced
by the charge and discharge currents.
Table 3. Cyclic voltammetry data of carbon paste electrodes.
Scan rate
Samples
(V/s)
Before electrodeposition 0,1
After electrodepsition 0,1
ISSN 2085-014X
electrodes, namely Pt electrode, Ag/AgCl
electrode and carbon paste electrodes. Pt
electrode as an comparison electrode,
Ag/AgCl electrode as a reference electrode
and carbon paste electrodes as the working
electrode (Himmaty and Endarko, 2013).
Tests carried out at the scan rate 100
mV/s using an electrolyte solution of H2SO4
0.1 M.
Calculation of the current charge and
discharge specific capacitance was taken at
the midpoint of each curve (Herniyanti et
al., 2014; Rizki et al., 2015). Charge and
discharge current value of the electrode can
be known from the voltammogram obtained
and the specific capacitance values can be
calculated using the following equation:
Cs =
Cs is the specific capacitance (nF/g),
Ic and Id respectively charge and discharge
currents (nA), v is the scan rate (V/s) and m
is the mass of carbon on the electrode.
Mass (g) Ic (nA) Id (nA) Cs (nF/g)
0,12 1,820 -6,073 657,75
0,12 4,708 -3,945 721,08
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Vol.8. No. 20, December 2015
Table 3 showed the larger charge and
discharge currents, the greater the value of
specific capacitance generated. The
resulting value was still very low compared
with the results of research conducted by
Gao et al. (2015) regarding the EDLC
material from rice husk with a specific
capacitance of 367 F/g. This was because
the method of making electrodes used are
different and the amount of carbon used was
too little (Rizki et al., 2015; Suwandana and
Susanti, 2015).
CONCLUSION
The surface area of rice husk carbon
before and after the extraction of silica and
after activation with an activator H3PO4 in a
row were 57.2833 m2/g, 180.5378 m2/g and
184.6074 m2/g. Cu electrodeposition with
ultrasonic irradiation can increase the value
of specific capacitance of silica free rice
husk activated carbon. The value of specific
capacitance of silica free rice husk activated
carbon before and after electrodeposition of
Cu with ultrasonic irradiation were 657.75
nF/g and 721.08 nF/g.
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