Article

Polypropylene/Short Glass Fibers Composites:

Effects of Coupling Agents on Mechanical Properties,
Thermal Behaviors, and Morphology
Jia-Horng Lin 1,2,3 , Chien-Lin Huang 4 , Chi-Fan Liu 5 , Chih-Kuang Chen 6 , Zheng-Ian Lin 1 and
Ching-Wen Lou 7, *
Received: 13 October 2015; Accepted: 20 November 2015; Published: 2 December 2015
Academic Editor: Wen-Hsiang Hsieh
1

2
3
4
5
6
7

Laboratory of Fiber Application and Manufacturing, Department of Fiber and Composite Materials,
Feng Chia University, Taichung City 40724, Taiwan; jhlin@fcu.edu.tw (J.-H.L.);
chengyen0624@gmail.com (Z.-I.L.)
School of Chinese Medicine, China Medical University, Taichung City 40402, Taiwan
Department of Fashion Design, Asia University, Taichung City 41354, Taiwan
Department of Fiber and Composite Materials, Feng Chia University, Taichung City 40724, Taiwan;
clhuang@mail.fcu.edu.tw
Office of Physical Education and Sports Affairs, Feng Chia University, Taichung City 40724, Taiwan;
cfliu@fcuoa.fcu.edu.tw
The Polymeric Biomaterials Laboratory, Department of Fiber and Composite Materials,
Feng Chia University, Taichung City 40724, Taiwan; chihkchen@fcu.edu.tw
Institute of Biomedical Engineering and Materials Science, Central Taiwan University of Science and
Technology, Taichung City 40601, Taiwan
Correspondence: cwlou@ctust.edu.tw; Tel.: +886-4-2451-7250 (ext. 3405); Fax: +886-4-24510871

Abstract: This study uses the melt compounding method to produce polypropylene (PP)/short
glass fibers (SGF) composites. PP serves as matrix while SGF serves as reinforcement. Two
coupling agents, maleic anhydride grafted polypropylene, (PP-g-MA) and maleic anhydride grafted
styrene-ethylene-butylene-styrene block copolymer (SEBS-g-MA) are incorporated in the PP/SGF
composites during the compounding process, in order to improve the interfacial adhesion and create
diverse desired properties of the composites. According to the mechanical property evaluations,
increasing PP-g-MA as a coupling agent provides the composites with higher tensile, flexural, and
impact properties. In contrast, increasing SEBS-g-MA as a coupling agent provides the composites
with decreasing tensile and flexural strengths, but also increasing impact strength. The DSC results
indicate that using either PP-g-MA or SEBS-g-MA as the coupling agent increases the crystallization
temperature. However, the melting temperature of PP barely changes. The spherulitic morphology
results show that PP has a smaller spherulite size when it is processed with PP-g-MA or SEBS-g-MA
as the coupling agent. The SEM results indicate that SGF is evenly distributed in PP matrices, but
there are distinct voids between these two materials, indicating a poor interfacial adhesion. After
PP-g-MA or SEBS-g-MA is incorporated, SGF can be encapsulated by PP, and the voids between
them are fewer and indistinctive. This indicates that the coupling agents can effectively improve
the interfacial compatibility between PP and SGF, and as a result improves the diverse properties of
PP/SGF composites.
Keywords: polypropylene (PP); Short glass fibers (SGF); coupling agent; mechanical properties;
thermal behaviors

Materials 2015, 8, 82798291; doi:10.3390/ma8125451

www.mdpi.com/journal/materials

Materials 2015, 8, 82798291

1. Introduction
Thermoplastic polymer has formed a new trend in material development, and it has the
advantages of low production cost, great diversity, sufficient sources, light weight, good physical
properties, and chemical resistance, as well as various efficient manufacturing process. Therefore,
there are a great number of plastic products commercially available.
Polypropylene (PP) is the most consumed polymer globally, and it has a comparably light
weight. Because of its good processing features, high chemical stability, and electrical insulation, PP
has been commonly used in the spare parts of vehicles, bicycles, electronic products, civil necessities,
medical instruments, and chemical products. However, it has low mechanical properties and does
not have any functions, which restrict its application ranges [15]. Current studies reinforce PP in
order to have greater mechanical properties; reinforcing materials include rigid particles fillers, such
as nanoclay [68], calcium carbonate [9], and silicon dioxide [10,11], as well as short fibers, such as
glass fiber, carbon fiber [1217], and basalt fiber [18]. In particular, short glass fiber causes PP to be
the strongest mechanically.
PP is a nonpolar polymer and has a poor interfacial adhesion with short glass fiber (SGF). This
disadvantage is improved by using a coupling agent [1926] or increasing the surface roughness
of fibers during the compounding process [2729]. Wong et al. examined three coupling agents
for the mechanical properties and interfacial compatibilities of composites made of PP and recycled
carbon fibers (CF). The test results showed that the tensile and flexural strengths of the composites
were significantly improved. The interfacial compatibility of PP and CF was dependent on the
acid anhydride group and molecular weight [30]. Broughton et al. used aminosilane and titanate
as the coupling agent for glass flake and PP and found that the improved interfacial adhesion
of the composites resulted in greater tensile, flexural, and impact strengths [31]. In contrast,
Eslami-Farsani et al. added nanoclay to basalt fiber/polypropylene composite in order to increase
the roughness of the fibers. The test results indicated that after the adhesion of nanoclay to the basalt
fibers, the layered structure improved the interfacial adhesion of two materials, and thereby improved
the mechanical properties of the composites [27]; however, the reinforcement was not permanent. In
contrast, using a coupling agent can improve the interfacial adhesion between constituent materials,
and this method forms a chemical reaction between the matrix and fibers, thereby effectively and
permanently improving the mechanical properties of the composites.
This study aims to produce composites that meet the requirements of different products and to
expand the applications of the composites, and compares different characterizations of the PP/SGF
composites produced with two different coupling agents. In this study, short glass fibers that
possess high strength, high modulus, and good thermal stability are synthesized with PP in order
to reinforce the mechanical properties of PP. Two coupling agents (i.e., maleic anhydride grafted
polypropylene, PP-g-MA, and maleic anhydride grafted styrene-ethylene-butylene-styrene block
copolymer, SEBS-g-MA) are used for a greater combination between PP and SGF. PP-g-MA has
the same molecular structure that PP has, and thus enhances the bonding between two materials.
Similarly, SEBS-g-MA, an elastomer, has a structure that includes an ethylene-butylene segment that
is compatible with PP. Therefore, SEBS-g-MA can improve the compatibility between PP and SGF,
and provides the composites with impact resistance. Finally, the influences of these coupling agents
on the mechanical properties, thermal behaviors, spherulite structure, and interfacial adhesion are
examined. This study can thus serve as a reference for the selection of a coupling agent according to
the diverse applications of the composites.
2. Experimental Section
2.1. Materials
Polypropylene (PP; YUNGSOX 1080; Formosa Plastics Corporation, Taipei, Taiwan) was a
homopolymer with a melt flow rate of 10 g/10 min (ISO1133). Short glass fiber (SGF; 202P; Taiwan

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Materials 2015, 8, 82798291

Glass Ind. Corp., Taipei, Taiwan) had a length of 3.2 mm and a diameter of 13 m, and was
treated with a silane coupling agent. Maleic anhydride grafted polypropylene (PP-g-MA; DuPont
Fusabond P613) was purchased from DuPont, Wilmington, DE, USA. Maleic anhydride grafted
styrene-ethylene-butylene-styrene block copolymer (SEBS-g-MA; Kraton FG1901X) was purchased
from Kraton, Houston, TX, US. Physical properties of materials are summarized in Table 1.
Table 1.
Physical properties of materials.
Polypropylene, PP; Short Glass Fiber, SGF;
Maleic Anhydride grafted Polypropylene, PP-g-MA; Maleic Anhydride grafted Styrene-EthyleneButylene-Styrene block copolymer, SEBS-g-MA.
Material

Density
(g/cm3 )

Melt Index
(g/10 min)

0.900
0.903
0.910

10 (230 C / 2.16 Kg measured)

120 (190 C / 2.16 Kg calculated)
22 (230 C / 5 Kg measured)

PP
SGF
PP-g-MA
SEBS-g-MA

Diameter Length
(m)
(mm)
13
-

3.2
-

Graft Weight
(%)
0.5
1.5

2.2. Methods
Various amounts of PP, a specified amount of 25 wt % of SGF, and 2, 4, 6, or 8 wt %
of a coupling agent (PP-g-MA or SEBS-g-MA) were mixed to form different PP/SGF/PP-g-MA
blends and PP/SGF/SEBS-g-MA blends. Different blends were dried in an oven at 80 C for
8 h in order to remove moisture, after which they were made into PP/SGF/PP-g-MA pellets and
PP/SGF/SEBS-g-MA pellets via a single screw extruder (SEVC-45, Re-Plast Extruder Corp., Miaoli,
Taiwan), in which the temperatures of the three barrels and the die were 210 C, 220 C, 230 C, and
210 C, respectively, and the screw speed was 36 rpm.
The pellets were then dried in an oven at 80 C for 8 h, followed by being made into composites
by using an injection machine (Ve-80, VICTOR Taichung Machinery Works Co., Ltd., Taichung,
Taiwan), in which the temperatures of three barrels and the nozzle were 210 C, 220 C, 230 C,
and 210 C, respectively. The control group was the pure PP/SGF composites made of 25 wt % SGF
and 75 wt % PP.
2.3. Measurements
2.3.1. Tensile Tests
An Instron 5566 Universal Tester (Instron, Canton, MA, USA) was used to measure the
tensile strength and tensile modulus, as specified in ASTM D638-10. Samples were made into
dumbbell-shapes according to ASTM D638 Type IV. The crosshead speed was 5 mm/min. There
were a total of 5 samples for each specification.
2.3.2. Flexural Tests
The flexural test was performed by using an Instron 5566 Universal Tester (Instron, Canton,
MA, USA), as specified in ASTM D790-10. The load and flexural modulus of the samples was
measured. There were a total of 5 samples for each specification, and each sample had a size of
127 mm 12.7 mm 3.2 mm. The test speed was 2 mm/min, and the support span was 50 mm. The
test results were then used to calculate the flexural strength with the following Equation (1):
f max

3PL
2bd2

(1)

where P is the load (N); L is the support span (mm); b is the sample width (mm); and d is the sample
thickness (mm).

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Materials 2015, 8, 82798291

2.3.3. Izod Impact Tests

This test followed ASTM D 256-10. An Izod impact strength tester (CPI, ATLAS, Mount Prospect,
IL, USA) was used to measure the impact strength of the samples. The samples had a 45 V-shaped
cut with a depth of 0.25 mm, and were sized as 63.5 mm 12.7 mm 3.2 mm. There were a total of
5 samples for each specification.
2.3.4. Differential Scanning Calorimetry (DSC)
Composite samples of 810 mg were then placed in the DSC (Q200, TA Instruments, New Castle,
DE, USA). Samples were heated from 40 C to 200 C at 10 C/min increments, and were isothermally
kept at 200 C for 10 min, in order to delete the thermal history. Next, samples were cooled to
40 C with the same increments. During the second cycle, the samples were heated and then cooled
between these two temperatures with the same increments. The crystallinity of composites was
calculated from Equation (2). The enthalpy corresponding to the melding of 100% crystalline PP
is 209 J/g [32,33].
Hm
XC
(2)
p1 f q
Hm
where XC is crystallinity; Hm is the apparent enthalpy of crystallization; H m is the enthalpy
corresponding to the melting of 100% crystalline PP; and f is the weight fraction of SGF.
2.3.5. Polarized Light Microscopy (PLM)
The spherulite morphology of the samples was observed by using a PLM (BX51, Olympus,
Tokyo, Japan). A small amount of sample was placed on a glass slide and was then melted to form a
film at 200 C. Samples were then cooled to 130 C at 10 C/min increments, and were kept at 130 C
for the observation of spherulite morphology.
2.3.6. Scanning Electron Microscope (SEM)
Samples were affixed to the sample holder by using carbon paste and were then coated with a
thin gold layer. The fractured surface of the samples was then observed by using an SEM (S3000N,
Hitachi, Tokyo, Japan) at a voltage of 15 kV.
3. Results and Discussion
3.1. Effects of Two Coupling Agents (PP-g-MA or SEBS-g-MA) on Mechanical Properties of
PP/SGF Composites
The tensile properties of various PP/SGF composites are compared to those of pure PP/SGF
composites (i.e., the control group), as indicated in Figure 1 and Table 2. The composites that are
incorporated with 8 wt % PP-g-MA have a tensile strength of 79.0 MPa, in comparison to that of
the control group (67.6 MPa). The tensile strength of the composites is proportional to the amount
of PP-g-MA. In contrast, the composites that are incorporated with 8 wt % of SEBS-g-MA have a
lower tensile strength (50.6 MPa) than that of the control group. The tensile strength is inversely
proportional to the amount of SEBS-g-MA.
The tensile modulus of the PP/SGF composites incorporated with 8 wt % PP-g-MA is 2004 MPa,
which is greater than that of the control group (1998 MPa). However, increasing PP-g-MA hardly
influences the modulus of the composites. Conversely, the tensile modulus of the composites
incorporated with 8 wt % SEB-g-MA is 1683.6 MPa, which is lower than that of the control group.
Furthermore, the tensile modulus has a decreasing trend with increasing SEBS-g-MA.
Figure 2 and Table 2 indicate the flexural properties of various PP/SGF composites that are
in conjunction with different coupling agents. The incorporation of 8 wt % of PP-g-MA results
in a greater flexural strength of the composites (123.4 MPa) in comparison to that of the control

8282

Materials 2015, 8, 82798291

Materials 2015, 8, pagepage

group (99.3 MPa). The flexural strength increases as a result of the increasing PP-g-MA. However,
incorporation
of 8 wt
of SEBS-g-MA
decreases
the flexural
strengthstrength
of the composites
to 81.3 MPa.
the
incorporation
of 8% wt
% of SEBS-g-MA
decreases
the flexural
of the composites
to
Moreover,
the
flexural
strength
of
the
composites
shows
a
declining
trend
with
increasing
81.3 MPa. Moreover, the flexural strength of the composites shows a declining trend with increasing
SEBS-g-MA content.
content.
SEBS-g-MA

Figure
1. (a) Tensile
strengthstrength
and (b) tensile
modulus
PP (Polypropylene)/SGF
(short glass fiber)
Figure
1. (a) Tensile
and (b)
tensile of
modulus
of PP (Polypropylene)/SGF
(shortcomposites.
glass
fiber) composites.
Table 2. Mechanical properties of pure PP matrices and PP/SGF composites treated with various
amounts
coupling agents.
Table
2. of
Mechanical
properties of pure PP matrices and PP/SGF composites treated with various
amounts
of coupling agents.T (MPa)
Composite
PP
21.0 0.8
Composite
T 67.6
(MPa)
PP/SGF25
0.9
PP
21.0
0.8
PP-g-MA (2 wt %)
76.8
0.2
PP/SGF25 (4 wt %)
67.677.7
0.9
PP-g-MA
0.4
PP-g-MA (2 wt %)
76.8 0.2
PP-g-MA
(6
wt
%)
80.0
0.6
PP-g-MA (4 wt %)
77.7 0.4
PP-g-MA
wt %)
0.5
PP-g-MA
(6 wt(8%)
80.079.0
0.6
PP-g-MA
(8 wt %)
0.5
SEBS-g-MA
(2 wt %) 79.061.3
1.5
SEBS-g-MA (2 wt %)
1.5
SEBS-g-MA (4 wt %) 61.357.8
0.9
SEBS-g-MA (4 wt %)
57.8 0.9
SEBS-g-MA
(6
wt
%)
53.4

SEBS-g-MA (6 wt %)
53.4 0.8 0.8
SEBS-g-MA
wt %) 50.650.6
0.9
SEBS-g-MA
(8 wt(8%)
0.9

ET (GPa)
0.8 0.032
E1.9
T (GPa)
0.026
0.81.9
0.032
0.008
1.91.9
0.026
0.013
1.9 0.008
2.0

0.022
1.9 0.013
0.016
2.02.0
0.022
2.01.8
0.016
0.035
1.8 0.035
1.8 0.014
1.8 0.014
0.016
1.71.7
0.016
0.012
1.71.7
0.012

F (MPa)
47.9 1.3
99.3
F (MPa)
2.7
47.9
1.3
120.0
4.2
99.3
2.7
123.3
1.0
120.0 4.2
127.2

0.9
123.3 1.0
123.40.9
2.8
127.2
123.4
97.8 2.8
2.9
97.8 2.9
90.6 1.0
90.6 1.0
84.8
1.0
84.8 1.0
81.41.2
1.2
81.4

EF (GPa)
1.3 0.051
3.5EF(GPa)
0.045
1.30.268
0.051
3.2
3.5

0.045
3.4 0.031
3.2 0.268
3.5
3.40.032
0.031
3.6
3.50.035
0.032
3.60.320
0.035
3.2
3.2 0.320
3.2 0.031
3.2 0.031
3.0
3.00.052
0.052
2.9
2.90.076
0.076

IS (J/m)
44.8 0.0
(J/m)
73.7IS
3.3
44.8
0.0
101.9 7.5
73.7
3.3
103.5 10.1
101.9 7.5
103.5
3.6
103.5
10.1
97.5
5.6
103.5
3.6
5.6
77.797.5
0.0
0.0
82.077.7
3.5
82.0 3.5
86.286.2
2.7
2.7
90.390.3
2.7
2.7

Note.TTisisthe
the tensile
ET EisT the
tensile
modulus;
F is the
strength;strength;
EF is the flexural
modulus;
Note.
tensilestrength;
strength;
is the
tensile
modulus;
Fflexural
is the flexural
EF is the
flexural
and IS is the impact strength.
modulus; and IS is the impact strength.

The
The flexural
flexural modulus
modulus of
of the
the PP/SGF
PP/SGF composites increases to 3565.9 MPa as a result of the
the
incorporation
incorporation of
of 88 wt
wt %
% PP-g-MA,
PP-g-MA, in
in comparison
comparison to
to that
that of
of the
the control
control group
group(3503.4
(3503.4MPa).
MPa). The
The
flexural
does not
notfluctuate
fluctuatewith
withincreasing
increasingPP-g-MA.
PP-g-MA.InIn
contrast,
flexural
modulus
of
flexural strength does
contrast,
thethe
flexural
modulus
of the
the
PP/SGF
composites
decreases
to 2937.6
MPa,
comparisontotothe
the control
control group. The flexural
PP/SGF
composites
decreases
to 2937.6
MPa,
inincomparison
modulus
modulus is
is inversely
inversely proportional
proportional to
to the
the content
content of
of SEBS-g-MA.
SEBS-g-MA.
The
The impact
impact strength
strength of
of the
the PP/SGF
PP/SGF composites that are incorporated with different coupling
agents
agents is
is indicated
indicated in
in Figure
Figure 33and
andTable
Table2.2.The
Theimpact
impactstrength
strengthincreases
increasesfrom
from73.6
73.6J/m
J/mto
to97.5
97.5J/m
J/m
when
the
PP/SGF
composites
are
incorporated
with
8
wt
%
of
PP-g-MA.
Meanwhile,
the
impact
when the PP/SGF composites
strength
composites are incorporated with
strength increases
increases from
from 73.6
73.6J/m
J/m to
to 90.2
90.2 J/m
J/m when the PP/SGF
PP/SGF composites
8 wt
wt%%ofof SEBS-g-MA.
SEBS-g-MA. In
In summary,
summary, increasing
increasing coupling
coupling agent,
agent, either
either PP-g-MA
PP-g-MA or
or SEBS-g-MA,
SEBS-g-MA,
improves
the
impact
strength
of
PP/SGF
composites.
Table
3
summarizes
the
variation
in tensile,
improves the impact strength of PP/SGF
Table
tensile,
flexural,
flexural, and
and impact
impact properties
properties as
as percentages.
percentages.
The
The tensile,
tensile, flexural,
flexural, and
and impact
impact strengths
strengthsof
ofPP/SGF
PP/SGF composites are proportional to the content
content
of
PP-g-MA
that
is
incorporated
with
the
composites.
The
mechanical
properties
are
reinforced
of
that is incorporated with the composites. The mechanical properties are reinforced due
due
to improved
the improved
interfacial
compatibility
between
PP and
There
is esterification
between
to the
interfacial
compatibility
between
PP and
SGF.SGF.
There
is esterification
between
the
the
hydroxyl
groups
on
the
surface
of
SGF
and
the
acid
anhydride
groups
of
PP-g-MA,
and
hydroxyl groups on the surface of SGF and the acid anhydride groups of PP-g-MA, and the covalent
the
covalent
is then
formed, asinindicated
Figure
4. As
a result, increases
PP-g-MAthe
increases
the
bond
is thenbond
formed,
as indicated
Figure 4.inAs
a result,
PP-g-MA
interfacial
interfacial
compatibility
between
PP and
SGF,
and thereby
improves
the mechanical
properties
of
compatibility
between PP
and SGF,
and
thereby
improves
the mechanical
properties
of the

composites [30,34,35]. However, when PP-g-MA reaches 8 wt %, the aforementioned properties of

the composites first exhibit an initial steep increase,
8283 followed by a gradual increase or even a steady
5

Materials 2015, 8, 82798291

the
composites
[30,34,35]. However, when PP-g-MA reaches 8 wt %, the aforementioned properties
Materials
2015, 8, pagepage
Materials 2015, 8, pagepage
of
the composites first exhibit an initial steep increase, followed by a gradual increase or even a
decrease,
which iswhich
ascribed
to a saturated
content ofcontent
acid anhydride
groups of PP-g-MA.
addition,
steady
decrease,
is ascribed
to a saturated
of acid anhydride
groups ofInPP-g-MA.
decrease, which is ascribed to a saturated content of acid anhydride groups of PP-g-MA. In addition,
theaddition,
tensile modulus
andmodulus
flexural and
modulus
of the
composites
changebarely
after the
conjunction
of
In
the tensile
flexural
modulus
of thebarely
composites
change
after the
the tensile modulus and flexural modulus of the composites barely change after the conjunction of
PP-g-MA. There
are twoThere
possible
factors.
SGF in
PP/SGF
composites
is composites
the major material
that
conjunction
of PP-g-MA.
are two
possible
factors.
SGF
in PP/SGF
is the major
PP-g-MA. There are two possible factors. SGF in PP/SGF composites is the major material that
withstands
by an externally
force.
PP-g-MA
only improve
interfacial
material
thatdeformation
withstands deformation
by anasserted
externally
asserted
force.can
PP-g-MA
can onlythe
improve
the
withstands deformation by an externally asserted force. PP-g-MA can only improve the interfacial
compatibility
between PP
and SGF,
butSGF,
cannot
resist
deformation.
Another
factor factor
is that
interfacial
compatibility
between
PP and
buthelp
cannot
helpthe
resist
the deformation.
Another
compatibility between PP and SGF, but cannot help resist the deformation. Another factor is that
and PP
similar
molecular
weights.
Therefore,
flexural
isPP-g-MA
that PP-g-MA
andhave
PP have
similar
molecular
weights.
Therefore,the
thetensile
tensilemodulus
modulus and flexural
PP-g-MA and PP have similar molecular weights. Therefore, the tensile modulus and flexural
modulus of
of the
the composites
composites are
are not
not correlated
correlatedwith
withthe
the conjunction
conjunctionof
ofPP-g-MA.
PP-g-MA.Such
Suchaa result
resultisis in
in
modulus
modulus of the composites are not correlated with the conjunction of PP-g-MA. Such a result is in
linewith
withthe
thefinding
findingof
ofthe
thestudy
studyby
byWong
Wongetetal.al.[30].
[30].
line
line with the finding of the study by Wong et al. [30].
Thetensile
tensileand
andflexural
flexuralstrengths
strengthsofofPP/SGF
PP/SGF composites
composites decrease
decrease as
as aa result
resultof
ofthe
thecombination
combination
The
The tensile and flexural strengths of PP/SGF composites decrease as a result of the combination
of SEBS-g-MA.
SEBS-g-MA. This
This coupling
coupling agent
agent isis an
an elastomer,
elastomer, which
which possesses
possesses low
low tensile
tensile and
and flexural
flexural
of
of SEBS-g-MA. This coupling agent is an elastomer, which possesses low tensile and flexural
strengths. A greater content of SEBS-g-MA causes the
the tensile
tensile and
and flexural
flexural strengths
strengths to
to decrease.
decrease.
strengths.
strengths. A greater content of SEBS-g-MA causes the tensile and flexural strengths to decrease.
However, the
the improved
improved compatibility between
to
However,
between SEBS-g-MA
SEBS-g-MAand
andSGF
SGFlends
lendslimited
limitedreinforcement
reinforcement
However, the improved compatibility between SEBS-g-MA and SGF lends limited reinforcement to
thethe
tensile
and
flexural
strengths
indicated
in in
Figure
5, 5,
thethe
combination
of
to
tensile
and
flexural
strengthsofofthe
thecomposites.
composites.AsAs
indicated
Figure
combination
the tensile and flexural strengths of the composites. As indicated in Figure 5, the combination of
SEBS-g-MA
results
turn improves
improves their
their
of
SEBS-g-MA
resultsininthe
thechemical
chemicalreaction
reactionbetween
betweenPP
PP and
and SGF,
SGF, which in turn
SEBS-g-MA results in the chemical reaction between PP and SGF, which in turn improves their
interfacial compatibility.
compatibility. This
forfor
elastic
deformation
of the
interfacial
Thisimproved
improvedinterfacial
interfacialcompatibility
compatibilityallows
allows
elastic
deformation
of
interfacial compatibility. This improved interfacial compatibility allows for elastic deformation of the
composites
under
an an
impact,
and
toughen the
the
the
composites
under
impact,
andthe
thedeformation
deformationcan
canthen
then absorb
absorb energy
energy and toughen
composites under an impact, and the deformation can then absorb energy and toughen the
composites, thereby
thereby increasing
increasing the
the impact
impactstrength.
strength. Although the toughness
toughness of
of the
the composite
composite
composites,
composites, thereby increasing the impact strength. Although the toughness of the composite
increases as
as aa result
result of
of the
the combination
combination of
of SEBS-g-MA,
SEBS-g-MA, the
the tensile
tensile and
and flexural
flexural strengths
strengths of
of the
the
increases
increases as a result of the combination of SEBS-g-MA, the tensile and flexural strengths of the
composites
decrease.
Elastomers
improve
the
toughness
of
the
composites
at
the
cost
of
sacrificing
composites decrease. Elastomers improve the toughness of the composites at the cost of sacrificing
composites decrease. Elastomers improve the toughness of the composites at the cost of sacrificing
theirrigidity
rigidityand
anddimensional
dimensionalstability
stability[36].
[36].
their
their rigidity and dimensional stability [36].

Figure 2. (a) Flexural strength and (b) flexural modulus of PP/SGF composites.
Figure
Figure2.2.(a)
(a)Flexural
Flexuralstrength
strengthand
and(b)
(b)flexural
flexuralmodulus
modulusofofPP/SGF
PP/SGF composites.
composites.

Figure 3. Impact strength of PP/SGF composites, as related to various coupling agents.

Figure 3. Impact strength of PP/SGF composites, as related to various coupling agents.
Figure 3. Impact strength of PP/SGF composites, as related to various coupling agents.
Table 3. Variations in tensile, flexural, and impact properties in percentage (%).
Table 3. Variations in tensile, flexural, and impact properties in percentage (%).
Coupling
Coupling
Agent
(wt %)
Agent (wt %)
PP/SGF25
PP/SGF25
2 wt %
2 wt %

T (%)
T (%)
0
0
14
14

ET (%)
ET (%)
0
0
3
3

PP-g-MA
PP-g-MA
F (%)
EF (%)
IS (%)
F (%)
EF (%)8284
IS (%)
0
0
0
0
0
0
21
9
38
21
9
38

T (%)
T (%)
0
0
8
8

SEBS-g-MA
SEBS-g-MA
ET (%) F (%) EF (%)
ET (%) F (%) EF (%)
0
0
0
0
0
0
8
2
8
8
2
8

IS (%)
IS (%)
0
05
5

Materials 2015, 8, pagepage

Materials 2015, 8, 82798291

4 wt %
6 wt %
8 wt %

15
2
24
4
41
14
11
9
8
18
1
28
1
41
21
14
15
13
Table 3. Variations in tensile, flexural, and impact properties in percentage (%).
18
0
24
2
33
25
15
18
16

Coupling
Agent (wt %)
T (%)
Materials
Materials 2015,
2015, 8,
8, pagepage
pagepage
PP/SGF25
0
wt %
%
14
442 wt
15
wt %
15
4 wt %
15
66 wt
18
wt %
%
18
6 wt
%
18
88 wt
18
wt %
%
18
wt
%
18

ET (%)

PP-g-MA
F (%)

3
2
2
2
111
000

21
24
24
24
28
28
28
24
24
24

EF (%)

IS (%)

T (%)

ET (%)

0
9
4
4
4
111
22

38
41
41
41
41
41
41
33
33

8
14
14
14
21
21
21
25
25
25

0
8
11
11
11
14
14
14
15
15
15

SEBS-g-MA
F (%)
EF (%)

Figure 4. Chemical reaction between PP-g-MA and SGF.

0
2
9
9
9
15
15
15
18
18
18

0
8
8
8
8
13
13
13
16
16
16

12
17
23
IS (%)
0
5
12
12
12
17
17
17
23
23
23

Figure
4.
Chemical
reaction
between
PP-g-MA
SGF.
Figure4.
4. Chemical
Chemical reaction
reaction between
betweenPP-g-MA
PP-g-MA and
andSGF.
SGF.
Figure
Figure
5. Chemical
reaction between
SEBS-g-MAand
and SGF.

3.2. Effects of Two Coupling Agents (PP-g-MA or SEBS-g-MA) on Thermal Behaviors of

PP/SGF Composites
In comparison to the crystallization temperature (Tc) and melting temperature (Tm) of pure PP
matrices and PP/SGF composites, PP/SGF composites that are incorporated with PP-g-MA have a
Figure
5. Chemical
reaction
between
SEBS-g-MA and
and
SGF.
Figure5.
Chemical reaction
reactionbetween
betweenSEBS-g-MA
andSGF.
SGF.
slightly greater Tc, but aFigure
similar5.TChemical
m, as indicated in
Figure SEBS-g-MA
6a,b, respectively.
The crystallization temperature of PP/SGF composites increases from 116.4 C to 118.8 C when
3.2.
Effects
of
Two
Coupling
Agents
(PP-g-MA
or
SEBS-g-MA)
on
Thermal
3.2. Effects
Effects of
of Two
TwoCoupling
CouplingAgents
Agents(PP-g-MA
(PP-g-MAor
orSEBS-g-MA)
SEBS-g-MA)on
onThermal
Thermal Behaviors
Behaviorsofof
of
3.2.
the composites
are incorporated
with 8 wt %
of PP-g-MA. For
PP/SGFBehaviors
composites,
SGF exists in PP,
PP/SGF
Composites
PP/SGF
Composites
PP/SGF
Composites
and is thus
able to increase the crystallization temperature of PP. The subsequent combination of
In
comparison
to
the
crystallization
temperature
(T
))and
and
melting
temperature
(T
m) of
pure
PP
In comparison
comparison
tothe
the
crystallization
temperature
(Tcc)cbe
and
meltingtemperature
temperature
(T
of pure
purehas
PP
PP-g-MA
enables SGF
to
becrystallization
effectively distributed
in and
compatible
with
PP. As a(T
result,
SGF
In
to
temperature
(T
melting
PP
mm)) of
matrices
and
PP/SGF
composites,
PP/SGF
composites
that
are
incorporated
with
PP-g-MA
have
andPP/SGF
PP/SGF
composites,
PP/SGF
are incorporated
incorporated
with
PP-g-MA
have aaa
amatrices
greater and
surface
area in
PP matrices,
whichcomposites
induced thethat
nucleation
of PP, andwith
eventually
augments
matrices
composites,
PP/SGF
composites
that
are
PP-g-MA
have
slightly
greater
T
c
,
but
a
similar
T
m
,
as
indicated
in
Figure
6a,b,
respectively.
slightly
greaterTTcc,,of
but
similar TTmm,, as
as indicated
indicated in
in Figure
Figure 6a,b,
6a,b, respectively.
respectively.
the
crystallization
PPaa[37].
slightly
greater
but
similar
The
The crystallization
crystallization temperature
temperature of
of PP/SGF
PP/SGF composites
composites increases
increases from
from 116.4
116.4 C
C to
to 118.8
118.8 C
C when
when
the
composites
are
incorporated
with
8
wt
%
of
PP-g-MA.
For
PP/SGF
composites,
SGF
exists
in
the composites are incorporated with 8 wt % of PP-g-MA. For PP/SGF composites, SGF exists in PP,
PP,
and
and is
is thus
thus able
able to
to increase
increase the
the crystallization
crystallization temperature
temperature of
of PP.
PP. The
The subsequent
subsequent combination
combination of
of
PP-g-MA
PP-g-MA enables
enables SGF
SGF to
to be
be effectively
effectively distributed
distributed in
in and
and be
be compatible
compatible with
with PP.
PP. As
As aa result,
result, SGF
SGF has
has
aa greater
greater surface
surface area
area in
in PP
PP matrices,
matrices, which
which induced
induced the
the nucleation
nucleation of
of PP,
PP, and
and eventually
eventually augments
augments
the
the crystallization
crystallization of
of PP
PP [37].
[37].

Figure 6.
6. DSC
DSC curves
curves for
for (a)
(a) melting
melting behavior
behavior and
and (b)
(b) crystallization
crystallizationbehavior
behaviorof
ofPP/SGF
PP/SGF composites.
composites.
Figure

The Tm of PP/SGF composites that are incorporated with PP-g-MA remains at 165.4 C.
The crystallization temperature of PP/SGF composites increases from 116.4 C to 118.8 C when
Furthermore, the melting temperature does not pertain to the amount of PP-g-MA. Namely, the
the composites are incorporated with 8 wt % of PP-g-MA. For PP/SGF composites, SGF exists in
conjunction of PP-g-MA is not correlated with the crystal structure and thermal stability of PP.
7(b)
Figure
Figure 6.
6. DSC
DSC curves
curves for
for (a)
(a) melting
melting behavior
behavior and
and
(b) crystallization
crystallization behavior
behavior of
of PP/SGF
PP/SGF composites.
composites.
8285
The
The TTmm of
of PP/SGF
PP/SGF composites
composites that
that are
are incorporated
incorporated with
with PP-g-MA
PP-g-MA remains
remains at
at 165.4
165.4 C.
C.
Furthermore,
the
melting
temperature
does
not
pertain
to
the
amount
of
PP-g-MA.
Namely,
the
Furthermore, the melting temperature does not pertain to the amount of PP-g-MA. Namely, the

Materials 2015, 8, 82798291

PP, and is thus able to increase the crystallization temperature of PP. The subsequent combination of
PP-g-MA enables SGF to be effectively distributed in and be compatible with PP. As a result, SGF has
a greater surface area in PP matrices, which induced the nucleation of PP, and eventually augments
the crystallization of PP [37].
The Tm of PP/SGF composites that are incorporated with PP-g-MA remains at 165.4 C.
Furthermore, the melting temperature does not pertain to the amount of PP-g-MA. Namely, the
conjunction of PP-g-MA is not correlated with the crystal structure and thermal stability of PP.
Materials
2015, 8, pagepage
Similarly,
in comparison to the Tc and Tm of pure PP matrices and PP/SGF composites,
the PP/SGF composites that are incorporated with SEBS-g-MA have a slightly greater Tc and a
Similarly,
in comparison to the Tc and Tm of pure PP matrices and PP/SGF composites, the
similar
Tm .
C when
PP/SGF
composites
that are
incorporated
with from
SEBS-g-MA
a slightly
greater
Tc and
similar Tm.
The Tc of PP/SGF
composites
increases
116.4 have
C to 118.8
they
are aincorporated
The
T
c of PP/SGF composites increases from 116.4 C to 118.8 C when they are incorporated with
with 8 wt % of SEBS-g-MA. For PP/SGF composites, the Tc of PP increases as a result of the
8conjunction
wt % of SEBS-g-MA.
For PP/SGFthat
composites,
the Tc of combined
PP increases
as athe
result
of the conjunction
of SGF. SEBS-g-MA
is subsequently
with
composites
serves asofa
SGF.
SEBS-g-MA
that
is
subsequently
combined
with
the
composites
serves
as
a
nucleating
agent,
nucleating agent, which causes nucleation of PP and thus augments the Tc of PP/SGF composites.

which
causes
nucleation
of
PP
and
thus
augments
the
T
c of PP/SGF composites.
In
addition,
the
of
In addition, the Tm of the PP/SGF composites increases from 166.21 C to 167.51 C whenTmthe
the
PP/SGF composites
increases
166.21
to 167.51 CAccording
when the to
composites
are incorporated
composites
are incorporated
withfrom
8 wt
% ofC
SEBS-g-MA.
the Tm results,
the Tm of

with
8
wt
%
of
SEBS-g-MA.
According
to
the
T
m results, the Tm of PP/SGF composites remains at 166.4 C,
PP/SGF composites remains at 166.4 C, which indicates that SEBS-g-MA does not correlate with
which
indicates
that SEBS-g-MA
not correlate
the crystal
structure
and thermaldoes
stability
of PP. with the crystal structure and thermal stability of PP.

3.3. Effects
Spherulite Morphology
Morphology of
of
Effects of
of Two
Two Coupling Agents (PP-g-MA or SEBS-g-MA) on Spherulite
PP/SGF Composites
PP/SGF composites
composites as
as related
related to
to various
various coupling
coupling agents
agents are
are indicated in
The PLM images of PP/SGF
Figure 7. Figure
Figure 7a
7a shows
shows that
that when
when SGF
SGF is
is combined
combined with
with PP,
PP, SGF serves as its nucleating agent.
The distribution of SGF in PP matrices results in an increasing amount of spherulites, which in turn
As aa result,
result, the
the spherulite
spherulite morphology is
prevents the spherulites from being formed completely.
completely. As
incomplete, and spherulites have a smaller size.
composites, SGF
SGF is evenly
When 8 wt % of PP-g-MA or SEBS-g-MA is incorporated
incorporated with
with SGF/PP
SGF/PP composites,
distributed in PP matrices, as indicated in Figure 7b,c. A phenomenon that is similar to that observed
namely, the spherulites have an incomplete structure and a smaller size with
in Figure 7a is found; namely,
the identical reason addressed for Figure 7a [36,38].
The optical microscopic images of PP/SGF
composites that
that have
have been
been treated
treated with
with different
different
PP/SGF composites
C, after
coupling agents are shown in Figure 8. PP is at a melting state when at a temperature of 200 C,
C, which
which the majority of spherulites start to crystallize along the fibers at a temperature of 130 C,
exemplifies that SGF is the nucleating agent for PP.
PP. Nevertheless, SGF is evenly distributed in PP as
a result of the combination of PP, and thus there are more nucleating points created. The majority of
PPs spherulites are formed surrounding the fibers, and at the same time increases the crystallization
PP, as
temperature of PP,
as indicated
indicated in
in Figure
Figure 6b
6b and
and Table
Table4.4.

Figure
PP/SGF
composites
that
areare
composed
of
Figure 7.
7. Polarized
PolarizedLight
LightMicroscopy
Microscopyimages
images(100)
(100)ofofthe
the
PP/SGF
composites
that
composed
(a)
0
wt
%
of
a
coupling
agent;
(b)
8
wt
%
of
PP-g-MA
as
a
coupling
agent,
and
(c)
8
wt
%
of
SEBS-gof (a) 0 wt % of a coupling agent; (b) 8 wt % of PP-g-MA as a coupling agent, and (c) 8 wt % of
MA
as a coupling
agent. agent.
SEBS-g-MA
as a coupling

8286

Materials 2015, 8, 82798291

Materials 2015, 8, pagepage

Figure
microscopy
images
(100)
of theofPP/SGF
composites
that arethat
composed
of (a) 0 wt
Figure8.8.Optical
Optical
microscopy
images
(100)
the PP/SGF
composites
are composed
of
%
of
a
coupling
agent;
(b)
8
wt
%
of
PP-g-MA
as
a
coupling
agent;
and
(c)
8
wt
%
of
SEBS-g-MA
as of
a
(a) 0 wt % of a coupling agent; (b) 8 wt % of PP-g-MA as a coupling agent; and (c) 8 wt %
coupling
agent.
SEBS-g-MA as a coupling agent.
Table
Table 4.
4. Thermal
Thermal behaviors
behaviors of
of PP/SGF
PP/SGFcomposites.
composites.
PP-g-MA
Hm (J/g) TPP-g-MA
m (C)
Tc (C) Xc (%)
H m (J/g)
T m ( C)
T c ( C)
X c (%)
PP
93.1
166.0
111.4
44.5
PP
93.1
166.0
111.4
44.5
PP/SGF25
61.5
165.2
116.4
39.2
PP/SGF25
61.5
165.2
116.4
39.2
116.8
44.8
2 2
68.4 68.4
165.7165.7 116.8
44.8
4 4
67.1 67.1
164.8164.8 116.9
45.1
116.9
45.1
6 6
75.5 75.5
165.4165.4 118.1
52.1
118.1
52.1
8
65.1
165.1
118.8
46.0
8
65.1
165.1
118.8
46.0

Coupling Agent
Coupling
Agent
(wt
%)
(wt %)

Hm (J/g)
H m (J/g)
93.1
93.1
61.5
61.5
66.0
66.0
59.2
59.2
62.6
62.6
59.6
59.6

SEBS-g-MA
SEBS-g-MA
Tm (C)
Tc (C)
Xc (%)
T m ( C)
T c ( C)
X c (%)
166.0
111.4
44.5
166.0
111.4
44.5
165.2
116.4
39.2
165.2
116.4
39.2
166.6
117.2
43.243.2
166.6
117.2
166.2
118.2
166.2
118.2
39.839.8
167.1
118.5
167.1
118.5
43.243.2
167.5
118.8
42.2
167.5
118.8
42.2

Note. Hm is the melting enthalpy, Tm is the melting temperature, Tc is the crystallization temperature, and Xc

Note.
H
m is the melting enthalpy, Tm is the melting temperature, Tc is the crystallization temperature,
is the
crystallinity.
2015, 8, pagepage
crystallinity.
andMaterials
Xc is the

3.4. Effects of Two Coupling Agents (PP-g-MA or SEBS-g-MA) on Spherulite Morphology of

PP/SGF Composites
Figure 9 illustrates the SEM images of PP/SGF composites that are made with different amounts
of coupling agent. The increasing amount of coupling agent, regardless of it being PP-g-MA or
SEBS-g-MA, decreases the pull-out of SGF and the interstices between SGF and PP. In addition, the
incorporation of a coupling agent also results in a rugged surface of PP/SGF composites. Therefore,
PP-g-MA and SEBS-g-MA can effectively improve the interfacial compatibility between PP and SGF.
Figure 10 shows the same images as those in Figure 9, but has a greater magnification. Figure 10
indicates that increasing PP-g-MA or SEBS-g-MA can distinctively decrease the interstices between
SGF and PP. Meanwhile, the PP remarkably adheres to SGF, and SGF does not exhibit a pull-out
phenomenon [30,34,35,37]. These results signify that the interfacial compatibility between PP and
SGF has been improved, and the composites thus have greater mechanical properties, as exemplified
in Figures 13 and Table 2. These results confirm the findings of the study by Tjong et al. [34,35,37].

Figure 9. SEM images (100) of PP/SGF composites, which are incorporated with (a) 0 wt % of a

Figure 9. SEM images (100) of PP/SGF composites, which are incorporated with (a) 0 wt % of a
coupling agent; (b) 2 wt %; (c) 4 wt %, (d) 6 wt %; and (e) 8 wt % of PP-g-MA; as well as (f) 2 wt %;
coupling
wt%;
%;and
(c)(i)4 8wt
(d)
6 wt %; and (e) 8 wt % of PP-g-MA; as well as (f) 2 wt %;
(g)agent;
4 wt %;(b)
(h) 62 wt
wt%,
% of
SEBS-g-MA.
(g) 4 wt %; (h) 6 wt %; and (i) 8 wt % of SEBS-g-MA.

8287
9

Materials 2015, 8, 82798291

3.4. Effects of Two Coupling Agents (PP-g-MA or SEBS-g-MA) on Spherulite Morphology of

PP/SGF Composites
Figure 9 illustrates the SEM images of PP/SGF composites that are made with different amounts
of coupling agent. The increasing amount of coupling agent, regardless of it being PP-g-MA or
SEBS-g-MA, decreases the pull-out of SGF and the interstices between SGF and PP. In addition, the
incorporation of a coupling agent also results in a rugged surface of PP/SGF composites. Therefore,
PP-g-MA and SEBS-g-MA can effectively improve the interfacial compatibility between PP and SGF.
Figure 10 shows the same images as those in Figure 9, but has a greater magnification. Figure 10
indicates that increasing PP-g-MA or SEBS-g-MA can distinctively decrease the interstices between
SGF and PP. Meanwhile, the PP remarkably adheres to SGF, and SGF does not exhibit a pull-out
phenomenon
[30,34,35,37].
These
results signify
thatwhich
the interfacial
compatibility
Figure 9. SEM
images (100)
of PP/SGF
composites,
are incorporated
with (a) between
0 wt % ofPP
a and
SGF coupling
has beenagent;
improved,
and
the
composites
thus
have
greater
mechanical
properties,
as
exemplified
(b) 2 wt %; (c) 4 wt %, (d) 6 wt %; and (e) 8 wt % of PP-g-MA; as well as (f) 2 wt %;
in Figures
13
These
results
confirm the findings of the study by Tjong et al. [34,35,37].
(g) 4 wt
%; and
(h) 6Table
wt %; 2.
and
(i) 8 wt
% of SEBS-g-MA.

Figure
Figure 10.
10. SEM
SEM images
images (800)
(800)of
ofPP/SGF
PP/SGFcomposites,
composites,which
whichare
areincorporated
incorporatedwith
with (a)
(a) 00 wt
wt %
% of
of aa
coupling
agent;
(b)
2
wt
%;
(c)
4
wt
%;
(d)
6
wt
%;
and
(e)
8
wt
%
of
PP-g-MA;
as
well
as
(f)
2
wt
coupling agent; (b) 2 wt %; (c) 4 wt %; (d) 6 wt %; and (e) 8 wt % of PP-g-MA; as well as (f) 2 wt %;
%;
(g)
4
wt
%;
(h)
6
wt
%;
and
(i)
8
wt
%
of
SEBS-g-MA.
(g) 4 wt %; (h) 6 wt %; and (i) 8 wt % of SEBS-g-MA.

4. Conclusions

10

This study successfully improves the compatibility between PP and SGF for their composites
by using PP-g-MA and SEBS-g-MA, and thereby augments the tensile strength, flexural strength,
impact strength, thermal behavior, and compatibility. The test results have proven that SGF is a
good reinforcing fiber, and the conjunction of 25 wt % of SGF improves the tensile, flexural, and
impact strengths of PP. In addition, the incorporation of 8 wt % of PP-g-MA as a coupling agent
provides the composites with 18% greater tensile strength, 24% greater flexural strength, and 33%
higher impact strength; however, it does not benefit their tensile modulus or flexural modulus.
Moreover, the incorporation of 8 wt % of SEBS-g-MA as a coupling agent provides the composites

8288

Materials 2015, 8, 82798291

with 23% greater impact strength, but 25% lower tensile strength, 16% lower tensile modulus, 18%
lower flexural strength, and 16% lower flexural modulus.
The test results also indicate that for PP/SGF composites, SGF serves as the nucleating agent,
which increases the crystallization temperature of PP, but decreases the size of the spherulites of PP.
Using PP-g-MA or SEBS-g-MA as the coupling agent allows for an even distribution of SGF, which
at the same time provides more nucleating points for PP. As a result, the crystallization temperature
of PP is increased and the spherulite size of PP is decreased. Hence, using these two coupling agents
positively improves the interfacial compatibility, which is exemplified by the facts that the PP matrices
enwrap the surface of SGF, and the mechanical properties of the PP/SGF composites are enhanced.
The PP/SGF composites proposed by this study can also provide feasibilities for different practical
applications by adjusting the amounts of PP-g-MA and SEBS-g-MA in order to render the composites
with desired synthetic properties and diverse uses.
Acknowledgments: The authors would especially like to thank Ministry of Science and Technology of Taiwan,
for financially supporting this research under Contract MOST 103-2221-E-035-027.
Author Contributions: In this study, the concepts and designs for the experiment, all required materials, as
well as processing and assessment instrument are provided by Jia-Horng Lin and Ching-Wen Lou. Data are
analyzed, and experimental results are examined by Chien-Lin Huang, Chi-Fan Liu, and Chih-Kuang Chen. The
experiment is conducted and the text is composed by Zheng-Ian Lin.
Conflicts of Interest: The authors declare no conflict of interest.

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