Composites: Part A 41 (2010) 154160

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Composites: Part A
journal homepage: www.elsevier.com/locate/compositesa

Chemical, morphological, and mechanical analysis of rice husk/post-consumer

polyethylene composites
Silvia Luciana Fvaro a, Milena Savioli Lopes a, Alberto Gonalves Vieira de Carvalho Neto a,
Ricardo Rogrio de Santana b, Eduardo Radovanovic a,*
a
Universidade Estadual de Maring, Departamento de Qumica, Grupo de Materiais Polimricos e Compsitos, Av. Colombo 5790, 87020-900 Maring, Paran, Brazil
b
Universidade Estadual de Maring, Engenharia Mecnica, Departamento de Engenharia Qumica, Av. Colombo 5790, 87020-900 Maring, Paran, Brazil

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

Article history: Composites were obtained from post-consumer high-density polyethylene (PE) reinforced with different
Received 13 November 2008 concentrations of rice husk. PE and rice husk were chemically modied to improve their compatibility in
Received in revised form 12 August 2009 composite preparation. Rice husk was mercerized with a NaOH solution and acetylated. The chemically
Accepted 28 September 2009
modied bers were characterized by FTIR and 13C NMR spectroscopy. The composites were prepared by
extrusion of modied and unmodied materials containing either 5 or 10 wt.% bers. The morphology of
the obtained materials was analyzed by SEM. The chemical modication of the ber surface was found to
Keywords:
improve its adhesion with matrix. Flexural and impact tests demonstrated that PE/rice husk composites
A. Polymermatrix composites
B. Fiber/matrix bond
present improved mechanical performance comparatively to the pure polymer matrix, on the contrary no
B. Mechanical properties benet is observed in the tensile strength over the pure PE.
E. Surface treatments 2009 Elsevier Ltd. All rights reserved.

1. Introduction use of rice husk as a thermoplastic composite reinforcement [13

In the last few years, recycled materials developed from post-
consumer polymers have gained increasing attention. Most poly-
mer wastes consist of polyolens, such as polyethylene (PE) and
polypropylene (PP) [1]. The development of new technologies to
prepare composites from post-consumer polymers as matrixes
and natural ber as reinforcement phases and the better under-
standing of their chemical, physical, and mechanical interactions
will increase their aggregated value and application in the produc-
tion of consumer goods and consequently reduce their environ-
mental impact as waste materials [2]. Natural bers have been
increasingly used in the production of composites in the last years
because of their inherent advantages, such as low cost, renewabil-
ity, biodegradability, abundance, and high specic strength. [35].
Natural bers, such as wood, jute, kenaf, hemp, sisal, pineapple,
rice husk, etc., have been successfully used to improve the mechan-
ical properties of plastic composites [610].
In the last years rice husk bers have been studied due to their
large availability. In fact, as consequence of the large production of
rice, approximately 600 million tons/year, there is a large amount
of rice husk waste (about 20 wt.%) [5]. Many studies have investi-
gated possible uses for all this husk, such as a fuel and the fuel res-
idue as activated carbon in cement and concrete production
[11,12]. Recently, a small number of studies have reported the
* Corresponding author. Tel.: +55 44 3261 3653; fax: +55 44 3261 4125.
E-mail address: eradovanovic@uem.br (E. Radovanovic).
15]. The majority of these works developed plastics with distinct
mechanical properties. However, similarly to any other hydrophilic
lignocellulosic ber used as hydrophobic plastic composite rein-
forcement, the relatively poor compatibility between the counter-
parts is a drawback. Thus, coupling agents are generally used to
modify the bermatrix interface and thereby enhance the ber
matrix adhesion [3,16].
This work reports on the mechanical and morphological proper-
ties of composites prepared with modied and unmodied post-
consumer high-density polyethylene (PE) matrixes and modied
and unmodied rice husk bers as the reinforcement phase. The
obtained composites were characterized by Fourier transform
infrared spectroscopy (FTIR), Fourier transform infrared spectros-
copy with horizontal attenuated total reectance (FTIR-HATR),
13
C Magic Angle Spinning Nuclear Magnetic Resonance (13C MAS
NMR), water contact angle, energy dispersive X-ray spectroscopy
in scanning electron microscopy (EDSSEM), exural tests, tensile
tests, and IZOD impact tests.
2. Experimental set-up
2.1. Composite preparation
2.1.1. Recycled polyethylene surface modication
Recycled high-density polyethylene was obtained from Plaspet
Polymer Recycling Industry Maring, PR, Brazil. Polymer samples
were previously hand-separated, washed with water, and cut into

1359-835X/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesa.2009.09.021
 S.L. Fvaro et al. / Composites: Part A 41 (2010) 154160 155

1.5-mm diameter pellets on site. The polyethylene pellets were Table 1

washed again and dried at 60 C for 8 h before the surface modi- Rice husk particle size distribution.

cation in laboratory. Surface modication conditions can be found Size (mm) Grit number (ASTM.E 11.79) Quantity (%)
elsewhere [17]: the pellets were immersed in a KMnO4 >1.180 16 23.50
(0.25 mol L1) solution in HCl (0.50 molL1) acidic medium at >0.850 and <1.180 20 15.74
25 C for 8 h. Hence, the oxidized polyethylene will be labeled PEox >0.710 and <0.850 25 10.59
and the untreated polymer, PE. >0.600 and <0.710 30 20.07
>0.425 and <0.600 40 13.44
>0.300 and <0.425 50 11.53
2.1.2. Rice husk surface modication <0.300 Remaining portion 3.33
Rice husk was obtained from a rice mill in Maring, PR, Brazil.
Rice husk was ground with a knife mill and size classied by a
mechanical separation bolter system. The rice husk particles were
trum obtained by recording 128 co-added scans of an empty HATR
washed with distilled water at 80 C for 1 h and dried in oven at
cell.
100 C for 5 h before composite preparation. Rice husk was mercer-
ized by immersion in 10% sodium hydroxide (NaOH) water solu-
2.2.3. 13C Magic Angle Spinning Nuclear Magnetic Resonance
tion at room temperature for 3 h. After mercerization, the husk
spectroscopy (13C MAS NMR)
particles were rinsed with water to remove the excess NaOH and 13
C MAS NMR spectra of rice husk particles were recorded in a
dried in oven at 100 C for 3 h. Next, the husk particles were acet-
Varian Mercury Plus BB 300 MHz spectrometer operating at
ylated by immersion in pure acetic acid at room temperature for
75.34 MHz for 13C with contact time of 1 ms, recycle time of 20 s,
1 h, followed by immersion in acetic anhydride acidied with
and 128 scans for signal accumulation.
0.1% sulfuric acid for 5 min at room temperature. Finally, the sam-
ples were rinsed with water until pH 7.0 was reached and dried
2.2.4. X-ray diffractometry
at 100 C for 5 h. The unmodied rice husk was labeled RH; the
X-ray diffractograms of the rice husk particles were obtained in
mercerized rice husk particles RHm, and the acetylated ones RHac.
an XRD-6000 Shimadzu diffractometer with 2h varying between
10 and 40 at 5/min.
2.1.3. Extrusion
The modied and unmodied rice husk particles were incorpo-
2.2.5. Scanning electron microscopy (SEM)
rated into PE (and PEox) at 5 and 10 wt.%. The components were
The PE, the rice husk particles and the composites were ob-
mixed in a lab-made monoscrew extruder with a 25-mm/70-cm
served using a Shimadzu SS 550 Superscan scanning electron
(diameter/length) screw L/D = 28. The cylinder temperature prole
microscope. The samples were gold-sputtered and observed under
was adjusted to 110, 155, and 185 C for the three heating zones
different magnications. The materials were analyzed by energy
and an average rotation of 40 rpm was used for all formulations.
dispersive X-ray (EDS) spectrometry. The composite was fractured
The extruded material was water-cooled down to room
after immersion in liquid nitrogen for 10 min and the fracture sur-
temperature.
face was analyzed.
2.1.4. Injection molding
2.2.6. Tensile testing
The mechanical test samples were obtained by injection mold-
The composite tensile strength and modulus assays were per-
ing in a Pavan Zanet 100 t injection machine with a 42-mm diam-
formed according to the ASTM D-638 test method. The samples
eter screw at 180 C and injection pressure of 35 bar. The prepared
were submitted to tensile tests in an EMIC DL 2000 machine at a
composites were labeled as in the example: PEox/RHac10, where
constant cross-speed of 50 mm/min. Tensile properties were deter-
PEox represents the oxidized polyethylene matrix with 10 wt.% of
mined for eight samples of each composition.
acetylated rice husk particles as reinforcement.

2.2.7. Flexural testing

2.2. Characterization techniques on polymers, rice husk bers, and
The composite exural strength and modulus were determined
composites
using the three-point bending test method following the ASTM
2.2.1. Water contact angle
The water contact angle by sessile drop method was measured
on the PE and PEox surfaces, with contact angle meter Cam Micro,
Tantec. Each contact angle value is an average of ve different
measurements in different parts of two samples obtained under
the same experimental conditions.

2.2.2. Infrared spectroscopy (FTIR and FTIR-HATR)

The IR spectra of the polymer lm were recorded in a FTIR
Pike Miracle ATR, Digilab Scimitar Series using Horizontal Attenu-
ated Totally Reectance Fourier Transformed Infrared spectroscopy
technique (FTIR-HATR) and the spectra of rice husk in KBr pellets
were recorded in a FTIR-BOMEM-100 spectrometer. The FTIR-
HATR technique works by passing a radiation beam through a crys-
tal made of a highly refractive infrared-transmitting material. The
beam is totally internally reected at the surface. The sample is
placed in contact with the totally reecting surface of the ATR crys-
tal and the evanescent wave is attenuated in regions of the infrared
spectrum where the sample absorbs energy. Each spectrum
represents 128 co-added scans rationed against a reference spec- Fig. 1. SEM micrographs of two rice husk particles.
156 S.L. Fvaro et al. / Composites: Part A 41 (2010) 154160

the particles were between 0.300 and 1.180 mm in size. The aver-
age size of an intact rice husk was 8 mm.
The mercerization process removes natural fats, waxes, lignin
and hemicelluloses from the cellulose ber surface, thus revealing
chemically reactive functional groups like OH. The removal of the
counts (U.A.)

surface impurities from the cellulose bers also improves the sur-
face roughness on both bers and particles, thus opening more hy-
droxyl groups and other reactive functional groups on the surface.
A NaOH may also react with all hydroxyl groups present in the back-
bone of the original cellulose [18], Eq. (1). Furthermore, the mer-
C K cerizing process can also improve the acetylation of the cellulose,
Au M
O K according to the chemical reaction proposed in Eq. (2).
Si K cellulose-OH NaOH ! cellulose-ONa H2 O impurities 1
B

0 1 2 3 4 5
X-ray energy (keV)
Fig. 2. EDX spectra of rice husk: outside (A) and inside (B) regions.
D-790-00 A test method. A 63 mm span was used in a 5 kN load
cell. The load was placed midway between the supports. The cross-
head speed applied was 20 mm/min. Flexural properties were
determined for eight samples of each composition.
2.2.8. Izod impact testing
The notched Izod impact strength tests were performed accord-
ing to ASTM D 256-00 A at room temperature in an EMIC-Al testing
machine using a 5.4 J hammer. The values obtained are averaged
measurements of ve samples.
3. Results and discussion
Table 1 presents the percentage size distribution of the rice
husk particles used in this work after grinding in a knife mill and
separating by mechanical bolter system. Seventy-three percent of
CH3 COOH=H
6 cellulose-OHCH3 CO2 O ! cellulose-OCOCH3 CH3 COOH
2
Fig. 1 shows a scanning electron micrograph of two rice husk
particles. They present different outside and inside region mor-
phologies. The outside region is formed by aligned and symmetri-
cal bumps composed mainly of silica onto the cellulose, while the
inside region presents a smooth cellulose surface. Fig. 2 presents
the energy dispersive spectrograms (EDS) of both the rice husk
particle regions. A silica layer predominates on the outside and
provides a protective barrier to the rice kernel against microorgan-
ism attack [18]. Fig. 3 shows micrographs of both regions outside
(Fig. 3A and B) and inside (Fig. 3C and D) of the rice husk particles,
before (Fig. 3A and C) and after mercerization (Fig. 3B and D). The
small particles on both surfaces (inside and outside) of the rice
husk were removed by mercerization. No other effect was ob-
served on the outside. However, on the inside, the protective layer
composed of waxes, hemicelluloses, and lignin was removed,
exposing the cellulose microbers.
The FTIR spectra of RH (A), RHm (B), and RHac (C) are shown in
Fig. 4. Compared with the curve of unmodied rice husk particles
(A), the spectra of mercerized (B) and acetylated cellulose (C) have

Fig. 3. Rice husk SEM micrographs: (A) unmodied outside region, (B) mercerized outside region, (C) unmodied inside region, and (D) mercerized inside region.
 S.L. Fvaro et al. / Composites: Part A 41 (2010) 154160 157

the C-4 signal at 89 ppm of crystalline cellulose decreased compar-

A atively to the signal at 84 ppm, as shown by the comparison of
spectrum A to spectra B and C. The C-6 signal in A shifted from
1735 64 ppm to 62 ppm in B and C, which may indicate that the crystal-
B line structure of cellulose was partially disrupted by the break of a-
Transmitance (A.U.)

cellulose hydrogen bonds by the mercerization and acetylation

C reactions [22]. The degree of substitution (DS) of 0.60 (substitution
1745
1235
2250 2000 1750 1500
-1
wavelength cm
Fig. 4. Rice husk FTIR-HATR spectra: unmodied (A), mercerized (B), and acetylated
(C).
important differences. After mercerization, the characteristic RH
peak at 1735 cm1, attributed to the lignin carbonyl groups, disap-
peared. After acetylation, a new acyl group was added to cellulose,
as indicated in curve C, with the expected acetyl group vibration at
1745 cm1 (C@O). The peak at 1235 cm1, characteristic of CO
stretching vibrations, was also intensied in the RHac spectrum
[19,20].
The mercerization and acetylation of rice husk cellulose were
also studied by solid-state 13C MAS NMR spectroscopy. The spectra
of RH (A), RHm (B), and RHac (C) samples are shown in Fig. 5. In the
spectrum A, all noticeable signals of the carbohydrate moiety car-
bon atoms occur between 50 and 110 ppm. The signal at 21 ppm in
RH spectrum is assigned to CH3 carbons of the hemicellulose acetyl
group. This signal disappears in RHm spectrum. The signals at
105 ppm (C-1), 89 ppm (C-4 of crystalline cellulose), 84 ppm (C-4
of amorphous cellulose), 75 ppm (C-5), 73 ppm (C-2 and C-3),
and 64 ppm (C-6) have all been reported before [21]. However,
of 20% in the three OH groups of each cellulose monomer) of RHac
was obtained by deconvolution of the area of the peak at 21 ppm in
spectrum C attributed to CH3 of the acetyl group generated by the
acetylation reaction and related to the deconvoluted area of the
peak at 105 ppm (C-1).
The X-ray diffractograms of RH (A) and modied rice husk par-
ticles (B and C) are displayed in the Fig. 6. In contrast with the NMR
results, which show a decrease in the degree of crystallinity of cel-
1250 1000 750 lulose, the sharper diffraction peaks of B and C comparatively to
those of A, reveals an increase in crystal size. This result can be ex-
plained by the preferential acetylation of small and imperfect cel-
lulose crystals. The reagent enters the crystalline region of the
small cellulose crystals and promotes the formation of amorphous
structures, which did not occur with the large cellulose crystals.
Fig. 7 shows the FTIR HATR spectra of PE and PEox samples. The
absorption peaks at 2916, 2848, 1463, and 719 cm1 in Fig. 7A are
attributed to methylene asymmetric stretch vibration, methylene
symmetric stretch vibration, methylene asymmetric changing an-
gle vibration, and methylene swing in plane vibration, respectively.
The main changes involving oxidized (spectrum B) and unmodied
polymers (spectrum A) are assigned to different C@O (between
1730 and 1650 cm1) and CO groups (between 1100 and
1000 cm1) generated on the polyethylene surface by the
KMnO4/HCl solution treatment.
The increase in the absorption peak intensities at 1645 and
909 cm1 in the FTIR spectrum indicates the formation of unsatu-
rated vinyl groups, as previously described by other authors
[23,24]. The sessile drop method is an optical contact angle tech-
nique used to estimate wetting properties of a localized region
on a solid surface. In this method, the angle between the baseline
of the drop and the tangent at the drop boundary is measured. The

6
OH CH2 OH OH

HO O O
4 5
OH OH OH
O 1 OH
O O
3 2
CH2OH OH CH2 OH
n
C

200 180 160 140 120 100 80 60 40 20 0

ppm
13
Fig. 5. Rice husk solid-state C MAS NMR spectra: unmodied (A), mercerized (B), acetylated (C) and cellulose molecular structure.
158 S.L. Fvaro et al. / Composites: Part A 41 (2010) 154160

650
Tensile Modulus 21
Tensile Strength
600 20

Tensile Strength (MPa)

Tensile Modulus (GPa)
550 19

C 18
Counts (A. U.)

500
17

450
16
B
400 15
1
0 0

--
PE

PEox

PE/RH5

PEox/RH5

PE/RHac5

PEox/RHac5

PE/RH10

PEox/RH10

PE/RHac10

PEox/RHac10
A

10 20 30 40
2 theta (degree)
Composites
Fig. 6. Rice husk X-ray diffractograms: unmodied (A), mercerized (B), and
acetylated (C). Fig. 8. Tensile properties of PE and PE/rice husk composites.

25
Flexural Strength
Flexural Modulus 24
1200 23
A 22
Flexural Modulus (GPa)

21

Flexural Strength (MPa)

20
19
Transmitance (u.a)

1000
18
B
17

800

0 0

--
PE

PE/RH5

PE/RHac5

PE/RH10

PE/RHac10
PEox

PEox/RH5

PEox/RHac5

PEox/RH10

PEox/RHac10
3500 3000 2500 2000 1500 1000
-1
Wavelength (cm )
Composites
Fig. 7. FTIR-HATR Spectra of PE (A) and PEox (B).
Fig. 9. Flexural properties of PE and PE/rice husk composites.

oxidation decreased the polyethylene surface water contact angle

in the sessile drop measurements, varying from 92.4 in PE to
60.0 in PEox, which decreased the polymer surface hydrophobic-
60
ity, but did not change the bulk characteristics [17].
IZOD Impact Strength (J/m)

The tensile properties of PE and PEox composites with 5 wt.%

and 10 wt.% of either RH or RHac are displayed in the Fig. 8. A
reduction in tensile strength for all the composite samples was ob- 50
served, however a gradual decrease in the tensile strength of PE/
rice husk composites was observed for the modied matrix and
the modied reinforced phase, while the composites with both
modied PEox and RHac presented the lowest tensile strength val- 40
ues. The decrease in the composite tensile strength values can be
explained by dewetting effect. The stress in the ber/matrix
boundary region is concentrated around the reinforcement parti-
cle. Consequently, the particlematrix interaction becomes weaker
0
probably leading to debonding at the boundary region. Moreover,
PE

PE/RH5

PE/RHac5

PE/RH10

PE/RHac10
PEox

PEox/RH5

PEox/RHac5

PEox/RH10

PEox/RHac10

--

the addition of rice husk to the polymer matrix increases the ten-
sile modulus signicantly from almost 450 GPa for PE to approxi-
mately 520 GPa for PE/RH10, PE/RHac10, and PEox/RHac10, an
increase of 16%. Composites PEox/RHac5 and PEox/RHac10 pre-
Composites
sented the lowest tensile modulus values comparatively to those
of the other composites with the same amount of reinforcement, Fig. 10. Izod impact properties of PE and PE/rice husk composites.
 S.L. Fvaro et al. / Composites: Part A 41 (2010) 154160
probably because both materials were modied in opposite ways;
the polymer surface became more hydrophilic and the rice husk
became more hydrophobic, probably decreasing the compatibility.
The exural properties of PE, PEox and four different composites
reinforced with either 5 or 10 wt.% rice husk are shown in Fig. 9.
The exural strength of PE/RH5, PEox/RH5, PE/RHac5, PE/RH10,
PEox/RH10, and PE/RHac10, compared with the exural strength
results of PE and PEox, were improved by approximately 10% and
15% in composites with 5 wt.% and 10 wt.% rice husk reinforce-
ment, respectively. As already observed in the tensile measure-
ments, the exural strength values of PEox/RHac5 and PEox/
RHac10 decreased when compared with those of composites with
the same quantity of reinforcement.
Izod impact tests were performed on notched samples at room
temperature. Fig. 10 shows the Izod impact strengths of PE, PEox
and rice husk polyethylene composites obtained with two different
compositions of rice husk. Relative to the pure PE Izod impact
strength, the values of acetylated rice husk composites (PE/RHac5
and PE/RHac10) are higher, 18% and 35%, respectively, and those
of unmodied material (PE/RH5 and PE/RH10) are lower. These re-
sults suggest that the presence of rice husk particles embedded in
the matrix can act to prevent the propagation of cracks generated
Fig. 11. SEM micrographs of composites: PE/RH10 (A), PEox/RH10 (B), PE/RHac10 (C), PEox/RHac10 (D) and (E).
159
during the impact tests. The Izod impact strengths of the PEox and
the other composites are similar to the values obtained for PE.
Overall, the oxidation of the PE surface had little effect on the com-
posite impact strength, whereas the acetylation of rice husk had a
composite toughening effect.
Fig. 11AE show the photomicrographs of the polyethylene
rice husk composites with 10 wt.% bers. The morphology of the
composite samples fractured in liquid nitrogen was characterized
by scanning electron microscopy (SEM). Fig. 11D and E display
the photomicrographs of the PEox/RHac10 composite. The images
show two opposite situations: a signicant interfacial interaction
between the ber and the matrix, which prevents the ber pullout
at the fracture (Fig. 11D), and ber pullout between nonadhered
phases (Fig. 11E). The interface adhesion allows stress transfer
from the matrix to the ber and accounts for the superior tensile
and exural modulus of the composites. However, the other micro-
graphs (not shown) show that phase nonadherance predominates
in PEox/RHac10, which explains its poor mechanical properties.
Nonadherance probably predominates due to the increase in the
hydrophilic character of the polymer surface, in opposition to the
increased hydrophobic character of the rice husk ber surface.
The high ber/polymer adhesion presented in Fig. 11D probably
160 S.L. Fvaro et al. / Composites: Part A 41 (2010) 154160
occurred in an unmodied polymer region, such as the inner part
of the polymer lm. This fact is in agreement with the micrograph
of the PE/RHac10 composite (Fig. 11C). In this micrograph, it is pos-
sible to observe a high adhesion between the inside of the modied
rice husk bers and the unmodied matrix. In the micrographs
presented in Fig. 11A and B of composites PE/RH10 and PEox/
RH10, respectively, it is possible to observe the nonexistence of
phase adherence. The presence of phase adherence between bers
and matrix (Fig. 11C) can act to prevent the propagation of the
cracks generated during the impact tests, meanwhile the not ad-
hered regions (Fig. 11A) probably contribute to increase the crack
propagation.
4. Conclusions
Unmodied and oxidized post-consumer polyethylene compos-
ites reinforced with unmodied and acetylated rice husk ber were
fabricated by extrusion and injection molding. The acetylated rice
husk bers were characterized by FTIR, Solid-state 13C MAS NMR,
EDS-SEM, SEM, and XRD. The bers are composed of an outside sil-
ica layer and an inside cellulose part. The latter was changed by
acetylation with a degree of substitution (DS) of 0.60. The mechan-
ical, chemical, and morphological aspects of different composite
compositions (polymer/ber) were studied. The incorporation of
rice husk bers into the PE matrix increased the tensile and ex-
ural modulus of the composite prepared with 10 wt.% of acetylated
rice husk ber and unmodied polyethylene matrix appreciably.
This composite presented an increase of 35% in Izod impact
strength comparatively to that of the pure matrix. SEM photomi-
crographs demonstrated the interfacial interaction between acety-
lated rice husk bers and unmodied PE and the better phase
compatibility afforded by acetylation. The modication of PE did
not improve its interaction with modied and unmodied bers,
which explains the poor mechanical properties of its composites.
Acknowledgements
The authors gratefully acknowledge funding support for this
work from CNPq and Fundao Araucria.
S. L. Fvaro also thanks CAPES (Brazil) for her master degree
scholarship.
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