1204 N.-S. Choi, K.

Takahashi
AE
Fracture
DF DF !
(Debonding) (Many FB) !
MCI
(Few FB)
CF
J I ll +1
0.0 0.2 0.4 0.6 0.8
(mm)
Figure 28. Characteristic behavior of AE peak amplitudes describing the fracture
process in short fiber-reinforced plastics: FB: fiber breakage; DF: damage forma-
tion; MCI: main crack initiation; CF: catastrophic fracture; MCP: main crack
propagation
4. Weathering effects on short fiber-reinforced PC/PBT compos-
ites
4.1. Experimental procedure
4.1.1. PC/PBT composites
Unreinforced and SGF-reinforced Xenoy thermoplastics were tested in this
study. Unreinforced Xenoy (Xenoy 522Ou produced by General Electric
Plastics Co.) was a thermoplastic blend of PC/PBT. The fiber weight
fraction in the composites was 31%. Injection molded panels, 2. 75mm
thick, were exposed to the following weathering conditions: (i) unweath-
ered; (ii) naturally weathered for 11 months outdoors in Perth, Western
Australia, under conditions which follow the Australian standard A1580-
457.1. According to this standard, the test panels should be shadow-free,
placed more than 60 cm above the ground, face north, and inclined at an
angle of 45 to the vertical plane; (iii) artificially weathered indoors for
1000 h, during which the irradiation was performed vertical to the panel
surface at 60 by ultraviolet rays with a 313 nm principal wavelength. Com-
pact tension (CT) specimens, 35 mm long and 35 mm wide, were machined
from the panel. As shown in Figure 29, the specimens were notched per-
pendicular (T direction) and parallel (L direction) to the mold fill direction
using a diamond wheel cutter with a thickness of 0. 4mm. A sharp notch
was made by pushing a razor blade into the initial notch tip. The initial
crack length, a
0
, was kept to 17.0 0. 2mm. Dumbbell type tensile speci-
mens were also obtained in the T and L directions, as shown in Figure 29.
In addition, microhardness and ultrasonic test specimens were machined
from the central part of the panels.
Handbook of Thermoplastic Polymers: Homopolymers, Copolymers, Blends, and Composites
Edited by Stoyko Fakirov
Copyright 2002 WI L E Y -V CH Verlag GmbH, Weinheim
ISBN : 3 -5 27 -3 0113 -5
Fracture Behavior of Fiber-Reinforced Polyester Composites
Mold fill direction
1205
IO
(M
I
l
10
L-notch
T-ncitch
+
3 1
' Lr
-
T
(t = 2.75 mm)
4
125 mm
Figure 29. Geometry of the injection molded panel and the compact tension (CT)
and dumbbell type specimens
4.1.2. Tensile testing and J-integral evaluation
Tensile testing was performed at a crosshead speed of 0. 5mm/min using
dumbbell type and CT type specimens. Five specimens were tested for each
experimental condition. The maximum stress obtained from the measured
nominal stress-strain curve was taken as a value corresponding to the yield
strength,

[61]. Based on the Landes and Begley method [62,63] em-

ploying several specimens, the values of the J-integral were obtained as a
function of the crack propagation length, , by the following equation
J =
Bb
(2)
where UT is the deformation energy obtained from the load P vs. displace-
ment curves of CT specimens, B the specimen thickness, b the ligament
length, the Merble and Corten' s compensation coefficient [63] for the
plastic region ahead the crack tip, the value of which varies with a/b and
is 2.27 at a/b = 1. The value of was obtained as an average of eight
measurements in order to consider the eventual curved shape of the crack
tip front. A number of identically cracked specimens were loaded up to vari-
ous displacements producing different amounts of crack extension, , and
then unloaded. To determine the values of J, slow-fracture surfaces of the
1206 N.-S. Choi, K. Takahashi
tested specimens were examined after impact fracture under a cryogenic
condition. Values of the critical fracture toughness, J
c
, were measured at
the intercept of the blunting line defined by equation
J =2,,
(3)
and the crack resistance, R, curve determined from Eq. (2) (see Chapter
16). Values of a
y
for CT specimens notched in the T and L directions were
obtained from averaged values of a
y
for dumbbell type tensile specimens
in the L and T directions, respectively (Figure 29).
4.1.3. Fracture surface observation
Fracture surfaces of CT specimens were observed under a scanning electron
microscope to study weathering effects on the fracture behavior.
4.1.4. Local ultrasonic velocity measurement
The ultrasonic velocity was measured at a location on a polished cross-
section of the plate employing a scanning acoustic microscope (HSAM 200,
Hitachi Co.) as shown in Figure 30. Longitudinal plane waves with a fre-
quency of 400 MHz traveled through distilled water and were point-focused
on the surface layer of the cross section by an acoustic lens. By analyz-
ing the variation in the amplitudes of the reflected waves with different
focusing depths (z direction) from the surface, the velocity of the elastic
surface waves, VR, propagating through the 10-30 deep surface layer
was measured using the following equation [64]
(4)
Polished
section
Incident longitudinal
waves (400 MHz)
\ ^ /
Figure 30. Measurement of the velocity, VR, of elastic surface waves propagating
locally in the surface layer using an acoustic microscope
Fracture Behavior of Fiber-Reinforced Polyester Composites 1207
where VQ is the longitudinal wave velocity of the water coupler; / the fre-
quency of the longitudinal waves; Az the average distance between focus-
ing depths corresponding to the continual peak amplitudes of the reflected
waves. Weathering effects on the local ultrasonic velocity were studied in
the thickness, ? /, direction.
4.1.5. Microhardness measurement
Using a dynamic microhardness tester (DUH-50, Shimadzu Co.), the rela-
tive microhardness, H^, of the polished surface of the unreinforced speci-
men was measured. The measurement was performed to obtain the value
of the indentation depth by a method of pushing a diamond triangular
indentor perpendicular to the specimen surface under an initial loading
rate of 1.9 x 10"
3
Ns"
1
, maximum load of 0.19 N and load retention time
of 20s. Weathering effects on the microhardness were investigated in the
thickness direction after the specimen surface was ground and polished.
Five microhardness measurements were carried out for each experimental
condition.
4.2. Yield strength
Results of yield strength, ^, measured from dumbbell type tensile spec-
imens are listed in Table 2. The reinforcement with 31wt%fibers of un-
weathered Xenoy resulted in an increase in

of 43%for L- and 32%

for T-specimens, respectively. The reinforced specimens showed that a
y
for L-specimens was much higher than that for T-specimens, since fiber
alignment in the L-direction has a strong reinforcing effect [60,65]. In un-
reinforced specimens, higher a
y
values were obtained for T-specimens; this
is understandable in view of the fact that the microstructural anisotropy
is formed during injection molding of the plates [43,65]. The values of a
y
for unreinforced and SGF-reinforced specimens were hardly changed by
weathering for 11 months. A reduction in ductility of reinforced Xenoy and
a gradual increase in

of glass fiber-reinforced Xenoy with increasing UV-

radiation exposure time were reported in the literature by Campeotto et
Table 2. Weathering effects on the yield strength, ^, of unreinforced and SGF-
reinforced Xenoy specimens
Material Loading
direction Unweathered
L 47.8'?
Unreinforced Xenoy . '
T 44. 3
+
L 68.72'.3
a
y
(MPa)
Weathered
48
68
for 11 months
0+1.6

y
-3.1
7+2.0
'-2.0
02'.9
SGF 31 wt%-Xenoy
+0

9
1208 N.-S. Choi, K. Takahashi
[36]. Qayyum and White [29] reported that a
y
of PP and polyoxymethy-
lene (POM) scarcely changed with weathering for 3 years, whereas PA66
exhibited a 30%decrease in a
y
when weathered for an initial period of 1.5
years, and thereafter a
y
approached a constant value. The fracture strain
was lessened greatly for these plastics in the order PA66 > POM > PP.
The severe deterioration of PA66 was considered to be mainly due to the
influence of humidity in air. The present study revealed that weathering for
a period of 11 months rarely affected

of the thermoplastic blend Xenoy.

4.3. Fracture toughness and R-curve
Figure 31 shows effects of weathering on the load vs. crack opening dis-
placement curves of unreinforced and SGF 31 wt%-reinforced specimens
notched in the L-direction. As compared to unweathered specimens, unre-
inforced Xenoy weathered for 11 months exhibited a very slight increase
in the maximum load. In contrast, reinforced Xenoy showed a considerable
loss in ductility, together with a slight decrease in the maximum load.
Figure 32a shows -R-curves for unreinforced specimens with L notches.
The material weathered for 11 months exhibited lower J-integral values by
about 5. 4kJm~
2
and a similar slope of the -R-curve, dJ/d(Aa), throughout
the whole range of , as compared to the unweathered material. Unrein-
forced specimens with T notches also showed reduction in J-integral similar
to the above, caused by the weathering (see Figure 32b). This consistency
in reduction of J-integral for each crack propagation length may indicate
that the weathering affected the deterioration of unreinforced Xenoy. -R-
curves obtained for SGF-reinforced specimens with L notches are shown
400-
300-
200-
100-
Unreinforced Xenoy
4 6
(mm)
10
Figure 31. Typical load-displacement curves of unreinforced and SGF-reinforced
Xenoy CT specimens with L-notches: () unweathered and () weathered for
11 months
Fracture Behavior of Fiber-Reinforced Polyester Composites
90-
1209
(a)
\
1.5
(b)
I I
3.0 4.5
(mm)
6.0
Figure 32. J-integral as a function of crack propagation length, , for unrein-
forced Xenoy unweathered (D) and weathered for 11 months (): (a) L-notched
and (b) T-notched specimens
in Figure 33a. Weathering for 11 months induced considerable degradation
of the reinforced material; the value of dJ/d(Aa) for the weathered ma-
terial was significantly lower than that for the unweathered material and
the reduction in J-integral was by about 2. 9kJm~
2
at ~ 2. 0mm, but
this value was much larger (15. 2kJm~
2
) at ~ 7. 5mm. The -curve of
1210 N.-S. Choi, K. Takahashi
Figure 33. J-integral as a function of crack propagation length, , for the
SGF-reinforced Xenoy unweathered (D) and weathered for 11 months (): (a) L-
notched and (b) T-notched specimens
weathered T-notched specimens had features similar to those in Figure 33b.
It should be noted that the SGF-reinforced specimens revealed a
stronger decrease in the value of dJ/d(Aa) than did unreinforced ones.
Taking into account that the slope of the -curve indicates the tearing re-
sistance to stable crack growth [63], it is believed that the tearing resistance
Fracture Behavior of Fiber-Reinforced Polyester Composites 1211
Table 3. Weathering effects on the critical J-integral, J
c
, of unreinforced and
SGF-reinforced Xenoy specimens
Material Loading
direction
Je (kJ/m
2
)
Unweathered Weathered for 11 months

. r ,

L 11.6 9.3
Unreinforced Xenoy ^
1 0 0
_
1 lo. U .
SGF 31 wt%-Xenoy ^ 5J^ ^
J. O. 4. 0
of SGF-reinforced specimens was deteriorated by weathering. This may be
the result of some degradation of the Xenoy matrix and of the interface
between matrix and glass fibers. The unreinforced specimens experienced
a simple degradation mechanism, characteristic of Xenoy. Values of J
0
for
each kind of specimen are listed in Table 3. The filling with 31 wt%SGF
caused a large reduction in J
c
: 60-71%. Unreinforced and SGF-reinforced
specimens with T notches exhibited higher J
0
values than the corresponding
specimens with L notches. After being weathered for 11 months, unrein-
forced specimens with T notches exhibited the greatest degradation in J
0
by about 33%, whereas J
c
of SGF-reinforced specimens decreased, on the
average, by 14%. It is believed that the weathering induced considerable
degradation, mainly in toughness of the thermoplastic Xenoy matrix, and
short glass fibers had a good stabilizing effect on the decrease in J
0
.
4.4. Local ultrasonic velocity
Values of VR, of elastic surface waves were measured for the unreinforced
plate as a function of depth from the weathered surface; they are shown in
Figure 34. The value for the unweathered surface layer was approximately
2.21 1O
3
InS"
1
. The unweathered specimen exhibited a rather uniform
velocity distribution, except for a small portion in the interior where the
values were smaller. Weathering for 11 months caused a considerable de-
crease in VR to a depth corresponding to two-thirds of the plate thickness
from the weathered surface, giving an average value of 2.13 x 10
3
ms"
1
. On
the contrary, a specimen irradiated with UVR for 1000 h showed a slight
decrease in VR for the irradiated surface layer and, unlike the weathered
case, an increase was established in the volume. Natural weathering must
have involved a moisture effect in addition to the effect of degradation by
sunlight. Consequently, one can expect induced deterioration not only in
the surface layer but also in the volume of the plate.
The velocity of Rayleigh waves that travel along the free surface of an
elastic half-space can be expressed as follows [66]
1212 N.-S. Choi, K. Takahashi
2400
Thickness, 2.75 mm
Figure 34. Values of local ultrasonic velocity, VR, measured through the plate
thickness for unreinforced Xenoy plates, showing significant changes with weath-
ering conditions: (D)unweathered; (Q) weathered for 11 months; () subjected
to UV irradiation for 1000 h
where E is the elastic modulus of the medium, the density, and v Poisson's
ratio. The increase and/or decrease of VR in Figure 34 is believed to be
caused mainly by the change in elastic modulus. This is because only slight
variation was assumed to occur in the density and Poisson's ratio of the
material [64]. The natural weathering might have induced some variation in
the material microstructure, which might have reduced E of the surface and
core layers. A plausible reason for the increase of VR in the volume of the
UV irradiated specimen may be some change of the compressive residual
stress which could be normally formed in the volume of the injection molded
plate [29]. This scenario might increase the value of E.
4.5. Microhardness
Figure 35 shows results of H\ j obtained from the surface (skin) and core
portion of the unreinforced plate. For the unweathered specimen, the av-
erage values of H\ j of the core were smaller than those of the skin layer.
This may be reasonable, taking into account that the microstructure and
residual stresses were differently distributed through the volume during the
injection molding process [43,65]. Little effect of the natural weathering on
HU was observed. Because the degree of hardness is not affected exclu-
Fracture Behavior of Fiber-Reinforced Polyester Composites 1213
v
e

m
i
c
r
o
h
a
r
d
n
e
s
s
I

1

t
O

t
U
l

O

C
I

I
+3
JS
a* -
S kin
Core
1
I
I
Unweathered
S kin
I Core
1
I
I
Naturally weathered
for 11 months
Irradiated
skin
Irradiated by
UV rays
for 1000 hour
Figure 35. Effects of natural weathering and UV irradiation on the relative mi-
crohardness, HU, of unreinforced Xenoy plates
sively by the elastic modulus, but also by the plasticity, HU was shown to
differ from that in Figure 34 where lower values of VR were observed for
the weathered skin. Irradiation for 1000 h by artificial UV rays caused an
increase of 26% in H\j of the surface part. It is thought that irradiation by
sunlight including UV rays induced an increase in hardness of the speci-
men surface, whereas water absorption of the skin layer due to rain and/or
moisture would cause a material softening, ie., a decrease in hardness.
4.6. Fracture surface morphology
Figure 36 shows scanning electron micrographs taken from the fracture
surface of the weathered unreinforced CT specimen. The fracture surface
near the initial notch tip was quite flat (see enlarged photograph of area A in
Figure 36b). On the contrary, the fracture surface far from the tip became
considerably thinner because of the large plastic deformation emanating
from the surface layer to the volume. Qayyum and White [29] reported that,
for PA66 and POM, surface microflaws developed; they were caused by the
increase of residual tensile stress by weathering which produced multiple
surface cracks during tensile testing, ie., a different failure mechanism,
whereas PP did not show much visible surface deterioration on weathering.
In this study, the fracture pattern of the weathered surface layer, ie., the
skin part of the Xenoy material showed little difference from that of the
1214 N.-S . Choi, K. Takahashi
Notch tip
Weathered
surface
Initial
surface
Deformed
Unweathered
Figure 36. (a) S canning electron micrograph taken from the fracture surface of
an unreinforced CT specimen with an L notch weathered for 11 months. Fracture
direction is from left to right. This picture is slightly asymmetric due to tilting
during microscopic observation, (b) Magnification of area A in (a)
Fracture Behavior of Fiber-Reinforced Polyester Composites 1215
Notch tip
Weathered
(a)
20
(b)
Notch tip
Figure 37. Scanning electron micrographs taken from the fracture surface of an
SGF-reinforced CT specimen with an L notch weathered for 11 months, (a) The
weathered side; (b) the opposite unweathered side. Fracture direction is from left
to right
1216 N.-S . Choi, K. Takahashi
opposite unweathered side. Figure 37 shows scanning electron micrographs
taken on the fracture surface of a weathered S GF 31 %wt-reinforced CT
specimen, where (a) and (b) are from the skin part and from the opposite
unweathered skin part, respectively. Little change was shown in the fracture
surface due to weathering, i.e., differences in fracture patterns of fibers,
matrices and their interfaces. It is believed that the visible fractures of the
present materials were rather insensitive to the weathering effect.
4.7. Material performance sensitivity to the weathering effects
Polymers are prone to deteriorate in mechanical performance when they
are affected by natural weathering [29-38]. Table 4 summarizes weather-
ing effects of unreinforced and S GF-reinforced Xenoy plates. In respect to
global-scale performance, a
y
and the fracture surface morphology of the
materials were little influenced by weathering for 11 months. However, a
significant decrease in J
c
was established for the unreinforced material.
Filling with S GFs exhibited a good antidegradation effect on J
c
, but in-
duced a stronger decrease in dJ /d(Aa) for stable crack propagation due
to weathering. On a local scale, a strong decrease in J
0
was shown to a
depth of two-thirds of the plate thickness from the weathered side for the
unreinforced plate. However, weathering effects on H\j were hardly shown.
On the contrary, an unreinforced plate irradiated for 1000 h with artificial
ultraviolet rays exhibited an increase in H\j and a slight deterioration in
VR of the surface layer. It is thus believed, for the Xenoy materials, that
global-scale performances of J
c
and dJ /d(Aa) and local-scale VR and H\j
were sensitive to the weathering conditions.
Table 4. S ummary of weathering effects on unreinforced and S GF-reinforced
Xenoy plates
Material performance Unreinforced Xenoy
Natural
weathering
Irradiation
by UV rays
S GF-reinforced Xenoy
Natural
weathering
a
y
Little change
J
0
Large decrease
Global
d(Aa)
Fracture Little change
morphology
skin Large decrease Decrease
y/p>
core Large decrease Increase
Local
skin Little change Increase
HU
core Little change Little change
Little change
Decrease
Large decrease
Little change
Fracture Behavior of Fiber-Reinforced Polyester Composites 1217
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