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Article history: Tensile fatigue behavior of tapered glass/epoxy laminates is investigated. The effect of nanoclay addition
Received 26 February 2014 into the epoxy resin is examined. It is shown that the relative orientation between the adjacent belt layer
Received in revised form 22 May 2014 and the cut layer has important inuence on the fatigue life. The fatigue crack starts at the resin pocket
Accepted 29 May 2014
and propagates along the interface between the belt layer and the core layer in the thicker section of the
Available online 10 July 2014
laminate. Crack propagation is mainly due to mode II crack failure. The addition of the clays enhances the
resistance against this mode II crack propagation, and thus prolongs the fatigue life of the laminate.
Keywords:
2014 Elsevier Ltd. All rights reserved.
A. Glass bers
A. Nanoclays
A. Polymer matrix composites (PMCs)
B. Fatigue
B. Matrix cracking
http://dx.doi.org/10.1016/j.compscitech.2014.05.038
0266-3538/ 2014 Elsevier Ltd. All rights reserved.
S. Helmy, S.V. Hoa / Composites Science and Technology 102 (2014) 1019 11
wide array of property improvements with only very low fractions Fiber orientation Sample conguration
of clay, including the improved thermal stability [22,23], decreased Cross-ply (CPS) [02/902/02/902/02/902/02/902/02a/902a]s
moisture and gas permittivity [24] and better ame retardation Cross-ply (CPN) [02/902/02/902/02/902/02/902/902a/02a]s
[25]. The nanoclay, in particular, exhibited ameliorating effects Quasi-isotropic (QIS) [02/902/+452/ 452/02/902/+452/ 452/02a/902a]s
on fracture and fatigue resistance of carbon ber composites: e.g. a
Orientation of the dropped ply.
increased mode I delamination resistance [26], developed impact
damage resistance and tolerance [27] and better static and impact
resin by hand with a spatula. Next, the high speed homogenizer
fracture toughness [28,29]. It is clear from the literature review
up to a maximum rotational speed of 25,000 rpm for 20 min was
that nano clay reinforced polymers have better dynamic and fati-
used to disperse the clay. Temperature of the suspension was clo-
gue behavior over the pristine matrix. The objective of the present
sely monitored using a thermometer and was kept below 100 C
study is to investigate the fatigue behavior of tapered composite
throughout the process to avoid self-polymerization.
beam structure made of glass ber and epoxy resin modied with
The resin was prepared by the following procedure: The exact
nanoclay.
amount of hardener (35 phr) was rst added to neat epoxy or
epoxyclay mixture (after dispersion with high speed homoge-
2. Experimental nizer) at room temperature. The mixture and hardener were then
mixed slowly with a stirrer for 5 min to avoid air entrapment. To
The tapered specimens are composed of three sublaminates as remove air bubble, the mixture was then degassed in a vacuum
shown in Fig. 1: one internally dropped sublaminate, and two oven at a vacuum of 25 mmHg for 25 min at room temperature.
outer continuous sublaminates (belt sublaminates) that cover the Hand lay-up and autoclave molding processes were used to fab-
dropped sublaminate. All of the laminates investigated are sym- ricate all samples. At rst, the bers were cut from the ber roll
metric. The ber orientations for all samples are summarized in according to the orientation of lay-up using standard knives with
Table 1. The laminates were tapered from 40 plies to 32 plies replaceable blades into the appropriate lengths for hand lay-up.
through a taper angle of approximately 10. The dropped sublami- The laminate panels were made using a ply ll-in technique shown
nate contains 8 plies and terminates at the midplane of the lami- in Fig. 2 whereby an equivalent tapered section was built up on the
nates. The triangular section in Fig. 1 represents a resin rich region. other side of release plies. Formation of laminate panel (for 4032
It is noted that in a real engineering structure, the lay up layers) was done following the steps below:
sequence is more complicated and there are more drop-off regions.
However in order to understand the mechanisms for the crack 1. The lower ll-in plies were placed on the mold (4 cured layers
propagation and fatigue behavior, a simple tapered arrangement of the same composite material).
such as that in Fig. 1 can provide better insight without the burden 2. The lower belt plies (16 layers) were laid-up.
of complexity. 3. The dropped plies (8 layers) were laid-up.
Table 1 shows three different lay up sequences, all with the 4. The upper belt plies (16 layers) were laid-up.
same number of plies. In the rst lay up sequence (CPS), the ber 5. The upper ll-in plies (4 cured layers of the material) were
orientation in the last belt plies is 90 whereas that of the rst nally placed.
cut plies is 0. In the second lay up sequence (CPN), the ber orien-
tation of the last belt plies is 90 and that of the rst cut plies is also This technique allows tapered panels to be made between at
90. In the third lay up sequence (QIS), 45 layers are added in addi- plates and produces good consolidation without the need for spe-
tion to the 0 and 90 layers. Also, the last belt plies have orienta- cial tooling. All of the full length plies for the laminates have in-
tion of 45 while that of the rst cut plies is at 0. These features plane dimensions of approximately 210 mm long, and 15 mm
have important inuence on the fatigue performance of the wide. The internally dropped plies that make up the ply-drop step
samples. are also 15 mm wide and 100 mm long.
The laminates were fabricated from the following materials. The specimens were cut by high speed diamond wheel/water
Unidirectional S-glass bers were manufactured by AGY World cooled cut-off saw in order to avoid any surface defect/damage
Headquarters and supplied by Aerospace Composites Products within the dimensions shown in Fig. 3. The thin and the thick
Inc. Organoclay Nanomer I.30E was supplied from Nanocor Inc. regions of the specimen are made of the same length; 101 mm
The resin and hardener are EPON 828 and EPICURE 3046, respec- whereas the length of the tapered region is 6 mm. Prior to conduct-
tively, both supplied by Hexion Specialty Chemicals. A high-speed ing the tests, strain gages are bonded to the specimens. Gages of
stirring method is used to disperse the clay in resin. type Vishay CEA-06-125UW-350, manufactured by micro-Mea-
The procedure for dispersing nanoclay in the resin is as follows: surement of Measurements Group, Inc., are used and attached onto
The resin was rst preheated to 45 C to reduce the viscosity. Then the specimens with M-Bond 200 adhesive as prescribed by Instruc-
2 wt.% of nanoclay was added to the resin. The clay was mixed in tion Bulletin B-127-6.
For all specimens, one strain gauge is bonded longitudinally at
the center of one surface to monitor the axial strain. The strain
gauge is located on the side of the thin section, 10 mm from the
end of the thick section as shown in Fig. 4.
2.4. Testing
Fig. 4. Location of strain gauge on the specimen. Tension tests were conducted prior to fatigue testing using a
digitally controlled (MTS) Servo Hydraulic Testing Machine at a
crosshead rate of 2 mm/min. Output from the load cell of the test-
samples, of the lay up sequence CPS. In Fig. 5a (no nanoclay), exam- ing machine namely, strains and load, and crosshead displacement
ining the central part of the gure, one can see the last belt plies (0 were continuously monitored with MTS Recorder. Tensile strength
and 90 layers) before the cut plies (0 and 90 plies). It can be is calculated by dividing the maximum load over the cross-sec-
observed that the last 90 belt plies are not stable. A signicant tional area of thin part of the tapered specimen. The fatigue testing
amount of bers from these plies fall into the cavity created by of the specimen was conducted in force-controlled mode. All fati-
the cut. As such the cavity is not just a resin rich area but it is also gue tests were carried out under a load ratio (rmin/rmax) of
partially lled with bers. In Fig. 5b (with nanoclay) a similar sit- R = 0.1 and at a frequency lower than 10 Hz to avoid temperature
uation is observed. The difference between the situations in rise especially at high stress levels. Three specimens were tested
Fig. 5a and b is that in the case of no nanoclay (Fig. 5a), there is at each stress level namely, 0.8, 0.6, 0.5, and 0.35Sut. Development
more disorder in the bers in the cavity area as compared to the of damage during the tests was observed and monitored using a
case with nanoclay (Fig. 5b). The presence of the clay seems to long-distance Questar QMI (Maksutov-Cassegrain Catadioptric)
dampen the ow of the 90 bers into the cavity. Also, the cavity telescope manufactured by Questar Corporation. The light source
is lled more in the case with clay. This has a signicant effect (lamps) was placed on the side opposite to the strain gauge to
S. Helmy, S.V. Hoa / Composites Science and Technology 102 (2014) 1019 13
700
CPNF
CPSF
600 CPNU
CPSU
QISF
500
QISU
Stress (MPa)
400
300
200
100
0
0 0.005 0.01 0.015 0.02 0.025 0.03 0.035 0.04
Strain (mm/mm)
Fig. 5. Micrographs at the cut-off section of CPS samples. (a) Sample without
3.1.2. Tensile failure observations
nanoclay and (b) sample with nanoclay.
Fig. 7 shows a typical image of fracture surface after the appli-
cation of tensile tests on lled laminates. The failure modes in both
minimize the thermal effects on the strain gauge. More impor- laminates (lled and unlled) are similar. It is observed that the
tantly, the position of the light source was properly adjusted to failure is dominated by the fracture of longitudinal delamination
maximize the shade contrast inside the specimen for a clearer between the 90, for cross ply laminates, or 45, for quasi isotro-
crack progress monitoring. Specimen monitoring was focused at pic laminates, (8th layer) and 0 (9th layer). This is due to high
the edges. Any damage to the specimen edges was easily recog- interlaminar stresses between layers with different orientations.
nized as bright areas on the surface. In some cases when a noise Delamination is accompanied with crack between the dropped
(indicating the occurrence of cracking within the laminate) was and continuous belt plies.
reported, the experiment was stopped for observation. The exper-
iment was then continued until the specimen failed completely. 3.2. Fatigue tensile loading tests
Delamination
0 layer
Crack between
90 layer dropped plies
and continues
plies
8 plies
Delamination along interfaces adopted. According to this criterion, failure is dened when bers
break and total separation of the specimens is attained. The fatigue
strength can be expressed in terms of maximum stress level versus
logarithmic number of cycles to failure. Fig. 12 shows the fatigue
behavior of the three stacking congurations for both lled and
unlled laminates.
Closely examining the above gure, it can be clearly shown that,
for the same level of maximum applied stress, laminates with
Crack at tip of resin pocket nanoclay exhibit longer fatigue life than laminates without nano-
clay. This is true for all stress levels and for all stacking sequences.
Fig. 8. Resin crack and delamination damage along two interfaces toward thick
region in tapered beam. For (CPN) stacking sequence, a maximum improvement of about
50% in fatigue life is achieved at a load equivalent to 50% of the ten-
sile strength of the specimen. On the other hand, a minor improve-
ment of about 5% in fatigue life is achieved at a load equivalent to
Delamination along thin region Delamination along interfaces along thick region 80%. For (CPS) stacking sequence, a maximum improvement of
about 50% in fatigue life is achieved at a load equivalent to 50%
of the tensile strength of the specimen whereas a minor improve-
ment of about 2% is achieved at a load equivalent to 80%. Finally,
for (QIS) stacking sequence, a fatigue life improvement of about
46%, 54%, and a minor improvement of about 7% are achieved al
loads equivalent to 35%, 50%, and 80% of the tensile strength of
Fig. 9. Typical delamination damage before nal failure.
the specimen, respectively.
Results also indicate that, as far as fatigue life improvement is
concerned, nanoclay modication is more effective at low stress
levels (or high cycle regime) and less effective at high stress levels.
At high stress levels, the nanoparticles are less resistive in sup-
Fiber breakage
dropped plies pressing the propagating cracks.
As for the effect of stacking sequence, the following is observed:
Resin
pocket
600
CPNF Fig. 14(a) shows a photograph of a typical initial crack at point
500
CPSF (T). Fig. 14(b) shows the crack as it grows to the thick region,
CPNU
whereas Fig. 14(c) shows delamination along the entire length of
Max. Stress (MPa)
CPSU
400 QISF thick region (about 81 mm long). The mode of crack propagation
QISU
in fatigue is similar to that in static loading.
300 Fig. 15 compares the crack propagation lengths in the thick
region as a function of fatigue cycles for QISF and QISU specimens.
200
The curves are plotted under two stress levels namely, high level at
100
0.8Sut and a low level at 0.5Sut. The delamination length is mea-
sured in the direction shown in the small insert.
0 Clearly, the lower is the stress level, the longer is the fatigue life.
3 3.5 4 4.5 5 5.5 6 6.5
It can be seen that for both stress levels and at the early stage of
Cycles Log (N)
fatigue, the lled composites exhibit more damage than the
Fig. 12. Tensile fatigue strength, SN curves, for all specimens. unlled composites. Here, the early stage refers to the crack ini-
tiation stage in which it grows to around 10 mm from tip of resin
pocket in direction of thick section. After the initial damage period,
the lled composite specimens in general sustain a relatively
The improvement in fatigue lives in CPN laminates upon adding longer stable period with low damage indices for the rest of fatigue
nanoclay is higher than that in CPS laminates. More specically, life. The nal failure takes place much earlier in the unlled com-
the fatigue life for CPNF laminates is about 1.181.54 higher posite than in the lled ones.
than that for CPNU laminates. There can be a few reasons for the improvement in the fatigue
life due to the addition of nanoclay. First is the situation of the ll-
ing of the bers into the cavity as shown in Fig. 5. The presence of
3.2.3. Fatigue crack growth rate the clay aids in more complete lling of the cavity. This reduces
Specimens were periodically inspected visually during the fati- stress concentration at the cut area. Second is the enhancement
gue testing to monitor the delamination growth at the edges. The in fracture resistance at the interface between the belt plies and
following observations are observed. the core of the cut plies. It was shown in [29,3133] that addition
of clay greatly improves the fracture toughness of epoxies.
The crack initiates in the specimens at the tip of resin pocket. Figs. 16 and 17 show the crack lengths for lled and unlled CPS
Then, delamination seems to start always from this crack tip to and CPN respectively. It is shown that CPS and CPN laminates have
the interface between the belt plies and the adjacent resin the same behavior of QIS laminates where adding the nanoclay
pocket as shown in Fig. 13(a). These cracks are faint but visible improves the crack propagation rate in both low and high stresses.
on the tapered beam surface during testing. This improvement is more signicant in low stress levels.
Once a crack is formed, delaminations grow from the crack Fig. 18 shows a comparison of delamination length between
toward the thick region at both interfaces between dropped three congurations at different stress levels. It is observed that
plies and belt plies simultaneously, Fig. 13(b). These delamina- CPS and CPN have crack growth rates less than QIS. The reason of
tions grow in a stable and steady manner until they approach this difference in crack growth rates may be related to the presence
around 20 mm along the thick region. of the 45 layers in the QIS laminates, which give rise to shear
Finally, an unstable delamination occurs as delaminations grow stresses. The difference in crack growth rates is more signicant
faster along the entire length of the thick region as shown in at low stress levels. In addition, the comparison of CPS and CPN
Fig. 13(c). laminates shows that the latter are more resistant to crack growth
16 S. Helmy, S.V. Hoa / Composites Science and Technology 102 (2014) 1019
Fig. 13. Delamination starting at tip of dropped plies and growing in to interfaces.
Initial crack at resin pocket (a) have the same orientation, 90. The interlaminar stresses are
higher in the former than in the latter.
T
3.2.4. Fatigue damage index
The fatigue damage index, D, is dened as: D = 1 (Er/Eo),
Crack growth where E is the elasiticity modulus of specimen, with the subscripts
(b) (0) and (r) referring to the undamaged state and residual value
after a certain fatigue life, respectively. D varies between 0 and 1.
A low D value means little modulus reduction due to fatigue. Thus,
T D is a macroscopic measure of fatigue damage since the structural
changes on the microscopic scale (due to matrix cracks, ber/
matrix interfacial failure, etc.) are characterized by a macroscopic
delamination along thick region reduction of the modulus [34,35]. Fig. 19 shows the damage index,
(c) D, plotted a function of fatigue cycles for QISF and QISU composites
at 0.8 and 0.5 stress levels.
It can be seen from Fig. 19(a) that in the early stage of fatigue
T (say, 0400 cycles), the lled laminates exhibit more damage than
the unlled ones. After the initial damage period, the lled speci-
mens sustain a relatively longer stable period with low damage
Fig. 14. Delamination evolution of tapered beam specimen.
indices for the rest of fatigue life. The nal failure takes place much
than the former. This may be explained by the interlaminar stress earlier in the unlled composite than in the lled ones. It is also
between adjacent dropped and belt plies. In CPS, the adjacent belt observed that at low stress level, the same behavior of lled and
and cut plies are 90 and 0 plies while in CPN the adjacent plies unlled composite, Fig. 19(b).
(a)
Delamination Length (mm)
QISU,0.8Sut
QISF,0.8Sut
Direction of
crack growth
N (Cycles)
QISU,0.5Sut (b)
Delamination Length (mm)
QISF,0.5Sut
N (Cycles)
Fig. 15. Crack growth lengths for QIS of lled and unlled laminates: (a) at 0.8Sult and (b) at 0.5Sult.
S. Helmy, S.V. Hoa / Composites Science and Technology 102 (2014) 1019 17
CPSU,0.8Sut
(a) QISU,0.8Sut (a)
CPSU,0.8Sut
CPSF,0.8Sut
CPNU,0.8Sut
N (Cycles)
N (Cycles)
QISU,0.5Sut
(b)
CPSF,0.5Sut CPNU,0.5Sut
N (Cycles)
Fig. 18. Comparison between the three congurations at different stress levels.
N (Cycles)
Fig. 16. Crack lengths for CPS of lled and unlled laminates: (a) at 0.8Sult and (b)at
0.5Sult. 0.6
0.4
CPNU,0.8Sut (a)
Delamination Length (mm)
CPNF,0.8Sut 0.3
0.2
0.1
0
0 500 1000 1500 2000 2500 3000
Fatigue Life (cycles)
N (Cycles) 0.8
QISF, 0.5 Sut (b)
0.7
QISU, 0.5 Sut
Damage Index, D
CPNF,0.5Sut
0.5
0.4
0.3
0.2
0.1
0
0 20000 40000 60000 80000 100000 120000
Fatigue Life (cycles)
N (Cycles)
Fig. 19. Fatigue damage variable for QIS laminates, D, plotted as a function of
Fig. 17. Crack lengths for CPN of lled and unlled laminates: (a) at 0.8Sult and (b) fatigue life: (a) at 0.8Sut, and (b) at 0.5Sut.
at 0.5Sult.
QISU
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