D. S.

Forsyth
Graduate Student,
Department of Electrical Engineering.
Thermal Fatigue of Composites:
S. 0. Kasap
Professor,
Department of Electrical Engineering.
Ultrasonic and SEM Evaluations
Results are presented on the evaluation of thermal fatigue in three fiber reinforced
polymer composites, using ultrasonic techniques and scanning electron microscopy.
1. Wacker The composites examined were (a) continuous carbon fibers in a vinylester matrix
Graduate Student, (b) continuous aramid fibers in a vinylester matrix and (c) randomly oriented
Department of Mechanical Engineering. aramid fibers in a polyphenylene matrix. Specimens of these composites were sub-
jected to thermal fatigue by thermal cycling from -25°C to 75°C. Changes in
ultrasonic attenuation and velocity were monitored during thermal cycling, and
S. Yannacopoulos scanning electron microscopy was used to qualitatively evaluate any damage. It was
Associate Professor, observed that ultrasonic attenuation is sensitive to thermal fatigue, increasing with
Department of Mechanical Engineering.
increasing number of thermal cycles. SEM evaluations showed that the primary
damage due to thermal fatigue is due to fiber-matrix debonding.
University of Saskatchewan,
Saskatoon, Saskatchewan,
Canada, S7N 0W0

1 Introduction
In the past few decades, composite materials have been re-
placing traditional engineering materials in many applications,
especially where high specific strength is required. A composite
is generally defined as any man-made material consisting of
two or more macroscopic components with a definite interface
[1-3]. Because of this formulation, composites are uniquely
susceptible to thermal fatigue. Temperature variations result
in the development of stress at the matrix-reinforcement in-
terface due to the different thermal expansion properties of
the components.
In many service environments, composite materials are re-
quired to undergo temperature variations as much as 100°C
even many times a day, as in an automobile engine compart-
ment. The electronics industry is beginning to recognize ther-
mal fatigue as an important reliability criterion for the
performance of chip packages and solder joints, which share
the problem of bonded materials with different thermal ex-
pansion coefficients [4-7]. The many variables which influence
the properties of a composite make it difficult to generalize
results, and there have been relatively few experimental studies
of thermal cycling-induced damage in composites [8-20].
Ultrasonic testing of materials is a well documented tech-
nique (see for example [21-23]). Ultrasonic velocities are re-
lated to the elastic moduli of the medium. Ultrasonic
attenuations are influenced by voids, cracks, and other defects
in the medium. Ultrasonic methods have been applied to the
study of the properties of composites by many authors (for
example [10, 18, 20, 24-27]).
Contributed by the Materials Division for publication in the JOURNAL OF
ENGINEERING MATERIALS AND TECHNOLOGY. Manuscript received by the Mate-
rials Division October 9, 1992, revised manuscript received May 12, 1992. As-
sociate Technical Editor: D. Hui.
Previously, the authors have studied the changes in ultra-
sonic propagation as a function of thermal fatigue in E-glass
fiber reinforced polyester resin composites, in correlation with
flexural strength testing and SEM examinations [18, 19]. This
work examines the changes in ultrasonic velocity and atten-
uation in three fiber-reinforced polymers as a function of ther-
mal fatigue damage. SEM examination is used to provide a
qualitative evaluation of the damage.
2 Materials
Three different polymeric fiber composites were examined
in this work. Two geometrical arrangements were examined,
continuous uniaxial fiber and short randomly oriented fiber.
All materials were obtained from Goodfellow Metals Limited
of Cambridge. These were:
composite 1: carbon fiber uniaxial in a vinylester matrix
composite 2: aramid (Kevlar®) fiber uniaxial in a vinylester
matrix
composite 3: aramid fiber randomly oriented in a poly-
phenylene sulphide (PPS) matrix
Uniaxial composites such as composites 1 and 2 are used in
aerospace applications for secondary structures such as skins
[1, 2]. Composite 3 can be injection molded, and has appli-
cations as a dielectric structural material for electronics ap-
plications [2].
Some relevant properties of the components of the experi-
mental materials are shown in Table 1. It is important to note
the large difference in the thermal expansion coefficients be-
tween the polymer matrix materials and the fiber materials,
which is responsible for thermal fatigue damage in the spec-
imens. These numbers are for the axial properties of the fibers.

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 Table 1 Thermal properties of the component materials of
the composite systems
Coefficient of Thermal
thermal expansion
1 conductivity Specific heat
1
Material (lxlO^KT ) (Wrrr'K~r) (Jkg-'K" )
Carbon fibers - 0 . 5 (axial) 50 (axial) 700
Aramid fibers - 2 (axial) 0.05 (axial) 1400
Vinylester 50 0.2 1500
Polyphenylene 50 0.29 1100
sulphide
Table 2 Fiber content of the composites
Material Vf
Composite 1 0.50 0.62
Composite 2 0.61 0.70
Composite 3 0.30 0.31
The thermal conductivity of the materials is also significant
here. All the materials other than carbon fiber have very low
thermal conductivities. This means that temperature gradients
will develop across the specimens during thermal cycling. This
limits the size of the specimens, because it is desirable to min-
imize the stresses due to thermal gradients across the specimen
in comparison to the stresses induced by the different thermal
expansions of the components.
The fiber volume fraction Vf of the composite samples was
determined from image analysis and density measurements.
The results are displayed in Table 2, with the weight fraction
Wp Fiber content is known to influence the magnitude of the
interfacial stresses due to thermal cycling [28].
Composites 1 and 2 were pultruded continuous fiber spec-
imens in the form of long cylindrical rods of diameter 10 mm.
Composite 3 was in the form of a square plate, about 7 mm
thick and 150 mm square. All samples were cut using an oil
cooled diamond saw. It was found that the saw caused damage
visible under the SEM. The faces to be mounted on the trans-
ducers were then polished to remove this damage. Unpolished
specimens were more attenuating, most likely due to this dam-
aged surface layer.
For composites 1 and 2, two different sample shapes were
cut to examine ultrasonic propagation parallel and perpendic-
ular to the fiber direction. For propagation parallel to the fiber
axis, sections of the rod were cut off simply perpendicular to
the fiber axis. To examine propagation perpendicular to the
axis, specimens were cut as above, and then cut again parallel
to the axis, leaving a thin section of the rod that was approx-
imately rectangular.
Thicknesses of the samples in the direction for wave prop-
agation were measured using a Sylvac electronic measuring
probe to a precision of 1 x 10~3 mm. This probe has a contact
surface area of about 1 mm2. Thicknesses were measured at a
number of places on each specimen surface to determine how
close to parallel the faces were. All specimens used were parallel
within better than 0.1 mm.
3 Thermal Cycling
Thermal cycling of the specimens was carried out in an
apparatus which used a motor to drive a chain, as shown in
Fig. 1. Samples were moved from a furnace to a refrigerated
airspace and back in holders attached to the chain. Soak times
in each are controlled by the user from a personal computer.
The number of cycles to be performed in a run is also controlled
from the personal computer.
Two different thermal cycle schedules were used in these
measurements, denoted by schedule 1 and schedule 2. The first
cycle schedule involved four minute soak times in each cham-
ber, with a higher furnace temperature than the second cycle
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FURNACE
sample holders
\
•Jj
REFRIGERATION thermocouples
Wj
personal computer
strip chart recorder
and power to furnace
and refrigeration units
Fig. 1 A schematic diagram of the thermal cycling apparatus
schedule, which used six minute soak times to achieve greater
range and smaller thermal gradients in the specimens.
The temperature of the refrigeration unit was kept constant
throughout all the experiments at - 35°C. This was measured
by attaching a thermocouple directly to the specimen holder
and allowing it to reach equilibrium in the refrigeration unit.
The thermocouple used by the refrigeration controller was in
a slightly different location, and this thermocouple measured
a variation of ±3°C during experiments.
For thermal cycle schedule 1, the furnace temperature was
kept at 85°C at specimen height, measured as above. Thermal
cycle schedule 2 used a temperature of 80°C. The oven tem-
perature was very consistent with time, varying by less than
±2°C.
The actual temperature ranges experienced by the specimens
during the experiments were determined by attaching ther-
mocouples to actual specimens and using a strip chart recorder
to plot the results. Two thermocouples were used in each case.
One thermocouple was placed in a hole drilled to the approx-
imate center of the specimen, and the other fixed to the spec-
imen surface. Not only does this provide information about
cycle temperatures, but also the temperature gradient across
the specimen. For the axial fiber specimens, only the rod shaped
specimens were examined, as the flat specimens were very thin
and would have developed similar temperatures but much
smaller gradients.
For composite 1, a 15 mm length was cut off the rod and
thermocouples fixed to the center through a hole, and at the
outside of the rod at the center position. The specimen was
taken from room temperature to the furnace, then to the re-
frigeration chamber. A 7 mm long rod-shaped specimen of
composite 2 and a 10 mm x 10 mm x 6.5 mm specimen of
composite 3 were also tested for temperature profiles in cycle
2. Figure 2 shows approximate temperature-time curves for
this experiment, as estimated from the above measurements.
It was found that the maximum and minimum temperatures
did not change more than 1-2°C after the first cycle from
room temperature.
4 Ultrasonic Measurements
Measurements of the longitudinal ultrasonic velocity v and
attenuation a were made to evaluate the effect of thermal
fatigue in the composites. In the uniaxial composites 1 and 2,
the velocity and attenuation measurements were made parallel
(yn and aj) and perpendicular (v± and a±) to the fiber direction.
Composite 3 being isotropic does not require this distinction.
Transactions of the ASME
 100 schedule 1 the first peak of the excitation voltage waveform and the first
peak of the received signal. The transit time could be measured
75 to a precision of about 2 to 5 ns, depending on the time scale
being used. This corresponds to an error for an individual
50 measurement of less than 0.5 percent.
specimen The ultrasonic velocities are related to the elastic coefficients
temperature
(C) 25
and the densities of the material. Using cartesian coordinates
with directions X!, x2, x3; for the case of the isotropic composite
3, the axis Xi is chosen arbitrarily as the direction of propa-
gation. The velocity Vt is given by:

E(l-»<)
(1)
/P(1 + I.)(1-2J0
0 2 4 6 12 18 24 where c H is the elastic constant associated with the direction
of longitudinal propagation, and p is the density of the com-
time (minutes)
posite. Equation (1) also relates c n to the Young's modulus
E and Poisson's ratio v for isotropic materials.
schedule 2 For the uniaxial composites 1 and 2, the fiber axis is chosen
to be the Xi direction, and the velocity parallel to the fibers

V|| = (2)

The velocity perpendicular to the fibers is:

C22
= v2 = (3)

The composites 1 and 2 are transversely isotropic, so no dis-

tinction is made between the directions of propagation per-
0 2 4 8 12 16 pendicular to the fiber axis.
time (minutes) The attenuation measurements were also performed from
the oscilloscope. The peak to peak voltages of the excitation
Fig. 2 Dependence of specimen temperature on time for thermal cycle
schedules pulse and the received pulse were measured directly. The at-
tenuation coefficient a (an and a± for composites 1 and 2)
was defined from Eq. (4):
oscilloscope signal VR=Vjexp[-aL] (4)
delay
generator
© ©© where VR and VT are the amplitudes of the waves at the re-
ceiving and transmitting transducers, and L is the path length
pulse through the sample. The authors estimate the measurement
9 9 generator error in a to be in the order of 1-2 percent, depending on the
specimen being studied.
The success of these measurements depends critically on the
consistency of the bonding effects between the specimen and
the transducers. This bond affects both velocity and atten-
uation measurements, and may be a larger source of error than
actual measurement errors. It is possible to evaluate the re-
peatability of the bond indirectly by the measurement of the
absolute attenuation in a material as described by Read and
Dean [25].
To find the absolute attenuation in the specimen material,
the experimenter measures the amplitude of the initial wave
Fig. 3 A schematic diagram of the apparatus used for ultrasonic meas- VT at the transmitting transducer, and of the received wave
urements
VR at the receiving transducer. There is assumed to be one
reflecting surface at each boundary layer, with coefficients of
A modification of the sing-around method [29] was used to transmission given by k\ and k2. The measured received am-
measure ultrasonic velocity and attenuation, and is displayed plitude can be expressed in terms of the measured initial am-
schematically in Fig. 3. Matec Penetran® transducers with a plitude as:
nominal resonance frequency of 4 MHz were excited through V^k^Vje-*1 (5)
an amplifier by a signal generator operating in gated mode.
The transducers were sufficiently broadband to allow meas- The attenuation coefficient in the material can be isolated
urements to be made from frequencies of 3 MHz to 5 MHz. from Eq. (5) and written as:
One trigger source was used for both the signal generator and ln(frAr2) . V 1
the oscilloscope, but the trigger pulse was delayed before the a—— — MyR (6)
signal generator. This allows the oscilloscope sweep to start
before the excitation. The terms on the right side of Eq. (6) are measured values. If
To determine the ultrasonic velocity, the transit time between these values are plotted against L~\ the result should be a
two peaks was measured on the oscilloscope. The peaks were straight line with slope -ln(kik2) and a^-axis intercept of a,

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 1.10

B m
a
1.05 m T "
normalized r- - T T - |
attenuation a
0 O
0
r •O' ' "
' b' o o

l.OOi
^ f c - V7 B 5.00MHz
a ~1a
V 4.00MHz
--• O 3.00MHz

0.95
7 8 9 10

normalized
velocity

,h 8 S
• • & 8 g • 5 3
2 3 4 5 6 7
hundreds of thermal cycles (schedule 1)

Fig. 5 Graph of attenuation and velocity changes for composite 1:

2 3 4 5 6 7 8 longitudinal wave perpendicular to fiber axis (thermal cycle schedule 1)
hundreds of thermal eycles (schedule 2)

Fig. 4 Graph of attenuation and velocity changes for composite 1:

longitudinal wave parallel to fiber axis (thermal cycle schedule 2)
normalized
attenuation

the actual material attenuation. For a number of different

specimens, this plot will only yield a straight line if the product
of the bond line terms k\ki is constant.
Measurements of the absolute attenuation were performed
for each of the composites examined here (in the fiber direction
only for composites 1 and 2). In every case, when the data
was fit to Eq. (6), the correlation coefficient of the linear fit
was greater than 0.9800, indicating a very consistent bondline
effect.
B 5.00MHz

5 Results and Discussion normalized ~^ v 4.00MHz

velocity
Thermal cycling of the composite materials and the ultra- O 3.00MHz
sonic measurements were carried out as described in Sections
3 and 4. All of the materials examined showed some evidence
of damage due to thermal fatigue, as demonstrated by the
dependence of ultrasonic velocity and attenuation on the num- 8 8^A_ X
ber of thermal cycles. Curves drawn on these plots are not • s •••*• • - - !

meant to represent any mathematical relationship, but are

merely visual aids. Error bars shown for the first point on each
graph are estimates of measurement error for the graph. The
leftmost number at the bottom of the SEM photographs in-
dicates the bar length in microns. hundreds of thermal cycles (schedule 2)

Composite 1 was affected the most by thermal cycling. Par-
allel to the fibers, attenuation increased but velocity showed
no change as shown in Fig. 4. Perpendicular to the fiber axis,
ultrasonic velocity decreased and attenuation increased as
shown in Fig. 5 and Fig. 6. This is true for all three frequencies
as apparent in Figs. 5 and 6. Ultrasonic attenuation changes
were larger at higher frequencies, which was observed in all
the specimens. Models of interfacial stress indicate the highest
stress levels at the ends of the specimens [1, 28] and a very
sharp drop from this level toward the center of the specimen.
If this is the case we should expect a highly damaged surface
layer on the fatigue-tested specimens, with damage decreasing
toward the center.
The specimens of composite 1 examined for axial change
Fig. 6 Graph of attenuation and velocity changes for composite 1:
longitudinal wave perpendicular to fiber axis (thermal cycle schedule 2)
were cylindrical and all within 1 mm of 15 mm length. The
increase in attenuation without velocity change seems to in-
dicate a surface layer change that does not affect the bulk
properties (especially elastic moduli along the axis) of the spec-
imens. The SEM photographs of Fig. 1(a) and (b) also indicate
fiber pullout at these faces, which would create a surface layer
of different acoustical properties. Figure 1(a) shows an un-
fatigue-tested specimen of composite 1, while Fig. 1(b) shows
a fatigued specimen (after 800 cycles in schedule 2) with fiber
pullout and matrix cracking radially outwards from the fibers.

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 1.05

nonnalized
attenuation

~. '0
_0_ _ - -

1.00
...

0.95 L-----L_---:'----,'-----L_---:'-_'----'-_---:'-_'--'
o 10

1.05

normalized ... 4.00MHz

velocity
o 3.00Ml-j:z

Fig.7(a) SEM photograph 01 composite 1, unlatigued. See Fig. 7(b) for

~
comparison. 1.00
- ~~~~d~.~.-~-._~ _!: __

0.95 '---------L_---:'-_'---1-_---:'-_'-----L_---:'-_'--'
o 10
hundreds of IhclmuJ cycl~s (schedule 2)

Fig. 8 Graph 01 altenualion and velocity changes for composite 2:

longitudinal wave perpendicular to fiber axis (thermal cycle schedule 2).

Fig. 7(b) SEM photograph 01 composite 1 after 800 cycles (schedule

2)

This increases scattering [30], and causes the increase in at-

tenuation that is observed. The damaged layer is likely to be
very thin in the direction of wave propagation, and thus in-
significant in producing an observable change in the acoustic
transit time. This explains the insensitivity of ultrasonic ve-
locity to the damage.
Flg.9(a) SEM photograph 01 composite 1, unlatigued
Stress relaxation due to fiber end pullout reduces the effect
of further cycling, as shown in the decrease in attenuation
change after the initial jump in all materials examined. For all
materials examined here, it was found that rates of damage
accumulation were initially very high but quickly slowed. This
is in agreement with observations of Kasap et al. [18] and
Hartung [20].
Perpendicular to the fiber direction, composites I and 2
showed increased attenuation and decreased velocity, as illus-
trated in Fig. 5, Fig. 6, and Fig. 8. SEM examination also
showed clear evidence of damage, examples of which are shown
in Fig. 9, Fig. 10, and Fig. 11. Matrix cracking and fiber
debonding from the matrix appear to be the main mechanisms
of damage, similar to observations made on E-glass reinforced
composites by Yannacopoulos, et al. [19]. The causes of in-
creased attenuation are likely the same as for the previous case,
with a surface layer that is cracked and contains even broken
fibers. The velocity decrease may be due to the fact that the
path length for these specimens was much smaller than that Fig. 9(b) SEM photograph of composite 1 after 1000 thermal cycles
for the axial specimens, due to specimen geometry and atten- (schedule 2)
u!!tion. The weakened layer may now be significant in size.
Due to the very high attenuation perpendicular to fiber axis The experimental error is apparent in the scatter in Fig. 8. For
in composite 2, it was very difficult to evaluate properties in more confidence in the measurement of damage in composite
this direction, and the signal to noise ratio at the 5.00 MHz 2, perpendicular to fiber direction, more specimens need to be
test frequency was too small to permit accurate measurements. examined, with higher excitation voltages.

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 Fig.10(a) SEM photograph of composite 1, prior to lesting Fig. 11(a) SEM photograph of composite 2, prior to testing

Fig.10(b) SEM photograph of composite 1 after 1000 thermal cycles Fig. 11(b) SEM photograph of composite 2 after 1000 thermal cycles
(schedule 2) (schedule 2)

1.05

In the fiber direction, composite 2 showed little degradation normalized

of properties due to thermal fatigue in ultrasonic examination attenuation

as apparent in Fig. 12, and only inconclusive evidence was

found using SEM (Fig. 13). The fatigue-tested sample shown
in Fig. 13(b) appears to show some damage at the surface,
possibly due to fiber pullout. Some attenuation increase was
T 4.00MHz
found for composite 2 in the fiber direction at the test fre-
• 3.00MHz
quencies of 3.00 MHz and 4.00 MHz. Attenuation at 5.00
MHz was too high to permit accurate measurements for this
direction in composite 2.
Composite 3 consisted of polyphenylene sulphide (PPS) ma-
trix material with randomly oriented aramid fibers .• The fiber 1.05
content is 30 percent by volume. This implies that the me-
chanical properties of composite 3 are not as dependent on normalized
velocity
fiber as the other composites, due to the low fiber content.
For this composite, attenuation increased and velocity de-
creased with increasing number of thermal cycles, as shown
1.00
in Fig. 14. The magnitude of the velocity chang6was very
small. SEM examination of this material showed detachment
of fiber ends from the matrix after cycling. Figure 15(a) shows
an unfatigue-tested sample where the fiber surface is flat with
the matrix surface after polishing. Figure 15(b) andFig. 15(c)
0.95 '----'-_-'--'-_--'-----':_....L-~'--_'____.L___'
show a fatigued-tested specimen where the fiber is. curled up o W
out of the matrix, much like the specimen of composite 2 shown hUOl.lreds of thelma I cydes (s~hedulc 2)
in Fig. 11. There is no visible matrix cracking.
The mechanisms of damage for composite 3 appear to be Fig. 12 Graph of attenuation and velocity changes for composite 2:
longitudinal wave parallel to fiber axis (thermal cycle schedule 2)
debonding of fibers from the matrix material, especially at
fiber ends, where stress concentrations are going to be largest.
This creates scattering centers for ultrasound, leading to in- that the debonding is not occurring over a significant interface
creased attenuation. Even after 1800 cycles the velocity de- area.
crease is very small, less than 1 percent. This demonstrates Results from this work indicate that the main mode of dam-

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 Fig. 13(8) SEM photograph of composite 2, prior to testing. See Fig. Fig. 15(8) SEM photograph of composite 3, prior to testing. See Fig.
13(b) for comparison. 15(b) and Fig. 15(c) for comparison.

Fig. 15(b) SEM photograph of composite 3 after 1000 thermal cycles

(schedule 2)
Fig. 13(b) SEM photograph of composite 2 after 1000 thermal cycles
(schedule 2)

LOS

nonnalized •
attenuation
•
...
••
-~-II .,~-
__ .... ..,-T. O.-.r:--_'.O'O
~~Q.Q.~.o·O·o·~ 0 0 0
1.00 .
• S.OOMHz

.. 4.00MHz
o 3.00MHz

0.95 L---l._...L-_L.-.....L_..L...--'_--'-_.l---l_-'
o III 12 14 16 18 20

1.05
Fig. 15(c) SEM photograph of composite 3 after 1000 thermal cycles
(schedule 2)
nonnalized
velocity

age due to thermal fatigue is fiber-matrix debonding. The

carbon fiber composite, composite 1, also showed significant
1.00 matrix microcracking in the region surrounding the fiber. Ow-
ens and Schofield [12] and Hartung [20] found similar damage
mechanisms, with different strength changes in different com-
positions. Ultrasonic examinations indicate that the modulus
of these particular composites is not significantly affected by
0.95 _--'-_.l---l_-'-_-'----'-_...L..._L---'-_-' thermal fatigue cycling.
o 10 12 14 16 18 20

hundreds of thermal cych::s (schedule I)

6 Conclusions
Fig. 14 Graph of attenuation and velocity changes for composite 3:
longitudinal wave in random fiber orientation (thermal cycle schedule Changes in ultrasonic velocities and attenuations were ex-
1). amined as a function of number of thermal fatigue cycles in

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 three fiber reinforced polymers, two uniaxial continuous fiber
composites and one randomly oriented fiber composite. It was
observed that, in general, ultrasonic attenuation increased and
ultrasonic velocities decreased with number of cycles. In all
cases ultrasonic attenuation changes increased with frequency.
No frequency dependence of velocity changes was found. SEM
evaluations of the specimens after thermal cycling indicated
that damage occurred in the form of fiber-matrix debonding
and matrix microcracking.
In the uniaxial composites, which were carbon fiber 50 per-
cent by volume in vinylester and Kevlar fiber 61 percent by
volume in vinylester, it was found that the carbon fiber com-
posite was more damaged by thermal fatigue cycling. Ultra-
sonic velocities perpendicular to the fiber direction were
sensitive to thermal cycling. Ultrasonic attenuations, both par-
allel and perpendicular to the fiber axis, increased with number
of cycles. SEM examinations showed damage to consist of
fiber-matrix debonding and matrix microcracking in the area
immediately adjacent to the fibers.
The randomly oriented fiber composite was Kevlar 30 per-
cent by volume in polyphenylene sulphide. Ultrasonic atten-
uation increased and ultrasonic velocity decreased with
increasing number of thermal cycles. SEM examination of this
composite showed damage to occur in the form of fiber-matrix
debonding. No matrix microcracking was observed.
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