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Microporous and Mesoporous Materials 197 (2014) 316323

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Microporous and Mesoporous Materials


journal homepage: www.elsevier.com/locate/micromeso

The synthesis and characterization of high purity mixed microporous/


mesoporous activated carbon from rice husk using chemical activation
with NaOH and KOH
Lingeswarran Muniandy a, Farook Adam a,, Abdul Rahman Mohamed b, Eng-Poh Ng a
a
b

School of Chemical Sciences, Universiti Sains Malaysia, 11800 Penang, Malaysia


School of Chemical Engineering, Universiti Sains Malaysia, Engineering Campus, 14300 Nibong Tebal, Pulau Pinang, Malaysia

a r t i c l e

i n f o

Article history:
Received 1 April 2014
Received in revised form 12 June 2014
Accepted 19 June 2014
Available online 28 June 2014
Keywords:
Rice husk
Activated carbon
Chemical activation
Surface area
Porous carbon

a b s t r a c t
Activated carbon (AC) with high purity and surface area was synthesized from rice husk (RH) using alkali
leaching at room temperature. Regular and pyridine FT-IR analysis had shown that the AC sample consists mainly of C@C aromatic bonds and did not have Brnsted or Lewis acid sites respectively. In addition, the XRD patterns indicate that all AC samples were amorphous with slight micro-crystalline features
due to the appearance of broad peaks at 2h = 24 and 44 respectively. The maximum surface area
obtained from the BET analysis was 2696 m2 g1 for the KOH activated carbon at 850 C with an impregnation ratio of 1:5 (RHC:KOH) under nitrogen ow. The SEM images also revealed the highly porous nature of the AC resulting in the high surface area. The TGA-DTG analysis of the AC samples showed that the
samples are thermally stable up to 900 C in nitrogen atmosphere.
2014 Elsevier Inc. All rights reserved.

1. Introduction
Activated carbons (AC) are usually characterized by their large
surface area, high micro-porosity and adsorption capacity, enabling
them to be utilized as an effective adsorbent in water treatment
processes [1]. Furthermore, AC has also been used as a support for
catalysis in various reactions [2,3]. In addition, AC has been utilized
as storage for natural gasses [4].
However, the commercial production of AC is not cost effective
and together with the fact that the regeneration of used AC is
extremely difcult, much attention has been given to synthesizing
amorphous activated carbon from renewable sources. Recently,
various types of agricultural wastes were used as the source for
the production of AC. Some recent examples are the use of coconut
shells, rice husks and empty fruit bunches of oil palm [57] to produce AC. This is also an approach to reduce environmental
pollution contributed by these agricultural wastes. There are, however, other alternative carbon sources such as animal waste and
polymers [8,9] which have been proven to be excellent precursors
for the synthesis of AC.
The synthesis of AC mainly comprises of two stages. Firstly, the
precursors/raw materials are carbonized at lower temperatures

Corresponding author. Tel.: +60 46533567; fax: +60 46574854.


E-mail addresses: farook@usm.my, farookdr@gmail.com (F. Adam).
http://dx.doi.org/10.1016/j.micromeso.2014.06.020
1387-1811/ 2014 Elsevier Inc. All rights reserved.

(<800 C) to produce the black colored char which would be followed by activation at higher temperature [1]. AC is basically synthesized via chemical or physical activation. In the physical
activation process, the charcoal/carbonized materials are activated
at high temperature in the presence of steam or carbon dioxide. On
the other hand, chemical activation involves the impregnation of
chemicals such as potassium hydroxide (KOH), sodium hydroxide
(NaOH), zinc chloride (ZnCl2), and phosphoric acid (H3PO4) with
the carbonized char followed by activation in an inert atmosphere
usually under nitrogen aeration [10].
Rice husk or rice hull (RH) is an agricultural waste found in
abundance in rice producing countries mainly around the Asean
region. RH is the hard sheath that would be formed through the
absorption of silica from the soil to protect the rice grains within.
RH has been reported to consist mainly of organic ligno-cellulosic
biomass and ash [11]. The ash is mainly composed of about, 99
wt.% silica [12]. The silica from RH has been extensively studied
as a support in the eld of heterogeneous catalysis.
Ironically, the high silica content in RH remains a barrier
towards synthesizing pure amorphous carbon with large surface
area. Previous studies have reported the use of alkali leaching with
sodium hydroxide to produce high quality AC from RH [11,13]. This
method, however requires the RH to be reuxed with dilute
sodium hydroxide (NaOH) solution at a high temperature for a
certain period of time in order to remove the silica in the form of
sodium silicate solution.

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L. Muniandy et al. / Microporous and Mesoporous Materials 197 (2014) 316323


Table 1
Various studies conducted on the synthesis of activated carbon and the surface area of
the porous carbon produced.
Author

Source

Poinern et al. [1]

Macademia nut
shells
Kalderis et al. [10] Rice husk
Nakagawa et al.
[9]

Liou et al. [11]

Sugarcane
bagasses
PET
Rice husk
Rice husk

Lin et al. [13]

Rice husk

Present study

Rice husk

Method of activation Surface area


(m2 g1)
1100 C Physical/
CO2
700 C Chemical/
ZnCl2
700 C Chemical/
ZnCl2
500 C Physical/
steam & H2O
500 C Chemical/
ZnCl2
500 C Chemical/
H3PO4
800 C Chemical/
NaOH
850 C Chemical/
KOH

602
811
864
394
2434
1741
1015
2696

Table 1 shows related work concerning the synthesis of activated carbon from several carbon precursors. In this particular
study, however, AC, with high carbon content and surface area
(>2000 m2 g1) was successfully produced from RH by removing
silica via alkali leaching at room conditions (ca. 30 C).
2. Experimental

Table 2
AC samples prepared under various conditions from 1.0 M NaOH pre-treated RH.
Sample Impregnation ratio
(RHC:Activation
agent)

Activation
temperature
(C)

Activation Gas Activation


time (min) ow agent

AC-A
AC-B
AC-C
AC-D
AC-E
AC-F
AC-G
AC-H
AC-I
AC-J
AC-K
AC-L
AC-M
AC-N
AC-O
AC-P
AC-Q
AC-R
AC-S

450
450
450
450
450
750
750
750
750
750
750
750
750
750
750
850
950
850
850

60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
30
120

1:1
1:2
1:3
1:4
1:5
1:1
1:2
1:3
1:1
1:2
1:3
1:4
1:5
1:6
1:7
1:5
1:5
1:5
1:5

Air
Air
Air
Air
Air
N2
N2
N2
N2
N2
N2
N2
N2
N2
N2
N2
N2
N2
N2

NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
NaOH
KOH
KOH
KOH
KOH
KOH
KOH
KOH
KOH
KOH
KOH
KOH

samples as indicated in Table 2. After activation, all samples were


washed with distilled water and dilute nitric acid (1.0 M) until the
pH of the rinse became neutral (pH 6.87.2), followed by drying at
105 C for 24 h. The samples prepared were labelled as presented
in Table 2.

2.1. Materials
The chemicals used were sodium hydroxide pellets (Qrec, 99%),
potassium hydroxide pellets (Qrec, 99%) and nitric acid (Qrec, 69%).
The rice husk (RH) was obtained from a rice mill in Penang,
Malaysia. All chemicals were of analytical grade and used without
further purication.
2.2. Preparation of the charcoal and activated carbon
2.2.1. Carbonization of rice husk waste (RHW)
About 30.0 g of clean RH was weighed and stirred with 1.0 M
HNO3 for 24 h to remove the metallic impurities. The RH was later
rinsed several times with distilled water to remove the remaining
acid content. It was then dried at room temperature and stored to
be used as a precursor for the synthesis of RHC. About 25.0 g of the
acid treated RH was stirred for 24 h in 500 mL of 1.0 M NaOH for
the removal of silica. The RHW (reddish brown solid after the
removal of silica from RH via sodium silicate solution) was ltered
and dried at 105 C for 24 h. This was followed by carbonization at
400 C for 4 h as described elsewhere, [14] under atmospheric conditions to obtain the black colored RHC. The RHC obtained was further processed by stirring it in 300 mL of 1.0 M NaOH at room
temperature for 20 min to remove any excess silica impurities in
order to obtain charcoal with high carbon content/purity. The charcoal was then ltered and rinsed with distilled water before being
dried at 105 C for 24 h.
2.2.2. Preparation of rice husk activated carbon (RHAC)
The activation was carried out by adding 3.0 g of RHC with 40%
(w/w) of the activating agent (NaOH or KOH) solution under various impregnation ratios (RHC:Activation agent) and stirred for
30 min at room conditions followed by sonication for 15 min.
The samples were then dried at 105 C for 48 h before activation
under normal atmospheric ow with a heating rate of 10 C min1
to achieve the nal activation temperature as listed in Table 2.
Activation was also carried out similarly under N2 ow for other

2.3. Physical characterizations


2.3.1. FT-IR and pyridine adsorption analysis
All the AC samples were analyzed for the identication of the
basic functional groups by FT-IR Spectroscopy (Perkin Elmer Spectroscopy 2000 FT-IR Spectrophotometer, in the range of 4000
400 cm1) using sample pellets made by mixing with anhydrous
KBr. The samples and the KBr salt were oven dried at 110 C for
24 h prior to analysis. Pyridine adsorption analysis (Thermo Scientic NICOLET IR200 FT-IR) was carried out using pellets of activated carbon without KBr. The pellets were heated up to 250 C
under vacuum conditions and the pyridine vapor was introduced
briey for the chemi-adsoprtion process to take place. After
1 min, the pyridine vapor was pumped out and the IR spectra
was recorded.
2.3.2. XRD analysis
The samples were characterized by powder X-ray diffraction
(Siemens Diffractometer D5000 Kristalloex, equipped with Cu
Ka radiation, k = 0.154 nm) with a step size of 0.05 from 10 to
90 (high angle). The voltage supplied was 40 kV with a current
of 30 mA.
2.3.3. N2 adsorptiondesorption studies
The surface area and porosity of the prepared samples were
assessed using N2 adsorptiondesorption analysis (Micromeritics
ASAP 2020 porosimeter). The samples were initially degassed at
110 C for 10 h under vacuum prior to being analyzed.
2.3.4. SEM-EDX/TEM analysis
The surface of the prepared samples was investigated using
scanning electron microscopy (SEM Leica Cambridge S360) tted
with energy dispersive X-ray (EDX) for elemental analysis. The
topography of the samples was studied using transmission electron microscopy (TEM Phillips CM12 TEM).

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L. Muniandy et al. / Microporous and Mesoporous Materials 197 (2014) 316323

2.3.5. TGA-DTG analysis


Thermal analysis (TGA/SDTA 851eMettler Toledo) was conducted under nitrogen ow to investigate the thermal stability of
the prepared AC samples. The heating rate was xed at 20 C min1
from 30 C to 900 C.
3. Results and discussion
3.1. Characterization of the AC samples
3.1.1. FT-IR and pyridine analysis
The FT-IR spectra were obtained from the AC samples in Fig. 1
which were prepared under varying conditions from RH. The broad
peaks around 33003400 cm1 in the spectra were due to the
stretching vibrations of the OH bonds of water molecules which
were adsorbed onto the matrices of the samples [15]. The appearance of peaks in the region between 1500 and 1600 cm1 indicate
the presence of C@C bonds of aromatic compounds [16]. The sharp
band at 1384 cm1 is due to the residual nitrate ions (NO
3 ) as a
result of washing the AC samples with 1.0 M nitric acid [17]. Broad
bands were also observed around the region of 10501070 cm1
which could be attributed to the stretching vibrations of the CO
bonds of esters, phenols, alcohols or ethers [18]. However, the AC
samples prepared at 450 C (Fig. 1a) in atmospheric conditions
exhibited weak bands at 28002900 cm1 indicating stretching
vibrations of the CH bonds of the methylene groups (CH2)
[5]. These bands were, however, not present for the AC samples
that were activated at 750 C. This could be due to the decomposition of the CH bonds to form a more stable aromatic C@C bond at
the higher activation temperature [6].
Pyridine FT-IR analysis was also conducted to determine the
presence of Lewis and Brnsted acid sites in the synthesized AC
sample as shown in Fig. 2. The spectra has shown that the AC samples have weak interaction with the pyridine vapor, thus indicating
that there might not be any Brnsted or Lewis acid sites on the surface of the AC sample. The presence of Brnsted acid would be
identied by the appearance of bands in the 14001700 cm1
region after pyridine adsorption [19]. The Bronsted acids are due
to the presence of specic groups in the material that can undergo
ionization to form hydrogen ions. These functional groups can be
identied as silanol (SiOH), carboxylic acid (COOH), amines
(NH), etc. The illustrations presented in Scheme 1 shows the
mechanism of adsorption of these acidic groups with pyridine
vapor through chemi-sorption. The samples tested in the present
study, however, consist primarily of C@C aromatic bonds.
Therefore, all the AC samples did not show the IR bands of the
pyridine-adsorbed species.
3.1.2. XRD analysis
The XRD patterns for all the prepared AC samples (Fig. 3) exhibited a broad peak in the range of 2030 and a broad hump in the
range of 4050 which could be attributed to the reection from
the (0 0 2) and (1 0 0) planes [20]. These broad peaks are the characteristics of amorphous carbon with carbon rings that disorderly
stack up [20]. Therefore, it could be justied that there are some
degree of micro-crystallinity with turbostratic graphite structure
in the AC samples [20]. The increased background signal between
10 and 20 is expected due to the presence of micropores in the
samples. These micropores eventually scatter the X-ray beam,
causing elevated background signal [21].
The interlayer spacing, d002 of the AC samples was calculated
using Braggs equation as follows

d002

k
2 sin h

Fig. 1. FT-IR spectra of the AC samples prepared under various activation temperatures, time and activating agent. Refer to Table 2 for the activation conditions of
samples in (a), (b), (c) and (d).

L. Muniandy et al. / Microporous and Mesoporous Materials 197 (2014) 316323

319

Fig. 2. The FT-IR spectra of sample AC-P: before and after pyridine adsorption.

(A)

+ Si

OH

Si

(B)

+ R

O
OH

O
(C)

+ R
N

O
R

Scheme 1. Several illustrations depicting the chemi-adsorption process when


pyridine vapor was introduced to samples with different functional groups.

in which the k is the X-ray wavelength (k = 0.154 nm) and h is the


angle of the peak position.
The average crystallite size along the c-axis, Lc and the size of
the layer planes, La were obtained by using the Scherrer Eq. (2).

Kk
B cos h

K is the value of the shape factor in which K = 0.9 and K = 1.84


are used for the purpose of calculation of the Lc and La, respectively.
The Lc and La values are based on the appearance of the peaks at
(0 0 2) and (1 0 0) planes respectively. B is the value of the line
broadening at half width of the peak or better known as FWHM
(full width half maximum) in radians.
The values of d002, d100, Lc and La are listed in Table 3. The interplanar spacing, d002 values for all the AC samples were found to be
in the range of 0.34 to 0.38 nm, which is actually larger than that of
graphite (d002 = 0.335 nm). Similar results were also reported previously by Prahas et al. [22] and Hadoun et al. [23]. However,
Hadoun et al. [23] justied that the high d002 value was attributed
to the fact that the AC samples were disordered and proper graphitization had not taken place. On the other hand, disordered AC
samples were found to exhibit better porosity and hence result
in a higher surface area with excellent adsorption capability [22].

Fig. 3. The XRD patterns obtained for the AC samples which were prepared under
various conditions. Refer to Table 2 for the activation conditions for samples in (a),
(b) and (c).

3.1.3. N2 Adsorptiondesorption analysis


The textural properties of the AC samples were determined by
applying the BarrettJoynerHalenda (BJH) method. The surface
area, pore volume and width of the samples prepared are shown
in Tables 4 and 5. The surface area of the AC samples is usually
inuenced by four main factors such as the type of the activating
agent, the amount of the activating agent, activation temperature
and the duration of treatment. From Table 4, it was observed that
KOH acts as a better activating agent compared to NaOH. The activation by KOH results in a larger surface area. This could be attributed to the fact that KOH activation would lead to the production
of more micropores generating higher micropore volume, therefore
resulting in porous carbon with higher surface area [24].
The pore width of the AC samples shows a decline as the
impregnation ratio of KOH increases up to 1:5 (RHC: KOH). As
the impregnation ratio of KOH increases, the larger pores collapsed

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Table 3
Interlayer spacing and micro-crystalline properties of the activated carbon samples
prepared from rice husk under various conditions.
Sample

d002 (nm)

d100 (nm)

Lc (nm)

La (nm)

AC-A
AC-B
AC-C
AC-D
AC-J
AC-K
AC-L
AC-M
AC-N
AC-O
AC-P
AC-Q
AC-R
AC-S

0.38
0.38
0.37
0.38
0.36
0.34
0.34
0.38
0.36
0.36
0.36
0.35
0.35
0.36

0.22
0.21
0.21
0.22
0.21
0.22
0.21
0.21
0.22
0.21
0.21
0.21
0.20
0.21

2.38
2.53
2.82
2.11
2.03
3.03
2.41
2.47
2.25
1.86
3.23
4.30
2.44
3.25

3.77
3.58
4.77
3.94
6.49
5.64
5.02
4.27
3.97
5.07
4.84
5.09
7.20
5.37

Table 4
The textural properties of the charcoal and activated carbon synthesized from NaOH
pre-treated rice husks under different conditions as summarized in Table 2.
Sample

RHC
AC-B
AC-G
AC-J
AC-K
AC-L
AC-M
AC-N
AC-O

SBET (m2 g1)

1.750
155.5
594.9
682.6
1075
1394
2121
886.1
990.6

Vpore (cm3 g1)


Total

Micro

Meso

0.192
0.340
0.401
0.636
0.837
1.022
0.655
0.818

0.028
0.192
0.228
0.362
0.345
0.589
0.176
0.097

0.150
0.121
0.172
0.260
0.444
0.243
0.359
0.515

DKJS (nm)

Yield, C (%)

12.80
8.410
7.210
9.592
8.543
3.714
6.490
6.168

23.80
19.83
18.24
18.96
18.09
17.61
17.21
16.74
16.02

Table 5
BET results of the activated carbon produced from NaOH pre-treated rice husks by
KOH activation at various activation temperatures and time as listed in Table 2.
Sample

AC-M
AC-P
AC-Q
AC-R
AC-S

SBET (m2 g1)

2121
2696
1592
1499
1908

Vpore (cm3 g1)


Total

Micro

Meso

1.022
1.496
1.293
0.882
1.038

0.589
0.274
0.052
0.319
0.442

0.243
0.691
1.056
0.383
0.374

DKJS (nm)

Yield, C (%)

3.714
2.634
3.150
4.845
4.258

17.21
17.05
16.58
17.45
16.65

and smaller micro-pores began to develop which eventually contribute to the increase in the surface area of the AC samples, from
683 m2 g1 to 2121 m2 g1. Consequently, this also leads to the
samples having higher micro-pore volume as shown in Table 4.
However, impregnation ratio higher than 1:5 (RHC: KOH) seemed
to be detrimental for the surface area of the AC samples resulting
in the surface area of the samples to decrease to 991 m2 g1.
The activation temperature of the samples is also instrumental
for the development of the micro-pores ensuring the production of
AC samples with large surface area. The highest surface area
obtained for the AC sample was 2696 m2 g1 (impregnation ratio
1:5, RHC: KOH) at an activation temperature of 850 C. Activation
at 750 C and 950 C however, produced AC samples with a relatively lower surface area (2121 and 1592 m2 g1 respectively).
Increasing the activation temperature usually enhances the activation process, which is crucial for the creation of new pores [25]. On
the other hand, very high activation temperatures are reported to
cause violent gasication reactions which would lead to the
destruction of the micro-pores and ultimately lowering the surface
area of the AC [26].

Fig. 4. The N2 adsorptiondesorption isotherm plots for the various AC samples


derived from RH after pre-treatment with NaOH. The plots are presented in two
separate diagrams for clarity.

The activation time plays a crucial role in the growth of the


micro and mesopores in AC samples. Previous studies had reported
that longer activation time would yield AC with higher surface
area. This could be traced back to the fact that longer activation
time would eventually cause the decomposition of the volatile
compounds resulting in better porosity for the AC samples [18].
The N2 adsorptiondesorption isotherm plots (Fig. 4) yields
important information regarding the porosity of the carbon samples. From the plots, it could be deduced that the AC samples consist of both mesopores and micropores which is the combination of
type I and type IV isotherms. However, it is revealed that upon
increasing the activation temperature from 750 C to 950 C
(KOH activation), the isotherm plot becomes more distinctly type
IV, indicating that higher activation temperature is not benecial
for the development of micropores and in turn promotes the
growth of mesopores. Similar results were also reported by Prahas
et al. [22], in which the authors have stated that increasing the
activation temperature would result in the widening of the micropore to mesopore.
The total surface area for the porous carbon samples increased
as the activation time was increased from 30 min (AC-R) to 60 min
(AC-P). This is expected because longer activation time would
allow more carbon particles to react with KOH, inducing higher

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L. Muniandy et al. / Microporous and Mesoporous Materials 197 (2014) 316323


Table 6
EDX analysis of the porous carbons derived from rice husk.
Samples

RHC
AC-B
AC-G
AC-M
AC-P

Elements
C

Si

Na

71.45
63.44
83.79
85.78
91.34

25.47
31.78
15.27
11.90
8.14

0.25
3.39
0.94
0.61
0.12

2.83
1.39

1.71
0.41

activated carbon decreased as shown in Table 5. Prolonged heat


treatment/activation would only cause the existing pores to collapse or be destroyed [28].
Fig. 5 exhibits the pore size distribution of AC samples prepared
under nitrogen ow. It was observed that the AC samples consists
mostly of micropores (<2 nm) which is one of the major characteristics found in AC samples.
Fig. 5. The pore size distribution of several AC samples prepared during the course
of the optimization study.

level of volatilization and eventually result in the creation of new


pores [27]. However, subsequent increase of the activation time
to 120 min (AC-S) became detrimental as the surface area of the

3.1.4. SEM-EDX analysis and TEM images of the prepared carbon


samples
Fig. 6(c and d) exhibits the highly developed porous structure of
the AC samples from the relatively non-porous RHC (Fig. 6a and
6b). It was observed that the RHC was brous and had no hollow

Fig. 6. The transformation of the non-porous RHC (Fig. 6a and b) to porous carbon as shown in Fig. 6c (AC-M) and Fig. 6d (AC-P) respectively upon activation. The TEM images
of AC-M and AC-P (Fig. 6e and f) indicating the presence of carbon nanoparticles.

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L. Muniandy et al. / Microporous and Mesoporous Materials 197 (2014) 316323

Fig. 7. TGA-DTG thermograms for the (a) RHC and (b) AC-P samples under N2 ow similar to the activation process.

structures which eventually lead to its very low surface area as


proven from the BET analysis. In addition, the low surface area of
the RHC could also be attributed to the fact that the pores of the
charcoal were lled with carbonaceous products due to the incomplete combustion at 400 C [29]. However, upon activation, the
non-porous structure of RHC transformed into the porous AC as
shown in Fig. 6c and d. This transformation is attributed to the
decomposition of the volatiles due to the activation process at high
temperatures which could be described by the equation [30];

6KOH
2K 3H2 2K2 CO3

A previous study had also reported the presence of metallic


potassium in the furnace, which was proven by TPD experiments
[30]. The potassium carbonate, however, would decompose during
activation and the CO2 gas would be released. The reaction
between the activating agent and the carbon precursor would lead
to the decomposition of the volatile organic compounds which in
turn would form the porous surface of the AC samples. In another
study [31], porous AC samples were prepared from intense gasication of carbonaceous material by the heat treatment process.
Therefore, it could be justied that heat treatment with the suitable activating agent is extremely crucial for the development of
the pores in AC samples.
The TEM images in Fig. 6e and f revealed that the AC samples
consist mostly of carbon particles which tend to agglomerate. This
could be due to the very ne nature of the carbon particles which
tend to stack up in aqueous solutions. The TEM images also
revealed that the carbon samples are turbostratic in nature [32]
which corroborates with the results from the XRD analysis. In addition, the carbon particles were observed to be extremely small
which could easily reach nano-scale level, hence indicating the
usefulness of this material as a support for catalytic reactions.
The elemental analysis conducted on the charcoal and AC samples are presented in Table 6. The high content of carbon indicates
the purity of the samples which was synthesized from rice husk. In
addition, the EDX analysis show that alkali leaching with dilute
solutions of NaOH at room temperature is more than sufcient
for the removal of silica from the rice husk in order to obtain porous carbon with large surface area (>2000 m2 g1). This is in stark
contrast of needing the rice husk to be heated or reuxed at high
temperatures as were reported in previous studies [11,13,33].
3.1.5. TGA-DTG analysis
The TGA-DTG analysis was conducted to determine the thermal
stability of the synthesized AC sample (Fig. 7). RHC showed three
main stages of weight loss which rst occurred between 30 and
165 C with 2.598 wt.% loss. This was attributed due to the evaporation of the water molecules which were adsorbed on the surface
and within the pores of the charcoal [34]. The second stage of

weight loss for RHC happened between 165 and 600 C with
18.35 wt.% loss followed by another stage from 600 to 900 C with
10.85 wt.% loss. These two stages of weight losses could be attributed to the violent gasication of the organic volatiles [35] and the
decomposition of the lignin found in the charcoal respectively [36].
The rst stage of weight-loss of the AC sample was observed
around 30150 C whereby 14.87 wt.% loss took place. The higher
weight loss of the AC sample indicates its excellent adsorptive
properties in which it could trap more water molecules due to its
micro-porous nature compared to the charcoal which is relatively
non-porous. The second/nal stage of weight loss of the AC sample
was observed to be around 150900 C with 9.683 wt.% loss. This is
attributed to the decomposition of the most tightly held organic
volatiles within the carbon matrix such as lignin, similar to the
results obtained from RHC [35].
4. Conclusions
It was observed that alkali leaching at room temperature was
sufcient for the removal of silica from RH. Highly porous AC
was synthesized having a high surface area (>2000 m2 g1). Activation using KOH seemed to be more effective than NaOH due to the
higher reactivity of the potassium metal (Eq. (3)) and the charcoal.
Carbon samples activated at high temperatures (P750 C) with
KOH consist predominantly of aromatic C@C bonds indicating a
thermally stable compound.
Acknowledgement
We would like to thank the Government of Malaysia for the
Research University Grant (Ac. No. 1001/PKIMIA/814127) which
partly supported this work. We would also like to thank the
Malaysian Ministry of Higher Education for providing MyBrain15
Scholarship to L.M.
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