Composites Part B 146 (2018) 145–154

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Composites Part B
journal homepage: www.elsevier.com/locate/compositesb

The effects of silane coupling agents on the mechanical properties of basalt T

fiber reinforced poly(butylene terephthalate) composites
Cagrialp Arslana,b, Mehmet Doganb,∗
a
Department of Textile Engineering, Bartin University, 38039, Bartin, Turkey
b
Department of Textile Engineering, Erciyes University, 38039, Kayseri, Turkey

A R T I C LE I N FO A B S T R A C T

Keywords: In the current study, the effects of three different silane coupling agents, namely (3-aminopropyl) triethoxysilane
Basalt fiber (AP), (3-Glycidyloxypropyl) trimethoxysilane (GP) and (3-trimethoxysilyl) propylmethacrylate (MA) are in-
Poly (butylene terefthalate) vestigated on the mechanical properties of the basalt fiber (BF) reinforced poly (butyleneterefthalate) (PBT)
Composite composites. The tensile, flexural, impact, thermomechanical and morphological properties of the composites are
Mechanical properties
investigated. According to the test results, the remarkable increase in tensile strenght and elastic modulus is
observed, whereas slight improvement in flexural strenght and no change in impact properties is observed.
According to flexural strength and elastic modulus values, the effectiveness of the silane coupling agents can be
ranked as follow: GP > AP > MA. It is clearly shown that the increase in mechanical properties arises from
improvement in interfacial adhesion between BF and PBT. It is concluded that the covalent bond formation
causes the highest improvement in mechanical properties including tensile and flexural strenght and elastic
modulus.

1. Introduction adhesion between polymer and the fiber [6,8,13,22–30,35,36]. In the

Poly (butyleneterephthalate) (PBT), a kind of polyester based
thermoplastic engineering polymer, has great importance owing to the
exclusive features including high thermal resistance, excellent electrical
insulation, easy processability and good surface apperance. These
properties provide wide applications in automative, electrical and
packing applications [1,2]. In the literature, PBT is reinforced with
various chopped fibers including carbon [3–5], glass [6–14] and natural
fibers [15] for improving its mechanical performance. As seen from the
literature, the glass fiber is the most widely used reinforcing material.
Basalt fiber (BF), known as non-pollution green material of 20th
century, is produced from volcanic basalt rocks [16]. It has superior
properties such as high tenacity, high fire performance, heat and sound
insulation, alkaline resistance and dimensional stability than E-glass
fiber [17–21]. These exclusive characteristics provide widely use in
such areas including aviation, civil application, defense industry and
agriculture. BF is seemed to be the best alternative of E-glass fiber in
terms of cost and mechanical properties. In the literature, BF in various
form is used as reinforcing material in various polymers [20–34].
Glass fiber and BF have hydroxyl groups on their surface.
Accordingly, the modification with silane coupling agents is the most
preferred method for improving the dispersion and the interfacial
literature, different silane coupling agents are used in glass fiber re-
inforced PBT composites [6,8,13,36]. Ishak et al. investigated the me-
chanical properties of (3-Aminopropyl) triethoxysilane (AP) modified
glass fiber reinforced PBT composites manufactured by injection
molding technique. It was concluded that the used silane coupling
agent improved the tensile properties of the composites significantly
[6]. Bergeret et al. examined the mechanical and the interphase prop-
erties of the AP modified glass fiber reinforced PBT composites. The use
of silane coupling agent improved the interfacial adhesion and in-
creased the impact strength of the composites [8]. Yang et al. synthe-
sized a novel phosphorus-containing coupling agent. They investigated
the effect of synthesized coupling agent on the mechanical and flame
retardant properties of the glass fiber reinforced PBT composites. It was
found that the use of synthesized silane coupling agent significantly
enhanced the fire retardant properties and improved the tensile prop-
erties [13]. Zhou et al. studied the mechanical properties of the (3-
Glycidyloxypropyl) trimethoxysilane (GP) modified long glass fiber
reinforced PBT composites. The use of the silane coupling agent im-
proved the tensile, flexural and impact properties of the composites
[36].
In the literature, only two studies that investigated the mechanical
performance of the BF reinforced PBT composites were found. Baets

∗
Corresponding author.
E-mail address: mehmetd@erciyes.edu.tr (M. Dogan).

https://doi.org/10.1016/j.compositesb.2018.04.023
Received 2 January 2018; Received in revised form 6 April 2018; Accepted 9 April 2018
Available online 10 April 2018
1359-8368/ © 2018 Elsevier Ltd. All rights reserved.
C. Arslan, M. Dogan Composites Part B 146 (2018) 145–154

et al. investigated the effect of the non-isothermal process conditions on

the crystallization characteristics and the mechanical properties of ba-
salt roving and woven basalt fabric reinforced PBT composites [37].
Hao et al. examined the effects of the various process temperatures on
the mechanical properties of the woven basalt fabric reinforced PBT
composites [38]. In these studies, BF is either roving or woven fabric
form and there is no compatibilizer or coupling agent is used. To our
best knowledge, this is the first study that investigates the mechanical
performances of the chopped BF reinforced PBT composites. In the
current study, the effects of three different silane coupling agents on the
mechanical and thermo-mechanical properties of the chopped BF re-
inforced PBT composites. The properties of the composites are char-
acterized by tensile, flexural, impact tests and dynamic mechanical
analysis (DMA). The tensile and impact fractured surfaces of the com-
posites are also inspected by scanning electron microscopy (SEM)
analysis.

2. Experimental

2.1. Materials
Fig. 1. Chemical structures of the silane coupling agents.
PBT under the trade name of Tecodur® PB70 NL 1.31 g/cm3, was
purchased from Interplast. Chopped BF with length and diameter of
6 mm and 13–20 μm was supplied from Tila Kompozit. The specifica-
tions of the raw materials given by the suppliers are given in Table 1.
Three kinds of silane coupling agents, (3-Aminopropyl) triethoxysilane
(AP) (0.946 g/cm3 and 221.37 g/mol), (3-Glycidyloxypropyl) tri-
methoxysilane (GP) (1.07 g/cm3and236.34 g/mol) and 3-(Trimethox-
ysilyl) propylmethacrylate (MA) (1.045 g/cm3and 248.35 g/mol) were
purchased from Sigma Aldrich. The chemical structures of the silane
coupling agents are given in Fig. 1.

2.2. Silane treatment of basalt fiber

In order to remove the coated sizing on the fiber surface applied by

the producer, BF was heated in a furnace at 500 °C for an hour prior to
the silane treatment process. The silane treatment of the BF (100 g) was
made with 5 wt% three different silanes in ethanol/water (1:1 by
weight) mixture at 85 °C for 5 h. After the silane treatment, BF was
washed with ethanol several times in order to remove unreacted silane
coupling agent. The characterization of the fiber samples were made
with attenuated total reflectance – Fourier transform infrared spectro-
Fig. 2. FTIR spectrum of neat and modified BFs.
scopy (ATR-FTIR) analysis. The modified BF samples are coded as AP-
BF, GP-BF and MA-BF for (3-Aminopropyl) triethoxysilane, (3-
Glycidyloxypropyl) trimethoxysilane and 3-(Trimethoxysilyl) pro- injection-molding machine (DSM Xplore 12 ml Micro-injection Molder,
pylmethacrylate modified BF, respectively. Netherlands) at a barrel temperature of 240 °C and the mold tempera-
ture of 28 °C.
2.3. Production of the composites
2.4. Characterization methods
PBT and BF and were dried at 85 °C for 8 h prior to the com-
pounding process. The constant amount of neat and modified BF (20 wt ATR-FTIR was used to characterize the silane modified BF at an
%) containing composites were prepared via laboratory type co-ro- optical resolution of 4 cm−1 with 32 scans. Tensile and flexural tests
tating twin screw extruder (L/D:40; Φ:16 mm), (GULNAR MAKINA, were carried out on Shimadzu AG-X universal testing machine equipped
Istanbul, Turkey) with a temperature profile of 50-210-215-220-215- with 50 kN load cell, according to ASTM D 638 and ASTM D-790
210 °C at 150 rpm. The extrudate was chopped into small pellets and standards at room temperature. Tensile tests were conducted on the
stored in sealed plastic bag until the injection molding process. The dog-bone shaped samples (7.4 × 2.1 × 80 mm3) at a crosshead speed of
specimens for mechanical tests were molded by a laboratory scale 5 mm/min. Tensile strength and percentage elongation at break values
were recorded. The flexural tests were performed on the specimens with
Table 1 the nominal dimensions of 13 × 125 × 3.2 mm3, setting the span
Mechanical properties of raw materials.
length of 55 mm and a cross-head speed of 1 mm/min. Charpy Impact
Material Tensile Strength Percentage Strain Tensile Density (g/ tests were performed on unnotched samples with the dimensions of
(MPa) (%) Modulus (GPa) cm3) 3.2 × 6.5 × 130 mm3 using Coesfeld-Material impact tester at room
temperature according to ASTM D256. All mechanical test results re-
PBT 45–55 ≤70 2.5 1.31
BF 2825 3.15 89 2.8 presented an average value of five samples with standard deviations.
DMA experiments were carried out using Perkin Elmer DMA 8000 in

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C. Arslan, M. Dogan
Fig. 3. Tensile fracture surfaces of the composites with a magnification of ×45.
dual cantilever bending mode at a frequency of 1 Hz, in the temperature
sweep mode from −50 to 140 °C at a heating rate of 10 °C/min. The
tensile and impact fracture surfaces of the composites after sputtering
with Au/Pd alloy were examined in SEM (LEO 440 computer controlled
digital, accelerating voltage of 20 kV).
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Composites Part B 146 (2018) 145–154
3. Results and discussions
3.1. FT-IR analysis
The FTIR analyses are performed for proving the presence of the
silane coupling agents on the BF surface. The FTIR spectrum of neat and
modified BFs are shown in Fig. 2. As seen from Fig. 2, BF shows
C. Arslan, M. Dogan Composites Part B 146 (2018) 145–154

Fig. 4. SEM images of the tensile fractured surfaces at magnifications of ×250 (left side) and ×1000 (right side).

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C. Arslan, M. Dogan Composites Part B 146 (2018) 145–154

characteristics peaks seen at 880, 1650 and 3320 cm−1, which corre-
spond to Si – OH and OH vibrations on the surface of the BF [2,13,39].
With the silane treatment, the additional peaks are seen at 2970, 2880,
1380, 1085 and 1040 cm−1. The peaks seen at around 2880 and
2970 cm−1 are attributed to the symmetrical and asymmetrical C-H
stretching vibrations in CH2, respectively [40,41]. The characteristics
Si-CH2 bending mode vibrations are seen at 1380 cm−1 [42,43]. The
peaks seen at 1085 and 1040 cm−1 are attributed to Si–O–C and Si–O
stretching vibrations, respectively [13,44]. The peaks related with the
chracteristics functional groups of silane coupling agents (amine for AP,
ether and epoxy for GP, double bond for MA) are overlapped with the
other peaks. Amine group shows two characteristic peaks at about 1615
and 3400 cm−1 due to the N–H stretching vibration and the bending
mode of free NH2 [13,45]. Ether group have characteristic peaks seen at
1150 and 1050 cm−1due to the antisymmetric streching of C-O-C
bridge and the skeletal vibrations of C-O streching [46]. The epoxy
group has characteristic peaks seen at 910 and 3050 cm−1 owing to the
asymmetrical ring stretch and C-H stretching, respectively [44,47]. The
double bond has characteristic peaks seen at 1640 cm−1 [48,49]. These
findings clearly show that the silane treatment on BF is made success-
fully.

3.2. Morphological analysis

SEM analyses are performed on the tensile and impact fracture

surfaces of the composites for providing precious information related
with the dispersion of the BF, the interface properties and the fracture
mechanism. Fig. 3 shows the tensile fracture surfaces of the composites
with a magnificationof 45×. As seen in Fig. 3, the matrix material
except for the PBT/MA-BF undergoes brittle failure with a character-
istic patchwork pattern on the whole fracture surface. In the SEM
photograph of PBT/MA-BF, the ductile failure mode of matrix material,
which is shown in white circle, is observed in a localized region. The
plastic deformation of the matrix material is related with the micro-
failure behavior of the short fiber reinforced composites [50,51]. The
SEM images of the tensile fractured surfaces at magnifications of × 250
(left side) and × 1000 (right side) are shown in Fig. 4. The arrows in
white, red and yellow color are used for long fibres, pull out fibres and
fibres embedded into matrix, respectively. Both pristine and modified
BFs are homogeneously dispersed in PBT matrix. The fiber pull out is
observed in all composites either as standing fibers or as black holes.
The observed difference between the use of pristine and modified BFs is
the number and length of the pull out fibers. With the use of silane
coupling agents, the less pull out BFs with shorter lengths is observed.
Most of the pull out fibers has clean surface owing to the poor fiber/
matrix adhesion without using any silane coupling agent. The matrix
material adheres on the BF surface after tensile test with the use of
silane coupling agents. These observations show that the use of silane
coupling agents regardless of their type improves the interfacial adhe-
sion between BF and PBT. However, no meaningful difference is ob-
verved between the modified BF containing composites. These findings
are also supported by the mechanical test results.
The impact fracture surfaces of the composites at a magnification
of × 250 are shown in Fig. 5. The matrix material is fractured in brittle
manner in all composites. Fiber pull-out, debonding and fiber break-
down are observed in all composites. With the use of silane coupling
agents, less fiber debonding and pull-out are observed. These results
also show that the use of silane coupling agents improves the interfacial
adhesion between BF and PBT.

3.3. Tensile test

The stress–strain curves of the composites are shown in Fig. 6 and

Fig. 5. Impact fracture surfaces of the composites at a magnification of ×250.
the relevant tensile test data are listed in Table 2. The pristine PBT
ruptures in ductile manner. With the addition of the pristine and
modified BFs, the composites fail in brittle manner due to the

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strength increase. The possible interactions of silane coupling agents

with PBT matrix are shown in Fig. 7. It is well known fact that the
covalent bond formation causes the highest interfacial adhesion among
the possible adhesion mechanisms of the silane coupling agents [56].
Although AP and GP modified BF has covalent bond formation with
PBT matrix, no considerable difference is observed among the modified
BF containing composites when the stardart deviations are considered.
In the literature, such increase in tensile strength with the use of AP, GP
and MA is observed in different fiber/thermoplastic polyester based
matrix systems [6,8,36,58–60].

3.4. Flexural properties

The load-deflection curves of the neat PBT and the composites are
shown in Fig. 8. Flexural test data of the samples are given in Table 2.
The shape of the load deflection curve gives precious information re-
lated with the failure mode of the material. As seen in Fig. 8, PBT shows
Fig. 6. Stress–strain curves of the composites. almost linear deformation up to reach its ultimate load bearing capa-
city. Then the gradual decrease of the flexural strength, which is the
indication of the shear failure mode, is observed. All BF containing
catastrophic crack propagation. The Youngs' modulus of the PBT in-
composites fail mainly in flexural mode, which is observed as in-
creases with the addition of the BF regardless of the modification type.
stantaneous flexural strenght drop, due to catastrophic crack propaga-
It is concluded that PBT becomes stiffer with the addition of the BF.
tion [61,62].
However no significant effect of silane modifications is observed on
The flexural modulus of the PBT increases with the addition of the
Youngs' modulus value since it is measured at low deformations. Thus,
BF, whereas no significant effect of the silane modifications is observed
the interfacial adhesion does not remarkably affect the modulus value
on it when the standart deviations are considered. On contrary to the
[52]. The tensile strength of the PBT remains almost same with the
tensile test results, the addition of the pristine BF significantly increases
addition of 20 wt% pristine BF, whereas the strain at break value re-
the flexural strength of the PBT at about 25%. During the tensile test,
duces drastically. BF, which has hydroxyl groups on its surface, is more
the composite is subjected to tensile forces to whole cross section and
hydrophilic than the matrix. Accordingly, the adhesion between pris-
the load bearing capacity of the composites predominantly determined
tine BF and PBT is poor owing to the polarity difference. Without the
by the interface properties. With the poor adhesion between BF and
strong interfacial adhesion between BF and PBT, the load transfer from
PBT, the matrix can not perfectly transfer load to BF. The composite is
matrix to fiber is low. Thus, the tensile strength is not change. The
forced to bend during the flexural test. It is subjected to compression
pristine BF containing composite fails at lower elongation value than
(upper surface) and tension (lower surface) in the direction of the load
those of modified BF containing ones due to the poor adhesion which
applied and shear forces in the asymmetric direction [50,54]. Fibers are
favors further the catastrophic crack propagation [53–55]. The tensile
forced to buckling in the compression side of a flexural specimen re-
strength of the modified BF containing composites increases at about
gardless of the fiber-matrix quality [63,64]. Thus, the flexural strength
30% with respect to pristine BF containing one. The silane modification
of composite is higher than tensile strength with the use of pristine BF.
has positive effect on the tensile strength regardless of their type due to
Similar results are observed with different fiber/matrix systems in the
the improvement in the interfacial strength between BF and PBT. The
literature [65–67]. The silane modifications of AP, GP and MA further
increase in interfacial strength stems from different mechanisms in-
improves the flexural strenght of the composites at about 5, 12 and 3%,
cluding the increase in hydrophobocity, covalent bonding, inter-
respectively. The increase in flexural strength arises from the im-
molecular entanglement and secondary bond interactions depending on
provement in interfacial adhesion between PBT and BF, as stated before
the silane coupling agent type [56]. In the studied matrix fiber system,
in the tensile test section in details. The highest improvement in flexural
the increase in hydrophobocity is the reason for the increase in inter-
strength is achieved with the use of GP which has ability to make
facial strength for all silane coupling agents. For AP, hydrogen bonding
covalent bond with hydroxyl and carboxyl end groups of the PBT. It is
and covalent bond formation increase the interfacial strength, as well.
worthy of note that the increase in flexural strength with silane mod-
The AP has primary amine structure which makes especially hydrogen
ificition is lower than that in tensile strenght. It thought that the ob-
bonding with hydroxyl and carboxyl end groups and reacts with the
served trend arises from the load bearing capacity of pristine BF during
carboxyl end groups of the PBT. For GP, covalent bond formation also
the flexural test. Thus, the effect of the interfacial adhesion improve-
increases the interfacial strength. GP has epoxy group which can reacts
ment on flexural strength remains low.
with carboxyl and hydroxyl end groups of the PBT via nucleophilic
substitution reaction [57]. For MA, the increase in hydrophobocity and
intermolecular entanglement are the possible causes of the interfacial

Table 2
Mechanical properties of the composites.
Sample Code Tensile Properties Flexural Properties Impact Properties

Tensile Strength (MPa) Percentage Strain (%) Youngs' Modulus (GPa) Flexural Strength (MPa) Flexural Modulus (GPa) Impact Strength (kJ/m2)

PBT 48.9 ± 0.54 22.2 ± 0.53 1.9 ± 0.2 76.5 ± 0.96 2.4 ± 0.05 29.9 ± 1.40
PBT/BF 47.6 ± 0.89 3.1 ± 0.23 3.6 ± 0.1 95.3 ± 1.29 4.4 ± 0.02 20.0 ± 0.31
PBT/AP-BF 63.4 ± 1.75 6.2 ± 0.22 3.7 ± 0.2 99.8 ± 0.59 4.2 ± 0.07 24.0 ± 1.95
PBT/GP-BF 62.0 ± 0.92 4.3 ± 0.40 3.6 ± 0.2 106.4 ± 2.30 4.5 ± 0.21 20.5 ± 0.31
PBT/MA-BF 61.9 ± 1.07 5.3 ± 0.05 3.6 ± 0.2 97.8 ± 0.81 4.2 ± 0.22 21.7 ± 0.94

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Fig. 7. Possible interactions of silane coupling agents with PBT matrix.

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Fig. 8. Load-deflection curves of the neat PBT and the composites.

3.5. Impact test

Impact test is performed on unnotched samples using the pendulum

hammer of 1 J. Table 2 shows the related impact test results. The neat
PBT has the highest impact strength. The addition of the pristine and
modified BFs causes sharp reduction in impact strength owing to the
easier initiation of the crack arising from the stress concentration cen-
ters at fiber ends. The impact resistance of the fiber reinforced polymer
composites depends mainly on the inherent characteristics of the matrix
and fiber material, their amounts, and the interface properties
[58,67,68]. The compositions of the studied composites are the same
and the difference among the composites stems from their interfacial
properties. The main energy dissipation mechanisms seen in fiber re-
inforced polymer composites are the matrix fracture and deformation,
fiber fracture, pull out and debonding [58,67,68]. The fracture me-
chanisms of matrix and fiber fracture, fiber pull out are observed in all
SEM photographs (Fig. 5). With the use of modified BFs, less fiber pull
out and more fiber breakage is observed due to the improvement in
interfacial strength. Although the fracture mechanism changes from
fiber pull out to fiber breakge with the use of modified BFs, neglible
change in the impact strenght of the composites is observed when the
standart deviations are considered. It is concluded that the improve-
ment in interfacial adhesion has no remarkable effect on impact
strenght of the composites. It is thought that crack growth is dominated
by matrix and fiber breakage. Accordingly, the effect of interfacial
adhesion on impact strenght stays negligible.

3.6. Dynamic mechanical analysis

DMA analyses are performed on the neat PBT and BF containing

composites. Elastic modulus, loss modulus and tan δ versus temperature
graphs are shown in Fig. 9. Elastic modulus of the all samples show
declining trend, which is attributed to the thermal transitions occurred
in PBT, as the temperature increases. The prominent decrease in elastic
modulus is observed at about 60 °C which corresponds to α relaxation
related to glass transition temperature [69,70]. The addition of the
pristine and modified BFs, which has higher stiffness than the PBT,
improves the elastic modulus. The use modified BFs further improves
the elastic modulus to whole temperature range owing to the enhanced
adhesion between BF and PBT. The increase in elastic modulus is more
prominent below the glass transition temperature. Above 100 °C, no Fig. 9. Elastic modulus, loss modulus and tan δ versus temperature graphs.
considerable difference in elastic modulus is observed between pristine
and modified BF containing composites. The highest improvement in several monomer units of PBT chain [8]. The glass transition tem-
elastic modulus is achieved with the use of GP-BF which makes covalent perature increases at about 4 °C with the addition of BF regarless of the
bonding with the PBT. modification type owing to the constraints exerted by BF on the seg-
As seen from loss modulus versus temperature graph, the PBT shows mental mobility of the PBT [66]. All BF containing composites show
a relaxation peak at 56 °C which is related to cooperative motions of

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higher loss modulus value than neat PBT at glass transition tempera-
ture. The loss modulus further increases with the use of modified BFs
and the highest value is observed with use of GP-BF.
The tan δ, which is also known as the damping factor, gives precious
information related with the interfacial adhesion between filler and
matrix material. It is well known fact that the height of tan δ is reduced
with the better interfacial adhesion between filler and matrix. The
lower tan delta indicates that material behaves more elastic [24,71].
The neat PBT shows the highest peak among the samples. The stiff filler
carries a greater extent of stress and allow only small part of it to strain
at the interface. Accordingly, the addition of BF reduces the height of
the tan δ peak. With the use of AP and MA, no meaningful change is
observed in the height of the tan δ. The tan δ is further reduced with the
use of GP-BF. As stated in the previous sections, the most improvement
in interfacial strength is observed with the use GP.
4. Conclusion
In this study, we evaluated the effect of three diffent silane coupling
agents on the mechanical and the morphological properties of the BF
reinforced PBT composites. The composites were characterized by
tensile, flexural, impact, DMA and SEM analyses. It followed from the
test results that the use of silane coupling agents improved the inter-
facial adhesion between BF and PBT with different mechanisms. The
improvement in interfacial adhesion increased the ultimate strength of
the resulting composites both in tensile and in flexural configuration,
whereas tensile, flexural stiffness and impact strength are not notice-
able influenced. According to the flexural strength and elastic modulus
values, the effectiveness of the silane coupling agents were in the order
of GP > AP > MA.
Acknowledgement
This work is supported by Erciyes University Scientific Research
Unit under grant no BAP- FDK – 2017-7749.
Appendix A. Supplementary data
Supplementary data related to this article can be found at http://dx.
doi.org/10.1016/j.compositesb.2018.04.023.
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