Composites: Part A 41 (2010) 1012–1018

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

Study on sound absorption property of ramie fiber reinforced poly(L-lactic acid)

composites: Morphology and properties
Dakai Chen a, Jing Li a, Jie Ren a,b,*
a
Institute of Nano- and Bio-Polymeric Materials, School of Material Science and Engineering, Tongji University, Shanghai 200092, PR China
b
Key Laboratory of Advanced Civil Engineering Materials, Ministry of Education, Tongji University, Shanghai 200092, PR China

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

Article history: The effect of ramie fiber, flame retardant and plasticizer on sound absorption property of ramie fiber rein-
Received 16 January 2010 forced PLLA composites was investigated. We used press molding process to prepare the ramie fiber/PLLA
Received in revised form 31 March 2010 composites, with short ramie fiber and ramie plain weave fabric as the reinforcement. The dispersivity of
Accepted 9 April 2010
flame retardant ammonium polyphosphate (APP) was indirectly tested by thermogravimetric analysis
(TGA). The result of sound absorption property measurement shows that the composites with short ramie
fiber have better sound absorption property than the ramie fabric reinforced PLLA composites. And the
Keywords:
addition of APP and plasticizer poly(butylene adipate-co-terephthalate) (PBAT) improves the sound
A. Ramie fiber
A. Poly(L-lactic acid)
absorption property of ramie fabric/PLLA composites. Moreover, morphological studies by scanning elec-
B. Sound absorption property tron microscopy (SEM) demonstrate the micro-phase separation in the PBAT/PLLA composites and the
porosity of the single ramie fiber bundle. The results suggest that these special structures are the main
reason for the better sound absorption property.
Ó 2010 Elsevier Ltd. All rights reserved.

1. Introduction reduction are often fabricated by the method of compression mold-

Noise refers to the irregular and chaotic sound which disturbs
people’s work and impairs people’s health. In recent years, with ra-
pid development of modern industry and transportation, noise pol-
lution has become increasingly prominent, and has become a
major cause of environmental pollution and personal unhealthi-
ness. There are two main methods to control the noise pollution.
One is the control of the noise sources, that is, to make the big vo-
cal sound inaudible through a small device or equipment; the other
one is to use a variety of noise reduction materials with special
structures, in terms of transmission route. In the last few years,
acoustics and materials science experts have introduced new noise
reduction materials and there are more and more applications of
fibers in the control of noise pollution. Noise reduction materials
are divided into two broad categories. One is the sound-absorbing
material and the other is acoustic material. Many of the fiber rein-
forced composites are used as sound-absorbing material and only a
small number of them are also used as acoustic materials.
Plant fibers and their products, such as cotton, flax fibers, sugar
cane fibers and wood fibers are the whole biodegradable
sound-absorbing materials. This type of plant fibers used for noise
* Corresponding author at: Institute of Nano- and Bio-Polymeric Materials,
School of Material Science and Engineering, Tongji University, Shanghai 200092, PR
China. Tel.: +86 21 65989238; fax: +86 21 65976823.
E-mail address: renjie6598@163.com (J. Ren).
ing or in the form of non-woven fabric which provides poor fire
prevention, anti-corrosion property and moisture resistant. Due
to relative cheapness, recyclability, the strength per unit weight
and the worldwide availability, natural fibers have been used as
reinforcement of different thermosetting and thermoplastic resins.
Natural fiber/PLLA composites have attracted great attention not
only because they can replace fossil resource but also for the posi-
tive environmental benefits gained by such materials [1–3]. Hard-
ness and brittleness of PLLA, thermal sensitivity at the temperature
of compounding processes and flammability of natural fiber/PLLA
composites limit their development and practical application [4].
Therefore, several modifications have been proposed to improve
processibility and mechanical properties. Among the several mod-
ifications, polymer blending is regarded as a useful and economical
way to produce new materials with a wide range of properties.
Blends of PLLA and other polymers, such as natural poly(3-
hydroxybutyrate) (PHB), atactic poly(3-hydroxybutyrate) (a-PHB),
and poly(butylene adipate-co-terephthalate) (PBAT), have been
studied to modify the properties and expand its practical applica-
tion [5–13]. In the field of flame retardation of natural fiber/PLLA
composites, some halogen-free flame retardants containing phos-
phorus–nitrogen have been extensively studied and reviewed in
literature for its low-toxicity and high efficiency [14–16]. APP,
which is widely studied and used, can be called intumescing flame
retardant, for it is combined with char forming agent and nitrogen-
containing components. The main purpose of the research is to

1359-835X/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesa.2010.04.007
 D. Chen et al. / Composites: Part A 41 (2010) 1012–1018
investigate the effects of ramie fiber, flame retardant and plasti-
cizer on sound absorption property of ramie fiber reinforced PLLA
composites.
2. Materials and methods
2.1. Materials and reagents
PLLA, weight-average molecular weight of 150 kDa, polydisper-
sity of 2 (GPC analysis) was obtained from Tong-Jie-Liang Biomate-
rial Co., Ltd. (China). PBAT (Ecoflex FBX 7011, BASF Corp.) with
density of 1.26 g/cm3 has a weight-average molecular weight of
145 kDa, polydispersity of 2.40 (GPC analysis), and a glass transi-
tion temperature and melting point of 30 and 122 °C (DSC anal-
ysis), respectively. Both polymers were supplied in granular form
and used as received. Silane coupling agent KH550 that is 3-Ami-
nopropyltriethoxysilane (APS) H2N(CH2)3Si(OC2H5)3 used to im-
prove the interaction between the ramie fibers and polymer was
purchased from Shanghai Yaohua Chemical Plant (China). APP
(Mn > 1000) was obtained from Shanghai Xunshen Flame Retardant
Co., Ltd. (China). Ramie fibers used were purchased from Feng-Ling
Co., Ltd. (China).
2.2. Methods
2.2.1. Preparation of the blends of PBAT and PLLA (PBAT–PLLA)
PBAT and PLLA were dried and mixed and a series of materials
were melt-mixed with a twin-screw extruder (LEISTRITZ) at about
170 °C with a rotor speed of 25 rpm for 10 min.
2.2.2. Preparation of short ramie fiber treated by permanganate
acetone solution and silane coupling agent (ksFIB) and ramie fabric
treated by permanganate acetone solution and silane coupling agent
(ksFAB)
Firstly, short ramie fiber and ramie fabric were treated with
0.8% permanganate acetone solution [17,18]. Secondly, the surface
of short ramie fiber and ramie fabric were treated with 0.4% silane
coupling agent (weight percentage with respect to the fibers) dis-
solved in acetone at 25 °C. Then, the fibers were immersed in the
solution for 8 h under agitation. Afterwards, the fibers were dried
at 70 °C until the fibers were completely dry.
2.2.3. Preparation of PLLA with flame retardant (F-PLLA), PBAT–PLLA
with flame retardant (F-PBAT–PLLA) and ks-FAB with flame retardant
(F-ksFAB)
The flame retardant (APP) was dried under vacuum at 80 °C for
10 h to remove moisture. Then PLLA and APP were mixed and a
Table 1
The compound formulation of the biocomposites.
1013
series of materials were melt-mixed with a twin-screw extruder
(LEISTRITZ, Germany) at about 170 °C with a rotor speed of
25 rpm for 10 min. The preparation of F-PBAT–PLLA was conducted
by the procedure same as that for F-PLLA. The ramie fabric was im-
merged in APP ethanol solution for 24 h under agitation. Then the
fibers were dried at 70 °C until completely dry, and F-ksFAB was
obtained.
2.2.4. Composites processing
To ensure that all absorbed moisture was removed and to pre-
vent void formation, ramie fibers and PLLA matrix resin were dried
at 80 °C under vacuum for 10 h before processing. Ramie fiber/PLLA
composites with 30% w/w ramie fibers were chosen to test the
sound absorptivity. The same fiber content was used for all tests
to determine the optimal mechanical properties [19,20]. The short
ramie fibers and PLLA were blended using a two roll plastics mill in
the following order. First, one half of the PLLA was placed inside
the mixing chamber for about 1 min at 30 rpm; then ramie fibers
were added over a period of 3 min. Then, the other half of the PLLA
was placed inside the mixing chamber and the mixing speed was
increased to 60 rpm for 5 min. The total mixing time was 9–
10 min. The ramie fabric/PLLA composites containing 30% w/w ra-
mie fabric were produced by press molding using the powder-
stacking procedure. Bed lay-ups were prepared in the sections
where fibers were stacked up with PLLA powder layers on either
side [21,22]. The weights of PLLA sheets and ramie fibers were
measured before processing so as to determine the wt.% of ramie
fibers and PLLA in the resulting composite. All the biocomposites
obtained were then molded into sheets by hot pressing at 170 °C
and 20 MPa for 4 min, followed by cooling to room temperature
at 5 MPa. The compound formulations of different sheets prepared
for structure characterization and properties measurements were
as shown in Table 1. The specimens for the sound absorption prop-
erty testing were obtained from these laminates according to GBJ
88-85 standards with diameter of 110 mm and thickness of 3 mm.
2.2.5. Thermogravimetric analysis(TGA)
TGA was performed on a Q100 thermogravimetric analyzer
(Tainstsh, USA) at a heating rate of 20 °C/min. Samples were exam-
ined under flowing air (80 ml/min) over a temperature range from
ambient to 700 °C.
2.2.6. Sound absorption property measurement
Sound absorption property was tested by standing-wave tube
method which is the normal incidence sound-absorbing determi-
nation. The devices were installed with the main tube equipment,
support device, sound source apparatus and sound accepter.
1014 D. Chen et al. / Composites: Part A 41 (2010) 1012–1018
Fig. 1. (a) Normal incidence sound absorptivity testing system and (b) computing formula for sound absorptivity test.
Fig. 2. TGA results of PLLA, F-PLLA, ksFAB/PLLA and F-ksFAB/F-PLLA.
Moreover, the profile of the main tube should be a circular cross-
section. The main tube used in our research has the inside diameter
of 110 mm, the overall length of 2500 mm and the thickness of
5 mm. Besides, the operating frequency was from 100 C/S to
1600 C/S. The frequency of determination frequency was 100 C/S,
and at intervals of 1/3 octave band frequency domain. The proce-
dure of the test was as follows. The sound-absorbing materials
were placed into one end of standing-wave tube, the specific deter-
mination frequency was produced in the other side and one stim-
ulant plane wave field was formed. After the incident plane wave
passed the sound-absorbing materials, the reflected wave formed
the standing-wave in the tube. By measuring the Pmax and Pmin of
the standing-wave pressure and converting the reflectivity of the
materials, the sound absorptivity was determined. The computing
formula and the testing system were as shown in Fig. 1.
2.2.7. Scanning electron microscope (SEM)
The surface morphologies of the alkali treated ramie fibers were
observed by Quanta 200 FEG (FEI Company) with field emission
gun and accelerating voltage of 10 kV was used to collect SEM
images of the surface of ramie fibers. The morphologies of the frac-
tured surfaces of the biocomposites were observed by SEM at room
temperature and analyzed by a scanning electron microscopy
(SEM) (Hitachi S-2360N, Tokyo, Japan). Before testing, the samples
were sliced and mounted on SEM stubs with double-sided adhe-
sive tape, and then gold sputtered for 5 min to a thickness of about
10 nm under 0.1 torr pressure and 18 mA current to make the sam-
ple conductive. Micrographs were recorded at different magnifica-
tions to assure clear images.
3. Results and discussion
3.1. Thermal stability
Fig. 2a and b presents comparison of TGA curves of PLLA, F-
PLLA, ksFAB/PLLA and F-ksFAB/F-PLLA. In the case of ksFAB/PLLA,
after initial loss of moisture and desorption of gases at about 50–
150 °C, a major decomposition takes place from 280 to 390 °C. Nev-
ertheless, the addition of APP changes the decomposition pattern.
For F-ksFAB/F-PLLA, the starting decomposition temperature is
 D. Chen et al. / Composites: Part A 41 (2010) 1012–1018 1015

becomes worse. It is reported that APP decomposes at high tem-

perature and phosphoric acid, poly-phosphoric acid and nonflam-
mable gas are released; the resulting acid is contributed to
intramolecular or intermolecular dehydration, and then dehydrog-
enization, charring of ramie. On the other hand, the acid from the
pyrolysis of APP catalyzes break of the –C–O– bond to produce
many oligomers and small molecular substances at lower temper-
atures. According to these facts, it is believed that the first weight
loss stage is due to the APP pyrolysis and advance decomposition
of ramie fibers caused by acid released from APP decomposition.
The char residue for F-ksFAB/F-PLLA in air at 400 °C are
21.90 wt.% that is remarkably higher than that of 8.85 wt.% for
ksFAB/PLLA in the same experimental conditions. As for the
flame-retarded composites, by adding APP residues increases sig-
nificantly at high temperature. The presence of APP enhances the
charring process for composites. In the range of 300–400 °C, it is
a consequence of initial physical interaction of both fiber and intu-
mescent via partial liquefaction and subsequent mixing of adjacent
contact zones. When the temperature increases above 400 °C, the
matrix and the intumescent component begin to fully develop a
bonded char structure. During the char formation, the heat and
the amount of burning’s volatile products are drastically reduced,
and thermally stable char in high temperature is contribute to
the thermal and flame protection to matrix. Thermogravimetric
analysis of the trace random sampling of the PLLA, F-PLLA,
ksFAB/PLLA and F-ksFAB/F-PLLA, and then the burning curve tests
indirectly determine the distribution of the flame retardants in the
composites. Through above test results, it can be seen that the
flame retardant in the PLLA and ramie fiber reinforced PLLA com-
posites have a better dispersion.

3.2. Sound absorptivity

By comparison between the properties of PLLA, PBAT–PLLA,

Fig. 3. Sound absorptivity, real part of impedance ratio and imaginary part of
impedance ratio of PLLA composites: (a) PLLA, (b) PBAT–PLLA, (c) ksFIB/PLLA, (d)
ksFAB/PLLA, (e) ksFAB/PBAT–PLLA and (f) F-ksFAB/F-PBAT–PLLA.
lowered significantly. At the same time, two significant mass loss
stages appear on the curve from 240 °C to 280 °C and from
300 °C to 385 °C respectively indicating that thermal stability
ksFIB/PLLA, ksFAB/PLLA, ksFAB/PBAT–PLLA and F-ksFAB/F-PBAT–
PLLA as shown in Fig. 3a, it can be concluded that the presence
of ramie fiber, flame retardant and plasticizer can greatly affect
the sound absorptivity of the composites. In terms of the data for
the operating frequency from 0 Hz to 1000 Hz, there are no sharp
differences in sound absorptivity of the PLLA composites. After
1000 Hz, a significant change took place in the sound absorptivity
of the various PLLA composite materials. The sound absorptivity of
ksFIB/PLLA is greater than that of PLLA and ksFAB/PLLA because
there is no specific orientation uniform distribution of ksFIB in
the composites. Due to the porous nature of ramie fiber, when
the sound waves hit the surface of ksFIB/PLLA, the non-vertical an-
gle fiber with the orientation of the incident wave can absorb a
part of the sound waves. However, the distribution of ksFAB in
the composites, and precisely, the direction of the fiber is vertical
to incident sound waves, so its sound-absorbing effect is not satis-
factory. Due to incompatibility between the plasticizer PBAT and
PLLA, micro-phase separation exists in the interface of PBAT–PLLA.
While the existence of such a fine slit is beneficial to absorption of

Table 2
Effect of ramie fiber, flame retardant and plasticizer on sound absorption coefficient.

Sample Frequency (Hz)

250 400 600 800 1000 1200 1400 1600 Average
PLLA 0.089 0.081 0.057 0.048 0.044 0.047 0.058 0.081 0.063
PBAT–PLLA 0.078 0.061 0.055 0.05 0.069 0.13 0.274 0.247 0.121
ksFIB/PLLA 0.104 0.069 0.058 0.048 0.047 0.059 0.097 0.147 0.079
ksFAB/PLLA 0.116 0.081 0.055 0.046 0.041 0.045 0.057 0.091 0.067
ksIAB/PBAT–PLLA 0.084 0.06 0.061 0.039 0.059 0.162 0.133 0.114 0.089
F-ksFAB/F-PBAT–PLLA 0.114 0.075 0.066 0.059 0.059 0.116 0.298 0.353 0.143
1016 D. Chen et al. / Composites: Part A 41 (2010) 1012–1018

Fig. 4. SEM photomicrographs of ramie fibers: (a) 100 lm (at 500), (b) 10 lm (at 4000), (c) 100 lm (at 400) and (d) 20 lm (at 2000) with (a and b) showing their
surface features; (c and d) showing their cross-sectional features.

Fig. 5. SEM micrographs of the quenching fault surface of: (a) PBAT–PLLA and (b) ksFIB/PLLA; SEM micrographs of the quenching fault surface and marginal surface of (c)
ksFAB/PLLA and (d) F-ksFAB/F-PBAT–PLLA.

sound waves. The effect of flame retardants on sound absorptivity holes caused by flame retardants, and it is a reflection of the poor
of the composites was also examined. It is found that the compos- compatibility between fire retardants and matrix resin. Comparing
ite materials with the flame retardants is superior to the materials the sound absorption curve of PBAT–PLLA and ksFAB/PBAT–PLLA,
without the flame retardants, which may be due to the molecular there is abated effect of sound-absorbing from the operating fre-
 D. Chen et al. / Composites: Part A 41 (2010) 1012–1018
Fig. 6. Horizontal–vertical organization of ramie fabrics in ksFAB/PLLA, chaotically distributed organization of short ramie fibers in ksFIB/PLLA and the hierarchical
organization of fiber.
quency of 1400–1600 Hz in the composites with ksFAB. And com-
paring the sound absorption curve of PBAT–PLLA and F-ksFAB/F-
PBAT–PLLA, there is increasing tendency of sound-absorbing from
the operating frequency of 1400–1600 Hz in the composites with
fire retardants. The sound absorptivity of PLLA, PBAT–PLLA,
ksFIB/PLLA, ksFAB/PLLA, ksFAB/PBAT–PLLA and F-ksFAB/F-PBAT–
PLLA at different operating frequency are shown in Table 2.
Fig. 3b and c shows the impedance ratio of different kinds of PLLA
composites. The larger the impedance ratio value is, the lower the
sound absorptivity is. In value, the impedance ratio of PLLA is lar-
ger than that of PBAT–PLLA, ksFAB/PLLA has larger impedance ratio
than ksFIB/PLLA and ksFAB/PBAT–PLLA has larger impedance ratio
than F-ksFAB/F-PBAT–PLLA, and all of the results are in accord with
the result of sound absorption property measurement.
3.3. Morphology analysis
SEM micrographs of the surface and the quenching fault surface
of ramie fiber are presented in Fig. 4. As shown in Fig. 4a and b, the
surface of ramie fibers is very dense, there is no apparent minute
crevices, but from the observations of the quenching cross-section
of fiber, we can see that the structure of fiber is a dense hollow
structure as can be seen in Fig. 4c and d. This porous structure
has a certain effect on the empty for the sound absorption, further
this is also related to the distribution of fibers in the composites.
For the short ramie fiber, due to its random distribution in the
composites, there is a considerable portion of porous structure,
which can absorb sound waves. But for the ramie fabric, due to
its tightly arranged structure, when the sound waves hit the dense
fiber bundle wall, they reflect. Pectin, lignin and hemicellulose and
other low-molecular weight materials can form a dense layer on
the surface of ramie fibers, so the reflection is higher. As shown
in Fig. 5a, the fault surface of PBAT–PLLA is not compact and mi-
cro-phase separation can be clearly seen. As is shown in Fig. 5b,
a lot of short ramie fibers is arrayed with random distribution in
the ksFIB/PLLA composites. The SEM micrographs of Fig. 5c and d
shows that the marginal surface of ksFAB/PLLA and F-ksFAB/F-
PBAT–PLLA is very dense and with the horizontal–vertical arrange-
ment fiber bundlesmaking the sound cannot be absorbed by the
composites easily. Fig. 6 demonstrates the porosity of the single
1017
ramie fiber bundle and the distribution of short ramie fiber and
ramie fabric in the PLLA composites. There are many micropores
and continuous bubbles in the porous structure of single ramie
fiber bundle. When the sound wave is incident on the surface of
porous structure of ksFIB/PLLA, the air motion and compression
in micropores caused by sound wave vibration can cause the fric-
tion with micropore wall and let the air that close to the micropore
wall cannot move easily. Because of the friction and viscous forces,
there are a considerable part of the sound energy can be converted
to heat energy and cause sound energy attenuation. On the other
hand, the heat loss caused by heat exchange between the air in
the micropores and the micropore wall can also cause sound en-
ergy attenuation. The random distribution of ksFIB in the PLLA
composites can let most of the sound waves hit the micropores
of fiber bundle and strengthen the sound absorption effect. These
special structures and the distribution are the main reason for
the acoustical absorptivity.
4. Conclusions
The data of sound absorption property measurement show that
the composites with short ramie fiber have better sound absorp-
tion property than the ramie fabric reinforced PLLA composites.
And the adding of flame retardant APP and plasticizer PBAT has po-
sitive effect on the sound absorption property of the ramie fabric/
PLLA composites. Moreover, morphological studied by SEM reveal
the micro-phase separation in the PBAT/PLLA composites, the
porosity of the single ramie fiber bundle and the distribution of
short ramie fiber and ramie fabric in the PLLA composites. These
special structures and the distribution are the main reason for bet-
ter acoustical absorptivity.
Acknowledgements
This work is supported by the National High Technology Re-
search and Development Program of China (No. 2006AA02Z248),
the Program of Shanghai Subject Chief Scientist (No. 07XD14029)
and the fund of Shanghai International Co-operation of Science
and Technology (No. 075207046).
1018 D. Chen et al. / Composites: Part A 41 (2010) 1012–1018

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