Composites: Part A 40 (2009) 218224

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

Poly(vinyl alcohol) nanocomposites reinforced with cellulose brils isolated

by high intensity ultrasonication
Qingzheng Cheng *,1, Siqun Wang *, Timthy G. Rials
Tennessee Forest Products Center, University of Tennessee, 2506 Jacob Dr., Knoxville, TN 37996-4570, USA

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

Article history: Cellulose brils in micro and nanoscales generated from biomass are relative new reinforcing materials
Received 24 April 2008 for polymer composites, which have potential lightweight and high strength and are biodegradable. The
Received in revised form 5 November 2008 objective of this study was to reinforce biodegradable polymers by cellulose brils generated from sev-
Accepted 22 November 2008
eral cellulose sources by ultrasonic treatment in order to utilize biomass to fabricate high-value products.
The geometrical characteristics of the brils were investigated by polarized light microscopy (PLM) and
atomic force microscopy (AFM). The degree of brillation of the bers evaluated by water retention value
Keywords:
was signicantly increased after treatment. The treated cellulose and separated brils were used to rein-
A. Polymer-matrix composites (PMCs)
B. Mechanical properties
force poly(vinyl alcohol) (PVA) to make biodegradable nanocomposites by lm casting. The mechanical
D. Mechanical testing properties of PVA were signicantly improved by most of the small brils. The morphological character-
E. Casting istics of the nanocomposites were investigated with PLM, scanning electron microscopy, and AFM.
2008 Published by Elsevier Ltd.

1. Introduction homogenizer treatment [5,6], and high intensity ultrasonication

Cellulose is the most abundant natural biopolymer in the world,
which is renewable and biodegradable. Fibrils in nano and micro
scales generated from cellulose bers have much higher mechani-
cal properties than those of single bers. It was reported that the
cellulose crystal regions had Youngs modulus of up to 137 GPa
measured by X-ray diffraction [1]. The elastic modulus of Lyocell
brils with diameter from 150 to 180 nm was evaluated to be
98 GPa using nanoscale three-point bending in AFM [24]. Isolat-
ing cellulose brils and reinforcing polymers by them to make
nanocomposites are very attractive [49]. Nanocomposite is de-
ned as composite that includes at least one-dimension of one
component in the composite at the nanometer scale (1100 nm)
[10]. A denition of a bril as a small, slender ber or lament is
used in this paper. It may include cellulose crystals or whiskers,
microbrils, and bundles of microbrils.
Cellulose brils can be generated by chemical or mechanical
treatment. The chemical method, such as strong acid hydrolysis,
removes the amorphous regions of cellulose ber and produces
nano-size brils. Wood bers [11], cotton [12], sea animals [13],
and sugar beet [14] were used as raw materials to isolate brils
by chemical method. Mechanical method includes a high-pressure
rener treatment [15], a grinder treatment [16], a high-pressure
* Corresponding authors. Tel.: +1 865 946 1120; fax: +1 865 946 1109.
E-mail addresses: chenggq@hotmail.com (Q. Cheng), swang@utk.edu (S. Wang).
1
Present address: Division of Forestry and Natural Resources, West Virginia
University, Morgantown, WV 26506-6125, USA.
[4,17,18]. The brils made by these mechanical methods could be
bundles of microbrils, or cellulose nanobers. For nanocompos-
ites reinforced by brils or llers, there are several common fabri-
cation methods: such as lm casting by vaporizing the solvents
[19,20], freeze drying followed by classical compression or extru-
sion processes [21], compounding dry polymers and cellulose
whiskers suspension using a corotating twin screw extruder [22],
hot press molding dried mats of microbrillated cellulose with
phenol-formaldehyde resin [23,24], ltration mats followed by a
compressive molding [4,7].
Lyocell ber, a regenerated cellulose ber (RCF), is produced by
dissolving wood pulp in a solution and then spinning the solution
into bers. The process orients the cellulose molecular chains,
which form cellulose brils. Lyocell differs from other RCF by its
high crystallinity, high longitudinal orientation of crystallities, high
amorphous orientation, and low lateral cohesion between brils
[25,26]. RCF was treated by high intensity ultrasonication (HIUS)
to generate cellulose brils [4,17,18]. An obtained mixture of brils
in micro and nanoscales was used to reinforce poly(vinyl alcohol)
(PVA) and polypropylene [7], and poly(lactic acid) [8].
The purposes of this study were to characterize the brils sep-
arated from the mixtures of treated RCF (Lyocell), pure cellulose
ber (PCF, TC180), and microcrystalline cellulose (MCC, Avicel)
treated by HIUS and to investigate the physical and mechanical
properties of PVA composites reinforced with these brils. The
brils were characterized by PLM and AFM. The degree of brilla-
tion of the bers was evaluated indirectly by water retention value. PVA
nanocomposites were prepared by lm casting. The mechanical

1359-835X/$ - see front matter 2008 Published by Elsevier Ltd.

doi:10.1016/j.compositesa.2008.11.009
 Q. Cheng et al. / Composites: Part A 40 (2009) 218224
properties and morphologies of the composites were evaluated and
compared by tensile test, and observations of PLM, scanning elec-
tron microscopy (SEM) and AFM, respectively.
2. Experiment
2.1. Materials
Regenerated cellulose ber (RCF, Lyocell, Lenzing, Austria), pure
cellulose ber (PCF, TC180, by CreaFill Fibers Corp.), and microcrys-
talline cellulose (MCC, Avicel PH-101, FMC BioPolymer) were used
as raw material. Commercial microbrillated cellulose (MFC, 10%
solid slurry, Daicel Chemical Industries, Ltd., Japan) was used as a
reference. Biodegradable polymer: poly(vinyl alcohol) (PVA,
99 + % hydrolyzed, typical average MW 85,000124,000, purchased
from SigmaAldrich) was used as matrix.
2.2. Fibril isolation and composite preparation
The short RCF, PCF, and MCC were soaked in distilled water for
more than 24 h (concentration: 2% in mass) and then treated
30 min with 80% power by high intensity ultrasonication (HIUS)
(Sonic Newtown, CT, 20 kHz, Model 1500 W) to isolate brils. HIUS
produces very strong mechanical oscillating power, so cellulose
brils can be isolated from cellulose bers by the action of hydro-
dynamic forces of ultrasound [4,17,18]. Centrifuge (Accuspin 400)
was used to separate brils from the treated materials with rela-
tive centrifugal force of 500 g and 5 (RCF) or 10 (PCF and MCC) min.
After setting for 5 min, the top portion (small brils) and/or bottom
portion (big brils) were used to reinforce PVA. The treated sam-
ples before centrifuging was called treated cellulose or bers.
PVA water solution (10 wt%) and cellulose bril water suspen-
sion (1 wt%) were mixed and stirred manually and then dispersed
by ultrasonic treatment (Sonic Newtown, CT, 20 kHz, Model
1500 W) for about 1 min with 50% power level. The mixtures were
degassed in a desiccator with vacuum and evaporated at room
temperature (T: 20 C) and relative humidity (RH) of 30% until
lms were formed, and then the lms were heat treated in an oven
at 70 C for more than 4 h [7]. The samples were kept in a desicca-
tor before the mechanical properties were performed. The compos-
ites with three levels of bril loading (2%, 6%, and 10%) were
manufactured and tested. The nominal thickness was 150 lm.
2.3. Fibril characterizations
The appearance and dimensions of the treated and untreated
RCF and small brils were investigated by PLM (Olympus-BX51).
The Morphology of the small brils was examined using an AFM
(PASI XE-100) with non-contact mode after a small drop of bril
suspension was dried on a silicon wafer. More than three images
were taken and chosen to observe the morphology of all samples.
At least ve brils with similar diameters were selected randomly
and measured in the micrographs. The aspect ratios of the brils
were estimated using SEM images [7].
Water retention value (WRV) can be used to measure the de-
gree of homogenization or microbrillation of bers [5]. WRV is
a percent ratio of the water contained in the sample after centri-
fuged in certain force and time to the dry weight of the sample.
The force of 900 g and time of 30 min were used in this study [7,8].
2.4. Nanocomposite characterizations
The mechanical tests were performed using an Instron testing
machine (model 5567, load cell 30 kN). The crosshead speed was
1 mm/min. The crosshead extensions were used as the specimen
219
deformations. The samples were cut to dogbone shapes with width
of 5 mm for the narrow portion and total length of 40 mm (gauge
length was 20 mm). According to the ASTM D1708 standard [27],
at least ve specimens were tested for each composition. Tensile
modulus was tangent modulus from the linear portion in the
stressstrain curves with ignoring the initially unstable part. Mul-
tiple comparisons by the Statistical Analysis System (SAS) (t Tests
(LSD)) were used to detect the overall signicant differences of
the inuences on the tensile elastic modulus and strength of com-
posites (a = 0.05).
The morphology of the fractured surfaces of the composites
after tensile test was investigated using a SEM (LEO 1525). The
fractured surfaces were coated with gold on an ion sputter coater,
and operating voltages of SEM were 510 kV. PLM was also used to
observe the distributions of the brils in the composites from sur-
faces. To observe the cross-sections by AFM with non-contact
mode, the RCF bril reinforced lms were embedded in epoxy resin
and cut to get smooth surfaces by an ultramicrotome with dia-
mond knives. A silicon cantilever with nominal spring constant
of 42 N/m, resonant frequency of 330 kHz was used (PPP-NCH,
Nanosensor). At least three images were taken and chosen to ob-
serve the morphology, but only some of the features selected ran-
domly in the micrographs were measured [7].
3. Results and discussions
3.1. Morphology of bers and brils
Fig. 1 shows PLM image of untreated cellulose and AFM image
of small brils for MCC. Fig. 2 shows one AFM image of small
PCF brils. And the PLM and AFM images of treated RCF bers
and small RCF brils are shown in Fig. 3. A mixture suspension of
ber and brils with diameter ranging from microns to tens of
nanometers was obtained from all the three materials after
30 min ultrasonic treatment. The separated brils had a wide range
of diameter and length as well as the aspect ratio, which was
approximately from 10 to 80 and different for different raw mate-
rials, i.e., it was smaller for MCC than those of PCF and RCF [7]. It
can be seen that many small RCF brils with diameter less than
1 lm were peeled from the bers (Fig. 3).
3.2. Water retention value (WRV) of untreated and treated cellulose
The WRV of treated RCF bers was increasing with the HIUS
treatment time increasing [7]. For MCC, PCF, and RCF treated
30 min by HIUS, the WRVs were dramatically increased as shown
in Fig. 4. This means the degree of microbrillation of the treated
bers increased because WRV is related to bril and microbril
surface and volumetric phenomena [5]. The higher WRV of MCC
indicated that it was much easier to break down to small brils
than PCF and RCF bers.
3.3. Mechanical properties of the composites
The tensile modulus and strength of neat PVA and its compos-
ites reinforced by untreated and treated MCC, and small MCC bril
with 2, 6, and 10 wt% are shown in Fig. 5. The tensile modulus of
neat PVA was decreased signicantly by 2% of untreated MCC,
but not much change for 6% and 10%. The PVA modulus was in-
creased by treated MCC and small MCC brils. The tensile strength
of PVA was decreased signicantly by untreated and treated MCC,
but it did decreased by small MCC brils. The treated MCC was bet-
ter than untreated MCC for modulus but similar to strength. These
demonstrated that untreated MCC might not be used as PVA rein-
forcement mainly because of its low aspect ratio; while treated
220 Q. Cheng et al. / Composites: Part A 40 (2009) 218224

Fig. 1. Structure and appearance of untreated MCC (PLM, left) and small MCC brils (AFM, right).

Fig. 4. WRV of the three materials before and after 30 min treatment by HIUS.

The tensile modulus and strength of PVA composites reinforced

Fig. 2. AFM image of small PCF brils.
MCC, especially the small brils with high aspect ratio could rein-
force the mechanical properties of PVA. Similar results were dis-
cussed that MCC does not demonstrate an improvement of the
tensile modulus value in the carboxymethyl cellulose composite
[12].
by 2% (m/m) separated small and big brils from treated MCC for
30 min by HIUS were 5.2 0.2 and 5.3 0.3 GPa, and 103 6 and
104 5 MPa, respectively. No signicant difference was found be-
tween the reinforcement of small and big brils, which were much
higher than those of untreated MCC reinforced composites
(4.1 0.2 GPa and 79 7 MPa). Fig. 6 shows the tensile modulus
and strength of PVA and its composites reinforced with 2% (m/m)
untreated and treated PCF, and small and big brils from PCF trea-
ted for 30 min by HIUS. The small bril reinforced composites had

Fig. 3. PLM (a) and AFM (b) images of treated RCF (Lyocell) bers and small RCF brils.
 Q. Cheng et al. / Composites: Part A 40 (2009) 218224
Fig. 5. Tensile modulus and strength of PVA and its composites reinforced by untreated and treated MCC, and small MCC brils.
much higher mechanical properties (both modulus and strength)
than those of neat PVA, untreated and treated PCF reinforced com-
posites, but big bril did not change much of the mechanical prop-
erties. Untreated PCF decreased both modulus and strength of PVA
signicantly, while treated PCF only decreased the strength but not
changed the modulus. Unlike MCC brils, small PCF bril rein-
forced composites had higher improvement for both modulus
and strength than those of big brils. This may be because small
PCF brils had higher mechanical properties than those of big -
brils [3,4], and PCF brils had higher aspect ratio than that of
MCC brils.
The tensile modulus and strength of neat PVA and its compos-
ites reinforced by untreated and treated RCF bers, small brils,
and MFC of 2, 6, and 10 wt% are shown in Table 1. The tensile mod-
ulus of neat PVA was increased by the three weight contents of all
the bers, brils, and MFC except 2% and 6% of untreated RCF, but
the modulus changes were not signicant among the loadings of
2%, 6%, and 10% except between the 2% and 6% of MFC. The tensile
strength of PVA was not signicantly changed by untreated RCF
and MFC except 10% of MFC. It was increased signicantly by only
2% of treated RCF bers and all the three contents of small brils.
Adding more ber and brils did not increase more strength. The
results indicated that small brils had better reinforcement for
the strength of PVA than the treated ber; and the treated ber
had better reinforcement for both the modulus and strength of
PVA than untreated bers. The reinforcement of RCF brils was
much better that that of MCC and PCF brils. The possible reasons
Fig. 6. Tensile modulus and strength of PVA and its composites reinforced by
untreated and treated PCF, and small and big PCF brils.
221
may be the aspect ratio of RCF brils was higher; the elastic
modulus of RCF brils was higher than that of natural bers [3];
and the crystallinity of treated RCF ber was increased, while it
was decreased for treated MCC cellulose [4,7,18].
The improvements of PVA were not as high as those of microbers
generated from wood pulp [28] and soybean [20]. The tensile
strength was doubled (from 42 to 102 MPa), and the stiffness
was increased from 2.3 to 5.2 GPa by 5% microber loading of
wood microbers [28]. The tensile strength was increased from
65 to 103 MPa; and the stiffness was increased from 2.3 to
6.2 GPa by 5% microber loading of soybean nanobers [20]. This
may be because the sources of neat PVA were different, and lm
making conditions, e.g., drying temperature and time, which may
inuence the adhesion between the bers and the polymer matrix,
the uniform distribution of the brils, aspect ratio and orientation
of the bers, and the degree of crystallinity of the matrix [29]. So
that the properties of neat PVA were much different (modulus
2.3 vs. ours 5.7 GPa, strength 42 or 65 vs. ours 112 MPa). The re-
sults of neat PVA in this study were similar as those of microber
reinforced composites. The other reason may be that the brils and
MFC had some bigger brils (>1 lm); and the brils may not be
even and ne enough, which had more defects and low mechanical
property than those of smaller brils [3,4].
3.4. Morphology of the composites
Fig. 7 shows PLM surface proles of PVA composites reinforced
with 2% (m/m) of untreated MCC and small MCC brils. The disper-
sion of MCC particles and MCC brils from the surface were uni-
form, but SEM cross-section images of fracture surfaces (Fig. 8)
demonstrated that some brils were aggregated and clear gaps
were observed between cellulose and polymer, especially for un-
treated MCC particles. The PLM and SEM techniques provide infor-
mation of different dimensional scales. The PLM images were from
surfaces; while SEM images were from the cross-sections. These
along with the low aspect ratios may be the main reasons that
the tensile strength and modulus of the composites were not im-
proved much by the small brils; and the strength of PVA was de-
creased by untreated and treated MCC (Fig. 5).
The SEM images of PVA composites reinforced with 2% of
untreated PCF and small PCF brils are shown in Fig. 9. The frac-
ture surfaces of untreated PCF demonstrated clear gaps between
bers and polymer. This was one reason that the composites
reinforced with untreated ber and the treated ber had lower
tensile strength than pure PVA (Fig. 6). The small PCF brils from
the cross-section were not clear (Fig. 9b). The bril dispersion in
the PVA matrix could be more uniform than that of untreated
PCF.
222 Q. Cheng et al. / Composites: Part A 40 (2009) 218224

Table 1
Tensile modulus and strength with standard deviations of PVA and its composites reinforced with untreated and treated RCF bers, small RCF brils, and MFC.

Materials Modulus (GPa) (PVA: 5.7 0.2) Strength (MPa) (PVA: 112 6)
2% 6% 10% 2% 6% 10%
Untreated 6.0 0.4 6.1 0.3 6.3 0.4 108 6 107 7 105 8
Treated 6.6 0.2 6.7 0.2 6.5 0.4 125 6 118 7 115 7
Small 6.5 0.4 6.8 0.4 6.8 0.3 127 6 124 7 130 7
MFC 6.3 0.3 7.1 0.3 7.2 0.4 112 10 113 8 101 7

Fig. 7. PLM surface proles of PVA composites reinforced with 2% untreated MCC (Avicel) and small MCC brils.

Fig. 8. SEM images of the fractured cross-sections of PVA composites reinforced with 2% untreated MCC and small MCC brils.

Fig. 9. SEM images of the fractured cross-sections of PVA composites reinforced with untreated PCF (TC180) and separated small PCF brils.
 Q. Cheng et al. / Composites: Part A 40 (2009) 218224 223

Fig. 10 shows PLM images of surface and cross-sections (inset)
of PVA composites reinforced with small RCF brils and MFC (as
reference). It indicated that the dispersions from the surfaces of
both RCF and MFC brils were uniform, but SEM images of fracture
surface after tensile test (Fig. 11) and AFM images of cross-sections
after cut by microtome (Fig. 12) from the PVA composites rein-
forced by small RCF brils demonstrated that the dispersion of
brils from the cross-section was not absolutely uniform. Some
brils were aggregated and some were pulled out after tensile test.
These are the main reasons that the increments of tensile strength
and modulus of the composites were not very high, especially after
the bril loadings of more than 2% in weight. Fig. 13 shows SEM
images of the fractured cross-sections of PVA composites rein-
forced with 2% and 10% of RCF brils. The relative ber and bril
dispersion in 10% loading was worse, which demonstrated that
more ller may be not further reinforcing PVA composites.
4. Conclusions
After treated by high intensity ultrasonication, a mixture of
ber and bril in micro and nanoscales was obtained from regen-
erated cellulose ber (RCF), pure cellulose ber (PCF), and micro-

Fig. 10. PLM images of surface and cross-sections (inset) of PVA composites reinforced with small RCF brils and MFC.

Fig. 11. SEM images of the fractured cross-sections of PVA composites reinforced with small RCF brils.

Fig. 12. AFM topography and phase images of the cross-sections of PVA composites reinforced with small RCF brils.
224 Q. Cheng et al. / Composites: Part A 40 (2009) 218224
Fig. 13. SEM images of the fractured cross-sections of PVA composites reinforced with 2% (a) and 10% (b) treated RCF bers.
crystalline cellulose (MCC). Both of the mixture and small brils of
RCF can be used to increase the tensile modulus and strength of
PVA. The small brils of PCF and MCC had better reinforcement
than that of untreated ones. PLM and AFM observations show that
the sizes of the brils have a wide diameter range from tens of
nanometers to several micrometers; the dispersion of cellulose
was uniform from surfaces but not absolutely uniform in the ma-
trix from the cross-sections; and there were some gaps between
the polymer matrix and brils.
Acknowledgements
We thank Dr. John R. Dunlap, Dr. David Harper, and Dr. Cheng
Xing at the University of Tennessee, for valuable assistances in
SEM, PLM, and AFM experiments; USDA Wood Utilization Research
Program and Tennessee Agricultural Experiment Station Project #
96 for funding.
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