Original Article

Effects of heat treatment on the thermal

and mechanical properties of ramie
fabric-reinforced poly(lactic acid)
biocomposites

Journal of Reinforced Plastics

and Composites
2015, Vol. 34(1) 2836
! The Author(s) 2014
Reprints and permissions:
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DOI: 10.1177/0731684414562222
jrp.sagepub.com

Xie Chen1, Jie Ren1,2, Naiwen Zhang1, Shuying Gu1,2

and Jianbo Li1,2

Abstract
Laminated biocomposites based on ramie fabric and poly(lactic acid) were prepared through hot compression molding
followed by direct cooling (without heat treatment) or melt crystallization (with heat treatment). The effects of heat
treatment and ramie fabric reinforcement on the thermal and mechanical properties of poly(lactic acid) composites were
studied. X-ray diffraction and differential scanning calorimetry measurements confirmed that the heat treatment was able
to promote the formation of crystals and enhance the crystallinity of poly(lactic acid), and the addition of ramie fabric
also accelerated the crystallization rate of poly(lactic acid). Hence, heat treatment and ramie fabric reinforcement both
can improve the thermal stability of poly(lactic acid) biocomposites remarkably. The heat deflection temperature of
poly(lactic acid)/24 wt% ramie fabric biocomposite with heat treatment was up to 149.3 C, with a highest increase of
90.7 C. The mechanical properties of the ramie fabric-reinforced poly(lactic acid) biocomposites were also improved
after heat treatment.

Keywords
Poly(lactic acid), ramie fabric, reinforcement, composites, thermal properties, mechanical properties

Introduction
Fiber reinforcement is an eective approach for
improving the mechanical properties of polymer materials. The traditional ber-reinforced polymer composites have been widely used in the automobile, airplane,
and electronic industries where materials with high
strength, stiness and thermal stability are required.
In the past decades, the growing concerns about oil
crisis and environmental protection have led to the
development of green composites with natural
reinforcement and biodegradable resin matrix. To
obtain practical green composites, considerable attention has been given to natural bers such as kenaf,13
ax,46 hemp,79 jute,10,11 ramie,12 bamboo,1315 pulp
bers,16 and microbrillated cellulose (MFC)1719 as
reinforcements in composites manufacturing, because
biodegradable natural bers with outstanding mechanical properties are cheaper and lighter than glass ber.20
Ramie ber is especially highlighted by many
researches, because it provides best heat resistance

and superior tensile strength and modulus than that

of jute, ax, hemp, and sisal.12,21
Among all the available biodegradable resins,
poly(lactic acid) (PLA), a naturally resourced thermoplastic resin, is the most extensively researched and utilized biopolymer as a substitute for conventional
petroleum-based polymers. It is widely used in disposable packaging and items, agriculture, garments, medical devices, and automobiles.22,23 However, the
practical applications of PLA have still been limited

1
Institute of Nano and Bio-Polymeric Materials, School of Material
Science and Engineering, Tongji University, Shanghai, China
2
Key Laboratory of Advanced Civil Engineering Materials (Tongji
University), Ministry of Education, Shanghai, China

Corresponding author:
Jianbo Li, Key Laboratory of Advanced Civil Engineering Materials (Tongji
University), Ministry of Education, Shanghai 201804, China.
Email: lijianbo@tongji.edu.cn

Chen et al.
by its inherent properties, such as the lack of toughness,
low heat deection temperature (HDT), and low thermal stability.
Our previous studies have indicated that the mechanical properties of PLA, such as tensile, exural,
and impact strength, can be much improved by
adding ramie or jute short bers, and ramie fabric
(RF) using the two-roll mill or hot compression molding technique.12,2426 Furthermore, natural bers and
inorganic llers can improve the thermal and crystallization properties of polymers.27,28 The degree of crystallinity can also be increased by annealing.29 Up to
now, the eects of heat treatment on the thermal and
mechanical properties of PLA/RF laminated composites were rarely investigated and deserve further studies
due to the potential applications in automobile and
electronic elds.
In this study, we prepared the PLA/RF laminated
biocomposites through hot compression molding followed by direct cooling (without heat treatment) or
melt crystallization (with heat treatment). The eects
of heat treatment and RF reinforcement on the thermal
and mechanical properties of the RF-reinforced PLA
biocomposites were studied through HDT test, X-ray
diraction (XRD), dierential scanning calorimetry
(DSC), dynamic mechanical analysis (DMA), and
mechanical properties testing.

Experimental
Materials
Ramie fabric (RF) as reinforcement layer was supplied
by Jintan Jinlan Ramie Fiber Factory (Jiangsu, China),
and was in the form of plain weave fabric with area
density of 120 g/m2. PLA lm as biodegradable
matrix material with area density of 350 g/m2 was
obtained from Shanghai Tong-Jie-Liang Biomaterials
Co., Ltd.

Fabrication of the laminated composites

The RF and PLA lm were dried in a vacuum drying
oven at 60 C for 24 h before use to ensure that all the
absorbed moisture was removed. Pre-drying should
help prevent void formation during the hot pressing
process. The multilayer lm-stacking procedure and
compression molding were applied to prepare PLA
composites with dierent ramie content. Lay-ups were
prepared in which the RF was laminated with PLA lm
layers on either side. Fabrics were laminated with the
same warp direction. The weights of fabrics and PLA
lms were recorded before composite fabrication to
monitor the weight percentages of the ramie. The
laying-ups were rst pre-heated at 175 C for 2 min,

29
hot pressed at 1 MPa for 1 min, and then hot pressed
into sheets at 6 MPa for 3 min. After hot compression
molding, the melted samples were either cooled directly
in a cold press machine at 2.5 MPa to obtain amorphous samples (samples without heat treatment), or meltcrystallized in another hot-press process at 115 C for
1 h followed by natural cooling to obtain highly crystallized samples (samples with heat treatment). The composites obtained (170 mm  170 mm  3.5 mm) were
then cut into desired shapes for mechanical and other
evaluation.

Characterization
Mechanical properties. Tensile properties of RF-reinforced PLA biocomposites were determined according
to GB/T 1447-2005.30 The type I tensile specimens were
tested by a CMT5105 universal testing machine
(Shenzhen Sansi Material Instruments Ltd., China)
with a drawing speed 5 mm/min. Flexural properties
were measured according to GB/T 1449-2005.31
The dimensions of each specimen were 80 mm 
10 mm  3.5 mm, and tested by a DXLL-5000 universal
testing machine (Shanghai D&G Measure Instrument
Co. Ltd., China) with a loading speed of 2 mm/min.
The Charpy impact tests were performed by an
impact tester in accordance with GB/T 1043-2008.32
The size of notched specimen was 80 mm  10 mm 
3.5 mm. All of the results are the mean values of ve
measurements.
Dynamic mechanical analysis. DMA was carried out on a
Q 800 dynamic mechanical analyzer (Tainstsh, USA) in
the 3-point bending mode with a frequency of 10 Hz.
The specimens were heated from 30 C to 130 C at a
heating rate of 2 C/min. The dimensions of each specimen were 60 mm  10 mm  3.5 mm.
X-ray diffraction. XRD analysis was performed on a
Rigaku-D/max 2550VB3+/PC X-Ray diractometer
(Rigaku International Corporation, Japan) with the
copper target. The scanning range and rate were 5 45
and 5 /min. The accelerating voltage was set at 40 kV.
Heat deflection temperature. HDT was tested according
to GB/T 1634-200433 by a XWB-300 apparatus
(Chengde Kecheng Testing Machine Co., Ltd.,
China), with a constant exural stress of 0.45 MPa at
the center of a three-point exural test sample. The
specimens were heated at a heating rate of 2 C/min
from room temperature up to 200 C.
Differential scanning calorimetry. DSC measurements were
performed on a Q100 thermal analysis system
(Tainstsh, USA). The samples were tested at a heating

30
rate of 10 C/min from room temperature up to 200 C
under nitrogen ow (50 ml/min). The weight of each
sample was 510 mg.

Results and discussion

Effects of heat treatment and the presence of RF
on the crystallinity of PLA
The eect of heat treatment and the eect of RF
reinforcement on PLA crystallization performance
were evaluated by XRD and DSC analyses. Figure
1(a) shows the XRD of amorphous neat PLA (the
melted samples with direct cold-pressing) and crystallized neat PLA (the melted samples with melt-crystallization at 115 C for 1 h). Figure 1(b) shows the
patterns of PLA/24 wt% RF biocomposite with and
without heat treatment. No peak appeared in either
neat PLA or PLA/24 wt% RF biocomposite without
heat treatment which revealed an amorphous nature.
However, the neat PLA and biocomposite with heat
treatment exhibited higher and sharper peaks at the
angular positions around 16.6 and 19.0 . These reection peaks corresponded to the 110 and 020 plane of
PLA crystal, which were in agreement with previous
conclusions reported by other studies.34,35 The results
revealed that heat treatment brought about the formation of prefect crystals and increased the degree of
crystallinity.28
The DSC results of neat PLA and PLA/24 wt% RF
biocomposite without heat treatment are shown in
Figure 2. The glass transition temperature (Tg), cold
crystallization temperature (Tcc), and melt temperature
(Tm) of PLA/24 wt% RF biocomposite were similar to
those of neat PLA. Moreover, the Tcc of PLA/24 wt%
RF biocomposite is 108.4 C which is slightly lower

Journal of Reinforced Plastics and Composites 34(1)

than that of neat PLA (110.8 C). Thus, the PLA/
24 wt% RF biocomposite has a quicker start of crystallization than that of neat PLA. These results revealed
that the RF acts as nucleating agent for the composite,
and accelerates the crystallization of PLA.35,36

Heat deflection temperature

HDT can be used to describe indirectly the thermomechanical property of polymer, which can be inuenced by the crystallinity and other factors such as
the reinforcement. Figure 3 shows the HDT testing
results of neat PLA and PLA biocomposites. The
HDT of neat PLA without heat treatment is 53.0 C,
which is far below the heat-resistant temperature of
products used in daily life (above 90100 C).28 With

Figure 2. DSC thermogram of neat PLA and PLA/24 wt% ramie

fabric biocomposite.

Figure 1. XRD of (a) PLA and (b) PLA/24 wt% ramie fabric biocomposite with or without heat treatment.

Chen et al.
the addition of RF, the HDTs of PLA/RF biocomposites were improved by only 1.55.5 C, without obvious
increment. It is worth noting that after heat treatment
there is a great increase (47.5 C) of the HDT of neat
PLA. It is mainly because the increased degree of crystallinity promotes the improvement of HDT in PLA
biocomposites. Moreover, PLA biocomposites with
reinforcing fabric and after heat treatment show an
even greater increase of HDT. The higher the ramie
proportion, the greater will be the increase of the
HDT of PLA. The HDT of PLA/24 wt% RF biocomposite is about 149.3 C, with the greatest increase
(90.7 C). The addition of RFs promotes the faster
and larger growing of PLA crystals around ramie
bers compared to the growing of crystals in neat
PLA with heat treatment. A similar phenomenon was
reported by Shi et al.28 However, the HDT of PLA/
38 wt% RF biocomposite is slightly lower than that

31

Figure 3. HDT of neat PLA and PLA/RF biocomposites with

and without heat treatment.

Figure 4. Tensile properties of neat PLA and PLA/RF biocomposites with and without heat treatment.

32
of PLA/24 wt% RF biocomposite. That could be
caused by the weakened interlayer adhesion. As the
mass percent of RF increases, PLA matrix resin is
insucient to cover the increased surface of ramie
ber bundles.

Mechanical properties
Tensile, exural, and impact properties of the neat PLA
and PLA/RF biocomposites were studied to evaluate
the eect of heat treatment and ramie reinforcement
on the mechanical performance of PLA composites.
Figure 4 shows the tensile properties of PLA and composites. As the weight percentage of RF increases, tensile strength as well as tensile modulus and elongation
at break of the PLA/RF biocomposites without heat
treatment increases. Compared with neat PLA, the tensile strength of PLA/24 wt% RF biocomposite
increases from 29.37 MPa to 66.33 MPa, and the modulus is also improved from 944.57 MPa to 1642.91 MPa.
Knitting structure and high strength of ramie ber
bring out the improvement which indicates good interfacial adhesion between PLA and RFs. But a reduction
of mechanical properties occurs in PLA/38 wt% RF
biocomposite. The higher use level of ramie results in
the decrease proportion of PLA matrix resin in the
biocomposite, so that the bonding strength between
PLA matrix and RFs is lowered. The stress distribution
and transfer from PLA matrix to RFs are aected by
lower interfacial adhesion.12,37
The PLA and PLA/RF biocomposites with heat
treatment have higher tensile strength and modulus,
but lower elongation at break when compared to their
counterparts without heat treatment. After heat

Journal of Reinforced Plastics and Composites 34(1)

treatment, the tensile strength of neat PLA is increased
from 29.37 MPa to 54.52 MPa, and the tensile modulus
is increased from 944.57 MPa to 1240.01 MPa, while
the elongation at break is decreased from around 4%
to 3%. It is because the crystallization of semi-crystalline polymer results in brittlement of the polymer so
that the elongation at break is declined.38 It is obvious
that the tensile strength and modulus of PLA/RF biocomposites are improved by heat treatment. The tensile
strength of PLA/24 wt% RF biocomposite reaches to
76.07 MPa, and the strength of PLA/38 wt% RF biocomposite is also increased from 51.14 MPa to
68.27 MPa. Although the crystallization of PLA
makes the tensile strength and modulus of PLA/
38 wt% RF biocomposite improved, the tensile properties are not better than those of PLA/24 wt% RF biocomposite. The eect of weakened interfacial adhesion
surpasses the reinforcing eect of PLA crystallization
and RF.
As shown in Figure 5, exural strength and modulus
of PLA/RF biocomposites without heat treatment
increased along with increasing RF content, whereas
PLA/38 wt% RF biocomposite appeared to have a
downtrend due to the decreased interfacial adhesion.
After heat treatment, the neat PLA and biocomposites
had better exural properties. The exural strength of
neat PLA was increased from 41.15 MPa to 88.59 MPa,
and the exural modulus was increased from
3479.41 MPa to 3603.19 MPa. The exural strength
and modulus of PLA/24 wt% RF biocomposite
reached to 116.22 MPa and 5069.41 MPa, respectively.
The reduction of interfacial adhesion made the exural
properties of PLA/38 wt% RF biocomposite inferior to
those of PLA/24 wt% RF biocomposite, although the

Figure 5. Flexural properties of neat PLA and PLA/RF biocomposites with and without heat treatment.

Chen et al.

33
crystallization was benecial to improvement of exural properties.
The impact strength of PLA/RF biocomposite without heat treatment increased from 3.02 kJ/m2 to
11.53 kJ/m2 with increase of the ramie percentage to
24% as shown in Figure 6. When the ramie content
reaches to 38%, the impact strength of PLA/RF biocomposite decreases because of the weakened interfacial adhesion between PLA matrix and RF. The
PLA/RF biocomposites with heat treatment shows
slight improvement in impact strength. A similar
trend exists in the tensile and exural properties of
PLA/RF biocomposites.

Dynamic mechanical analysis

Figure 6. Impact properties of neat PLA and PLA/RF biocomposites with and without heat treatment.

DMA of the neat PLA and PLA/RF biocomposites

were performed to evaluate the eects of RF reinforcement and heat treatment on the thermo-mechanical

Figure 7. DMA thermograms of neat PLA and PLA/RF biocomposites without heat treatment.

34

Journal of Reinforced Plastics and Composites 34(1)

Figure 8. DMA thermograms of neat PLA and PLA/RF biocomposites with heat treatment.

properties of PLA composites. Figure 7 shows the storage modulus, loss modulus, and tan d of neat PLA and
PLA/RF biocomposites without heat treatment. Figure
7(a) showed that the storage modulus of neat PLA
below Tg is 3000 MPa. Then it drops to 5 MPa at
around 85 C, and climbs to 400 MPa at around
105 C. The uptrend of storage modulus is caused by
the cold crystallization of the amorphous PLA.35 The
addition of RF improves the storage modulus and loss
modulus of PLA composites. Compared with neat
PLA, the PLA/24 wt% RF biocomposite obtains the
largest storage modulus and loss modulus. The trend
is in accord with those of mechanical properties of
PLA/RF biocomposites. The peak in loss factor is in
connection with the glass-transition temperature (Tg).
The reinforcer RF rarely inuences Tg of PLA/RF biocomposites without heat treatment.
Figure 8 shows the DMA thermograms of neat
PLA and PLA/RF biocomposites with heat treatment.
From Figure 8(a), it can be seen that with increasing
temperature, the storage modulus of PLA composites

shows almost no change in the glassy state below

60 C, and then gradually decreases. It is probably
because the PLA is not fully crystallized after heat
treatment and -relaxation of amorphous structure
leads to the slow decline of storage modulus
around Tg.35 The storage modulus of PLA/RF biocomposites with heat treatment is improved compared
with that of PLA/RF biocomposites without heat
treatment. The heat treatment improves the storage
modulus of neat PLA at 30 C from 3000 MPa to
4000 MPa, whereas at around 84 C the storage modulus increases from 5 MPa to 600 MPa. The peak of loss
modulus remarkably decreases after heat treatment,
and the loss modulus of PLA/RF biocomposites with
dierent ramie content is close. From Figure 8(c), the
Tg of PLA/RF biocomposites with heat treatment
shows a slight shift to the high temperature region,
and the magnitude of the tan d peak decreases in evidence, which is believed to be attributed by the
increased crystallization and the restriction of the
chain movement of PLA.

Chen et al.

Conclusions
XRD and DSC analyses revealed that heat treatment
promoted the formation of PLA crystal and enhanced
the crystallinity of PLA, and the RF as nucleating agent
accelerated the crystallization rate of PLA. Remarkable
increase in HDT of PLA/RF biocomposites was
obtained due to the heat treatment and RF reinforcement. The HDT of PLA/24 wt% RF biocomposite is
149.3 C with a greatest increase (90.7 C). Mechanical
tests show that the mechanical properties of biocomposites improved along with increase in ramie content,
whereas PLA/38 wt% RF has a downtrend due to the
decreased interfacial adhesion. Heat treatment
improves the mechanical properties of neat PLA and
biocomposites. DMA measurements conrmed that the
addition of RF improved the storage modulus and loss
modulus of PLA/RF biocomposites. After heat treatment, the storage modulus of PLA/RF biocomposites
were improved, and the peak of loss modulus obviously
decreased. The Tg of PLA/RF biocomposites with heat
treatment showed a slight shift to high temperature,
and the magnitude of the tan d peak decreased in evidence. The RF-reinforced PLA biocomposites with
improved thermal and mechanical properties can
potentially be used in the automobile and electronic
industry applications which require high strength, stiness, and thermal stability.
Conflict of interest
None declared.

Funding
This work was supported by the National Natural Science
Foundation of China (Grant No. 51203118), the National
Key
Technology
R&D
Program
(Grant
No.
2012BAI17B05), the Shanghai Automotive Industry Science
and Technology Development Foundation (Grant No. 1006),
the Fundamental Research Funds for the Central
Universities, and the Open Funds for Characterization of
Tongji University.

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