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Keywords: In this relatively unique study, the impact of adding nanoparticles (NPs) on the fatigue properties of antisym-
GFRP metric glass fiber reinforced polymer (GFRP) laminate has been investigated. Antisymmetric GFRP laminates
CNTs (+45/02/902/02/-45) were prepared and reinforced once with 0.1 wt% of single-walled carbon nanotubes
Graphene (SWCNTs) and then with 0.1 wt% of Graphene nanoplatelets (GNPs). The NPs reinforced GFRP laminates are
Antisymmetric laminate
termed here GFNRP nanocomposites. Ultrasonication method was used to disperse the NPs using carefully
Fatigue properties
chosen process parameters. Fatigue tests were analyzed based on S-N curves, stiffness degradation and hysteresis
loops. The results showed that the use of 0.1 wt% of SWCNTs led to an increase in the fatigue strength coefficient
(FSC) and the fatigue strength exponent (FSE) of GFNRP nanocomposite specimens by 51% and 24%, respec-
tively, while the use of similar wt.% of GNPs enhanced the FSC and FSE by 33% and 25%, respectively.
Consequently, fatigue life of GFNRP nanocomposites are surprisingly enhanced by about three and twelve times
when GNPs and SWCNTs are used, respectively. The findings would give designers much more confidence in
using antisymmetric composite laminates in specific elastic tailoring structures.
∗
Corresponding author.
E-mail address: mbourchak@kau.edu.sa (M. Bourchak).
https://doi.org/10.1016/j.compscitech.2018.07.047
Received 19 June 2018; Received in revised form 25 July 2018; Accepted 31 July 2018
Available online 01 August 2018
0266-3538/ © 2018 Elsevier Ltd. All rights reserved.
M. Bourchak et al. Composites Science and Technology 167 (2018) 164–173
can improve the fatigue life of carbon fiber reinforced polymer (CFRP) Table 2
composites. Product specifications of used GF fabrics.
Unfortunately, no specific case of using NPs to enhance fatigue Interglas style 92145
properties of antisymmetric composite laminates could be found in the Weave Pattern Plain, weave warp-reinforced (unidirectional)
literature. Consequently, in the current study, neat resin antisymmetric Yarn Description • Warp: EC-9-68 tex x 5 t0
GFRP composite laminates were reinforced with either 0.1 wt% of • Fill: EC 7-222 tex
Thread Count • Warp (per cm): 5.9
SWCNTs or with 0.1 wt% of GNPs. The 0.1 wt% ratio was chosen based
on what has been widely reported in the literature as being the most Weight
• Fill (per cm): 7.0
220 g/m2
efficient ratio [23]. The neat GFRP composite specimens were termed Mechanical data • Tensile strength: 630 MPa (warp)
here GFRP-N, while the specimens reinforced with SWCNTs were • Tensile modulus: 33 GPa (warp)
• Compressive strength: 510 MPa
termed GFNRP-S and the specimens reinforced with GNPs were termed
GFNRP-G. The laminate specimens were made of eight layers of UD • Flexural strength: 810 MPa
In the present study, fatigue tests were carried out at three different
The GFRP composites and GFNRP nanocomposites specimens were
stress (S) levels. The selected S values were 80%, 60% and 40% of UTS.
fabricated using a vacuum bag assisted wet layup technique. GFNRP
The number of cycles to failure (Nf) against the stress levels were re-
nanocomposites specimens made from three components: glass fiber,
corded. Then, the tests were stopped when the specimen completely
epoxy resin and randomly dispersed NPs. Both GFRP composites and
fractured or reached over a million cycles as applied in previous works
GFNRP nanocomposites specimens were fabricated with eight layers
[6]. Generally, six specimens were tested for each stress level to cal-
(+45/02/902/02/-45) and the average thickness was 2 mm. A sonica-
culate the average values of fatigue properties. The results obtained for
tion method was used to disperse either 0.1 wt% of SWCNTs to fabricate
the experiments were used to plot the stress-life (S-N) curves. Then, the
GFNRP-S nanocomposite specimens or 0.1 wt% of GNPs to fabricate
Basquin's formula shown below is used to model the fatigue behavior
GFNRP-G nanocomposite specimens.
[27].
2.3. Mechanical testing σa = σf (Nf )b (1)
Tensile properties of neat GFRP composite and GFNRP nano- where σa is the applied stress level, σf is fatigue strength coefficient
composite specimens were obtained as per ASTM standard D3039 [25] (FSC), Nf is the number of cycles at failure and b is the fatigue strength
at room temperature, using a MTS 809 axial/torsion system. The latter exponent (FSE). The S-N curves of GFRP-N composites, GFNRP-S na-
nocomposite and GFNRP-G nanocomposite specimens are shown in
Table 1 Fig. 3. There are two types of S-N curves known as “flat curve”, which
Typical mechanical data for a combination of resin L385 and hardener has a small slope, and “steep curve”, which has a larger slope, as re-
386. ported by Nijssen R.P.L [28]. Thus, as the flatness of the curve in-
Mechanical data of neat resin
creased, the specimen life and fatigue properties will increase.
After curve fitting the fatigue data, it can be seen from the con-
Density (g/cm3) 1.18–1.20 structed S-N curves that GFNRP-S nanocomposite specimens show
Modulus of elasticity (KN/mm2) [GPa] 3.3–3.6 better fatigue performance (longer lives at a given stress level) followed
Tensile strength (N/mm2) [MPa] 75–85
by GFNRP-G nanocomposite specimens and then GFRP-N composite
Compressive strength (N/mm2) [MPa] 120–140
Elongation of break (%) 6–8 specimens. In addition, the specimen life is closely related to the ap-
plied cyclic load. For instance, at higher applied load (80% of UTS) the
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M. Bourchak et al. Composites Science and Technology 167 (2018) 164–173
Fig. 1. Images of tested samples from left to right: GFRP-N, GFNRP-S and GFNRP-G.
Fig. 2. Tensile stress versus strain curves of GFRP-N and both GFNRP.
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M. Bourchak et al. Composites Science and Technology 167 (2018) 164–173
Fig. 4. Stiffness degradation curves of GFRP-N composites at various applied load levels.
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M. Bourchak et al. Composites Science and Technology 167 (2018) 164–173
Fig. 5. Stiffness degradation curves of GFNRP-S nanocomposites at various applied load levels.
degradation that occurs in the specimen leading to a shorter fatigue life. three phases could be clearly observed. Moreover, CDS of GFRP-N
In average, at N = 100 cycles the stiffness of the GFNRP-S nano- composite specimens occurred at about 12% of the total fatigue life.
composite specimens was degraded by 20% at the applied stress level of Figs. 8 and 9 show the normalized stiffness versus the normalized
80% of UTS and by 15% for applied stress level of 60% of UTS, while at number of cycles of GFNRP-S and GFNRP-G nanocomposite specimens
the applied stress level of 40% of UTS was 10%. Whereas the GFNRP-G at applied cyclic load of 60% of UTS. The three phases of the stiffness
nanocomposite specimens stiffness was degraded by 35%, 20% and degradation were also clearly observed. In addition, CDS point of both
15% at applied stress level of 80%, 60% and 40%, respectively. GFNRP-S and GFNRP-G nanocomposites occurred at about 24% and
Fig. 7 represents the normalized stiffness versus the normalized 20%, respectively, of the total fatigue life. Therefore, it can be stated
number of cycles of neat GFRP composite specimen at applied cyclic that the use of 0.1 wt% of SWCNTs and 0.1 wt% of GNPs help delay the
load of 60% of UTS. Generally, the stiffness degradation curve has three cracks saturated state which agreed with previous studies such as those
phases: (I) rapid degradation due to initiation and growth of matrix by Phong et al. [15] and Shen et al. [16] in which they reported that the
cracks in off-axis direction, (II) gradual or linear degradation due to use of NPs delayed the crack growth in FNRP nanocomposites.
almost stable transverse matrix cracks and interfiber fractures (marked
by dashed line in Figs. 7–9) and (III) rapid degradation or significant
3.4. Hysteresis loop
deterioration due to complete fiber fractures [16,28,31]. The transition
point between the first and second phases is called the characteristic
The hysteresis loop is used to evaluate the fatigue damage that oc-
damage state (CDS) [27]. At the CDS point, the number of the matrix
curred in the FRP composites [28–30]. It is plotted based on the peak
cracks in the off-axis direction of the FRP composites reach the satu-
and valley values of the displacement that occurs in the specimen due to
rated level, which has a great impact on the stiffness degradation of FRP
loading and unloading of the applied cyclic load [6]. In addition, the
composites [32]. Therefore, the majority of the stiffness degradation
energy dissipated due to fatigue loading could be calculated based on
can be attributed to matrix cracking. It is clear from Fig. 7 that all the
the area under the hysteresis loop curve as shown in Fig. 10 according
Fig. 6. Stiffness degradation curves of GFNRP-G nanocomposites at various applied load levels.
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to Equation (4), which is related to the crack growth in FRP composites S and GFNRP-G nanocomposite specimens, which led to shorter fatigue
specimen [29,30]: life of GFRP-N composite specimens under high stress fatigue loading.
Therefore, it can be deduced that there is a dependence relation be-
δmax
tween the dissipated energy due to fatigue and specimen fatigue life.
Ed = ∫ F . dδ
Fig. 12 shows the hysteresis loops of GFRP-N composite specimens
δmin (4)
at N = 2000 cycles for different applied loads. The hysteresis loops
were also shifted away from each other along the displacement axis for
where Ed is the dissipated energy, F is the applied fatigue load and
the purpose of better visualizing. The dissipated energy at an applied
(δmin ) and (δmax ) are the minimum and maximum displacements, re-
load of 80% of UTS was 0.54 kN mm, and then it was reduced by 50%
spectively.
and 87% when the applied load was reduced to 60% of UTS and 40% of
Fig. 11 shows the hysteresis loops of GFRP-N composite specimens,
UTS, respectively. Therefore, it is evident that the dissipated energy was
GFNRP-S and GFNRP-G nanocomposite specimens at N = 1000 cycles
decreased as the applied load decreased, or in other words, the higher
and applied load of 80% of UTS. The hysteresis loops were shifted away
the applied load, the higher the value of the dissipated energy. These
from each other along the displacement axis for clear representation. It
results could be observed clearly from the narrow elliptical topology of
can be seen that the hysteresis loops behavior has an ellipse shape. The
the hysteresis loops, which tend to become straight lines as the applied
dissipated energy (area of hysteresis loop) result of the GFRP-N com-
load decreases. In addition, it is worth noting that the dissipated energy
posite specimens was 2.26 kN mm, while the dissipated energy of the
results agreed with the results of stiffness degradation, because the high
GFNRP-S and GFNRP-G nanocomposite specimens results were reduced
applied load led to an increase in the number of matrix cracks, and
by 19% and 29% compared to GFRP-N composite specimens dissipated
therefore an increase in the damage occurring in the specimen as well
energy due to the use of 0.1 wt% of SWCNTs and 0.1 wt% of GNPs,
as the dissipated energy.
respectively. These results mean that high damage occurred in GFRP-N
Figs. 13 and 14 show the hysteresis loops of GFNRP-S and GFNRP-G
composite specimens compared to the damage that occurred in GFNRP-
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Fig. 11. Hysteresis loops comparison at N = 1000 cycles and applied load level of 80% of UTS.
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Fig. 12. Hysteresis loops of GFRP-N composites at N = 2000 cycles for various applied load levels.
rapid decrease at a specific cycle, and no significant changes were ob- due to a higher specific surface area and an additional failure mode of
served in the remaining cycles. This behavior could be observed in layer separation that enable more energy absorption than MWCNTs.
GFRP-N composite specimens and both GFNRP nanocomposite speci- However, in this work, instead of using MWCNTs, SWCNTs were used
mens, which agreed with what has been reported in the literature and compared to graphene nanoplatelets (GNPs) with the former per-
[29,30]. It is worth noting that the drop in dissipated energy that forming better than the latter. SWCNTs have been reported by Davis
happened between the initial cycles in GFRP-N composite specimens et al. [13] to create an “a-SWCNTs reinforced region” of strengthened
was higher than that which happened in GFNRP-S and GFNRP-G na- and stiffened matrix material in CFRP composites resulting in overall
nocomposite specimens. Also, GFNRP-S specimens experienced more improvements of fatigue life. It is therefore envisaged that a similar
dissipated energy than GFNRP-G specimens. Then, there was a satura- mechanism is happening in GFRP composites but with a difference due
tion in the dissipated energy in all composite and nanocomposite spe- to the mismatch between glass fibers and CNTs. Moreover, due to the
cimens with almost the same value. Therefore, it can be stated that the antisymmetry of laminates in this work, high strains are induced on the
use of 0.1 wt% of SWCNTs and 0.1 wt% of GNPs led to reduced fatigue matrix due to the extension-twisting coupling experienced by these
damage in the nanocomposite specimens, as shown in Fig. 15. laminates under fatigue loading. Therefore, any increase in ductility
(within a limited range) would allow the matrix to perform better
compared to the un-toughened matrix which can exhibit higher strains.
3.5. Influence of fiber/matrix interface on fatigue performance It is therefore concluded that the fatigue performance is subject to the
behavior of mainly fiber/matrix interface and specifically its toughness
Taking symmetric GFRP composites that were enhanced by nano- since the design load level is usually much lower than the fiber strength.
particles as examples, it is found that the effect of the latter on fatigue The existence of a unique fiber/matrix layer with specific properties
performance differ from NP type to another as widely reported by re- other than the fiber and matrix has been initially suggested by Chamis
searchers. Knoll et al. [22] hypothesized that few layered graphene [33] many decades ago. It was later theoretically studied by some
(FLG) performed better than MWCNTs when added to CFRP composites
Fig. 13. Hysteresis loops of GFNRP-S nanocomposites at N = 2000 cycles for various applied load levels.
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Fig. 14. Hysteresis loops of GFNRP-G nanocomposites at N = 2000 cycles for various applied load levels.
authors [34,35]. Evans [36] then proved by chemical analysis and fatigue test was conducted for both GFRP composites and GFNRP na-
photomicrographs that a layer of finite thickness exists between the nocomposites which were subjected to three levels of cyclic loads (80%
fiber and the matrix and that it is chemically different from both fiber of UTS, 60% of UTS and 40% of UTS). By comparing the fatigue life of
and matrix. Lhotellier et al. [37] concluded that this layer poses a dif- GFRP-N, GFNRP-S and GFNRP-G specimens at the same applied cyclic
ficult problem because its thickness is only on the order of a micron. As load (220 MPa ( ± 5%)), the obtained results of the S-N curves show
a result, the mechanical properties of this region cannot yet be mea- that the fatigue life of GFNRP-G and GFNRP-S nanocomposite specimen
sured experimentally. Therefore there needs to be significant research were enhanced by about three and twelve times, respectively.
in determining its properties parameters and its true influence on the Additionally, the use of 0.1 wt% of SWCNTs led to an increase in the
load transfer in FRP composites. FSC and the FSE of GFRP specimens by 51% and 24%, respectively,
while the use of similar wt.% of GNPs enhanced the FSC and FSE by
4. Conclusions 33% and 25%, respectively. The stiffness degradation behavior of GFRP
composite specimens and GFNRP nanocomposite specimens were clo-
A comprehensive experimental investigation has been conducted in sely related to the applied cyclic loads. Moreover, the use of SWCNTs or
order to characterize the level of improvement in fatigue properties of GNPs slows down the stiffness degradation rate of GFNRP nano-
antisymmetric GFNRP composites that are enhanced with either composites compared to the GFRP composite, which led to longer fa-
SWCNTs or GNPs. Specimens made from antisymmetric and balanced tigue life. Specifically, the characteristic damage state (CDS) or cracks
(+45/02/902/02/-45) GFNRP nanocomposites laminates consisting of saturated state, was delayed by the inclusion of either SWCNTs or
0.1 wt% of SWCNTs and 0.1 wt% of GNPs, respectively were tested and GNPs. The obtained hysteresis loops show that most of the damage
their results were compared to neat GFRP composite specimens. The occurred in the first few cycles followed by a rapid decrease towards the
Fig. 15. Comparison between dissipated energy of GFRP-N composites and both GFNRP nanocomposites at 60% of UTS.
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