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Fatigue Performance of Kevlar/Epoxy Composites with Filled Matrix by Cork

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Article  in  Fibers and Polymers · December 2012

DOI: 10.1007/s12221-012-1292-4

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Fibers and Polymers 2012, Vol.13, No.10, 1292-1299 DOI 10.1007/s12221-012-1292-4

Fatigue Performance of Kevlar/Epoxy Composites with

Filled Matrix by Cork Powder
P. N. B. Reis*, J. A. M. Ferreira1, J. D. M. Costa1, and M. J. Santos2
Department of Electromechanical Engineering, University of Beira Interior, Covilha 6201-001, Portugal
1
CEMUC, Department of Mechanical Engineering, University of Coimbra, Coimbra 3030-790, Portugal
2
CEMUC, Department of Electrical and Computers Engineering, University of Coimbra, Coimbra 3030-790, Portugal
(Received February 6, 2012; Revised May 2, 2012; Accepted June 2, 2012)

Abstract: The objective of this study is to characterize the fatigue strength of a Kevlar/epoxy laminate composite as well as
the benefits obtained by using an epoxy matrix filled by cork powder. Twelve ply laminates, all in the same direction, of
woven bi-directional Kevlar 292, were prepared by hand lay-up, using an SR 1500 epoxy resin. The composite sheets were
produced by a vacuum moulding process. The addition of cork powder reduces the static strength, however, in terms of
fatigue strength a similar behavior was found for both laminates.
Keywords: Composite laminates, Aramid fiber, Fillers, Fatigue, Mechanical testing

Instruction The fatigue strength in wet air was lower than that in
laboratory air and the strength degradation under cyclic
Composite materials have been applied to various engineering loading by wet environment was much larger than that under
fields such as aircraft, space, automotive, sport and marine quasistatic tensile condition. The fatigue fractured fibers
industries but, particularly, in military applications. They under the sinusoidal and the positive pulse waveform in air
offer an attractive potential for reducing the weight as also broke with fiber splitting, similar to the case of the
consequence of their high specific strength and stiffness. tensile test. Under the negative pulse waveform, the specimens
For military applications aramid fibers are a very important that fractured at 102-104 stress cycles broke with fiber splitting
reinforcement for advanced composites as consequence of and for fatigue lives higher than 105 stress cycles transverse
their high degree of toughness and damage tolerance. In fact crack to the fiber axis occur. Bunsell [27] subjected individual
these fibers do not present brittle behavior, like glass or Kevlar 49 fibers to sinusoidal tensile load and found that the
carbon fibers, but fail by a series of small fibril failures. minimum load required to develop fatigue failure of individual
These many small failures absorb much energy and, Kevlar 49 fibers was approximately 80 % of the UTS.
therefore, result in very high toughness. Similar tests were developed by LaFitte and Bunsell in
In this context the literature shows a really interest in these Kevlar 29 fibers [28]. Maximum stress levels between 56-
fibers and several studies can be found. To improve the 90 % of the fibers’ UTS were analyzed. Their results
interfacial adhesion, as consequence of the low surface indicate that, under cyclic loading conditions where the
energy and chemically inert surface of the Kevlar fiber, there maximum load is below about 75 % of the UTS, individual
are extensive works [1-9]. On the other hand to improve the Kevlar 29 fibers exhibit little or no reduction of lifetime
impact strength several techniques are proposed [10-19], compared to the creep lifetime under constant stress equal to
and, more recently the inclusion of fillers was also successful the maximum level used in the cyclic testing. At higher
used [20-24]. stress levels if the cyclic amplitude is small enough, such
For the industries mentioned above, structural components that the minimum stress applied during fatigue remains
are usually subjected to complex fatigue load histories. In above about 25 % of UTS, the creep behavior dominates and
this case the performance of the composite materials is lifetime is enhanced due to the intermittent exposure to high
strongly dependent of the fibers behavior. In case of aramid stress. On the other hand, when the cyclic amplitude is great
fibers shows time-dependent mechanical behavior, indicating enough to cause the minimum stress to fall below about
that their viscoelasticity may play an important role on the 25 % of UTS, fatigue damage ensues and lifetime is reduced.
fracture behavior of the composites [25]. Tanaka et al. [26] However for bending fatigue the main mechanisms that
investigated the influences of stress waveform and wet promoted strength degradation are: compressive fiber buckling,
environment on the fatigue fracture behavior of aramid kinking and fiber-to-fiber surface abrasion [29,30]. These
single fiber (Kevlar 49). They observed that, in air, the mechanisms result from the high tensile modulus of the fiber
fatigue strength under negative pulse waveform was higher coupled with its low compressive and transverse strengths
than those under sinusoidal and positive pulse waveforms. [31,32].
The fatigue behaviour of Kevlar fibre reinforced composites
*Corresponding author: preis@ubi.pt is a subject requiring a better understanding, particularly the

1292
Kevlar/Epoxy Composites with Filled Matrix Fibers and Polymers 2012, Vol.13, No.10 1293

fatigue behavior of the Kevlar fiber reinforced composites changed. A load cell was used to monitor the load. The load
with filled matrix. In this context the aim of this work is wave was sinusoidal, having a stress ratio of R=0.1 and a
study the bending fatigue response of a Kevlar/epoxy frequency of 25 Hz.
composite with filled epoxy matrix by cork powder. Cork The nominal bending stress (σ) was calculated using:
presents an alveolar structure and it is characterized by high
3PL
specific strength and stiffness, near zero Poisson coefficient, σ = -----------2 (1)
high damage tolerance to impact loads, impervious to liquid 2bh
and gases, resistance to reactive agents and microorganisms, being P the load, L the span length, b the width and h the
resistance to wear and fire, very low thermal conductivity, thickness of the specimen.
good acoustic insulation capacity and excellent damping The water effect on the flexural properties of the laminates
characteristics [33-36]. was also analyzed. In order to obtain the water absorption it
was used the following procedure, in accordance with BS
Material and Experimental EN ISO 62:1999. The samples were placed in an oven at
80 oC for 2 hours, then cooled and weighed in order to obtain
Twelve ply laminates, all in the same direction, of woven the dry weight (DW). Afterwards, a series of samples were
bi-directional Kevlar 170-1000P (170 g/m2), were prepared immersed in water and periodically weighted to obtain the
by hand lay-up and the overall dimensions of the plates were current wet weight (CWW). The water absorption in weight
330×330×3 mm and the fiber weight fraction was 66 %. SR percentage (W%) was calculated from equation (2):
1500 epoxy resin and a SD 2503 hardener, supplied by
Sicomin, were used. The system was placed inside a vacuum W% = CWW – DW- × 100
--------------------------- (2)
bag and a load of 2.5 kN was applied for 24 hours in order to DW
maintain a constant fiber volume fraction and uniform
laminate thickness. During the first 10 hours the bag remained Results and Discussion
attached to a vacuum pump to eliminate any air bubbles
existing in the composite. The post-cure was followed The flexural properties of the Kevlar/epoxy composites
according to manufacturer datasheet (epoxy resin) in an with pure resin and filled by cork powder were obtained by
oven at 40 ºC for 24 hours. 3PB static tests. Typical load-displacement curves for both
With the same manufacturing process were produced materials are plotted in Figure 1. Both materials show a
composite laminates with filled epoxy matrix by cork linear elastic behavior, in an early stage, with a non-linear
powder. The bulk density of the cork powder is 0.1095 gcm-3 region that starts around 150 MPa. After peak stress the load
and the particles’ size, in terms of percentile, is: d(0.1)= decreases, however, the drop is more significant for filled
18.6 µm, d(0.5)=78.9 µm and d(0.9)=208.3 µm. More details laminates. The soft decreasing of the load-displacement
about the powder characterization can be found in [37].
Before being added into the resin, the cork powder was dried
in an oven-dried (Heraus, model UT 6060) at about 120 oC
for 2 h. When dried it was placed in a desiccators, cooled to
room temperature, and stored until use.
The mixture, epoxy resin and the cork powder, was
conducted at 900 rpm for 2 hours and, at same time,
subjected to ultrasonic bath sonicator. The filler content
employed was 3 wt.% of the epoxy resin-hardener mixture.
The mixture was degassed in a vacuum oven followed by
addition of hardener agent. Special care occurs in this
process to avoid the formation of bubbles.
The specimens used in the static and fatigue three point
bending tests, were cut from these plates, with dimensions of
60×10×3 mm and tested with a span of 45 mm. The static
tests were performed according the recommendations of
ASTM D 2344 Standard in an electromechanical Shimadzu
AG-10 universal testing machine, equipped with a 5 kN load
cell and TRAPEZIUM software. Four specimens were
tested for each material. The fatigue tests were carried out in
constant displacement control, at room temperature in an Figure 1. Typical load-displacement curves for Kevlar laminates
electromechanical machine where the stress ratio can be with pure epoxy resin and filled by cork powder.
1294 Fibers and Polymers 2012, Vol.13, No.10 P. N. B. Reis et al.

Figure 3. Water absorption curves.

are more pronounced as consequence of the high compressive

stress concentration in the pin load contact region [39].
Figure 3 shows the water absorption curves for two
material configurations. All these configurations show water
absorption up to 100 days (2400 hours) and the same trend is
expected after this value. According with the open literature,
for Kevlar-reinforced composites the hygroscopic nature of
the resin and the fiber must be considered [40]. For epoxy
resins the water absorption varies substantially, depending
Figure 2. S-scan observations: (a) specimens before tested, (b) on the resin type and the curing system. Eckstein [41], for
laminates with pure resin after tested, and (c) laminates filled by example, shows that the water absorption may differ by a
cork powder after tested. factor of ten between different epoxy resins, and to a factor
of up to three for the same resin with a different curing
agent. On the other hand, aramid fibers are strongly
curve, for Kevlar with pure resin laminates at maximum hygroscopic and often with values higher than the matrices.
load, denotes a more stable grow of the damage mechanisms A maximum moisture content of 6 % was reported by the
than the one observed for filled composites. In this case it is manufacturers for Kevlar-49 at room temperature 96 % RH
possible conclude that the fillers change the mechanical [40]. In this context, the water absorption was studied for the
behavior of the matrix and agrees with the study developed system SR 1500 epoxy resin and SD 2503 hardener, and it is
by Reis et al. [37], where was found that the introduction of presented in Figure 3 also, in order to understand better the
cork powder in a polyester matrix decreases the flexural results for laminates.
strength. After 100 days, the epoxy system used present around
Figure 2 presents the damage obtained by S-Scan, using an 0.9 % of moisture content, value much lower than observed
Olympus phased array instrument, Omni-K-PA1664MW10. for the laminates. In fact when the Kevlar fibers were added
In detail, it is possible to observe that Figure 2(a) presents to the resin it was observed an increase of 2.5 times of water
the material without damages of a specimen before testing uptake, as consequence of their hygroscopic behavior [40],
and, by contrast, the specimen observed in Figure 2(b) and and around 3.6 times for laminates with fillers. Similar
2(c) shows significant delaminations (by absence of wave tendency was obtained by Reis et al. [37] when similar
transmission) for laminates with pure resin and laminates fillers were added to polyester resin.
filled by cork, respectively. In fact delaminations, for Kevlar Finally the UV effect on the flexural properties of the
composites, are the main energy absorption mechanism [38]. laminates was also studied. The samples were exposed around
At same time the aramid fibers do not fail by brittle cracking, 450 hours in a UV-Irradiation chamber BS-02 supplied by
as do glass or carbon fibers, but they fail essentially by a Dr. Gröbel UV-Elektronik GmbH. It was used four lamps,
series of small fibril failures. All these damage mechanisms type UVB, with intensity of 2.3 mW/cm2. According with
Kevlar/Epoxy Composites with Filled Matrix Fibers and Polymers 2012, Vol.13, No.10 1295

Woo et al. [42], photo-degradation of polymers due to UV aramid-fiber/epoxy-resin composites. An approximately 35 %

exposure occurs by activation of polymer macromolecules loss in the room-temperature flexural strength was observed
arising from the absorption of photons. This process generates in Kevlar-49/epoxy resin laminates at 5 % moisture uptake,
free radicals in the presence of air or oxygen, and induces apparently as a result of the ease of fiber buckling in a
dissociation of chemical bonds on the surface as well as plasticized matrix [40]. Finally the UV effect on flexural
inside the material by diffusion. Physical changes consist properties is negligible for the time of exposure tested.
mainly of discoloration and micro-cracking phenomenon. According with Woo et al. [42] it is possible to say that the
However for relatively short periods of exposure only some period of exposure was relatively short and insignificant
changes in surface morphology are observed, but, in extended changes in surface morphology (micro-cracks) and/or chemical
exposure to UV radiation, the elongation and rupture of bonds occurred. Consequently the flexural properties remained
polymers shows to be very sensitive to irradiation [42]. On unchanged.
the other hand the UV stability of Kevlar has been described The results of the fatigue tests are plotted in Figure 4 in
in the literature [43,44] and it is possible to conclude that its terms of maximum stress, at the beginning of the test, versus
light stability depends on the thickness of the exposed item. the number of cycles to failure (N). It was observed that
Very thin Kevlar 49 fabric when exposed directly to very fatigue strength depends significantly on the defined failure
high intensity sunlight for an extended period will lose about criterion, so the criterion of failure was defined as the
half its tensile strength within few days. In thicker items, moment when the loss of maximum stress reaches 25 % of
such as a half-inch diameter rope, the outer layer protects the the initial value. In terms of Kevlar fibers, its fatigue lifetime
majority of the rope and strength loss is minimized [44]. is dependent on the amplitude of the applied oscillatory load
Table 1 presents all results obtained in 3PB static tests, in as well as the maximum load to which the fiber is cycled
terms of the average values and standard deviation. Ultimate [27]. On the other hand these fibers show time-dependent
stresses, σUTS, were obtained using equation (1) with the mechanical behavior, indicating that their viscoelasticity
peak load values. It is possible to observe that the average may play an important role on the fracture behavior of the
value of the ultimate stress, at room temperature, is higher composites [25]. At same time the aramid fibers fail by a
for laminates with pure resin, around 10.4 %, in comparison series of small fibril failures, which can explain also the
with laminates filled by cork powder. According with fatigue performance for long fatigue life. The fatigue data
previous studies developed by the authors [37], it was also were analyzed according with the ASTM 719 and respective
observed a decrease of the flexural strength with the filler parameters are plotted in Figure 4. Comparing the results
content. This tendency was well fitted by the Nicolais and shown in Figure 4 it is possible to observe a similar behavior
Nikodemo model, which is specially used when poor adhesion for both laminates: medium and standard deviations of both
occurs between matrix and filler. The immersion in water parameters (A and B) of the two S-N curves have very
promotes decrease in terms of ultimate stress for both similar values.
laminates, relatively to dry ones. For laminates with pure Figure 5 shows the normalized stress range (∆σ/∆σ0)
epoxy resin the ultimate strength decreased around 23.1 % versus N/Nf curves for filled and unfilled laminates. ∆σ is the
while for laminates filled by cork powder this value was current stress range of the load cycle, ∆σ0 is the initial value
around 31.5 %. This can be explained by the fact that the of ∆σ, N the current number of cycles and Nf is defined by
laminates filled by cork powder absorb more moisture. For the number of cycles from which a stabilization of ∆σ
epoxy resins, according with Akay et al. [40], a drop in the
glass-transition temperature (Tg) of 15-20 oC per 1 % moisture
pickup have been widely reported and, consequently, matrix
plasticization and matrix/fiber interface degradation have
been shown to influence the mechanical properties of

Table 1. Three point bending properties for several environmental

conditions
Kevlar Average Std. dev.
Conditions
laminates σUTS (MPa) (MPa)
Room temperature 298.96 2.87
With pure
Immersed in water 229.79 7.07
resin
UV degradation 296.7 3.94
Room temperature 267.96 6.16
Resin filled by
Immersed in water 183.49 8.24
cork powder
UV degradation 265.97 8.47 Figure 4. Fatigue strength, S-N curves.
1296 Fibers and Polymers 2012, Vol.13, No.10 P. N. B. Reis et al.

occurs. These figures show an important dependency of the increases, the damage, quantified by the stress range decreasing,
initial stress range. When the cyclic displacement amplitude is faster. In all cases significant decreases of stress range
were observed, since the first cycles of fatigue life, caused
not only by matrix creep and microcracking, but essentially
by significant delaminations between laminate layers. In fact
delaminations, for Kevlar composites, are the main energy
absorption mechanism [38]. The curves presented in Figure
5 were fitted by a curve with following mathematical equation:
b
∆σ
--------- = a ⋅ ⎛ ----- + c⎞
N
(3)
∆σ0 ⎝ Nf ⎠
with
1/b
c = ⎛⎝ ---⎞⎠
1 (4)
a
The values of “a” and “b” are constants obtained by a
power trend line that fits the curves represented in Figure 4.
Parameter “c”, obtained by the equation (5), was found to
force the curve to start at 1. All constants are presented in
Table 2.
Figure 6 shows a direct comparison of the normalized
stress range, for filled and unfilled composites, relatively to
the tests carried out at initial σmax=135.9 MPa. It is possible
to observe that the curve for laminates with pure resin is
above of the curve for laminates with resin filled by cork
powder. This suggests that occurs a significant stress realize
and, consequently, a drop of the stiffness.
Figure 7 shows the UV effect on fatigue strength. Laminates
with epoxy resin filled by cork powder were exposed by 450
hours and compared with other ones without any exposition
time (control samples). The criterion of failure was defined,
Figure 5. Typical ∆σ/∆σ0 – N/Nf curves for: (a) Kevlar/epoxy again, as the moment when the loss of maximum stress
laminates and (b) Kevlar with epoxy filled by cork powder reaches 25 % of the initial value. It is possible to observe
laminates. that both laminates present similar performance, which is

Table 2. Constants of the equations that fitting the different curves

Maximum stress Constants Correlation
Material Curves
(MPa) a b c coefficient
126.5 0.929 -0.017 0.0131 0.940
135.9 0.913 -0.012 0.0005 0.970
Kevlar 176.0 0.705 -0.099 0.0293 0.966
+ ∆σ/∆σ0 – N/Nf 184.1 0.644 -0.116 0.0225 0.997
Epoxy resin 190.7 0.622 -0.095 0.0068 0.986
212.3 0.584 -0.125 0.0135 0.992
236.7 0.511 -0.107 0.0019 0.992
130.5 0.869 -0.030 0.0093 0.863
Kevlar 135.9 0.830 -0.051 0.0259 0.974
+ 154.6 0.775 -0.035 0.0007 0.893
Epoxy resin ∆σ/∆σ0 – N/Nf 185..4 0.710 -0.042 0.0003 0.987
filled by 198.0 0.650 -0.066 0.0015 0.985
cork powder 223.9 0.498 -0.093 0.0006 0.947
252.8 0.454 -0.094 0.0002 0.984
Kevlar/Epoxy Composites with Filled Matrix Fibers and Polymers 2012, Vol.13, No.10 1297

Table 3. Statistics of the roughness measurements

Control samples After UV
Statistics
(µm) radiation (µm)
Arithmetic average, Ra 0.0688±0.0589 0.0879±0.0401
Root mean square, Rq 0.0882±0.0377 0.1111±0.0101
Average peak to valley height, Rz 0.5174±0.0955 0.5927±0.0808
Evaluation length, Lo 0.8012±0.001 0.8020±0.0007
Core roughness depth, Rk 0.2158±0.1155 0.2731±0.0947
Reduced peak height, Rpk 0.0727±0.0487 0.1029±0.0183
Reduced valley depth, Rvk 0.1098±0.0874 0.1218±0.0572

Figure 6. Comparison of the normalized stress range for initial

σmax=135.9 MPa.

Figure 7. UV effect on fatigue strength, S-N curves.

Figure 9. Water effect on fatigue strength, S-N curves: (a) pure

epoxy resin and (b) epoxy resin filled by cork powder.

or chemical bonds. However, according with Woo et al. [42],

for relatively short periods of exposure some changes in
surface morphology are the main damage. In order to analyze
the presence of micro-cracks, because it is well known their
Figure 8. Typical roughness profile for: (a) control sample and (b) influence in the fatigue strength, Figure 8 shows the roughness
laminates exposed to UV radiation. profile for the two laminates. The roughness profiles were
obtained by a Mitutoyo equipment, model SJ-500, for an
according with the static tests. This suggests that the period evaluation length of 0.8 mm. Table 3 present the statistic of
of exposure was relatively short to produce significant the roughness measurements, where is evident that all
changes in terms of surface morphology (micro-cracks) and/ parameters are very close. As expected, the roughness
1298 Fibers and Polymers 2012, Vol.13, No.10 P. N. B. Reis et al.

parameters, measured before and after UV exposition, are Davies, J. Mater. Sci., 27, 5431 (1992).
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