Industrial Crops and Products 37 (2012) 93–99

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Industrial Crops and Products

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Extraction, preparation and characterization of cellulose fibres and nanocrystals

from rice husk
Nurain Johar a,b , Ishak Ahmad a,b,∗ , Alain Dufresne c
a
Polymer Research Center (PORCE), Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia
b
School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia
c
The International School of Paper, Print Media and Biomaterials (Pagora), Grenoble Institute of Technology, BP 65 - F-38402 Saint Martin d’Hères Cedex, France

a r t i c l e i n f o a b s t r a c t

Article history: Cellulose fibres and cellulose nanocrystals were extracted from rice husk. Fibres were obtained by submit-
Received 30 September 2011 ting the industrial rice crop to alkali (NaOH) and bleaching treatments. Nanocrystals were extracted from
Received in revised form 1 December 2011 these fibres using sulphuric acid (H2 SO4 ) hydrolysis treatment. The material obtained after each stage of
Accepted 14 December 2011
the treatments was carefully characterized and its chemical composition was determined. Morpholog-
Available online 7 January 2012
ical investigation was performed using scanning electron microscopy (SEM) and transmission electron
microscopy (TEM). Fourier transform infrared (FTIR) spectroscopy showed the progressive removal of
Keywords:
non-cellulosic constituents. X-ray diffraction (XRD) analysis revealed that the crystallinity increased with
Rice husk
Natural fibres successive treatments. The thermal stability of the rice husk fibres and cellulose nanocrystals was also
Purification investigated using thermogravimetric analysis (TGA).
Cellulose nanocrystals © 2011 Elsevier B.V. All rights reserved.

1. Introduction
Producing more sustainable and environmental friendly materi-
als has gained the attention of researchers at the international level.
It includes a search for alternatives to petroleum-based materials.
The development of biomaterials holds great promise to miti-
gate many of the sustainability problems, offering the potential
of renewability, biodegradation, and a path away from harmful
additives. The research reported here involves the development
of efficient techniques for the production of natural fillers as rein-
forcing agents for composite applications. Chemical composition,
morphological structure, physical and thermal properties of the
fibres can be evaluated to estimate their ability to be used as
filler in biocomposite applications. Alemdar and Sain (2008b) have
reported that nanofibres from wheat straw can be produced in the
range of 10–80 nm in diameter with a length of several microme-
tres. Moreover, the hierarchical structure of natural fibres allows
the preparation of nanoscale particles (Azizi Samir et al., 2005;
Wang et al., 2006).
In the last decade, research focusing on the use of cellulosic
waste as filler has grown rapidly. Agricultural wastes such as
coconut husk fibres (Rosa et al., 2010), cassava bagasse (Pasquini
∗ Corresponding author at: Polymer Research Center (PORCE), Faculty of Science
and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia.
Tel.: +60 3 89215441; fax: +60 3 89215410.
E-mail address: gading@ukm.my (I. Ahmad).
et al., 2010), banana rachis (Zuluaga et al., 2009), mulberry bark (Li
et al., 2009a,b), soybean pods (Wang and Sain, 2007), wheat, straw,
and soy hulls (Alemdar and Sain, 2008a), and cornstalks (Reddy
and Yang, 2005) have been studied as a resource in the produc-
tion of crystalline cellulose fibres. Various terms has been used
in the literature to describe these crystalline cellulose nanopar-
ticles which includes nanowhiskers, cellulose nanocrystals, NCC
(nanocrystalline cellulose), monocrystals, microcrystals or micro-
crystallites (Siqueira et al., 2010). Although a variety of natural
fibres were investigated in detail, the use of rice husk as a natu-
ral source for the production of cellulose nanocrystals has not been
widely explored yet.
Rice is the largest cereal crop in the world. Rice husk is an impor-
tant agricultural waste that can be easily found in some states of
Malaysia. The rice milling industry generates a huge quantity of rice
husks during the paddy milling process from the fields. It accounts
for 20% of the 500 million tons of paddy produced worldwide
(Bhammathidas and Mehta, 2004). Societies, especially among the
rice millers, often dispose of the rice husk waste using open burn-
ing. This situation directly leads to environmental concerns and
becomes a great environmental threat causing damage to the land
and the surrounding area in which it was dumped. Different meth-
ods for husk disposal, including finding a commercial use for the
waste have been suggested; however, it has proven to be a difficult
fuel for gasification and fluidized bed combustion. This is a result
of the high ash content resulting in carbon conversion inefficiency.
Previous reports on the commercial use of rice husk have focused
more on surface modification to improve filler–matrix interaction

0926-6690/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.indcrop.2011.12.016
94 N. Johar et al. / Industrial Crops and Products 37 (2012) 93–99
in composite applications (Ahmad et al., 2007). The rice husk can
also undergo combustion to produce rice husk ash that is rich in
silica. Another way to use rice husk involves the exploitation of its
cellulose content. According to Jackson (1977), rice husk consists of
33% cellulose, 26% hemicellulose, and 7% lignin. Therefore, the use
of rice husk as the primary source for producing cellulose fibres and
nanocrystals is promising.
The aim of this study was to extract cellulose fibres from the rice
husk using alkali and bleaching treatments. The preparation of cel-
lulose nanocrystals from these natural fibres was also investigated.
2. Materials and methods
2.1. Materials
The rice husk used as raw material was obtained from Bernas
Malaysia Sdn. Bhd. Sodium hydroxide (99% purity) was used
for alkaline treatment. Sodium chlorite, acetic acid, and sodium
hydroxide were used as bleaching agents while sulphuric acid was
used for hydrolysis. All chemicals were purchased from System
ChemAR and Sigma–Aldrich and were used without further purifi-
cation.
2.2. Preparation of cellulose nanocrystals from rice husk.
2.2.1. Alkali treatment
The alkali treatment was performed to purify the cellulose
by removing lignin and hemicellulose from rice husk fibres. The
ground rice husk was treated with an alkali solution (4 wt% NaOH).
The mixture was transferred into a round bottom flask and treat-
ment was performed at reflux temperature for 2 h. The solid was
then filter and washed several times using distilled water. This
treatment was performed thrice.
2.2.2. Bleaching process
Following alkali treatment, the bleaching process was com-
pleted by adding a buffer solution of acetic acid, aqueous chlorite
(1.7 wt%) and distilled water at reflux (using a silicon oil bath at
100–130 ◦ C) for 4 h. The mixture was allowed to cool and was
filtered using excess distilled water. The bleaching process was
repeated four times.
2.2.3. Acid hydrolysis
The acid hydrolysis treatment was conducted on the fibres after
alkali treatment and bleaching at a temperature of 50 ◦ C using
10.0 mol L−1 of sulphuric acid (pre-heated) for 40 min under con-
tinuous stirring. The fibre content ranged from 4 to 6 wt%. The
hydrolysed material was washed by centrifugation at 10,000 rpm
at 10 ◦ C for 10 min. This centrifugation step was repeated several
times before the suspension was dialysed against distilled water
for several days until constant pH in the range of 5–6 was reached.
The resulting suspension was then sonicated for 30 min before kept
refrigerated for further used.
2.3. Characterization of rice husk fibres and nanocrystals
2.3.1. Chemical composition
The chemical composition of the rice husk at each stage of
treatment was determined according to the methods reported by
the Technical Association of Pulp and Paper Industry (TAPPI). The
cellulose and hemicellulose contents were accessed according to
TAPPI standard T203 OS-74 while the lignin content was measured
according to TAPPI standard T222 OS-83. The silica ash content was
determined using the thermogravimetric analysis (TGA) data. The
composition of silica ash was obtained at temperatures 900 ◦ C as
the residual ashes at this point can be attributed to the silica ash.
2.3.2. Microscopies
Scanning electron microscopy (SEM) (model Philips XL 30) was
used to observe the surface morphology of the rice husk fibres. The
effect of the different chemical treatments was assessed using a
comparison of the untreated, alkali treated, and bleached fibres.
Rice husk fibres were placed on the aluminium stub and incu-
bated in the oven at 60 ◦ C. The samples were then coated with gold
using a vacuum sputter coater (model SC 500). The thickness of the
gold layer was ca. 0.01–0.1 ␮m. The accelerating voltage was 15 kV.
Transmission electron microscopy (TEM) (model Philips CM 12)
was used to determine the dimensions of the cellulose nanocrystals
obtained from the rice husk fibres. A drop of a diluted suspension
(1 wt%) was deposited on the surface of a clean copper grid and
coated with a thin carbon film. As for contrast in TEM, the cellulose
nanocrystals were negatively stained in a 2 wt% solution of uranyl
acetate for 10 s then washed using 50 wt% of filtered alcohol. The
sample was dried at ambient temperature before TEM analysis was
carried out with an accelerating voltage of 80 kV.
2.3.3. Fourier transform infrared (FTIR) spectroscopy
Fourier transform infrared spectra were recorded using a
Perkin-Elmer FTIR spectrophotometer. Untreated, alkali-treated,
bleached, and acid-hydrolysed rice husk fibres samples were ana-
lysed. Samples were finely ground and mixed with potassium
bromide, KBr. The mixture was then compressed into pellet form.
FTIR spectral analysis was performed within the wave number
range of 400–4000 cm−1 .
2.3.4. X-ray diffraction (XRD)
X-ray diffraction was used to determine the crystallinity of the
rice husk fibres after different treatments. Each material in the
form of milled powder was placed on the sample holder and lev-
elled to obtain total and uniform X-ray exposure. The samples were
analysed using an X-ray diffractometer (D8-Advance Bruker AXS
GmbH) at room temperature (RT) with a monochromatic CuK␣
radiation source ( = 0.1539 nm) in the step-scan mode with a 2
angle ranging from 10◦ to 50◦ with a step of 0.04 and scanning time
of 5.0 min.
To characterize the crystallinity of the different samples, the
crystallinity index CrI, was determined based on the reflected
intensity data following the method of Segal et al. (1959):
I0 0 2 − Iam
CrI (%) = × 100
I0 0 2
where I0 0 2 is the maximum intensity of the (0 0 2) lattice diffraction
peak and Iam is the intensity scattered by the amorphous part of
the sample. The diffraction peak for plane (0 0 2) is located at a
diffraction angle around 2 = 22◦ and the intensity scattered by the
amorphous part is measured as the lowest intensity at a diffraction
angle around 2 = 18◦ .
2.4. Thermogravimetric analysis (TGA)
The thermal stability of the different samples was determined
by TGA measurements performed using a Mettler Toledo ther-
mogravimetric analyser (TGA/SDTA 85-F). The amount of sample
used for each measurement was ca. 1 mg. All measurements
were performed under a nitrogen atmosphere with a gas flow of
10 mL min−1 by heating the material from room temperature to
900 ◦ C at a heating rate of 10 ◦ C min−1 .
 N. Johar et al. / Industrial Crops and Products 37 (2012) 93–99
Table 1
Chemical composition of rice husk fibres at each stage of treatment.
Rice husks fibres Cellulose (%)
Untreated fibres 35
Alkali treated fibres 57
Bleaching treated fibres 96
3. Results and discussion
3.1. Chemical composition of fibres
The chemical composition of the rice husk was determined at
each stage of treatment and the data are summarized in Table 1.
The original rice husk fibres contained 35 wt% cellulose, 33 wt%
hemicelluloses, 23 wt% lignin, and 25 wt% silica ash. The cellulose
composition agrees quite well with the data published by Jackson
(1977), which reported that the untreated rice husks consist of
33 wt% celluloses, but shows a different in terms of hemicellu-
lose and lignin compositions which were 26 wt% hemicelluloses,
and 7 wt% lignin. In addition Real et al. (1996) and Patel et al.
(1987) reported that the rice husk contains silica ash in the range of
20–25 wt% which supported the value of silica ash that was deter-
mined in this research which is 25 wt%. Yussuf et al. (2010) also
reported that the general composition of rice husk was 38–45 wt%
cellulose, 12–20 wt% lignin, 20 wt% ash and 19 wt% silica. The chem-
ical compositions of rice husk were varied from sample to sample.
This difference was depending on the type of paddy, climatic, geo-
graphical conditions, sample preparation and method of analysis
which could be the reason for this variation (Chandrasekhar et al.,
2003).
Upon chemical treatment, the cellulose content continuously
increased as expected. The alkali treatment was efficient in
removing hemicellulose, which decreased from 33 wt% to 12 wt%
following treatment. Almost all of the silica content was removed
during alkali treatment. The lignin content remained practically
Fig. 1. Photographs of rice husk: (a) untreated rice husk, (b) alkali-treated rice husk, and (c) bleached rice husk.
95
Hemicelluloses (%) Lignin (%) Silica Ash (%)
33 23 25
12 21 –
– – –
constant. The bleaching treatment completely removed hemicel-
lulose and lignin, resulting in almost pure cellulose fibres, which
reached 96%.
3.2. Morphological investigation of the fibres
The visual macroscopic evolution of the rice husk fibres after
each stage of treatment is shown in Fig. 1. The colour of the
untreated rice husk is brown and changes to brownish-orange after
alkaline treatment. The bleached material is clearly different and
appears completely white. These colour changes are due to the
removal of non-cellulosic materials and other impurities such as
lignin, hemicelluloses, pectin, and wax upon chemical treatment of
the rice husks. The observed white colour of the final product is a
clear indication of almost pure cellulosic material and agrees with
the chemical composition data.
The chemical treatments used for cellulose purification from the
rice husks are also expected to induce morphological changes. The
structure of rice husk fibres was investigated using SEM (Fig. 2).
The smooth surface of untreated rice husk fibre is shown in Fig. 2a.
After alkali treatment (Fig. 2b), the fibre surface becomes rougher.
This could indicate the partial removal of the outer non-cellulosic
layer composed of materials such as hemicelluloses, lignin, pectin,
wax, and other impurities contained in the rice husk. Both wax and
pectin are known to surround the surface of natural fibres as a pro-
tective layer. Moreover, it is worth noting that the diameter of the
fibre bundles remains similar (around 170 ␮m) after alkali treat-
ment; this is attributed to the retention of the cementing lignin
96 N. Johar et al. / Industrial Crops and Products 37 (2012) 93–99

Fig. 2. Scanning electron micrographs of (a) untreated rice husk fibres, (b) alkali-treated rice husk fibres, and (c) bleached rice husk fibres.

material. Previous reports suggest that lignin forms a bridge bond of 100 samples of cellulose nanocrystals extracted from rice husk
with the cellulose ester and acts as a binder in the fibre compo- fibres are shown in Fig. 4. Most nanoparticles displayed a diameter
nents (Batra, 1981) thus preserving the bundle form after alkali and aspect ratio in the range of 15–20 nm and 10–15 respectively.
treatment. It was shown that pectin was fully removed from the
fibres by boiling the product in 0.4% NaOH solution (Batra, 1981),
3.3. Spectroscopic analysis (FTIR)
but for this study, the alkali treatment used a 4% sodium hydroxide
(NaOH) solution under reflux conditions for 2 h, with the expecta-
Fig. 5 shows the FTIR spectra recorded for (a) untreated rice husk,
tion that a majority of the pectin and hemicellulose content would
(b) alkali-treated rice husk (4% NaOH), (c) bleached rice husk, and
be removed.
(d) cellulose nanocrystals obtained from rice husk after hydroly-
The effect of the subsequent bleaching treatment was evident
sis with sulphuric acid. The different chemical treatments were
from the comparison of micrographs in Fig. 2b and c. It is observed
expected to induce morphological and chemical changes as shown
that the rice husk fibre bundles separate into individual fibres.
in the previous sections. The main peaks are reported in Table 2.
The diameter of the fibrous material decreased from an average
of around 170–7 ␮m. This decrease indicates that under the strong
chemical treatment conditions almost all the components that bind
the fibril structure of the rice husk were removed thus enabling
the fibres to separate into an individual form. This is further indi-
cation that the alkali treatment was unable to eliminate all the
non-cellulosic components.
The destruction of the natural fibre bundles after bleach-
ing treatment was reported by Hornsby et al. (1997b). Hornsby
observed a diameter reduction from 25–125 ␮m to 10–15 ␮m. This
size reduction was mainly attributed to the separation of the fibres’
primary cell wall due to the removal of hemicellulose and lignin.
An important consequence of the observed size reduction is the
increase in the fibre aspect ratio (L/d, L being the length and d the
diameter), which should provide higher reinforcing capability of
the fibres for composite applications.
Fig. 3 shows transmission electron micrographs obtained for
cellulose nanocrystals resulting from sulphuric acid hydrolysis of
purified rice husk fibres. Under controlled conditions, the acid
hydrolysis treatment was expected to cleave the amorphous region
of cellulosic microfibrils transversely keeping the straight crys-
talline domains intact. The treatment should eventually reduce the
size of the fibres from the micron to the nanometre scale (Azizi
Fig. 3. Transmission electron micrograph from diluted suspension of cellulose
Samir et al., 2005). The diameter distribution and the aspect ratio nanocrystals extracted from rice husk fibres.
 N. Johar et al. / Industrial Crops and Products 37 (2012) 93–99 97

Fig. 4. Diameter distribution and aspect ratio of cellulose nanocrystals extracted

from rice husk fibres.

Fig. 6. X-ray diffraction patterns of (a) raw, (b) alkali treated, (c) bleached, and (d)
acid hydrolysed rice husk.

The peak located around 1300 cm−1 in the spectrum of the

treated rice sample is representative of a change in the symmetry
of the C H group (Sun et al., 2005). The absorption phenomenon
around 1266–1200 cm−1 in the spectra in Fig. 6b and c refers to
the bending frequency of C H, O H, or CH2 , while the absorption
around 1060–1050 cm−1 and 890 cm−1 observed in the four spec-
tra refers to the C H stretching vibration of C O and the structure
of the cellulose component (Alemdar and Sain, 2008a).
No significant differences were observed between the spectra
corresponding to bleached and acid hydrolysed fibres. The results
indicate that the cellulose molecular structure remains unchanged
following acid hydrolysis.
Fig. 5. FTIR spectra recorded for (a) raw, (b) alkali treated, (c) bleached, and (d) acid
hydrolysed rice husk.
3.4. X-ray diffraction (XRD)

Cellulose has crystalline structure contrary to hemicellulose and

The peak near 3440–3400 cm−1 , which was observed in all spec-
tra, is representative of the C H and O H groups. The peak around
1640 cm−1 in all spectra corresponds to the absorption of water.
Both sets of peaks are ascribed to the stretching of hydrogen bonds
and bending of hydroxyl (OH) groups bound to the cellulose struc-
ture. These results indicate that the cellulose component was not
removed during the chemical treatment carried out on the rice husk
fibres and is the common material found in all samples.
A shoulder was observed around 1700 cm−1 in the spectrum
corresponding to the untreated rice husk. It is ascribed to the acetyl
and ester groups in hemicellulose or carboxylic acid groups in the
ferulic and p-coumeric components of lignin. The existence of this
shoulder was also reported by Alemdar and Sain (2008a) and Sun
et al. (2005) for untreated wheat straw. The peak disappears upon
chemical treatment of the rice husk showing the removal of non-
cellulosic materials.
lignin, which are amorphous in nature. According to Zhang and
Lynd (2004), cellulose has a crystalline structure due to hydrogen
bonding interactions and Van der Waals forces between adjacent
molecules. X-ray diffraction (XRD) analysis was completed to eval-
uate the crystallinity of the rice husk fibres after different chemical
treatment stages.
Chemical treatment performed on natural fibres can affect the
crystallinity of cellulose. For example, dilute acid has no effect on
the crystalline domains, but destroys the amorphous region of the
fibre (Fengel and Wegener, 1984). On the other hand, Mwaikambo
and Ansell (2006) also reported that the alkali treatment can be
performed onto the plant fibres to increase the stiffness of fibre
as the impurities present in the fibres can be removed during this
treatment. Therefore the crystallinity of chemically treated fibres
can be determined and compared to untreated fibres to access the
effectiveness of the chemical treatment.

Table 2
Peak absorption of rice husk at different stages of treatment.

Rice husk Involved groups

Untreated Alkali treated Bleached Acid hydrolysed

3430 3435 3411 3401 Strain O H

2929 2914 2914 2897 Strain C H
1643 1638 1639 1649 O H bond of water absorption
1077 1053 1053 1060 C O stretching and C H vibration in cellulose
899 897 898 898 C O stretching and C H vibration in cellulose
98 N. Johar et al. / Industrial Crops and Products 37 (2012) 93–99
Fig. 7. (a) TGA and (b) DTG curves of raw, alkali treated, bleached, and acid hydrolysed rice husk.
Fig. 6 shows the diffraction patterns obtained for (a) untreated,
(b) alkali treated, (c) bleached, and (d) acid hydrolysed rice husks.
They are typical of cellulose I with three well-defined crystalline
peaks around 2 = 16◦ , 22◦ , and 35◦ and no doublet at 2 = 22◦
(Klemm et al., 2005). These peaks become more defined upon
chemical treatment as expected.
The crystallinity index was determined for the various sam-
ples and the results are summarized in Table 3. A continuous
increase of the CrI value was observed upon the successive chemi-
cal treatments. The highest value (59.0%) corresponds to cellulose
nanocrystals, which also displayed the strongest and sharpest peak
at 2 = 22◦ .
The increased crystallinity following rice husk treatments com-
pared to the raw material was ascribed to the progressive removal
of amorphous non-cellulosic materials. The subsequent increase
of the CrI value upon acid hydrolysis of purified cellulose rice
husk fibres is indicative of the dissolution of amorphous cellu-
losic domains. During the hydrolysis process, hydronium ions can
penetrate the more accessible amorphous regions of cellulose and
allow the hydrolytic cleavage of glycosidic bonds, which eventually
releases individual crystallites (Lima and Borsali, 2004). In addi-
tion, during the preparation of cellulose nanocrystals the growth
and realignment of monocrystals may occur in parallel and thus
can improve the cellulose crystallinity (Li et al., 2009a,b). This phe-
nomenon could explain the narrowing of the diffraction peaks.
This increase in the cellulose fibres crystallinity was also
expected to increase their stiffness and rigidity, and therefore
strength. Thus, it was assumed that the potential mechanical
properties and reinforcing capability of treated fibres increased
(Bhatnagar and Sain, 2005; Rong et al., 2001).
3.5. Thermal stability
Thermogravimetric analysis (TGA) was measured to access the
thermal stability of both untreated and chemically treated rice husk
fibres. Fig. 7 shows the TGA and derivative thermogravimetry DTG
curves obtained for untreated, alkali treated, bleached, and acid-
hydrolysed rice husk. They correspond to the weight loss of the
sample upon continuous heating to 900 ◦ C.
Table 3
Crystallinity index (CrI) of rice husks fibres at different stages of treatment.
Sample CrI (%)
Untreated rice husk 46.8
Alkali treated rice husk 50.2
Bleached rice husk 56.5
Cellulose nanocrystals 59.0
An initial weight loss of the fibres occurs below 100 ◦ C regardless
of their treatment. The initial change is ascribed to the vaporisation
of water because of the hydrophilic character of the lignocellu-
lose fibres. The weight reduction was dependent on the initial
moisture content of the analysed fibre. At higher temperatures, a
sharper weight drop is observed. Compared to untreated and alkali
treated fibres, it was observed that the bleaching treatment induces
an increase in the materials thermal stability. This is due to the
presence of hemicellulose, lignin, and pectin in the chemical com-
position of the untreated and alkali treated rice husk fibres. These
components have a lower decomposition temperature compared
to cellulose (Moran et al., 2008) and their progressive removal
improves the thermal stability of the rice husk. The lower ther-
mal stability of alkali treated compared to the bleached fibres is
attributed to the partial elimination of non-cellulosic material.
As can be seen in Fig. 7, the amounts of residue at tempera-
ture around 400–700 ◦ C in raw rice husks fibre were remarkably
high which is at the range of 30–40%. The similar thermogram
patterns have also been reported on raw rice husk fibres (Ndazi
et al., 2007; Mansaray and Ghaly, 1998) which indicates higher
residue amount of rice husk fibres. The weight fraction of mate-
rial that still existing after heating above 400 ◦ C is representative
of the carbon content in the fibres, as reported by Hornsby et al.
(1997a). The increased residue amount at high temperature, or the
char fraction, for raw rice husk compared to chemically treated
fibres is due to the presence of ash as well as lignin (Ashori et al.,
2006; Fahma et al., 2011). The high silica content of the rice husk
is also a factor that contributes to the high char content for raw
fibres.
When rice husk fibre was burnt, the rice husk ash is gener-
ated. On burning, the cellulose and lignin were decomposed and
removed leaving behind silica ash. The residual ash for rice husk
fibres can be generally said as silica ash because it usually con-
tains almost over 95% of amorphous silica (Della et al., 2002). In
this research, the amorphous form of silica content was obtained
as reported by Yeoh et al. (1979) that rice husk ash can remain in the
amorphous form at combustion temperatures of up to 900 ◦ C. Based
on this, the silica ash content can be determined as mentioned in
characterization part of silica ash composition.
Alkali treated rice husk fibres showed a slightly decreased resid-
ual weight compared to raw rice husk fibres as most of the lignin
still obtained in the fibres. The acid hydrolysis treatment of the rice
husk fibres induces a significant decrease of the thermal stability
of the material. This is ascribed to the surface sulphation result-
ing from the sulphuric acid treatment. Moreover, this treatment
induces an increase in the char fraction compared to the bleached
fibres, which is due to the introduction of sulphated groups acting
as a flame retardant (Roman and Winter, 2004).
 N. Johar et al. / Industrial Crops and Products 37 (2012) 93–99
The determination of the thermal properties and thermal sta-
bility of the natural fibres is important for their potential use in
the processing of biocomposites. Indeed, most thermoplastic poly-
mers are processed at temperatures ranging between 150 and
250 ◦ C.
4. Conclusion
The chemical composition of the rice husk was determined
and its cellulose content was found to be ca. 31%. Purification
of cellulose was performed using classical chemical treatments
involving alkali and bleaching treatments. It was observed that the
former treatment was efficient in removing hemicellulose while
the latter fully removed lignin. Chemical composition determina-
tion, morphological investigation, infrared spectroscopy, and X-ray
diffraction analyses confirmed the removal of non-cellulosic mate-
rials. The chemical treatments induced an increase of the cellulose
content from 31% to 96%, and of the crystallinity index from 46.8%
to 59.0%, while the diameter decreased from 170 to 7 ␮m. The cel-
lulose fibres exhibit enhanced thermal stability but contrary with
the cellulose nanocrystals which showed lower thermal stability.
Cellulose nanocrystals were successfully extracted from the puri-
fied rice husk using an acid hydrolysis treatment. Their diameter
ranged from 10 to 15 nm.
Acknowledgements
The research work reported in this paper was funded by the
Ministry of Science, Technology and Innovation, Malaysia and Uni-
versiti Kebangsaan Malaysia (UKM). The French Embassy in Kuala
Lumpur is also acknowledged for financial support (French Scholars
in Malaysia).
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