Int. j. eng. sci., Vol(4), No (4), April, 2015. pp.

57-64

TI Journals

ISSN:

International Journal of Engineering Sciences

2306-6474

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Copyright 2015. All rights reserved for TI Journals.

Composites from Rice Straw and High Density Polyethylene:

Thermal and Mechanical Properties
Mohamed H. El Nemr *
Sidi Kereir Petrochemicals Company, Alexandria, Egypt

Yehia M.S. El Shazly

Alexandria University, Faculty of Engineering, Chemical Engineering Department, Alexandria, Egypt

Ashraf A. Mubarak
Alexandria University, Faculty of Engineering, Chemical Engineering Department, Alexandria, Egypt

Mohamed H. Zaki
Alexandria University, Faculty of Engineering, Chemical Engineering Department, Alexandria, Egypt
*Corresponding author: elnemrsidpec@yahoo.com

Keywords

Abstract

Thermo gravimetric analysis

Differential scanning calorimetry
High density polyethylene
Coupling agent
Composites

The use of rice straw along with high density polyethylene in the production of wood plastic composite is
investigated. PE wax, a by-product in the Sidi Kreir Petrochemicals Company-Egypt, is incorporated in the
matrix to act as a coupling agent or compatibilizer between the matrix and the straw. The polar C=O group in
the wax, confirmed by the FTIR analysis, is expected to bind the two phases. The mechanical properties of the
composite (tensile properties) for three different rice straw mass fractions have been examined. Preliminary
studies showed that the addition of this wax has improved the properties of the composite.
Thermal properties of rice straw (RS) filled high density polyethylene (HDPE) composites were measured
using the differential scanning calorimetry and thermo gravimetric analysis. Presence of RS in thermoplastic
matrix reduced the degradation temperature of the composites. Two main decomposition peaks were observed;
one for RS and one for HDPE. The HDPE sample exhibited higher crystallinity (XC) compared with the all
RS/HDPE composite formulations. The XC increased with increasing the RS content in all composite
formulations. The addition of PE wax increases the XC. This is due to the bonding between the RS and HDPE.
The addition of PE wax (coupling agents) improved the mechanical properties of the composites.

1.

Introduction

Fiber reinforced composites are materials that comprise strong load carrying material (known as reinforcement) imbedded in weaker material
(known as matrix). Reinforcement provides strength and rigidity, helping to support structural load. The matrix, or binder (organic or inorganic)
maintains the position and orientation of the reinforcement. Significantly, constituents of the composites retain their individual, physical and
chemical properties; yet together they produce a combination of qualities which individual constituents would be incapable of producing alone
[1]. An example wood is natural three-dimensional polymeric composite and consists primarily of cellulose, hemicellulose and lignin [2].
In addition, rice straw is an original and natural composite. Historical examples of composites are abundant in literature. Significant examples
include the use of reinforcing mud walls in houses with bamboo shoots, glued laminated wood by Egyptians and laminated metals in the forging
of swords. In the 20th century, modern composites were used in 1930s. Boats and aircrafts were built out of glass fiber composites, commonly
called fiber glass. Since the 1970s, the applications of composites have widely increased due to development of new fibers such as carbon, boron
and aramids, and new composite systems with matrices made of metal and ceramics.
Cellulose fiber is little used as filler in thermoplastics compared to the inorganic fillers, such as talc, mica and glass fiber, despite its offers many
advantages such as lower density, higher specific strength and modulus, renewable nature, lower fiber breakage during mixing and lower cost
[3,4]. When cellulosic fiber is compounded with thermoplastic polymers, the main problem encountered is the poor interfacial adhesion between
the hydrophobic polymer and hydrophilic filler. Coupling agents have been added to improve the dispersion, adhesion and compatibility between
the hydrophilic cellulose and hydrophobic matrix. These agents improved the interface by interacting with both the fiber and its matrix, to form a
stronger link between them [5]. Maleated polypropylene has received considerable attention as a coupling agent because of its effectiveness in
improving the mechanical properties of wood fiber-polypropylene composites [6].
A review of the cited literature showed that the main natural fibers used to reinforce thermoplastics mainly include wood, cotton, flax, hemp,
jute, sisal, and oil palm fibers [7]. The rice straw fiber is important reinforcing filler for thermoplastic composite because of its cellulosic
characteristics. The whole rice straw fiber used is composed of leaf sheath, straw leaf blade, straw stem and knot [8]. In Egypt rice cultivation in
the river Nile Delta produces large quantities of rice straw as an agriculture residue. The analysis of Egyptian rice straw is: cellulose (41 47%),
hemicelluloses (33%), lignin (8-19), residual ash (8-38%), [9]. The disposal of agriculture residue represents a serious environmental problems.
Due to its low nutrition value for cattle's and its bulk size, farmers tend to dispose of the rice straw by burning which results in the emission of
large volume of smokes. This causes a significant contribution to the air pollution known as the Black Cloud [9].
The use of compatibilizers in natural fiber reinforced polymer composites is to improve poor interface adhesion between the fiber and polyolefin
matrix. Among numerous compatibilizers are maleic anhydride grafted polyethylene and polypropylene (MAPE and MAPP). They are
considered to be the most effective interphase modifiers for polyolefin / natural fiber composite. Their success depends on the polar interaction
and covalent link between anhydride carbonyl and hydroxyl groups of the fiber surfaces [1013]. As well as their good compatibility with matrix
[1418].The improvements with the coupling agent are believed to be due to the formation of ester bonds between the anhydride carbonyl group
of MAPE and hydroxyl groups of the wood fibers [19, 20].
In this work, the wood plastic composites were prepared from a mixture of (HDPE) and rice straw particles (RS). The addition of PE wax as a
compatibilizer or coupling agent between the hydrophilic rice straw particles and the hydrophobic PE matrix was also studied. The IR spectrum
of PE wax produced as a by product from SIDPEC company, showed the presence of the C=O in the structure of the PE wax, which indicated

Mohamed H. El Nemr *, Yehia M.S. El Shazly, Ashraf A. Mubarak, Mohamed H. Zaki

58

International Journal of Engineering Sciences Vol(4), No (4), April, 2015.

it might play the role of the coupling agent by forming an ester group similar to the MAPE with the hydroxyl group of the rice straw. The
composite was compounded in a two roll-mill, and then compressed to form sheet or plate in a mechanical hot press, and tested for thermal
analysis and tensile properties.

2.

Materials and methods

2.1. Materials
High density polyethylene (HDPE) was obtained from Sidi Kerir Petrochemical Company (SIDPEC), with density 952 kg/m3, melt index 26
g/10min and melting temperature 126oC as indicated by the manufacture. PE wax was obtained also from SIDPEC with density 900 kg/m3 .The
structure of the PE wax has been characterized by infrared analysis which is illustrated in (Fig. 1), shows a peak at 720 cm-1 which is
characteristic of the =C-H group, a peak at 1465 cm-1 which is characteristic of the alkyl CH, a peak at 2920 cm-1, which is characteristic of the
alkane C-H, and a peak at 1638 cm-1, which is characteristic of the C=O group [21]. Differential Scanning Calorimetry showed that PE wax
melts at 99.7 oC. It starts to decompose at 205 oC. The ASTM D664 has shown it has an acid number of 1.2(mg KOH/g). Rice straw was
obtained from Egyptian farms. The straw was dried and milled to pass through a 20-mesh screen, the particle size distribution of RS was in the
range of 200-800m. the degradation of RS starts at 188.5oC. Chimasorb 944 UV stabilizer obtained from Ciba Specialty Chemicals, was used
as received with molecular weight >2500, and melting range (100-135oC) as indicated by the manufacturer.
5 0.0
45
40
90 8.86

35

390.34

964.81

30

579.95

%T

25
13 75.64

20
2848.72

15

722.68
163 8.18

3443 .36

10

2920 .39
1465.57

5
0 .0
4 40 0.0

4 00 0

3 00 0

2 00 0

1 50 0

1 00 0

5 00

3 50 .0

cm-1

Figure 1. FTIR for Polyethylene wax

2.2. Preparation the rice straw (RS) fiber / HDPE composites

The prepared rice straw fiber was further dried in an oven at 75oC for 10 hr to remove the moisture. The compounding process used for
preparing rice straw (RS) fiber / HDPE composites included two steps. First step:-all the HDPE was melted in the two roll-mill (Shaw Robinson
/ 2799), at 170 oC at a rotation speed of 60 rpm, then the PE wax and UV stabilizer were added. Later, the RS was added to the mixture and the
process continued till homogeneity was obtained. The second step:- The resulting blend was placed in a three-piece stainless steel molding set
and compression-molded in a (SAUMYA) hot press, at 30 tons/cm2 and 170C for 10 min.
At the end, it was allowed to cool to room temperature by cooling water passing through the press under the same pressure. The RS/HDPE
composites formulations in (Table 1). The RS/HDPE panels were firstly conditioned at 232C and RH of 50 5% for at least 40 hr according to
ASTM D618-99 before the tests.
Table 1. Composite formulations
Composite Code
vHDPE
A1
A2
A3
B1
B2
B3
C1
C2
C3
RS :- Rice Straw Fiber
CA :- Coupling Agent (PE wax)

Composite formulation
Virgin high density polyethylene
80% HDPE + 20% RS
77% HDPE + 20% RS + 3% CA
76.5% HDPE + 20% RS + 3% CA + 0.5% UV
65% HDPE + 35% RS
62% HDPE + 35% RS + 3% CA
61.5% HDPE + 35% RS + 3% CA + 0.5% UV
50% HDPE + 50% RS
47% HDPE + 50% RS + 3% CA
46.5% HDPE + 50% RS + 3% CA + 0.5% UV
vHDPE :- Virgin High Density Polyethylene
UV :- Ultra Violet Stabilizer

2.3. Differential Thermal Analysis (DTA)

Thermal analysis was conducted in a Shimadzu DTA-50, Japan (Sample weight: 3-5 mg, cell: Platinum, Atmosphere: air, rate flow: 20.00
ml/min, heating rate: 10oC/min, hold temperature: 600 oC). In the scanning, the whole samples were used for the average values of the thermal
properties thus, the influence of the degraded surfaces was reduced. The peak melting temperature (Tm) were determined from heating cycle. The
crystallinity (XC) was determined using the following equation:

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Composites from Rice Straw and High Density Polyethylene- Thermal and Mechanical Properties
International Journal of Engineering Sciences Vol(4), No (4), April, 2015.

Xc

Hf
100%
H 100 w

where, Hf is the heat of fusion or melting of the composites and Hf100 is the heat of fusion for a 100% polymer [22] and w is the mass fraction
of thermoplastic in the composite samples. The Tm is the peak temperature of melting during heating cycle. Melting of polymer is a change from
a solid, crystalline state into an amorphous state. The quantity of heat absorbed during the melting is called melting enthalpy. Enthalpy change
(Hm) of a specimen, expressed based on initial mass, is calculated from the area bounded by the melting or crystallization curves and the line
connecting the onset melting and end temperature. Higher values of crystallinity of the polymer indicate stronger secondary bonding and higher
density, higher strength, higher resistance to dissolution and softening by heating.
2.4. Mechanical Properties
2.4.1. Tensile Properties
The tensile tests were conducted for the different formulations according to ASTM D 638, with a Universal Testing Machine (Zwick / Roell Co).
The tests were performed at a crosshead speed of 5 mm/min and with 5 kN load cell. Samples in the form of dumppell with dimensions of
165mm 19mm 3.0mm (thickness).

3.

Results and discussion

3.1. Thermal Analysis (DTA)

The data presented in Table 2 and Figures 2-5 show thermal analysis and melting enthalpy of composites formulations indicate that the HDPE
sample exhibited higher melting enthalpy compared with the all RS/HDPE composite formulations. The melting enthalpy (Hm) decreased with
increasing the RS content in all composite formulations. The addition of PE wax increase the (H m), except for 50 wt.%RS composites which
decreased. This is due to the bonding between the RS and HDPE. The addition of UV stabilizer has no significant effect on (H m).
The crystallinity (XC) is presented in Figures 2-5, related to HDPE used in the stud. The crystallinity is increased with increasing the RS content
in all composite formulations. The addition of PE wax increases the XC due to the bonding between the RS and HDPE. The addition of UV
stabilizer has no significant effect on X C.
The melting temperature data presented in Figures.2-5, shows that the HDPE sample exhibited lower melting temperature (Tm) compared with
the all RS/HDPE composite formulations except for 20wt.%RS composites. The melting temperature is increased with increasing the RS content
in all composite formulations. The addition of PE wax and UV stabilizer has no significant effect on Tm.
Table 2. DTA data for the rice straw / HDPE composites.
HDPE
A1
A2
A3
B1
B2
B3
C1
C2
C3

T m; onset
102.0
111.0
110.9
114.6
95.5
99.4
99.4
93.0
99.0
97.0

Tm; OC
133.2
131.9
131.8
132.4
134.8
135.7
135.2
137.1
136.3
136.0

Hm;J/g
0.455
0.185
0.198
0.20
0.178
0.186
0.182
0.167
0.166
0.164

XC, Related to HDPE used in the study

-------51.10
56.51
57.46
60.18
65.93
65.04
73.4
77.62
77.51

Figure 2. DSC thermographs of the neat HDPE.

Mohamed H. El Nemr *, Yehia M.S. El Shazly, Ashraf A. Mubarak, Mohamed H. Zaki

60

International Journal of Engineering Sciences Vol(4), No (4), April, 2015.

PE wax addition created chemical bonds at the interface between the RS and the HDPE matrix and thereby improved the compatibility between
the RS and HDPE matrix, which in turn, enhanced the mechanical properties. This can be further supported by the increased Xc of PE wax
coupled composites. This was confirmed with the DSC analysis, which showed that the PE wax coupled composites had higher Xc as compared
to non-coupled composites Table 2.
The melting enthalpy of the HDPE based composite was the highest, which was decreased with the addition of rice straw, indicating the
decreased thermal stability of the composites. The Xc of the non coupled composite samples was lower than that of the neat HDPE which agree
with data presented by Stark NM [23]. The high Xc value for PE wax coupled composite may be due to chain branching of the C=O and better
coupling effect of the PE wax, which extended the predominance of the crystallization process which agree with Doh et,al., [24].

Figure 3. DSC thermographs of the 80% HDPE + 20% RS composites.

Figure 4. DSC thermographs of the 65% HDPE + 35% RS composites.

Figure 5. DSC thermographs of the 50% HDPE + 50% RS composites.

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Composites from Rice Straw and High Density Polyethylene- Thermal and Mechanical Properties
International Journal of Engineering Sciences Vol(4), No (4), April, 2015.

The addition of RS to HDPE matrix changes the crystallinity of HDPE. Although RS can act as a nucleating site for crystallization, it has been
found to physically hinder crystal growth at the higher fiber loading and, begins to hinder the molecular motion of HDPE resulting in lower
polymer crystallinity, which agree with pervious study by Stark et al. [25]. These data suggest that the crystallization mechanism of HDPE was
induced at a slightly higher temperature by incorporation of smaller wood fibers (which promote nucleation).
The use of coupling agent may act to induce crystallization of HDPE at a higher temperature.
Furthermore, the addition of a coupling agent to WPC seems to have played a larger role in HDPE crystallization. The reduction of crystallinity
and Tm could be due to the loss of structural integrity and debonding of the fibre from the matrix, resulting from the development of shear stress
at the interface due to absorbed moisture [26]. As the temperature increased, dehydration and decomposition of volatile components was
observed at about 260oC, followed by rapid weight loss for oxidative decomposition, and finally slow decomposition corresponding to the
formation of char [26].
3.2. Thermo gravimetric analysis (TGA) data
The obtained data indicate that HDPE-RS composites initial degradation was started at around 220 C, which is close to the main decomposition
temperature of the lignin extracted from wheat straws as reported to be around 210 C by Hornsby et. al.[27]. DTGA thermographs clearly show
two main decomposition peaks for both HDPE-RS composites. These peaks were shown on the Figures 6-9. The First peak was around 330 C
for RS based composites while the second peaks were around 460 C for HDPE based composites.
The main decomposition peak on the DTGA thermograph of the RS fiber was around 330C, which was pretty close to the decomposition
temperature of 320 C reported by Hornsby et. al [27]. It is believed that first peak of 330 C in RS fiber filled thermoplastic composites was
mainly from degradation of RS fiber. Second decomposition temperature peak for HDPE based composites was identical with the decomposition
temperature of neat HDPE (460 C).
Based on the TGA and DSC analysis during the manufacturing of the composites, it is recommended that extruder temperatures should be over
137 C to facilitate the melting of the matrix and should be less than 210 C to prevent the lignocellulosic material from degradation. According
to ASTM D 6662 it should also be noted that residence time of the material in the extruder is also important [28]. Higher processing temperature
can be set if the component passes through the extruder in a short time.

Table 3. Thermo gravimetric data for the rice straw/HDPE composites.

HDPE
A1
A2
A3
B1
B2
B3
C1
C2
C3

TG;OC; onset
376.1
215.0
217.6
210.0
220.0
250.0
248.0
218.0
212.0
210.0

1st Peak- RS;OC

-----------353.9
325.0
324.0
322.0
358.0
355.0
325.0
325.0
322.0

2nd Peak- HDPE; OC

485.0
468.0
467.0
465.0
468.0
465.0
463.0
465.0
466.0
465.0

The onset degradation temperature (TG), are presented in Figures 6-9, the HDPE sample exhibited higher (TG), compared with the all RS/HDPE
composite formulations. Onset degradation temperature is increased with increasing the RS content in all composite formulations. The addition
of PE wax increases the (TG), except for 50%RS composites. The addition of UV stabilizer decreases the (TG), in all composite formulations.

Figure 6. DTGA thermographs of the neat HDPE.

Mohamed H. El Nemr *, Yehia M.S. El Shazly, Ashraf A. Mubarak, Mohamed H. Zaki

62

International Journal of Engineering Sciences Vol(4), No (4), April, 2015.

Figure 7. DTGA thermographs of the 80% HDPE + 20% RS composites.

The first peak(1st peak) may be considered as the degradation peak of rice straw and the second peak(2nd peak) is the degradation peak of HDPE.
The 1st peak and 2nd peak, are presented for examples in (Figures.6-9). The 1st peak degradation, are decreased with increasing the RS content.
The addition of PE wax has no stable action. The addition of UV stabilizer decreases the 1st peak degradation in all composite formulations. The
neat HDPE sample exhibited higher degradation peak (2nd peak), compared with the all RS/HDPE composite formulations. The 2nd peak
degradation has no change with increasing the RS content. The addition of PE wax has no stable action. The addition of UV stabilizer decreases
the 2nd peak degradation in all composite formulations.

Figure 8. DTGA thermographs of the 35% HDPE + 65% RS composites.

Figure 9. DTGA thermographs of the 50% HDPE + 50% RS composites.

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Composites from Rice Straw and High Density Polyethylene- Thermal and Mechanical Properties
International Journal of Engineering Sciences Vol(4), No (4), April, 2015.

3.3. Mechanical properties

3.3.1. Tensile properties
The results of the tensile tests for all composite formulations are given in Figures 10, 11, and 12. The tensile strength is presented in Figure 10.
The HDPE sample exhibited higher tensile strength compared with the all RS/HDPE composite formulations. The tensile strength decreased
with increasing the RS content in all composite formulations. The addition of PE wax significantly increased the tensile strength, this is due to
the bonding between the RS and HDPE. The addition of UV stabilizer has no significant effect.

Tensile strength, MPa

25
20
15
10
5
0
vHDPE

A1

A2

A3

B1

B2

B3

C1

C2

C3

Composite formulation
Figure 10. Tensile strength of HDPE/RS composites.

The data presented in Figure 11, show the young's modulus (MOE), for the pure HDPE sample exhibited lower MOE compared with the all
RS/HDPE composite formulations. The increase in RS content has no significant change on MOE. The addition of PE wax increase the MOE of
the composites. The addition of UV stabilizer has no significant effect on MOE. For all composite formulations the MOE is identical, however a
sharp decrease was noticed for the samples of 50%RS without PE wax addition.

0.7

Tensile MOE, GPa

0.6
0.5
0.4
0.3
0.2
0.1
0
vHDPE

A1

A2

A3

B1

B2

B3

C1

C2

C3

Composite formulation
Figure 11. Tensile modules of HDPE/RS composites.

The data presented in Figure 12, indicate the elongation at break. The elongation at break decreased with increasing the RS content in all
composite formulations. The elongation at break of the RS-HDPE composites was much lower than that of pure HDPE samples. This decrease
may be attributed to the higher degree of brittleness introduced by the incorporating of RS into the HDPE matrix. The addition of PE wax
increased the elongation at break of the composites. The addition of UV stabilizer has no change in the elongation at break for 20%RS but for 35
and 50%RS a sharp decrease was noticed.

Mohamed H. El Nemr *, Yehia M.S. El Shazly, Ashraf A. Mubarak, Mohamed H. Zaki

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International Journal of Engineering Sciences Vol(4), No (4), April, 2015.

14

Elongation at break, %

12
10
8
6
4
2
0
vHDPE

A1

A2

A3

B1

B2

B3

C1

C2

C3

Composite formulation
Figure 12. Elongation at break of HDPE/RS composites.
The improvement with the PE wax addition is attributed to the formation of ester bonds between the(C=O) group of the oxidized PE (PE wax)
and hydroxyl groups of the RS fibers. This hypothesis is confirmed by previous studies showed the (C=O) group of functionalized polyolefin
coupling agents entered into an esterification reaction with the surface hydroxyl groups of RS fiber [16, 17]. The observed increase in the tensile
strength is attributed to the improved interfacial bonding between the rice straw and the HDPE matrix as well as the modification of individual
components which agrees with data presented by Lu et al., [29] and Balsuriya et al., [30].

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