Hadeer jalal

mustafa mohamed

Dimensional stability and mechanical behaviour of wood–plastic composites based

on recycled and virgin high-density polyethylene (HDPE)

Introduction .
The worldwide production of plastics is approximately 100 million tonnes per annum [1],
resulting in a significant proportion in municipal solid waste (MSW). For example, waste
plastics account for 11.8% of the 246 million tonnes of MSW generated in Unites States in
2005 [2]. Attempts have been made to recycle the post-consumer plastics in order to reduce
the environmental impact and consump- tion of virgin plastics. During 2004, plastics
recovery was about 8.25 million tonnes (39% of total amount of plastics consumed) in
Western Europe [3]; 35,000 tonnes (13.48% of total imported virgin plastics) in New Zealand
[4]; while
United States recycled around 5.7% of the plastics gener- ated in 2005 [2]. Previous studies
show that the properties of the recycled high density polyethylene (shortened as rHDPE)
obtained from the post-consumer milk bottles was not largely different from those of virgin
resin and thus could be used for various applications [5]. Also the recycled plastics are
cheaper than in the virgin form, for example, rHDPE pellets and flakes are 31–34% less
expensive than the virgin high density polyethylene (vHDPE) [6]. Thus, increased use of
recycled plastics offers the prospect of less- ening waste disposals and reducing the product
.costs
In wood industry, a large amount of wood waste is gen- erated at different stages of the
wood processing and such waste is mainly destined for landfill. In the United States, about
63 million metric tonnes of wood waste was gener- ated in 2002 [7]. The use of waste wood
in wood plastic
composites (WPCs) helps to offsets these disposal costs. It was well established that waste
wood in the form of wood flour, fibres or pulp is suitable as a filler for polyolefins [8 and 9].
As reported by Miller et al. [10] the Pinus radiata wood fibre possesses physical and
.mechanical properties suited to the reinforcement for plastics
There are a number of published studies on the reinforce- ment of vHDPE with wood fibre
with regard to the result- ing mechanical properties, dimensional stability, interfacial bonding
and durability [11–14]. However, studies on WPCs
based on recycled HDPE are very limited. Yam et al. [15] and Selke et al. [16] studied
rHDPE (simulated milk gallon) and wood fibre composites using extrusion moulding and
report that the performance was at least as good as the com- posites based on virgin plastic.
Li et al. [17] studied com- pression–moulded composites based on a combination of virgin
and recycled HDPE and pine wood flakes. It was found that the initial particle geometry of
the HDPE played an important role in the quality of the composites. Kamdem et al. [18]
studied the properties of compression–moulded composites made of rHDPE and wood flour
from untreated or chromated copper arsenate (CCA) treated pine wood, respectively. It was
observed that the composites with par- ticles from recycled CCA treated pine exhibited
higher flex- ural strength compared to composite from untreated pine. Sellers et al. [19]
demonstrated that for hot-pressed compos- ites of recycled pine wood fibres and recycled
polyethylene, these composites have mechanical properties suitable for construction
applications. Youngquist et al. [20] have shown that composites made from demolition wood
waste and waste plastics from milk bottles by thermoforming method exhibit a broad range
of properties similar to those made of virgin ingredients. Jayaraman et al. [21] studied the
performance of melt blending and injection-moulding com- posites made from Pinus radiata
fibres and rHDPE, and found that the tensile strength was 25% higher than those of
composites using vHDPE. Chen et al. [22] investigated the influence of wood particle size in
hot-pressed composites based on construction wood waste and rHDPE, and found that
.smaller sized wood particles improved water absorp- tion and thickness swelling
Most of the research on wood and rHDPE composites has concentrated on the use of either
a single type of plastic from the waste stream, or a simulated mixing of waste plas- tics or
mixing of recycled and virgin plastics. The post-con- sumer plastics waste stream may
contain many different grades, colors and contaminants, leading to varying perfor- mance
when these plastics are combined with wood fillers (fibres or flour). The impact of
post-consumer rHDPE in WPCs is still not fully understood, leaving open research
opportunities for the optimisation of the products and pro- cessing. This study aims to
explore the use of waste Pinus radiata sawdust and post-consumer rHDPE for the pro-
duction of the HDPE-wood flour composites. The effect of the wood flour loadings and
coupling agent addition on the dimensional stability, mechanical properties and
.microstructure is also investigated

Experimental
Materials .2.1
Sawdust of softwood radiata pine (Pinus radiata) was collected from a local sawmill. The
fresh sawdust was dried at 102 °C for 24 h to a moisture content about 2–3% and then
ground to finer flour by using a plate grinder. The sieve analysis found that most of the wood
particles fall in the 35– 45 mesh sizes with the corresponding diameter ranging between 0.18
and 0.5 mm. Recycled HDPE granules were procured from local plastic recycling plant,
which were derived mainly from post-consumer plastics wastes. The plastic granules were
thoroughly washed with water and dried at 65 °C for 12 h. The measured properties of
recycled HDPE show a MFI of 0.072 g/10 min at 190 °C. The cou- pling agent used was
-maleated polypropylene of grade Epo
. lene G-3015 polymer with a bulk density of 913 kg/m 3
Industrial grade virgin HDPE of grade GM4755F (melt flow index, MFI, of 0.1 g/10 min at 190
.°C and bulk density of 949 kg/m3) was also used for comparison studies
Composite preparation .2.2
The wood flour was compounded, separately, with recy- cled and virgin HDPE granulates in
a co-rotating twin-screw extruder. The barrel temperatures of the extruder were con- trolled
at 170 °C, 180 °C, 190 °C and 190 °C for Zones 1, 2, 3 and 4, respectively, while the
temperature of the extruder die was held at 200 °C. The screw speed was varied between
150 and 165 revolution per minute and the pressure from 33 to 47 bars, depending on the
materials being blended. The wood flour and HDPE were premixed before being fed into the
first zone of the extruder. The extruded strand passed through a water bath and was
.subsequently palletized
Before the panel was made, the compounded pellets were dried at 75 °C for 4 h to remove
the remaining mois- ture. The pellets were then moulded in an electrically heated platen
press by using an aluminium mould coated with a di-butylether releasing agent. The
hot-press platens were heated to 200 °C before placing the pellet-filled mould on the bottom
platen. The pellets were then hot-pressed for 4 min under a pressure of 1.0 MPa, followed
by another 5 min under a pressure of 5.0 MPa. The mould and panel were then transferred
to a cold press and pressed for fur- ther 5 min at 5.0 MPa. The panel thickness was
controlled by using 6.4 mm spacers. The final composite panel size was 165 · 152 · 6.4
(thickness) mm. Finally, the composite panels were conditioned at a temperature of 23 ± 2
°C and relative humidity of 50 ± 5% for at least 40 h according to ASTM D618-99 [23]. The
formulations of the composite

Dimensional stability tests

Water absorption and thickness swelling tests were con- ducted in accordance with ASTM
D570-98 [24], in which
 Mechanical properties measurements .2.​4
Type-I tensile bar specimens with dimensions of 165 · 19 · 6.4 (thickness) mm were cut and
machined from the hot-pressed composite panels. Tensile tests were per- formed in
accordance with ASTM D638-99 [25] using a standard material testing system (MTS-810
load frame with 5 kN load cell) at a crosshead speed of 5 mm/min. Strain was measured
over a 25 mm gage length using an extensometer. The flexural properties were measured in
three-point bend tests using a standard Material Testing System (MTS-858 load frame with
2.5 kN load cell) at a crosshead speed of 2.8 mm/min in accordance with ASTM D790 [26].
The flexural test specimens were also cut from the composite panels with dimensions of 130
· 12.7 · 6.4 (thickness)mm. The tensile and bending measurements were performed at
 ambient conditions of 23 ± 2 °C and 50 ± 5% relative humidity. Five replicates of each
.compos- ite formulation were tested
Micro-structural examination of fracture surfaces .2.​5
The fracture surfaces of the flexural test specimens were characterised with high-resolution
field emission scanning electron microscopy (FESEM). The FESEM was operated at an
accelerating voltage of 1 kV and emission current of 47 lA. Fracture surfaces were
sputter-coated with gold of approximately 50 nm in thickness. Specimens were ana- lysed at
.·magnifications of 100

Results and discussion​s .3

Moisture absorption and thickness swelling .3.1
Results of composite density, moisture absorption and
thickness swelling are given in Table 2. It is found that
3
the density of the composites ranges from 922 kg/m for

the entirely rHDPE panel to 1042 kg/m3 for the 50 wt% wood-rHDPE panels with 3 wt%
MAPP. The composites made with MAPP have higher density with lower porosity and thus
have better dispersion and better interfacial strength as compared to the composites without
.[the cou- pling agent [13,14,27
The water absorption increases with increasing wood content in the composites – a trend
that is true for both the 2 h and the 24 h water immersion tests. However, after 24 h
immersion the water absorption is almost doubled as given in Table 2. With the increase in
the wood content, there are more water residence sites thus more water is absorbed. On the
other hand, the composites made from higher plastic content have less water absorption
sites and thus lower water absorption. The water absorption of the entirely recycled HDPE or
the entirely virgin HDPE composite is only 0.03–0.04% after 2 h and 0.05% after 24 h
immersion in water. For the rHDPE based composites, the water absorption with 30 wt%
wood flour content is 0.39% after 2 h immersion and 0.98% after 24 h, while the corre-
sponding values for the composites with 50 wt% wood flour content are 1.7% and 4.1%,
respectively. Interestingly the composites made of rHDPE have lower water absorp- tion
compared to those made of vHDPE at the same wood content. It is also noted that addition
of MAPP can signif- icantly reduce the water absorption. The composites with 50 wt% of
wood flour and 3 wt% MAPP reduce the water absorption from 4.1% to 1.31% for the 24 h
immersion tests and this can be further reduced to 1.18% by adding 5 wt% of MAPP in the
same composite formulation. When the coupling agent is added, the influence of the plastic
to wood ratio is no longer important. For example, by adding 3 wt% of the coupling agent,
 the water absorption for com- posites with 40% wood flour is 1.24% at the 24 h immersion
.compared to 1.31% for the composites with 50 wt% of wood flour
The impact of wood to plastics ratio on the water absorption can be explained by the
differences in water
Table 3
Tensile and flexural properties of HDPE-wood flour composites
absorption between wood and plastics. The moisture absorption in composites is mainly due
to the presence of lumens, fine pores and hydrogen bonding sites in the wood flour, the gaps
and flaws at the interfaces, and the micro- cracks in the matrix formed during the
compounding pro- cess [28]. The presence of hydroxyl and other polar groups in various
constituents of the wood flour resulted in poor compatibility between the hydrophilic wood
flour and the hydrophobic plastics, which increases the water absorp- tion. Water absorption
by cellulose and hemicelluloses depends on the number of free hydroxyl groups thus the
amorphous regions are accessible by water. On the other hand, plastics are water repellent
and have much lower water sorption capability than wood. With the addition of MAPP (3–5
wt%) the compatibility between wood flour and HDPE is improved because the anhydride
moieties in MAPP entered into an esterification reaction with the sur- face hydroxyl groups of
.[wood flour [29
The thickness swelling (TS) of the HDPE-wood flour composites increases with the water
absorption and thus has similar trend to the water absorption regarding the impacts of wood
to plastics ratio and coupling agent (Table 2). The TS values for the 2 h water immersion
vary from 0.24% to 1.26%, and these values are increased after 24 h immersion, varying
from 0.42% to 2.50%. Samples made with lower content of wood flour have lower TS and
this is true both for the composites made from vHDPE and those made from rHDPE.
However, samples treated with MAPP show that thickness swelling is reduced at the same
wood content. In general, the composite made of virgin and recycled plastics have similar
dimensional stability properties without adding the coupling agent which is con- sistent with
.[previous findings by Chen et al. [22
Tensile propertie​s .3.2
The tensile strength of the HDPE-wood flour composite is found to lie in the range of 9.5 and
.(23.2 MPa (Table 3

The unfilled rHDPE composite exhibit higher tensile strength (23.2 MPa) compared with the
unfilled vHDPE composite (21 MPa) which is likely due to the stiffer poly- mer grades
present in the recycled plastic. Furthermore, composites based on rHDPE exhibit higher
tensile strength than those based on vHDPE for the same plastic to wood ratio. For example,
with a plastic to wood ratio of 60:40, composite based on rHDPE have a tensile strength
value of 14.5 MPa while the tensile strength of the composites based on vHDPE is 12 MPa.
 This is probably due to the presence of mixed type of polymer and chemical impurities in the
rHDPE, which might enhance interface bonding. In addition, the tensile strength of the
composites increases with decreasing wood content in the matrix. The Young’s modulus
(MOE) in tension for the composites without MAPP ranges from 1.4 to 1.7 GPa (Table 3),
which is much less variable than the tensile strength values. Com- posite of 30 wt% wood
and 70 wt% rHDPE exhibit the lowest MOE, while all other composites without coupling
agent have very similar MOE values. The results also show that the composites made from
the recycled plastics have MOE values similar to or higher than the composites made from
.the virgin plastics using the same formulations
It is observed that the addition of MAPP to the compos- ites based on 40–50 wt% wood flour
show the highest ten- sile strength and stiffness for all of the composites. For example, the
tensile strength of composite made from rHDPE with 50 wt% wood flour and 3 wt% MAPP is
almost 60% higher than the non-treated composites using a similar composite formulation.
The observed increase in the tensile strength and stiffness is attributed to the improved
interfacial bonding between the wood flour and the HDPE matrix as well as the modification
of individual
components [14,30]. Such improvements is due to the for- mation of ester bonds between
the anhydride carbonyl groups of MAPP and hydroxyl groups of the wood fibers [31,32]. This
hypothesis is confirmed by previous studies [29,32] that show anhydride moieties of
functionalized polyolefin coupling agents entered into an esterification reaction with the
surface hydroxyl groups of wood flour. Upon esterification, the exposed polyolefin chains
diffuse into the HDPE matrix phase and entangle with HDPE chains during hot pressing.
These changes create chemical bonds at the interface between the wood flour and the
HDPE matrix and thereby improve the compatibility between the wood flour and HDPE
.matrix. This, in turn, enhances the mechanical properties of the composites
The stress–strain behaviour of all the HDPE-wood flour composites under tensile loading is
presented in Fig. 1. The composite material becomes stiffer with the addition of wood flour,
however, the corresponding strain at failure decreases. As the wood flour loading increases
so do the yield stress, tensile modulus and tensile strength, but in opposing trend, the
ductility of the material falls. The MOE for these composites increases monotonically with
increasing of the wood flour loading. On the other hand, the composites with higher HDPE
content showed higher ductility and higher strain at fracture. In case of non-cou- pled
composites, lack of intimate bonding between wood flour and HDPE led to numerous
irregularly shaped micro-voids or micro-flaws, which make the transfer of stress from the
matrix to the fibers, was poor and the mechanical properties of the fibers were not fully
utilized. However, for the MAPP added composites, the maximum strength is increased but
.the maximum strain at failure is decreased as compared to the non-coupled composites
 Flexural properties .3.3
The flexural strength and stiffness of the composites mea- sured using 3-point bending tests
are shown in Table 3. The flexural strength exhibits a similar trend to the tensile strength
although less variation is observed in the flexural strength with different formulations than the
tensile strength. The composites based on rHDPE and wood flour have a flexural strength
varying from 15.6 to 25.5 MPa whereas those made of vHDPE have the corresponding val-
ues ranging from 14.4 to 17.9 MPa. Similarly, the bending MOE for the rHDPE composites
varies from 1.3 to 1.97 GPa and that of the composites using the vHDPE is from 1.06 to 1.34
.GPa
The flexural strength and MOE of the composites made from the rHDPE are slightly higher
than those using the vHDPE at the same plastic to wood ratio. It is also observed that the
flexural strength increases with decreas- ing wood content. For example, the flexural
strength of the composite made from rHDPE with 30 wt% wood flour content is 24.3 MPa as
compared to that made with 50 wt% wood flour content which is only about 15.6 MPa. As
expected, the flexural MOE of the composites increases with the wood content. With a
similar trend to the tensile test results, the addition of the coupling agents significantly
improves the flexural strength as well as the stiffness of the composites. Due to the similar
mechanism as explained in the previous section, the flexural strength of composites with
.MAPP coupling agent increases as compared that of non-coupled composites
The load–displacement curves of the entirely HDPE and the HDPE-wood flour composites
are shown in Fig. 2 which reflects the effects of the filler loading and MAPP addition. The
load–displacement curves for the HDPE- wood composites have relatively high slopes
initially, but
as failure occurred, the loads dropped off quickly as the material crumbled. However, the
pure HDPE specimen reached ultimate capacity after significant deformation (15 mm in this
case), and then the load decreased gradually until the test was concluded, indicating ductile
behaviour. The addition of wood flour in the composites increased the stiffness and
brittleness, however, reduced the elonga- tion at break. The stress concentration at the fiber
ends and poor interface bonding between wood and HDPE matrix have been recognized as
the leading causes for the embrittlement. Nevertheless, coupling agent (MAPP) improved
 interfacial bonding between the filler and the matrix and improved the flexural strength.
However, dur- ing loading, fractures occurred at the filler locations, and these fracture
locations were more brittle than other parts of the matrix. Hence these composites showed
little change in the specimen appearance in the initial stage of loading until the maximum
load was reached when the specimen failed suddenly with extensive breakage at the
interface between the wood flour and the matrix. The elongation at break of the HDPE-wood
flour composites was much lower than that of entirely HDPE panel. This decrease was
probably due to the higher degree of brittleness intro- duced by the incorporation of wood
fibers into the HDPE matrix. As in the case of modulus, improving the adhesion between
.fibers and HDPE did not enhance elongation at break
It was found that effect of wood was notable in material properties of the composites. Wood
is a lignocellulosic material made up of three major constituents (cellulose: 42–44%,
hemicelluloses: 27–28%, and lignin: 24–28%) with some minor constituents (extractives:
3–4%) [27]. The major portion of wood is crystalline cellulose. The aligned fibril structure of
cellulose along with strong hydrogen bond has high stiffness thus addition of the wood flour

can increase the stiffness of the thermoplastic based com- posites. Lignin as an amorphous
polymer does not greatly contribute to the mechanical properties of wood flour but plays an
important role in binding the cellulose fibrils that allows efficient stress transfer to the
cellulose molecules. Hence, wood filler increases the stiffness of HDPE without excessively
increasing the density. Furthermore, these com- posites have potential to take up water
under humid condi- tions due to the presence of numerous hydroxyl groups available for
interaction with water molecules via hydrogen bonding. The addition of a coupling agent
improved the compatibility between the wood filler and HDPE through esterification and thus
.reduced the water absorption and improved the stability and mechanical properties
Characterisation of fracture surfaces .3.4
Microstructure of the fracture surface of specimens tested in bending was examined using
FESEM. The bend- ing fracture surface of the HDPE-wood flour composites at a filler
loading of 30 wt% is shown in Fig. 3a in which
 numerous cavities and pulled-out fibers can be seen. The presence of these cavities and
pulled-out fibers confirms that the interfacial bonding between the filler and the matrix
polymer is poor and weak. In addition, localised bunch of fibers and patches of HDPE matrix
are seen, which indicates the poor dispersion of fillers within HDPE matrix. Hence, the
fracture surface of the composite with lower filler content appears to be dominated by
pull-out damage rather than fibers breakage. Figs. 3b and 4a show, respectively, the
micrographs of fracture surfaces of 50 wt% wood flour filled composites with virgin (Fig. 3b)
and recycled HDPE (Fig. 4a) matrix. In these composites, there are still distinct cavities
between the matrix and the fibers, indicating poor adhesion. It is also possible to observe the
wood fibres being weakly bonded to the matrix and thus pulled out from the matrix during
fracture. Fig. 4a also shows that part of the wood lumen is filled with plastic that could
increase the strength of the composites because of mechanical interlocking. The dispersion
of the wood fibers in the recycled HDPE matrix is uniform as compared to virgin HDPE
matrix. This may be due to
K.B. Adhikary et al. / Composites: Part B 39 (2008) 807–815 813

the different grade of plastics and other impurities in the recycled HDPE. When wood
content is increased, the poly- mer matrix is no longer continuously distributed and many
wood fibres are in direct contact with one another, result- ing in poor bonding at adhesion at
the interface. Fig. 4b shows the micrograph of fracture surface of the 3 wt% MAPP
incorporated composite filled with 50 wt% wood flour. The SEM image shows that there are
no clear gap between wood flours and HDPE matrix, indicating the good interface bonding. It
is also seen that a crack running through the wood fibre, and this could be an indication of
stress-transfer from the weaker matrix to the stronger wood fibre. The interfacial bonding
between the filler and the HDPE matrix is improved due to the esterification mechanism [30],
and the fracture occurred at the filler itself. This means that the stress is well propagated
between the filler and the matrix polymer, resulting in enhanced flexural strength and
modulus in response to stress. In addition, the fracture surface shows a very limited amount
of torn matrix, suggesting that the composite is more brittle.

4.Conclusions
In this work, WPCs were made from both recycled and virgin HDPE with Pinus radiata wood
flour. The dimen- sional stability and mechanical properties, which are important properties
in product utilisation, and the micro- structure of the fracture surfaces with regards to the
cou- pling agent, wood flour content and plastic types were investigated. Following
conclusions are drawn from the current work:
The composites made with hot-press have very low water absorption and thickness swelling
thus the products is stable in humid environment. The water absorption and thickness
swelling increase with the wood content, how- ever, adding coupling agent (MAPP) reduces
these proper- ties significantly. The composites of 50 wt% of recycled HDPE with the
3–5wt% MAPP coupling agent can achieve equivalent stability properties to those of the
com- posites made from 70 wt% of recycled HDPE without the coupling agent.
The mechanical properties of the composites made from post-consumer recycled HDPE are
similar to or, in some cases, better than the composites made from the virgin HDPE. The
composites with low wood content (or pure HDPE composite) and coupled with the MAPP
have better tensile strength than all of the non-coupled ones. However, the composites
made with lower wood content without the coupling agent show lower stiffness. The addition
of the MAPP reduces the ductility and elongation at the breaking point. Comparison of the
SEM images of the fracture sur- faces of HDPE-wood flour composites with and without the
coupling agent confirms that an addition of MAPP improves the interfacial bonding.
The results of the present work clearly show that recy- cled HDPE and wood sawdust can be
successfully used to produce stable and strong WPCs. Dimensional stability

Acknowledgements
The authors thank the Department of Chemical and Pro- cess Engineering and Department
of Mechanical Engineer- ing, University of Canterbury, for the technical supports, SCION
and AgResearch (New Zealand) for providing equipment, NZ Plastics Recycling Ltd. and
Canterbury Landscape Supplies for supplying materials. The PhD scholarship awarded by
NZAID is greatly appreciated.

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Dimensional stability and mechanical behaviour of wood–plastic composites based on

recycled and virgin high-density polyethylene (HDPE)
Kamal B. Adhikary a, Shusheng Pang a,*, Mark P. Staiger b
a Department of Chemical and Process Engineering, University of Canterbury, Private Bag
4800, Christchurch, New Zealand
b Department of Mechanical Engineering, University of Canterbury, Private Bag 4800,
Christchurch, New Zealand Received 10 March 2007; accepted 17 October 2007
Available online 4 November 2007
www.elsevier.com/locate/compositesb