Materials Science and Engineering A347 (2003) 338
/345

www.elsevier.com/locate/msea

Impact fracture toughness of short glass fiber-reinforced polyamide

6,6 hybrid composites containing elastomer particles using essential
work of fracture concept
S.C. Tjong a,*, S.A. Xu a,b, Y.W. Mai c,d
a
Department of Physics and Materials Science, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon, Hong Kong
b
Institute of Polymer Science and Engineering, East China University of Science and Technology, 130 Mei Long Road, Shanghai 200237, PR China
c
Department of Mechanical and Mechatronic Engineering, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong
d
Center for Advanced Materials Technology (CAMT), School of Aerospace, Mechanical and Mechatronic Engineering, The University of Sydney,
Sydney, NSW 2006, Australia

Received 22 May 2002; received in revised form 15 August 2002

Abstract

Polyamide 6,6 (PA6,6) hybrid composites toughened with maleated styrene
/ethylene butylene
/styrene (SEBS-g-MA) and
reinforced with 5, 10, 15, 20 and 30% short glass fiber (SGF) were prepared via melt blending followed by injection molding. The
matrix blend of composites consisted of 80 wt.% PA6,6 and 20 wt.% SEBS-g-MA. The impact fracture resistance of injection-
molded PA6,6/SEBS-g-MA 80/20 blend and its hybrid composites was investigated. Drop weight Charpy impact test showed that
the hybrids exhibit much higher notched impact strength than the PA6,6 polymer under various test velocities of 1
/5 m s 1. Tough
PA6,6/SEBS-g-MA 80/20 blend was not broken under the test velocities employed. The Charpy test is not a good technique to
characterize the impact fracture behavior of tough polymer blend. The impact fracture resistance of tough PA6,6/SEBS-g-MA 80/20
blend can be characterized successfully using the essential work of fracture (EWF) concept under a speed of 3 m s 1. Moreover,
impact EWF measurements indicate the specific essential fracture work of hybrids to decrease with increasing SGF content. The
specific non-essential plastic work was absent in hybrids owing to glass fibers restricting shear yielding of the matrix of composites.
# 2002 Elsevier Science B.V. All rights reserved.

Keywords: Impact; Fracture resistance; Essential work; Hybrid composites; Glass fiber; Elastomer

1. Introduction include ethylene
/propylene rubber [2], styrene
/ethylene

Polyamides (PAs) are engineering thermoplastics
widely used in industrial applications because of their
attractive combination of mechanical properties and
ease of processing. However, PAs suffer from moisture
absorption and notch sensitive characteristics. The
deficiencies of PAs can be improved by blending with
elastomers or with other polymers [1
/8]. For polymers
in industrial applications, the fracture toughness of
polymers is a critical factor in materials selection.
Adding impact modifiers can enhance the toughness of
PAs. The impact modifiers commonly used in PAs
* Corresponding author. Tel.: /852-27887702; fax: /852-27887830
E-mail address: aptjong@cityu.edu.hk (S.C. Tjong).
0921-5093/02/$ - see front matter # 2002 Elsevier Science B.V. All rights reserved.
PII: S 0 9 2 1 - 5 0 9 3 ( 0 2 ) 0 0 6 0 9 - 3
butylene
/styrene (SEBS) and maleated SEBS (SEBS-g-
MA) [3
/5]. The cavitation of elastomer particles and
associated matrix shear yielding are the key toughening
mechanisms for PA
/elastomer blends.
Generally, SEBS copolymer is grafted with maleic
anhydride (MA) prior to blending with PA to improve
the compatibility between the matrix and elastomer. The
MA functional group can react with amine and amide
end groups of PA, resulting in a finer dispersion of
elastomers. Paul and coworkers reported that PA6,6 can
be made super-tough by blending with SEBS-g-MA.
They indicated that melt blending of SEBS-g-MA with
PA6,6 can produce rubber particles within the optimal
size range for effective toughening [4]. The rubber
toughening of PAs is achieved at the expense of their
stiffness and strength characteristics. These parameters
 S.C. Tjong et al. / Materials Science and Engineering A347 (2003) 338
/345
can be restored in rubber-toughened PAs by adding
inorganic filler [9] or short glass fiber (SGF) reinforce-
ments [10
/14], leading to the formation of ternary or
hybrid composites. Numerous studies have been con-
ducted on the mechanical properties of glass fiber-
reinforced PA composites [15
/21]. In comparison, little
information is available on the toughening behavior of
PA hybrid composites.
In recent years, the essential work of fracture (EWF)
concept has been increasingly used to evaluate the
fracture toughness of ductile polymers and tough
composites [22
/30]. The total energy needed to fracture
a sample having a sharp crack (Wf) consists of the EWF
(We) and non-essential plastic work (Wp). We is the
work required to fracture the polymer in its process zone
and surface-related. Wp is the energy consumed by
various deformation mechanisms in the plastic zone and
volume-related. Mathematically, Wf can be written as
Wf We Wp ;
2
Wf we LBbwp L B;
Wf
wf  we bwp L;
LB
where wf is the specific total fracture work, we and wp are
the specific essential fracture work and specific plastic
work, respectively, L is the ligament length, B the
sample thickness, and b is a shape factor of the plastic
zone. Apparently, EWF concept is a simple method that
consists of testing specimens with different ligament
lengths, recording the area under the load displacement
curve (Wf), plotting wf vs L diagram and evaluating the
best-fit regression line. It should be noted that the
specimen must be fully yielded prior to crack initiation,
which can be easily evaluated for slow testing of double-
edge notched tensile specimen.
Polymer composites used in structural engineering
applications are frequently subject to high deformation
rates and impact loading. The knowledge of deforma-
tion and fracture behavior of composites under impact
loading conditions is crucial to an understanding of
toughening mechanism. Because of the high strain rate
sensitivity of polymers, materials that are ductile under
low strain rate loading can behave in a brittle manner at
high strain rates. Notched Charpy and Izod tests are
commonly used to evaluate the fracture behavior of
polymers and composites due to their simplicity. In-
strumented drop weight impact test is particularly
attractive because it is capable of testing materials at a
wide range of velocities [31
/33]. However, the impact
strength is not a good parameter to characterize the
toughness of ductile polymers because the samples are
frequently not fully broken. Better characterization of
the impact fracture energy can be obtained using EWF
methodology. Mai and coworker [34] have extended the
EWF concept to impact testing of ductile polymer
339
blends. Martinatti and Ricco [35] reported that it is
valid to apply the EWF method to assess high rate
fracture toughness of polypropylene-based materials.
Since then, some research has been conducted on the
validity of impact EWF concept to characterize the
toughness of ductile polymers and their blends [36
/41].
Taking into account the testing conditions and sample
geometries may not fully comply with the yielding
criterion of EWF method, Paul and coworkers modified
Eq. (2) into
U
 u0 ud L; (4)
A
where U /A is the total fracture energy per unit area, L
the ligament length, u0 the limiting specific fracture
energy and ud the dissipative energy density [36,39,40].
This work aims to study the impact fracture toughness
of PA6,6 hybrids reinforced with various SGF contents
(1) using EWF methodology.
(2)
(3) 2. Experimental
The polymer used in this study was PA6,6 purchased
from Mitsubishi Engineering Plastics Company (Tai-
wan). Maleic anhydride-grafted SEBS elastomer (Kra-
ton FG 1901X) was supplied by Shell Company. E-glass
fibers with a length of
/4 mm and a diameter of
/10
mm was obtained from Owens Corning. All materials
were dried separately in ovens prior to compounding.
Elastomer-toughened PA6,6/SEBS-g-MA 80/20 (wt.%)
blend designated as SGF0 in this paper was prepared as
matrix material for the hybrids. SGFs ranging from 5,
10, 15, 20 and 30 wt.% SGF were incorporated into the
PA6,6/SEBS-g-MA 80/20 (wt.%) blend to form the
hybrid composites. They were designated as SGF5,
SGF10, SGF15, SGF 20 and SGF30, respectively. The
composites were prepared by melt mixing using a twin-
screw extruder (Brabender Plasticorder). In the process,
dried polymer pellets and SGF were initially fed into the
extruder with operating temperature profiles of 260
/
270
/270
/260 8C. The extruded strands were granulized
with a pelletizer and dried. The dried pellets were fed
into an injection molder (Cheng Hsong Jetmaster 4
Mark II-C) to produce plaques of 200/80/3.2 mm3.
Notched Charpy impact specimens with dimensions
100 /13/3.2 mm3 were cut from these injection-
molded plaques. The bars for the standardized Charpy
notched impact test were notched according to ASTM
D256. The notch tip radius was 0.25 mm. A Ceast
Fractovise drop weight system was used to conduct
instrumented impact test at 21 8C. The system was
equipped with an instrumental tup. The mass of a striker
was 3.164 kg and the span of sample support was 60
mm. The sensor attached to the tup measured the force
340 S.C. Tjong et al. / Materials Science and Engineering A347 (2003) 338
/345

Fig. 1. SENB specimen geometry used for impact EWF method.

generated within the impact specimens during the test,

and the signal was fed to a computerized data acquisi-
tion system. Impact velocities of 1
/5 m s 1 range were
employed.
Single-edge notched bending (SENB) specimens with
dimensions of 100 /13 /3.2 mm3 were used for this test
(Fig. 1). They were cut from the injection-molded
plaques with the longitudinal direction of the specimens
parallel to the melt flow direction. The notches were Fig. 2. Drop weight impact energy vs velocity for the specimens
made by first forming sawcut slots, followed by shar- investigated.
pening with a fresh razor blade. This procedure was
adopted by several researchers [23,27]. The exact liga- techniques to determine the fracture behavior of poly-
ment length (L ) was measured by a traveling microscope meric materials at high strain rates. The Charpy and
(Topcon Profile Projector). The test was conducted at Izod impact specimens containing one single ligament
21 8C by placing the sample in Ceast Fractovise drop length have notch that are not sharp enough. Accord-
weight system with a span length (S ) of 60 mm. Impact ingly, the ductile polymer samples often experience no
velocity of 3 m s 1 was employed in the measurements. breakage or fracture during the test. Therefore, EWF
The fracture surfaces of the SENB specimens after methodology becomes an attractive method to evaluate
impact loading were examined in a scanning electron the impact fracture toughness of ductile polymers or
microscope (SEM; Jeol JSM 820). They were coated composites having sharp cracks with various ligament
with a thin gold film prior to SEM observations. lengths. According to literature, the impact EWF
approach is carried out under high impact velocity, i.e.
from 3 to 3.5 m s 1 [34,38
/41]. This implies that the
3. Results and analysis EWF method can be used to determine the high-rate
EWF according to Eq. (3).
Fig. 2 shows the variation of total impact energy with Fig. 3 shows the plot of the impact fracture energy vs
velocity for the specimens investigated. It is evident that
ligament length for unreinforced SGF0 blend under an
notched PA6,6 specimens exhibit very low impact
impact velocity of 3 m s 1. It can be seen that the plot
strength at various test velocities. Addition of 20 wt.%
SEBS-g-MA elastomer to PA6,6 improves its impact
strength significantly. The SGF0 blend is not broken
during the drop weight test under various impact
velocities employed. Thus, the fracture energy values
obtained are unreliable. The notched impact specimen
experiences fracture by adding 5 wt.% SGF to the
PA6,6/SEBS-g-MA blend. And this SGF5 sample ex-
hibits a ductile
/brittle transition in the plot of impact
strength vs velocity. Such a transition can still be
observed in the SGF10 composite, but its impact
strength is reduced considerably with the incorporation
of 10 wt.% SGF into the PA6,6/SEBS-g-MA blend. As
the SGF content is increased to 15 wt.% and above, the
impact strength of the hybrids is further reduced
independent of test velocity. The notched Charpy and
Izod impact tests are simple and fast measurement Fig. 3. Impact fracture energy vs ligament length for SGF0.
 S.C. Tjong et al. / Materials Science and Engineering A347 (2003) 338
/345
Fig. 4. Impact fracture energy vs ligament length for SGF5.
yields a regression line having a steep positive slope. The
specific essential fracture work (we) and non-essential
plastic work (wp) for the SGF0 blend is 19.53 and 11.68
kJ m 2, respectively. Stress whitening can be clearly
observed in the impact specimens of SGF0 for various
ligament lengths. Fig. 4 shows the impact fracture
energy vs ligament length plot for SGF5. It is apparent
that the SGF5 hybrid exhibits no specific plastic work
because the slope of the horizontal regression line is
zero. In other words, the fracture energy is dissipated in
the inner process zone, and no energy is consumed in the
outer plastic zone. This implies that the matrix plasticity
is constrained by adding 5 wt.% SGF to the PA6,6/
SEBS-g-MA blend. Similar horizontal regression lines
are obtained by adding 10 wt.% SGF and more (Fig.
5(a)
/(d)). The we of hybrids appears to decrease with
increasing SGF content. Cho and Paul [39] observed a
similar behavior in plots of impact fracture energy vs
ligament length for the glass fiber-reinforced PA com-
posites toughened with ABS at a speed of 3.5 m s 1.
They reported the dissipative energy density (ud) to be
reduced to zero or even a negative value by addition of
glass fibers to the compatibilized PA6/ABS blend.
However, plot of impact fracture energy vs the ligament
length for the unreinforced PA6/ABS blend yields a line
with a positive slope. Thus, a large amount of energy is
dissipated by plastic deformation about the fracture
plane [39]. Paul and coworkers [40] studied the effects of
glass fiber content on the impact fracture behavior of
the PA6/EPR-g-MA 80/20 (wt.%) blend. They showed
the dissipative energy density (ud) to depend on glass
fiber content. In the absence of glass fibers, the
regression line has a positive slope. The addition of 5
wt.% glass fiber to compatibilized PA6/EPR-g-MA 80/
20 blend decreases the slope of the line sharply, and by
adding 20 wt.% glass fibers the slope is essentially zero
[40].
Fig. 6(a) and (b) show the SEM fractographs of SGF0
blend specimens with ligament lengths of 4 and 8 mm,
341
respectively, after impact EWF measurements. Appar-
ently, the fractographs show the typical shear bending
morphology regardless of ligament length. Such a
morphology results from cavitation of elastomers and
subsequent shear yielding of the matrix. Fig. 7(a) and (b)
show the SEM fractographs of SGF5 hybrid with
ligament lengths of 4 and 8 mm, respectively. The
fracture surface is rather smooth indicating that incor-
poration of 5 wt.% SGF to the PA6,6/SEBS-g-MA 80/20
blend constraints the yielding of the matrix dramati-
cally. Debonding and pullout of SGF occurs. As the
SGF content is increased to 15 wt.% SGF (Fig. 8), the
matrix feature is relatively flat, indicating that matrix
fractures is the brittle mode under high impact loading
of 3 m s 1. A similar fracture features is observed for
hybrids containing 20% SGF and above. Thus, higher
SGF content in hybrids constraints the matrix from
yielding during a very short impact testing period.
From above observations, fiber debonding and pull-
out are derived from weak bonding between SGF and
matrix consisting of PA6,6 and SEBS-g-MA. Generally,
weak physical interaction can develop between SGF and
PA6,6 due to their polar structures. Moreover, MA
functional group of SEBS-g-MA can react with hydrox-
yl groups on the glass fiber surfaces during compound-
ing, i.e.
In this work, MA functional group of SEBS-g-MA has
reacted readily with amine groups of PA6,6, yielding an
imide linkage. Consequently, fewer remaining MA
groups grafted to SEBS are available to react with
hydroxyl groups on the SGF surfaces. Weak interfacial
fiber
/matrix bonding produces a clean fiber surface
feature in SEM micrographs. It is known that a good
fiber
/matrix interfacial bond and a fiber length longer
than a critical length factor (lc) permit effective load
transfer from the matrix to discontinuous fiber reinfor-
cement of the composite. The critical fiber length can be
determined from [42]
sf d
lc  ; (5)
2t
where sf is the ultimate fiber strength, d the fiber
diameter and t the interfacial shear strength that equals
to one-half of the matrix strength (sm/2). For the glass
fiber, sf /3.45 GPa [42], d /10 mm, and sm /39 MPa
[43]. Accordingly, lc is determined to be 0.885 mm. In
previous study [43], we have determined the fiber length
distribution of injection-molded PA6,6 hybrids. The
results showed that there is a large fraction of fibers
with a length between
/0.1 and 0.4 mm for the hybrids
after processing. This implies that the length of SGF is
342 S.C. Tjong et al. / Materials Science and Engineering A347 (2003) 338
/345

Fig. 5. Impact fracture energy vs ligament length for (a) SGF10, (b) SGF15, (c) SGF20, and (d) SGF30 hybrids.

reduced from original 4 mm to less than 0.4 mm due to According to the literature, the essential work per-
compounding and subsequent injection molding [43]. formed in the inner fracture process zone of SGF-
Thus, the critical fiber length of 0.885 mm is longer than reinforced composites is the energy required to debond,
exact fiber length of the hybrids after processing. Taking bridge and pullout of the fibers, to deform the matrix
into account weak fiber
/matrix interaction and short that include crazing, voiding or shear yielding [44]. For
fiber length of the hybrids, fiber pullout rather than SGF-reinforced hybrids, the mechanisms responsible for
broken occurs (Figs. 7 and 8). toughening of hybrids under quasi-static tensile loading
For the purpose of comparison, we present the results are fiber pullout and matrix shear yielding. There exists
of EWF using double-edge notched tension (DENT)
specimens under tensile loading speed of 1 mm min 1 Table 1
[43]. Table 1 lists the specific EWF (we) and non- Specific EWF (we) and specific plastic work (bwp) for specimens
investigated with DENT geometry under quasi-static tensile loading of
essential plastic work (bwp) of the PA6,6, SGF0 blend 1 mm min 1 [43]
and its hybrids under quasi-static tensile loading. It is
apparent that SGF additions to the PA6,6/SEBS-g-MA Sample we (kJ m 2) bwp (kJ m 2)
80/20 blend leads to an increase in we but to a decrease PA6,6 7.82 14.09
in bwp values. In other words, SGF additions are SGF0 13.90 14.47
beneficial in improving the fracture toughness of SGF5 25.31 11.95
SGF10 21.82 9.90
PA6,6 hybrids under tensile loading. Stress whitening
SGF15 32.65 4.44
in plastic zone can be observed in all hybrid specimens SGF20 29.98 3.14
(Fig. 9). The size of outer plastic zone begins to decrease SGF30 19.62 1.92
for SGF content greater than 15%.
 S.C. Tjong et al. / Materials Science and Engineering A347 (2003) 338
/345 343

Fig. 6. SEM fractographs of SGF0 blend specimens with ligament Fig. 7. SEM fractographs of SGF5 hybrid specimens with ligament
lengths of (a) 4 and (b) 8 mm after impact EWF measurements. lengths of (a) 4 and (b) 8 mm after impact EWF measurements.

a competition between the matrix deformation and

fiber-related toughening. The addition of fibers reduces
the volume of ductile matrix. Rigid fibers also restrict
the matrix deformation, leading to a decrease in specific
non-essential work (Table 1) and stress-whitening zone
(Fig. 9). For hybrids containing lower SGF content (5/
15%), the toughening mechanism is mainly derived from
shear yielding, and fiber-related damage. In contrast,
fiber debonding and pullout mechanisms predominate
in hybrids with SGF content ]/20% [43].
The toughening mechanism of hybrids under impact
EWF measurements is fiber debonding and pullout.
Upon introduction of SGF into PA6,6/SEBS-g-MA, the
matrix of hybrids becomes brittle under high impact
velocity of 3 m s 1. Plastic deformation does not take
place outside the fracture process zone owing to glass
fibers restricting shear yielding of the matrix during
impact tests. Accordingly, stress whitening is not Fig. 8. SEM fractograph of SGF15 hybrid with a ligament length of 4
observed in the plastic zone of hybrids. Fiber debonding mm after impact EWF measurements.
344 S.C. Tjong et al. / Materials Science and Engineering A347 (2003) 338
/345
Fig. 9. Macrograph showing stress whitening in outer plastic zone of (1) PA6,6, (2) SGF0, (3) SGF5, (4) SGF10, (5) SGF15, (6) SGF20, and (7)
SGF30 samples with the ligament lengths within 8.2
/8.8 mm after EWF measurements under quasi-static tensile loading of 1 mm min 1.
and pullout are caused by poor fiber
/matrix interfacial
bonding and by the length of fibers being smaller than a
critical value. Because of weak fiber
/matrix interfacial
bonding, matrix plasticity near the fiber ends does not
occur in the present PA6,6 hybrids. The impact-specific
fracture work of hybrids appears to be smaller than that
of the PA6,6/SEBS-g-MA matrix blend with the excep-
tion of SGF5 composite. On the other hand, matrix
plasticity near fiber ends takes place in maleated
polypropylene (mPP) hybrids reinforced with SGF and
toughened with SEBS elastomer under impact EWF
tests [45]. Synergistic toughening effects arises from the
matrix plasticity and fiber pullout result in SGF/SEBS/
mPP hybrid exhibits higher we than its matrix blend
material (SEBS/mPP). This implies that the incorpora-
tion of SGF enhances the impact fracture toughness of
the SEBS/mPP blend [45].
4. Conclusion
This work attempts to use the EWF methodology to
characterize the impact fracture toughness of ductile
PA6,6/SEBS-g-MA blend and its composites. The main
conclusions of the investigation can be summarized as
follows. (a) Drop weight impact measurements show
that notched PA6,6 polymer exhibits low impact
strength at various test velocities. The PA6,6/SEBS-g-
MA blend experiences no breakage under test velocities
employed. The hybrids exhibit much higher impact
strength compared with PA6,6, particularly for those
reinforced with lower SGF content. (b) EWF concept
can be used to evaluate the impact fracture resistance of
tough PA6,6. Incorporation of SGF content as low as 5
wt.% to the PA6,6/SEBS-g-MA blend results in diminish
of non-essential work in the hybrid under high impact
rate loading condition. This is due to SGF that
constraints the matrix from yielding during a very short
period of impact test. (c) Scanning electron microscopic
examination of the fracture surfaces of impact EWF
specimens reveals that the glass fiber debonding and
pullout are responsible for energy absorbing mechan-
isms in the hybrids during impact loading. Fiber
debonding and pullout are resulted from a weak
fiber
/matrix interfacial bonding and from a reduction
in the fiber length lower than a critical value after
processing.
Acknowledgements
The work described in this paper was fully supported
by a grant from the Research Grants Council of Hong
Kong Special Administrative Region, China (Project no:
CityU 1029/00E).
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