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Mechanical Properties of Injection-molded Natural Fiber-reinforced Polypropylene

Composites: Formulation and Compounding Processes
Zhan-Ying Sun, Hai-Shan Han and Gan-Ce Dai
Journal of Reinforced Plastics and Composites 2010 29: 637 originally published online 25 February
2009
DOI: 10.1177/0731684408100264

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 Mechanical Properties of Injection-molded
Natural Fiber-reinforced
Polypropylene Composites: Formulation
and Compounding Processes

ZHAN-YING SUN,* HAI-SHAN HAN AND GAN-CE DAI

State Key Laboratory of Chemical Engineering
East China University of Science and Technology, Shanghai 200237, China

ABSTRACT: In this study, the effects of material optimization and compounding processes on
the properties of natural fiber composites were studied. The thermal stabilities of sisal fiber and jute
fiber were compared by thermogravimetric analysis. The influences of fiber content, coupling agent,
fiber geometry, and fiber distribution on the properties were also researched. It was observed that
sisal fiber had more thermal stability than jute fiber. Addition of coupling agent, long fiber length,
and uniform fiber distribution led to higher performance composites. For the sisal fiber-reinforced
polypropylene composites, the critical fiber length was 2.27 mm and the interfacial shear strength
was 22.03 MPa with MAPP. The tensile strength of composites was also theoretically predicted
based on Kelly–Tyson model.

KEY WORDS: natural fiber composites, compounding, critical fiber length, distribution.

INTRODUCTION

ATURAL FIBER-REINFORCED THERMOPLASTIC composites have many applications in

N automotive and electrical industries. There are two main technologies in manufactur-
ing these materials. One is compression molding, which is mainly used for the production of
natural fiber mat-reinforced thermoplastic composites (NMT). The other is injection
molding. This is a major part of the plastics industry, consuming approximately 32 wt% of
all plastics [1]. Although compression molding is the predominant processing technology in
manufacturing natural fiber composites, the complex parts cannot be made by this process.
However, injection molding can be used for high quality complex parts. For example, the
Chrysler Composite Vehicle uses a set of mold tools weighing 450 tonnes each to manu-
facture the complex body shell by injection molding [2]. Moreover, among the different
processes compared, the injection molding process shows better mechanical performance
than the other processes [3]. It is receiving increased attention for producing natural fiber
composites. Nevertheless, there are several technical issues yet to be solved that limit use of
this processing technology, such as product consistency, thermal and moisture sensitivity,
tool design, and flow limitations [4]. Among the constituents, the properties of natural fibers
vary with types and geographic areas, and the same type of fiber can be different over

*Author to whom correspondence should be addressed. E-mail: dlwxtj@gmail.com

Journal of REINFORCED PLASTICS AND COMPOSITES, Vol. 29, No. 5/2010 637
0731-6844/10/05 0637–14 $10.00/0 DOI: 10.1177/0731684408100264
ß SAGE Publications 2010
Los Angeles, London, New Delhi and Singapore

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638 Z.-Y. SUN ET AL.

seasons and batches. Thermal sensitivity is another disadvantage of natural fibers. These
fibers are biomaterials, and therefore sensitive to thermal treatment. High processing
temperature can cause chemical and physical changes [5]. Thus, in order to improve thermal
stability, the suitable fiber type needs to be selected prior to manufacturing. Besides, the
incorporation of natural fibers to thermoplastics leads to flow limitation, which are
increased by the incompatibility of natural fibers and thermoplastics. The differences in the
interfacial tension between most thermoplastic polymers and reinforcing fibers result in
poor fiber wetting. A lot of methods have been used to solve this incompatibility problem,
and maleated polypropylene as a coupling agent has a better result [6–8].
The final properties of natural fiber composites manufactured by injection molding
depend not only on the properties of raw materials used and their compositions, but also on
processing methods. The constituent materials may interact in a synergistic way so as to
provide properties in the composite that are not accounted for by a simple volume-fraction
sum of the properties of the constituents [9]. There are several factors influencing the
mechanical properties of composites, such as fiber and matrix types, fiber loading, fiber
geometry (length, diameter, aspect ratio), fiber distribution in the matrix, and interface
adhesion between fiber and matrix. The compounding processes play a much more
important role in determining the performance of composites. Fiber geometry and fiber
distribution in the matrix can be greatly changed after processing. The pore ratio and fiber–
matrix interaction can also be affected by compounding processes [10]. For natural fiber
composites, compounding is normally divided into one-step (continuous mixers, such as
extruders) and two-step (batch mixers, such as two-roll mill and rotor mixers) processes [11].
Owing to the advantages of batch mixers such as the easy addition of fibers, the two-step
compounding process has a lot of applications. For example, Maldas and Kokta [12] studied
pulp and polystyrene composites with a two-roll mill system. Dányádi et al. [13] researched
wood flour and polypropylene composites by using an internal mixer. Rozman et al. [14]
compared the effects of an internal mixer and single-screw compounding processes on the
properties of oil palm empty fruit bunch-polypropylene composites. Although lots of research
has been carried out on the natural fiber composites, the commercial compounds based on
natural fibers have not been introduced in the market on a large scale. This may be due to the
lack of general guidelines for material optimization and processing [15].
The present article aims to study the effects of material optimization and compounding
processes on the properties of natural fiber composites. Two compounding technologies
followed by injection molding were performed. In order to select a suitable fiber, thermal
properties of two natural fibers (sisal and jute) were compared. Maleated polypropylene
was used as a coupling agent to improve interface adhesion. Mechanical properties, fiber
geometry, interface morphology, and fiber distribution were analyzed.

EXPERIMENTAL

Materials

Polypropylene Y1600 was purchased from the plastics of Shanghai Petrochemical

Complex, China, with a melt flow index of 16. Coupling agent A018 used in the study was
a maleated polypropylene (MAPP) supplied by Shanghai Zhongzhen Material Technology
Co., Ltd., China. The amount of grafting was 1.1% and the melt flow index was above 70.
Sisal fiber rovings were obtained from Dongfang Sisal Group Co., Ltd., China. Jute fibers
were purchased from Zhenjiang Li Da Co., Ltd., China.

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Injection-molded Natural Fiber-reinforced Polypropylene Composites 639

Processing

TWO-ROLL MILL COMPOUNDING

Sisal fiber rovings were first chopped to short-length fibers at 20 mm, then were dried in
an oven at 808C for 8 h. Then polypropylene, MAPP, and dried sisal fibers were
compounded in a SK-1600B two-roll mill (Shanghai Rubber Machinery Co., Ltd., China)
at 1908C. The blends were cut into pellets and molded into standard ASTM specimens at
1908C using a TTI-80 plastic injection machine (Dong Hua Machinery Co., Ltd., China).
The mold temperature was set at 608C.

EXTRUSION COMPOUNDING
Sisal fiber rovings were dried in an oven at 808C for 8 h prior to compounding.
Then polypropylene, MAPP, and sisal fibers were compounded in a twin-screw extruder at
1908C and 180 rpm. The fiber weight fraction was controlled by the extruder speed and the
matrix adding. The extrudates exiting from the twin-screw extruder were cooled by water
immediately and cut into pellets by a pelletizer. Then these pellets were dried at 808C for
over 10 h and molded into specimens by the same conditions as mentioned above.

Testing

MECHANICAL PROPERTIES
The tensile and flexural properties were measured on a CMT 4204 universal testing
machine (Shenzhen SANS Testing Machine Co., Ltd., China) at a cross-head speed of
2 mm/min. The tensile samples were prepared and tested according to ASTM D638, type I
specification. An extensometer with gauge length of 50 mm was used for modulus
measurements. The flexural specimens were conducted using the universal testing machine
in the three-point loading mode. The procedure ASTM D790 was followed, an 80 mm
support span, and a 2 mm/min cross-head speed were used. Notched impact strength was
tested on an XJU-22 cantilever beam impact machine (Chengde Testing Machine Co. Ltd.,
China) in accordance with ASTM D256. It is noted that in all the mechanical tests at least
five samples were tested at ambient conditions.

MEASUREMENT OF FIBER LENGTH AND DIAMETER

The tensile samples were cut into suitable sizes and used to analyze the fiber length.
Sisal fibers were extracted from the composites by dissolving the matrix in boiling xylene.
The extracted fibers were put into a beaker contained acetone. Then they were carefully
scattered on a glass plate. Magnified fiber images were taken by a reflectance light
microscope and loaded into a software called UTHSCSA image tool. The lengths and
diameters of at least 500 fibers from each sample were pictured and recorded. The average
fiber length (ln) and the corresponding standard deviation () of each sample were
calculated using the relations [16]:
P
ni li
ln ¼ P ð1Þ
ni
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
1 X n
¼ ðli  ln Þ2 ð2Þ
n1 1

where ni is the number of fibers and li is the fiber length.

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640 Z.-Y. SUN ET AL.

THERMOGRAVIMETRIC ANALYSIS
To compare thermal properties of sisal fiber and jute fiber, thermogravimetric
analysis of the two fibers was performed by a TG WRT-2P thermogravimetric analyzer
(Shanghai Precision and Scientific Instrument Co., Ltd., China). The experiment was
carried out at a heating rate of 108C/min in an air environment.

FRAGMENTATION TESTING
The specimens for the fragmentation test were prepared by embedding single sisal
fibers between two films of polypropylene of a thickness of about 500 mm and then placed
into a hot oven at 1908C. After polypropylene melting, they were pressed between two
aluminum plates at ambient temperature for 2 min. Then the specimens were cut from the
films, and the size dimension (L  W  H) was 95  16  1 mm [17]. Fragmentation testing
was measured on a CMT 4204 universal testing machine (Shenzhen SANS Testing
Machine Co., Ltd., China) at a cross-head speed of 2 mm/min and at least 10 specimens
were tested for each case. The fiber fragment lengths and diameters were measured by
UTHSCSA image tool software.

MORPHOLOGICAL CHARACTERIZATION
The morphology of composites and interface between fiber and matrix by different
processes were performed using a scanning electron microscope (SEM) (model JSM-
6360LV, JEOL, Japan).
For the interface study, the impact fracture surface of each sample was sputter-coated
with gold and analyzed using a SEM.
For morphological characterization, the fracture surface of the tensile specimen was
milled and polished by using sandpaper. Then the polished surface was sputter-coated
with gold and scanned by a SEM. The morphological images were analyzed using the
MATLAB 7.1 program.

RESULTS AND DISCUSSION

Fiber Type Selection

In order to select a changeless fiber during processing of composites, thermal stabilities

of different fibers need to be evaluated. Sisal and jute fibers were investigated by
thermogravimetric analysis. As can be seen in Figure 1, the weight of both fibers decreased
with increasing temperature. From room temperature to 1508C, there was a slow decrease in
weight, which was due to the water desorption. At 150–2408C, the dehydration of some
glucose units of cellulose contributed to the weight loss [18]. The degradation around
250–4008C was due to the decomposition of cellulose and hemicellulose [19]. The lignin
weight loss range was wider and appeared between 2008C and 5008C, with a maximum
at 3508C [20,21]. As shown in Figure 1, the sisal fiber had less weight loss than jute fiber
below 2508C, which indicated that sisal fiber had a better thermal stability than jute fiber
within the processing temperature range (170–2208C) of the composites.

Fiber Content and Coupling Agent

Tensile strength and modulus of composites manufactured by two-roll mill compounding

technology are shown in Figure 2. The materials contained a 5 wt% MAPP coupling agent.

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Injection-molded Natural Fiber-reinforced Polypropylene Composites 641

Figure 1. Thermograms of sisal fiber and jute fiber.

Figure 2. Tensile properties of composites compounded by two-roll mill.

As seen in Figure 2, the tensile modulus was increased greatly with the incorporation of
fibers, whether or not with the addition of coupling agent. It showed an increase of 147% at
30 wt% fiber loading. The tensile strength decreased with the fiber contents without
coupling agent, especially at higher fiber levels, whereas it increased by 56% at 30 wt% fiber
weight content with addition of MAPP coupling agent. Without coupling agent, the
decrease in the strength of natural fiber composites was due to the incompatibility between
fiber and matrix. Figure 3(a) and (b) shows that there were clearly gaps between fibers and
matrix without coupling agent, which indicated that the interfacial interaction was quite
weak. So, the stress was not effectively transferred from matrix to fibers, thus leading to
worse mechanical properties. Figure 3(c) and (d) shows better interface adhesion with
MAPP coupling agent. Without coupling agent, natural fiber composites showed a deceased
tendency for fiber loading. This phenomenon was quite different from glass fiber
composites, which showed an increased tendency whether coupling agent was used or
not. This may be attributed to the glass fibers being sized by a certain chemical agent before

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642 Z.-Y. SUN ET AL.

Figure 3. SEM microphotographs of the composites, fracture surface (a) after Izod impact test, (b) without
MAPP, (c), (d) with MAPP.

acting as reinforcements, such as silane coupling agent, which led to a good interface
between fibers and matrix. However, natural fibers are not sized by any chemical agent, so
surface modification must be carried out before use in composites; otherwise poor
mechanical properties would be achieved due to weak interface.
Figure 4 presents the flexural strength and modulus of composites manufactured by
two-roll mill compounding technology. As seen in Figure 4, the flexural strength was not
decreased without MAPP coupling agent, and it was not increased considerably with the
fiber loading. With coupling agent, the composites showed much higher flexural strength
than pure polypropylene, increasing by 90% at 30 wt% fiber content. Also, the flexural
modulus showed an increase of 217% at this fiber content. Thus, it was concluded that
better compounds could be achieved by adding coupling agent.
Impact strength of composites depends on the properties of fiber and matrix, and also
on the adhesion between fiber and matrix. The deformation and fracture energy can be
absorbed by fiber breakage, matrix deformation, and crack, interfacial debonding, fiber pull-
out, etc. [22]. Figure 5 shows the effects of fiber content and coupling agent on the impact
strength of composites, where the impact strength increased with fiber content. It was
observed that composites without coupling agent showed higher impact strength: this
tendency was opposite to the tensile and flexural strength, which indicated that better
interface resulted in worse impact strength. This phenomenon has been observed by many
other researchers [23,24].

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Injection-molded Natural Fiber-reinforced Polypropylene Composites 643

Figure 4. Flexural properties of composites compounded by two-roll mill.

Figure 5. Impact strength of composites compounded by two-roll mill.

Fiber Geometry and Distribution

The results from tensile testing on SEXM and STRM composites are summarized in
Table 1. SEXM represents sisal fiber composites with MAPP manufactured by extrusion
compounding, and STRM stands for sisal fiber composites with MAPP produced by two-
roll mill compounding. The fiber loading of these two composites were both controlled at
30% weight content. From Table 1, we can see that the tensile properties of STRM
composite are higher than that of SEXM composite. This phenomenon is attributed to the
fiber geometry and distribution.
The geometries of sisal fibers extracted from STRM and SEXM composites are shown in
Table 2. For the STRM composite, the average fiber length was 2.17 mm after processing,
which was much shorter than the original fiber length. However, the diameters of sisal
fibers did not change, and were equal to the diameters of original fibers (0.22 mm). So the
average aspect ratio was decreased. For the SEXM composite, although the average length

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644 Z.-Y. SUN ET AL.

Table 1. Tensile properties of SEXM and STRM composites.

Tensile Tensile
Process wt (%) vt (%) strength (MPa) modulus (MPa)

SEXM 30 20 41.98  0.16 3615  307.5

STRM 30 20 46.55  0.49 4109  71.3

Table 2. Geometries of sisal fibers extracted from SEXM and STRM composites.

Fiber type q (g/cm3) Process wt (%) vt (%) Length (mm) Diameter (mm) Aspect ratio
a
Sisal fiber 1.5 STRM 30 20 2.17 0.22 9.86
SEXM 30 20 1.87 0.20 9.35
a
The density of sisal fiber was obtained from Ref. [25].

was smaller than that of STRM composite, the diameters also had little change. So, the
SEXM and SEXM composites had almost an equal average aspect ratio at the same fiber
loading. However, as seen in Figure 6, the fiber length standard deviation of STRM
composite is smaller than that of SEXM composite, which indicates that the STRM
composite has greater load-bearing capabilities than SEXM composite. This confirms that
the properties of STRM composite are higher than that of SEXM composite.
The morphologies of materials are formed during processing, which closely relate to the
physical properties of materials. Identical materials (same fiber type and content, and same
matrix type and content) may have different physical properties owing to different
morphologies. In the morphologies of fiber-reinforced composites, fiber distribution is a
crucial problem. Uniform fiber distribution can lead to good mechanical properties. The
distribution of fibers was characterized by fluorescence technique [26], nearest neighbor
distance [27] and Dirichlet tessellations [28,29], etc. As a useful tool, fractal concepts were
widely applied for analyzing disordered systems. Ryszard used the fractal method to study
dispersion of second-phase inclusions: he pointed out that the fractal dimension grew as
homogeneity and regularity of dispersions became more pronounced [30,31]. According to
Ryszard’s method, the fiber distribution was studied by fractal concepts in this study.
Figure 7 shows the morphologies of composites manufactured by different compound-
ing processes. (a) and (c) were original images on the transverse cross-section of STRM
and SEXM composites, (b) and (d) were binary images of STRM and SEXM composites
through MATLAB program image processing. All the image sizes were 960 pixels high
and 1280 pixels width. The box-counting program was written by MATLAB language.
The fractal dimension analysis was performed using several scale lengths of different pixel
dimensions. Plotting the scale lengths vs. the value of filled cells in a log–log plot could get
the value of fractal dimension.
As shown in Figure 8, the fractal dimension of the STRM composite was larger than
that of the SEXM composite, which indicated that the fiber distribution of STRM was
more uniform than that of SEXM. So the mechanical properties of the STRM composite
were better than that of the SEXM composite.

Critical Fiber Length and Theoretical Prediction of Tensile Strength

Critical fiber length is an important parameter in theoretical prediction of the mechanical

properties of fiber-reinforced thermoplastic composites. There are two main methods used

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Injection-molded Natural Fiber-reinforced Polypropylene Composites 645

Figure 6. Fiber length distribution of composites (a) STRM; (b) SEXM.

to determine the critical fiber length. One is the fragmentation testing method, the other
method is based on the well-known equation of Kelly and Tyson [32]:

f d
¼ : ð3Þ
2lc

s is the interfacial shear strength,  f is the fiber strength, d is the fiber diameter, and lc is the
critical fiber length. When the interfacial shear strength is measured, the critical fiber
length can be calculated by Equation (3).
Fragmentation test is a direct method for measuring the critical fiber length, although
there is a lot of debate over this test. The critical fiber length is estimated from the mean
fiber fragment length by the Oshawa et al. equation [33]:

4
lc ¼ l: ð4Þ
3

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646 Z.-Y. SUN ET AL.

Figure 7. Morphologies of composites by different compounding processes: (a) original image of STRM;
(b) binary image of STRM; (c) original image of SEXM; (d) binary image of SEXM.

Since the interfacial shear strength is not easily measured, the critical fiber length
was determined by the fragmentation test in this study, and the interfacial shear strength
was obtained by using Equation (3).
According to Equations (3) and (4), the tensile strength of discontinuous fiber-
reinforced plastic composites could be predicted by the following equation [34,35]:
0 1
X li vi X  
lc A
uc ¼ 0 @ þ f vj 1  þ Em "f ð1  vf Þ ð5Þ
l 5l
d f l 4l
2lj
i c j c

where 0 is the fiber orientation factor in the composites, and considered as 0.375 for
in-plane orientation for these fibers of injection-molded composites. s is the interfacial
shear strength (estimated by Equation (3)),  f is the fiber strength, df is the fiber diameter,
lc is the critical fiber length, li and lj are the actual fiber lengths below and above
lc, respectively (determined by the fiber length distribution), vi and vj are the corresponding
volume fractions, Em"f ¼  m, which represents matrix strength at fiber failure strain, and vf
is the total fiber volume fraction [32].
The critical fiber lengths of SEXM and STRM composites were obtained by the fragmen-
tation test, and the interfacial shear strength was estimated, which are shown in Table 3.

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Injection-molded Natural Fiber-reinforced Polypropylene Composites 647

Figure 8. Fractal dimensions of composites by different compounding processes: (a) fractal dimension of
STRM; (b) fractal dimension of SEXM.

Table 3. Summary of the data used in the theoretical prediction.

Process wt (%) vt(%) lc (mm) rf (MPa) df (mm) Em (MPa) ef (%) s (MPa)

SEXM 30% 20% 2.27 500 0.2 1663 2.5 22.03

STRM 30% 20% 2.27 500 0.2 1663 2.5 22.03

As seen in this table, the critical fiber lengths of SEXM and STRM composites match the
assumed equal distribution of coupling agent in the composites. So the same value was
measured by the fragmentation test and the same interfacial shear strength was achieved.
In this study, the critical fiber length of SEXM and STRM was 2.27 mm, and the
interfacial shear strength was 22.03 MPa for the sisal fiber-reinforced polypropylene
system, which was similar to results of other researchers. Nyström et al. [15] reported that
the interfacial shear strength was 23 MPa with added MAPP in the wood fiber-reinforced
polypropylene composites. So we can estimate that the critical fiber length is 1.63 mm.
They also observed that the flax fiber-reinforced polypropylene composites showed a value
of 20 MPa of the interfacial shear strength with MAPP. Nechwatal et al. [36] reported that
the critical fiber length range of natural fiber composites was 1–10 mm for tensile strength

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648 Z.-Y. SUN ET AL.

Figure 9. Comparison of experimental values and theoretical prediction of tensile strength.

and would decrease with added coupling agent. They also pointed out that if the
reinforcing fibers were much longer than the critical fiber length, the effect of an improved
fiber matrix adhesion would be low. From their study, the mechanical properties would
not be increased by using long fibers above 10 mm.
The comparison of experimental values and theoretical prediction of tensile strength
of SEXM and STRM composites is shown in Figure 9. It is shown that both
the theoretical prediction values were higher than experimental values. They were 18.27
and 12.12% higher than actual values, respectively. The reason for the discrepancy of
experimental values and theoretical prediction values may be mainly due to these following
aspects: the fiber strength measurement for short fiber length above or below critical fiber
length was a quite difficult calculation, and the fiber strength used in Equation (5)
was an average value measured for long fibers. This led to an error prediction. Besides,
the interfacial shear strength based on the Kelly–Tyson equation was obtained by
the single-fiber composite test method, which was not the real situation in the actual
fiber composites. The interaction of fibers should not be neglected, especially at high
fiber content. Another important reason was the porosity produced by the compounding
and injection molding technologies. These reasons attributed to the discrepancy
of experimental values and theoretical prediction values. As seen from Figure 9, the
theoretical prediction for tensile strength of STRM was relatively accurate compared to
that of SEXM, which indicated that the STRM has more uniform microstructure.

CONCLUSIONS

Two compounding technologies followed by injection molding were performed to

produce natural fiber composites. The effects of fiber type, fiber content, coupling agent,
fiber geometry, and distribution on the properties of natural fiber composites were studied.
Sisal fiber and jute fiber were used as reinforcements. Thermogravimetric analysis showed
that sisal fiber had more thermal stability than jute fiber. Coupling agent had an important
influence on the mechanical properties. With coupling agent, the tensile strength and

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Injection-molded Natural Fiber-reinforced Polypropylene Composites 649

modulus of STRM increased by 56 and 147% at 30 wt% fiber loading, and the flexural
strength and modulus showed an increase of 90 and 217% at this fiber content,
respectively. However, the impact strength showed the tendency to decrease. The STRM
composite had greater load-bearing capabilities than the SEXM composite owing to its
longer fiber length and narrow fiber length distribution. Uniform fiber distribution in the
matrix resulted in higher mechanical properties. The critical fiber length and the interfacial
shear strength were 2.27 mm and 22.03 MPa with MAPP for the sisal fiber-reinforced
polypropylene system. The theoretical prediction of tensile strength showed higher values
than experimental results.

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