J Polym Environ (2014) 22:365372
DOI 10.1007/s10924-014-0676-5
ORIGINAL PAPER
Mechanical Properties of Microcrystalline Cellulose (MCC) Filled
Engineering Thermoplastic Composites
Alper Kiziltas Douglas J. Gardner
Yousoo Han Han-Seung Yang
Published online: 24 June 2014
Springer Science+Business Media New York 2014
Abstract In this study, engineering thermoplastic com-
posites were prepared from microcrystalline cellulose
(MCC)-filled nylon 6. MCC were added to nylon 6 using
melt mixing to produce compounded pellets. The MCC-
filled nylon 6 composites with varying concentrations of
MCC (from 2.5 to 30 wt%) were prepared by injection
molding. The tensile and flexural properties of the nylon 6
composites were increased significantly with the addition
of MCC. The maximum strength and modulus of elasticity
for the nylon 6 composites were achieved at a MCC weight
fraction of 20 %. The Izod impact strength of composites
decreased with the incorporation of MCC without any
surface treatments and coupling agent. This observation is
quite expected for filled polymer systems and has been
commonly observed. There was a strong correlation
between density and tensile (r = 0.94) and flexural mod-
ulus of elasticity (r = 0.9). MCC filled composites manu-
factured by injection method had highly uniform density
distribution through their thickness. The higher mechanical
results with lower density demonstrate that MCC can be
used as a sufficient reinforcing material for low cost, eco-
friendly composites in the automotive industry especially
for under-the-hood applications (engine covers, intake
manifolds and radiator end tanks) as well as in other
applications such as the building and construction indus-
tries, packaging, consumer products etc.
A. Kiziltas (&)  D. J. Gardner  Y. Han  H.-S. Yang
Advanced Structures & Composites Center, University of Maine,
Orono, ME 04469, USA
e-mail: alper.kiziltas@umit.maine.edu
A. Kiziltas
Department of Forest Industry Engineering, Faculty of Forestry,
University of Bartin, 74100 Bartin, Turkey
Keywords Microcrystalline cellulose (MCC)  Nylon 6 
Mechanical properties  Engineering thermoplastic
composites  Density
Introduction
Engineering thermoplastic composites have attracted a
great deal of interest over the last decades as a result of the
potentially superior properties (excellent chemical resis-
tance, high thermal stability, low creep compliance and
high tensile, flexural and impact strength) and wide range
of industrial and consumer applications such as automo-
tive, electrical and aerospace applications these materials
can show relative to commodity plastic composites [1].
Aliphatic polyamides are well known engineering ther-
moplastics in industry [1, 2]. Nylon 6 is in a major class of
aliphatic polyamides and has several advantages including
good chemical resistance, good abrasion resistance, ther-
mal and weather resistant and good mechanical properties
[1, 3]. A variety of inorganic materials such as clay min-
erals, glass fibers, talc, calcium carbonate and kaolin have
been used in nylon 6 composites as additives or rein-
forcement to improve mechanical and thermal properties of
nylon 6 composites [47]. In spite of technological interest
in nylon 6, only a few studies of cellulose filled or rein-
forced nylon 6 composites have been published in literature
[815].
The earlier research related to cellulose filled engi-
neering thermoplastics did not give encouraging results.
Materials exhibited severe discoloration and pronounced
pyrolytic degradation because of high melting point of
engineering plastics [911, 15]. Due to initial research,
scientists believed that the use of cellulose as a reinforce-
ment or additive in engineering thermoplastics cannot be
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366
effective because cellulose thermal degradation occurs at
temperatures needed to process these engineering thermo-
plastics [811]. The automobile and construction market
need low density and cheap reinforcement for engineering
thermoplastics. Because of this demand, researchers have
looked again at cellulose filled engineering thermoplastic
recently [8]. Jacobson et al. developed a unique com-
pounding method called low temperature compounding to
produce cellulose pulp fiber filled nylon 6 composites.
They found that mechanical properties for the 33 % cel-
lulose fiber filled nylon 6 composites were approximately
twice as stiff as neat nylon composites and had better
strength properties than the neat nylon composites. The
33 % cellulose fiber filled nylon composites were also
intermediated between approximately the same percent
glass fiber and wollastonite, which are extensively used in
automobile industry as filler for filled nylon composites.
They also found that the density, color and surface
appearance of these injection-molded materials appear
suitable for some automobile applications [10]. In another
study, Misra et al. used small quantities of Lithium chloride
(LiCl) during melt extrusion processing to decrease melt-
ing temperature of nylon 6. They realized that the addition
of LiCl to nylon 6 also decreased the crystallization tem-
perature and degree of crystallinity. They also exhibited
that both tensile modulus and strength increased with
reinforcement of modified nylon 6 with 40 % hemp fiber
[8, 16]. In 2008, Xiaolin Xu studied cellulose filled engi-
neering thermoplastics with different production methods
and found that for cellulose fiber/nylon 6 composites,
extrusioninjection molding gave better mechanical prop-
erties than extrusioncompression molding and low tem-
perature extrusion exhibited better properties than high
temperature extrusion. Xu [8] also found that modulus and
strength increased with the increase of fiber content.
Microcrystalline cellulose (MCC) is naturally occurring
substance and obtained from high quality wood pulp [17,
18]. MCC has the advantage of high specific surface area in
comparison with other conventional cellulose fibers and
can use as a cellulosic reinforcement for polymer matrixes
[18]. The MCC has been incorporated into a number of
different matrixes like poly (lactic acid) [18, 19], polysty-
rene [20] and polyethylene [2124]. However there is lack
of information about MCC filled engineering thermoplas-
tics. Although recent efforts have demonstrated the feasi-
bility of producing nylon/natural fiber composites, there is
not enough information related to natural fiber reinforced
nylon composites because of the difficulties in producing
the composites without considerable thermal degradation
of natural fibers and high cost of nylon compared to
commodity plastics [814]. The objective of this study was
to evaluate the utility of MCC to reinforce an engineering
thermoplastic, nylon 6, with melting point over 220 C.
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J Polym Environ (2014) 22:365372
MCC was incorporated over a content range from 0 to
30 wt%. Analyses were conducted using some mechanical
tests including tensile, flexural and impact test and physical
test including density.
Experimental Procedure
Materials
The nylon 6 used as the thermoplastic matrix polymer, was
supplied by Entec Co., USA. Nylon 6 has a density of
1.13 g/cm3. The MCC used as the reinforcement was a
powder with particle size range from 26 to 96 lm. The
average particle size is 50 lm. The MCC is highly crys-
talline cellulose and supplied by Sigma Aldrich Co. The
MCC was stored in sealed containers after being oven dried
for at least 16 h at 105 C to obtain low moisture content
which is less than 1 %. The lubricant (Struktol TPW 113)
processing aid, being a blend of a complex, modified fatty
acid ester and having a specific gravity of 1.005 and
drooping point of 6777 C respectively, was supplied by
Struktol Company of America.
Sample Preparation
The MCC and nylon 6 were dried to a moisture content less
than 1 % using oven at 105 C for 16-h. The matrix
polymer, nylon 6, was mixed with the MCC. The com-
pounding was conducted with a Brabender Prep-mixer
equipped with a bowl mixer and the process temperature
and torque changes were measured in real time. Melt
temperature and torque changes for every run were recor-
ded to determine optimum processability for the nylon 6
MCC composites. The basic melt processing parameters
are listed in Table 1. The temperature was set to 250 C
and rotor speed at 60 rpm. MCC was added to the mixer
when the polymer melt appeared visually well mixed. After
addition of the MCC, the melt mixture temperature drop-
ped sharply to 200 C and increased again as the mixing
progressed. The melt mixture was released from the mix-
ture immediately after the temperature reached 230 C.
According to our earlier experiments in our lab, these
temperature ranges and MCC residence times, approxi-
mately 3 min, were recognized as a relatively safe tem-
perature range to prevent severe thermal degradation with a
guarantee of composite processability. Mixing was done
for 10 min until torque became stabilized. The nylon 6
MCC compounds were granulated using a lab scale grin-
der. The ground particles were dried at an oven at 105 C
for 16 h before being injection molded into ASTM test
specimens. All materials were injection molded using a
barrel temperature of 250 C mold temperature of 250 C
J Polym Environ (2014) 22:365372 367

Table 1 Basic operating parameters of the Brabender Rheomixer for Unreinforced and Reinforced Plastics and Electrical
nylon 6 and MCC Insulating Materials, Test Method 1, Procedure A, i.e.
Stage level Set Melt RPM Mix melt Reaction three-point loading system utilizing centre loading, using
temp. temp. temp. time (min) an Instron 8801 with a 4.48 N load cell. The support span
(C) was 50 mm and tests were run at a test speed of 1.27 in/
1st stage 250 240 6070 8 min. At least six specimens were tested for each compo-
(nylon 6) sition and the results are presented as an average for tested
2nd stage 230 200240 50 Cont. under 2 samples.
(with MCC) 240 C

Impact Test
Table 2 Composition of MCC filled nylon 6 composites
The impact tests were conducted according to ASTM D
Sample code MCC content Nylon 6 Lubricant 256-06, Standard Test Methods for Determining the Izod
Neat nylon 6 0 95 5 Pendulum Impact Resistance of Plastics. The notches
2.5 NMCC 2.5 92.5 5 were added using a NotchVIS machine manufactured by
10 NMCC 10 85 5 Ceast. The specimens were tested on a Resil 50 B impact
20 NMCC 20 75 5 test machine, manufactured by Ceast. The specimen is
30 NMCC 30 65 5 clamped in the bottom of the test fixture and the hammer is
then released from a specified height. The depth under the
Values are percentage by weight (wt%)
notch and the specimen width is entered, and the machine
will then record the energy taken to break the specimen. A
injection pressure of 2,500 psi. The compositions of com- 2.75 J hammer was used to impact the specimens. At least
posites are shown in Table 2. seven specimens were tested for each composition.

Statistical Analysis
The tensile strength, tensile modulus, elongation at break,
flexural modulus, impact strength and density data were
compared using a one-way analysis of variance followed
by TukeyKramer Honestly Significant Differences (HSD)
test with JMP statistical analysis program [25].
Mechanical Properties
Tensile Test
All the tension tests were conducted according to the
American Society of Testing and Materials (ASTM) stan-
dard D 638-03, Standard Test Method for Tensile Prop-
erties of Plastics. The tensile behaviors of composites were
measured using an Instron 8801 with a 10 kN load cell. All
the tension tests were tested at a rate of 5 mm/min. An
extensometer was employed for elongation determination.
At least six specimens were tested for each composition, and
the results are presented as an average for tested samples.
Tensile modulus of elasticity, the relative stress at maximum
load and strain at failure of neat nylon 6 and MCC filled
composites were obtained from the stressstrain curve.
Flexural Test
The flexure tests were conducted according to ASTM D
790-03, Standard Test Methods for Flexural Properties of
Density Test
The density profile of the neat nylon 6 and MCC filled
composite specimens was measured using X-ray densi-
tometer (QMS, Model QDP-01). At least five specimens
were tested for each composition. The dimension of density
specimens was prepared to be 63.5 mm by 12.5 mm by
3.2 mm. Density determination by the QDP scanning sys-
tem is basically based on relationship between X-ray
attenuation and density as express in the following equa-
tion [26, 27].
I=I0 elmqt
where I = intensity of radiation beam after passing through
the sample, I0 = intensity of radiation beam without
passing through the sample, e = natural logarithm base,
lm = material mass attenuation coefficient (cm2/g),
q = material density (g/cm3), t = material thickness
(mm), respectively.
Scanning Electron Microscopy (SEM)
Studies on the morphology of the tensile fracture surfaces
of the composites were carried out using an AMR 1000
(AMRay Co.) scanning electron microscope. Images were
taken at 10 kV with 2009 and 2,0009 SEM micrograph
magnifications. All samples were sputtered with gold
before the microscopic observations were obtained.

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Results and Discussion 60

50

Tensile Strength (MPa)

Tensile Properties
40
The tensile behavior of the neat nylon 6 as well as the
composites reinforced from 2.5 to 30 % of MCC was 30

performed by tensile testing at room temperature and 50 % 20

R.H. Figures 1 and 2 show tensile strength and elongation
at break of the neat nylon 6 and MCC filled composites. 10
The tensile strength and elongation at break were deter-
0
mined form stress and strain curves. It was observed that
Neat Nylon 2.5 NMCC 10 NMCC 20 NMCC 30 NMCC
neat nylon 6 exhibits a non linear elastic behavior with a
Filler Loading (%)
tensile strength of 29.06 MPa and an elongation at break of
2.16 %. None of the materials including neat nylon 6 Fig. 1 Effect of MCC loading on tensile strength of MCC filled
showed signs of stress yielding. This led to believe that the nylon 6 composites
mechanism behind the elongation and rupture of the
composites was quite similar compared to neat nylon 6. 6
The composite reinforced with MCC displayed enhanced

Elongation at break (%)

tensile properties in comparison with the neat nylon 6. 5

Because of better compatibility between polar nylon 6

matrix and polar MCC as well as better stress-transfer
properties, tensile strength of composites was larger
(reaching values 52.7 MPa with addition of 20 % MCC).
Tensile strength increased by 81 % with 20 % MCC
addition. After 20 % MCC addition, tensile strength
decreased but it was greater compared to neat nylon 6. The
reason why tensile strength decreases after 20 % MCC
addition could be very little or no stress-transfer properties
in this highly MCC filled composites [28]. This behavior is
also mainly because of the high MCC content which cause
a brittleness of materials. Xiaolin Xu observed similar
reinforcements with cellulose fiber in nylon 6 composites.
The tensile strength increased until 20 % addition of cel-
lulose fiber and after 20 % MCC addition tensile strength
decreased but was still higher than neat nylon 6. The tensile
strength also increased by 23 % with 20 % cellulose fiber
addition with extrusioninjection molding methods [8].
Almost all filled polymer systems display smaller elonga-
tion at break compared to neat polymer matrix because of
deformability of a rigid interphase between filler and the
matrix material [29]. Our results seem to be contradictory
to this observation. In our case, elongation at break of
composites was longer (reaching values 4.8 % with addi-
tion of 20 % MCC). Like tensile strength, the elongation at
break also decreased after a critical MCC loading (after
20 % MCC). The reason for this, it might be better dis-
persion below 20 % MCC addition. At high MCC contents,
the degree of fillerfiller interaction became more promi-
nent and, as a consequence, a reduction in elongation at
break was seen in the MCC filled composites. [30]. Based
on the above results, it clearly shows that there is an
optimal amount of MCC needed in a composite to achieve
greatest improvement in its properties. Figure 3 shows the
4
3
2
1
0
Neat Nylon 2.5 NMCC 10 NMCC 20 NMCC 30 NMCC
Filler Loading (%)
Fig. 2 Elongation at break as function of MCC loading for MCC
filled nylon 6 composites
tensile modulus of neat nylon 6 and MCC filled compos-
ites. The tensile modulus of a polymeric material has been
shown to be significantly improved when nanomicro
composites are formed with cellulose [18, 19, 3134].
Tensile modulus of elasticity of neat nylon 6 was 1.41 GPa.
The tensile modulus of elasticity was first seen to decrease
with 2.5 % MCC addition however this value (1.38GPa)
was not significantly difference from neat nylon 6. The
tensile modulus of elasticity of MCC filled composites
after 2.5 % MCC addition systemically increased with
increasing MCC loading (reaching values 1.86 GPa with
addition of 30 % MCC). Xiaolin Xu observed similar
phenomena. Tensile modulus of elasticity of the compos-
ites increased with increasing cellulose fiber content [8]. A
similar effect was also reported by Caulfield et al. [9] for
Nylon 66/hardwood and softwood fiber composites.
Flexural Properties
The flexural behavior of the neat nylon 6 as well as the
composites reinforced from 2.5 to 30 % of MCC was

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2.0
Tensile Modulus (GPa)
1.5
1.0
0.5
0.0
Neat Nylon 2.5 NMCC 10 NMCC 20 NMCC 30 NMCC
Filler Loading (%)
Fig. 3 Tensile modulus of elasticity of neat nylon 6 and MCC filled
composites
5.0
Flexural Modulus (GPa)
4.0
3.0
2.0
1.0
0.0
Neat Nylon 2.5 NMCC 10 NMCC 20 NMCC 30 NMCC
Filler Loading (%)
Fig. 4 Flexural modulus of elasticity of neat nylon 6 and MCC filled
nylon 6 composites
performed by flexure testing at room temperature and 50 %
R.H. In Fig. 4, the average values of the flexural modulus
as a function of MCC are shown. As can be seen in the
figure, the flexural modulus of composites was higher than
neat nylon 6. Flexural modulus of elasticity of neat nylon 6
was 2.56 GPa. The modulus also increased with increasing
MCC loading (reaching values 3.76 GPa with addition of
20 % MCC). There was no statistical difference in terms of
flexural modulus of elasticity between 20 % MCC and
30 % MCC filled composites. Flexural modulus of elas-
ticity increased by 47 % with 20 % MCC addition. The
flexural modulus is strongly affected by MCC loading and
MCC orientation and less by neat nylon 6MCC interac-
tion [31]. A similar effect was also reported by Xiaolin Xu
for nylon 6/cellulose fiber composites [8]. Also Sears et al.,
used cellulose wood pulps as a reinforcement for nylon 6
composites and found that cellulose wood pulps increased
flexural modulus compared to neat nylon 6 composites
[11].
369
50
Impact Strength (J/m)
40
30
20
10
0
Neat Nylon 2.5 NMCC 10 NMCC 20 NMCC 30 NMCC
Filler Loading (%)
Fig. 5 Effect of MCC loading on impact strength of neat nylon 6 and
MCC filled composites
Impact Strength
The impact strength of the composites depends on the
amount of filler loading and the type of testing whether the
samples were notched or un-notched [35]. The impact
behavior of the neat nylon 6 as well as the composites
reinforced from 2.5 to 30 % of MCC was performed by
Notched Izod impact testing at room temperature and 50 %
R.H. Figure 5 shows the izod impact strength of neat nylon
6 and MCC filled composites. The izod impact strength of
composites decreases as the MCC loading increases and
this observation is quite expected for filled polymer sys-
tems and has been commonly observed [29, 3639]. Pos-
sibility of poor wetting of the particles in nylon matrix and
poor interfacial adhesion between the MCC and the neat
nylon 6 cause weak interfacial regions in Fig. 6 which
presents the tensile fracture surfaces of the composites
[29]. Figure 6a as a low resolution shows debonded traces
of MCC particles and Fig. 6b as a high resolution shows
the micro crack between MCC particle and nylon 6 matrix.
This poor wetting phenomena might cause lower impact
strength with addition of MCC loading. Another reason for
this observation is untreated filler surface which can cause
poor dispersion of the MCC in nylon 6 matrix. In this case,
the impact strength decreases quickly although at low filler
addition [29, 36]. On the other hand a relatively smalls
stress concentration might be formed in the nylon 6
because of the smooth rod like shape of MCC. This phe-
nomena cause a weak sensitivity of impact strength to filler
content [29]. During the impact test, cracks travel through
the polymer as well as along the weak interfacial regions,
which might be caused from poor wetting of the particles
by the nylon 6. As a result of cracks travel, the latter cannot
resist crack propagation as effectively as the polymer
region; therefore we can see lower impact strength [29].
Increasing MCC content only increase the interfacial
regions which cause to crack propagation. In addition
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Fig. 6 SEM pictures of 20 wt% (a)

MCC-filled nylon 6 composites.
a Tensile fracture surface 9200.
b Tensile fracture surface
92,000

Debonded traces
of MCC particle

(b)

Micro crack sbetween nylon

6 matrix and MCC

1.4

1.2
1.25
Density (g/cm3 )

1.0
Density (g/cm3 )

1.20
0.8
1.15
0.6

0.4 1.10
Neat Nylon 6
0.2 1.05 2.5 % MCC
10 % MCC
20 % MCC
30 % MCC
0.0 1.00
Neat Nylon 2.5 NMCC 10 NMCC 20 NMCC 30 NMCC 0.0 0.5 1.0 1.5 2.0 2.5 3.0
Filler Loading (%) Thickness (mm)

Fig. 7 Density as function of MCC loading for MCC filled nylon 6 Fig. 8 Average density profile of neat nylon 6 and MCC filled
composites composites

these, addition of MCC might cause polymer immobility. It
can cause lower impact strength. Figure 5 also shows that
the Izod impact strength of composites decreased from
41 J/m for neat nylon 6 to 20 J/m for 30 % MCC filled
composite. A similar effect was also reported by Xiaolin
Xu for nylon 6/cellulose fiber composites [8]. The impact
strength of the composite can be improved by providing
flexible and strong interfacial bonding in the composite or
by using some coupling agents or impact modifiers [29,
3739].

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Table 3 Tukey-Kramer HSD comparison at a = 0.05 for neat nylon 6 and MCC filled composites
Sample Code T.S (MPa) TMOE (GPa)
Neat Nylon 6 B CD
2.5 NMCC B (NC) D (NC)
10 NMCC A (?67 %) C (NC)
20 NMCC A (?81 %) B (?20 %)
30 NMCC A (?69 %) A (?32 %)
The same letters indicates no statistical difference between properties of composites and those arround it. NC is no siginificant change upon the
addition of MCC (a = 0.05) and paranthesis show that effect of MCC loading on the mechnaical propeties of composites in comparision with
neat nylon 6
T.S tensile strength, TMOE tensile modulus of elasticity, EAB elongation at break, FMOE flexural modulus of elasticity, I.S impact strength
Density
Figure 7 shows the density of neat nylon 6 and MCC filled
composites. The density of the composites slightly
increased with MCC loading. This was expected, since
MCC has a greater density compare to neat nylon 6.
Generally there is a certain correlation between density and
mechanical properties such as flexural strength and mod-
ulus of elasticity [39]. There is a strong correlation between
density and tensile (r = 0.94) and flexural modulus of
elasticity (r = 0.9). We assumed that these large
improvements in the mechanical properties come from
MCC and density. The strong hydrogen bond between the
MCC molecules, which lead to strong interaction between
fibers and fibrils, and great MCC flexibility, might cause
better mechanical properties in comparison with the neat
nylon 6 [31]. As a result from density study, we can say
that MCC provide the reinforcement (flexural and tensile
modulus) with a smaller increase in density should not be
discounted, especially for automobile industry [40]. As
expected neat nylon 6 and MCC filled composites manu-
factured by injection method had highly uniform density
distribution through their thickness in Fig. 8. Table 3
shows summary of the effect of MCC loading on the
mechanical properties and density of composites in terms
of statistical analysis.
Conclusions
This study shows that it is possible to produce MCC-filled
engineering thermoplastic with melt compounding fol-
lowed by injection molding without compatibilizers. There
was no statistical difference in terms of mechanical prop-
erties between neat nylon 6 and 2.5 % MCC filled com-
posites. The composite reinforced with high filler loading
MCC displayed enhanced tensile and flexural properties in
comparison with the neat nylon. Elongation at break of
composites was longer (reaching values 4.8 % with addi-
tion of 20 % MCC). Izod impact strength decreased, when
371
EAB (%) FMOE (GPa) I.S (J/m) Density (g/cm3)
B B A D
B (NC) B (NC) A (NC) D (NC)
A (?114 %) B (NC) B (-23 %) C (?4 %)
A (?122 %) A(?47 %) C (-41 %) B (?7 %)
AB (?66 %) A (?46 %) C (-52 %) A (?10 %)
in comparison with the controls, from 23 to 52 % when
MCC was added to nylon 6. The density of the composites
slightly increased with MCC loading. There was a strong
correlation between density and tensile (r = 0.94) and
flexural modulus (r = 0.9). It is assumed that these large
improvements in the mechanical properties come from
MCC and density. Overall, MCC filled composites showed
comparable or higher mechanical properties compared to
neat nylon 6. The higher mechanical properties and lower
density is suggesting that the MCC-filled nylon composites
could be especially relevant in thermally challenging areas
such as the manufacture of under-the-hood automobile
components such as engine covers, intake manifolds and
radiator end tanks.
Acknowledgments The republic of Turkey, Ministry of National
Education has been greatly acknowledged for the scholarship of the
researcher Alper Kiziltas to do this study at the University of Maine.
The authors thank Chris West for the sample preparation. The authors
would also like to thank Maine Agricultural and Forest Experiment
Station (MAFES) project ME09615-08MS and the Wood Utilization
Research Hatch 20072008 project. This is fourth paper of the Maine
Agricultural and Forest Experiment Station.
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