Theoretical and Applied Fracture Mechanics 95 (2018) 242–247

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Theoretical and Applied Fracture Mechanics

journal homepage: www.elsevier.com/locate/tafmec

Interfacial toughening of carbon/epoxy composite by incorporating styrene T

acrylonitrile nanofibers
⁎
Rasoul Esmaeely Neisianya,b, , Saied Nouri Khorasania, Jeremy Kong Yoong Leeb,c,
Mohammadreza Naeimiradd, Seeram Ramakrishnab
a
Department of Chemical Engineering, Isfahan University of Technology, Isfahan 84156-83111, Iran
b
Centre for Nanofibers and Nanotechnology, Department of Mechanical Engineering, National University of Singapore, Singapore 117575, Singapore
c
Lloyd’s Register Global Technology Centre, 1 Fusionopolis Place, #09-11, Galaxis, Singapore 138522, Singapore
d
Department of Materials and Textile Engineering, Faculty of Engineering, Razi University, Kermanshah, Iran

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

Keywords: In this research, Styrene Acrylonitrile (SAN) nanofibers, produced by the electrospinning method, were used in
Carbon/epoxy composites order to improve out-of-plane and impact properties of a conventional carbon fiber/epoxy composite. The
Interfacial toughening prepared SAN nanofibers were directly deposited on the surfaces of conventional carbon fiber fabrics. Vacuum
Mechanical properties assist resin transfer molding (VARTM) was employed for fabricating carbon/epoxy composite. The morpholo-
Electrospinning
gical study of the electrospun SAN nanofibers indicated the prepared SAN nanofibers were smooth, continuous,
Nanofibers
and without any formation of beads, with average diameters assessed to be 480 ± 102 nm. Mechanical prop-
erties studies of the composites indicated that embedding SAN nanofibers in the hybrid composite (carbon/
epoxy composite containing SAN nanofibers) led to 26%, 37%, 27%, and 8% of flexural strength, flexural work
to fracture, interlaminar shear strength, and impact absorption energy, respectively compared to acquired results
from control composite (without nanofibers). Statistical analysis was furthermore carried out to prove the sig-
nificant differences of the obtained results. Finally, fractographical analysis by field emission scanning electron
microscope (FE-SEM) confirmed that embedding nanofibers in the hybrid composite caused tougher fracture
during composite breakage.

1. Introduction weaker than mechanical properties of reinforcement phase leads to

Carbon/epoxy composites have been widely used in plenty of ap-
plications due to their excellent specific mechanical properties and
manufacturability as well as superior corrosion resistance compared to
metals which make them suitable for substituting metals in many ap-
plications including aerospace, ground vehicles, and wind turbines
[1–4]. The mechanical properties of polymer matrix composites are
predominantly determined by the mechanical properties of the com-
ponents (matrix and reinforcement phase), the volume fraction of each
phase, fiber-matrix interfacial interactions between matrix and re-
inforcement phase, fiber alignments, etc. [5]. In particular, the lami-
nated structure causes anisotropicity in materials with the in-plane
mechanical properties dominated by properties of reinforcement phase
(fibers). Therefore, the in-plane properties of laminated structures are
strong enough for a lot of applications., while properties of the matrix
dictate the out-of-plane mechanical properties of the laminated com-
posite [6]. The mechanical properties of the matrix are significantly
weak out-of-plane properties of laminated polymer matrix composites.
In addition, the ply-by-ply nature of the laminated polymer matrix
composites can be vulnerable to delamination because of the micro-
cracks creation and propagation in the frail resin-rich layer. This serious
problem prevents employing these type of materials in the critical ap-
plications [5]. Therefore, numerous researches have been conducted in
order to boost the mechanical properties of the matrix such as using
carbon nanotubes [7–11], inorganic and rubbery micro/nanoparticles
[12–15], using metallic micro/macro-fibers [16–20], curing process
modification [21,22], blending [23–26], and even combination of these
techniques [27]. Despite the aforementioned methods have led to me-
chanical properties improvement of the matrix, but causes in con-
siderable limitations that restrict their usefulness in composite mate-
rials including troubles in the nanofillers distribution and dispersion,
and increase in the viscosity of resins [28] which adversely influence
the manufacturing process and consequently mechanical properties of
fabricated parts. In addition, the researches confirm that modifications

⁎
Corresponding author: Department of Chemical Engineering, Isfahan University of Technology, Isfahan 84156-83111, Iran.
E-mail address: r.esmaeely@ce.iut.ac.ir (R.E. Neisiany).

https://doi.org/10.1016/j.tafmec.2018.03.006
Received 16 February 2018; Received in revised form 12 March 2018; Accepted 12 March 2018
Available online 13 March 2018
0167-8442/ © 2018 Elsevier Ltd. All rights reserved.
R.E. Neisiany et al.
Fig. 1. Schematic cross sections of the hybrid composite and control composite.
Fig. 2. (a) FE-SEM images of the electrospun SAN nanofibers (b) the diameter distribution.
in curing process cannot impressively improve the mechanical proper-
ties of the resins [29].
Dzenis and Reneker firstly proposed a developing composite
strengthening method, with use of nanotechnology, which has since
gathered much research interest. The technique involved embedding
un-oriented electrospun nanofiber mats between layers of the re-
inforcement phase in order to improve the mechanical properties of the
weak resin-rich area [29]. Using electrospinning technique for fabri-
cating nanofibers with surface area-to-volume ratios greatly higher than
their conventional micro fiber counterparts offers the facile and eco-
nomical method for improving mechanical properties of the resin-rich
area with minimal effects on the manufacturing process [5]. The use of
electrospun nanofibers in boosting the mechanical properties of resin-
rich layers of laminated composites has therefore been keenly in-
vestigated during recent years [30,31] as well as enhancing fracture
toughness of epoxy adhesives [32] and neat resins [33,34]. Previous
researches showed the nanofibers diameter, the nanofiber mat thick-
ness, the nanofiber type, and the interaction between nanofibers and
matrix strongly influence mechanical properties of the laminated
polymer matrix composites [35]. Chen et al. showed that surface-
functionalization of electrospun carbon nanofibers is highly effective in
improving impact energy absorption, interlaminar shear strength, and
flexural properties for both nano-epoxy resins and hybrid multi-scale
conventional carbon/epoxy composites [36].
The present research aims to study the influence of incorporating
SAN nanofibers on interfacial toughening of a conventional carbon/
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Theoretical and Applied Fracture Mechanics 95 (2018) 242–247
epoxy composite. Therefore, the SAN nanofibers were directly de-
posited on the surfaces of carbon fabrics and subsequently, subjected to
a wet-layup process (followed by VARTM) in order to fabricate hybrid
carbon/epoxy composite which the resin-rich area enriched with the
SAN nanofibers. The hybrid composite panel was then evaluated by
three-point bending, interlaminar shear strength, and impact tests to
determine the effect of SAN nanofibers incorporation on the interfacial
toughening of the prepared hybrid composite.
2. Experimental
2.1. Materials
SAN powder (Mw = 185 g/gmol, acrylonitrile 30 wt%) was pro-
vided by Sigma-Aldrich. N, N-dimethylformamide (DMF, 99.8%) were
also purchased from Sigma-Aldrich and used as the solvent of SAN
powder for electrospinning process. Same as our previous works
[37,38], the unidirectional carbon fiber fabric was supplied by
Shanghai Horse Construction. Moreover, the epoxy resin (EPON™ Resin
828), and its curing agent (EPIKURE™ Curing Agent F205) were pur-
chased from Hexion Inc and used as epoxy matrix.
2.2. Electrospinning
Based on the obtained results in our previous work [39] the 25 wt%
of SAN powder was dissolved in DMF using a magnetic stirrer for 24 h
R.E. Neisiany et al. Theoretical and Applied Fracture Mechanics 95 (2018) 242–247

Fig. 3. FE-SEM micrographs of (a) conventional unidirectional carbon fiber fabric, (b) the electrospun SAN nanofiber layer on the surfaces of unidirectional carbon fiber after 0.05 g m−2
deposition, (c) the SAN nanofiber layer on the surfaces of unidirectional carbon fiber after 1 g m−2 deposition.

Table 1
Mechanical properties of reinforced composite by incorporation of the electrospun SAN nanofibers and control composite.

Three-point test Short beam strength (MPa) Impact absorption energy (J/m)

Flexural strength (MPa) Work to fracture (kJ/m2)

Control composite [37] 472.07 ± 44.05 28.80 ± 1.60 28.32 ± 2.67 2017.94 ± 210.95
Hybrid composite 595.32 ± 25.10 39.44 ± 1.05 36.00 ± 1.65 2172.90 ± 165.35
Enhancements in comparison with control composite (%) 26 37 27 8
|tstat | 5.44 12.70 5.54 1.30
tCritical 2.45 2.36 2.36 2.31

at room temperature in order to obtain a homogeneous solution. The manufacturer’s specification.

obtained solution was filled in a 10 mL syringe with a blunted needle
gauge 23. The conventional unidirectional carbon fiber fabrics were
wrapped around a 20 cm diameter grounded drum. The electrospun
nanofibers were directly deposited on the surfaces of the unidirectional
carbon fiber fabric. The electrospinning process parameters were ad-
justed as follow: SAN solution feed rate of 0.3 mL h−1, a 15 cm an air
gap between the needle tip and collector, and a 19 kV DC voltage in
order to provide a stable electrospinning process for fabrication of the
uniform nanofibers without any signs of beads. Electrospinning was
held until one gram of the SAN nanofibers was deposited on one square
meter (1 g m−2) of the unidirectional carbon fabrics.
The hybrid composite panel was prepared to contain the epoxy
matrix reinforced by 6 layers of unidirectional carbon fabric (parallel
aligned) compromised 5 layers of the SAN nanofibers (in the resin-rich
area). A 27 mmHg vacuum pressure was applied during the first curing
step for 6 h and held for a further 12 h in order to completely cure at
room temperature. The hybrid composite panel was then post-cured in
an oven at 60 °C for 30 min. Furthermore, as described in our previous
work [37], the control composite was fabricated from six layers of
carbon fabric via hand lay-up method followed by VARTM without
nanofiber deposition between the carbon fiber layers. Fig. 1 schemati-
cally illustrates the cross-section of control and hybrid composite.

2.3. Composite preparation 2.4. Characterizations

As mentioned before, the carbon/epoxy composite panel was pre-
pared via hand layup technique followed by the VARTM method in
order to provide the highest wetting of the nanofibers and carbon fiber
fabrics by the mixture of resin and its curing agent. The epoxy resin and
its curing agent were mixed in the mass ratio 100:58 according to
2.4.1. Morphological investigations
The morphology of the electrospun SAN nanofibers and the mor-
phology of the SAN nanofibers on the surfaces of the carbon fabric, the
thickness of the nanofiber layers, and the surfaces of the fractured
composites were studied by using of a Hitachi S-4300 field emission

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R.E. Neisiany et al. Theoretical and Applied Fracture Mechanics 95 (2018) 242–247

uniaxial machine. Short beam shear strength test was conducted by a

1 kN load cell Instron 5500 machine. The cross-head speed (of short
beam shear strength test) was set at 1 mm min−1. Meanwhile the span-
to-thickness ratio was adjusted at 4. The Izod impact test was conducted
by employing a CEAST® Resil impactor machine. All the tests were
performed at room temperature (25 ± 2 °C). The obtained results were
compared with a control composite (without nanofibers). It should be
noted that statistical analyses were conducted to prove the significant
difference in the mechanical properties of control and hybrid composite
due to the incorporation of SAN nanofibers.

3. Results and discussion

3.1. Morphological studies

Fig. 2a and b show the FE-SEM micrograph of the electrospun SAN

nanofibers and nanofibers diameter distribution, respectively. From
Fig. 2a, it can be discerned that the electrospun nanofibers were pre-
pared without any signs of bead formation. To assess the average value
of the nanofiber diameter and distribution over 50 measurements of
nanofiber diameter were carried out by analyzing the FE-SEM micro-
graph using Image J software. The average nanofiber diameter was
determined to be 480 nm. The standard deviation of nanofiber dia-
meters was further determined to be 102 nm.
In order to assess the morphology of the deposited SAN nanofibers
on the surfaces of conventional unidirectional carbon fiber fabrics, FE-
SEM was again employed. Fig. 3a shows FE-SEM micrograph of carbon
fiber fabric, meanwhile, Fig. 3b indicates the electrospun SAN nanofi-
bers on the surfaces of unidirectional carbon fiber fabrics after
0.05 g m−2 deposition of the nanofibers on the fabric. It can be ob-
served that the SAN nanofibers randomly deposited on the surface of
carbon fiber fabrics and rotation of collector and transverse movement
of the needle did not have any effects on nanofiber orientation. Fur-
thermore, FE-SEM was used to assess the thickness of nanofiber layer
Fig. 4. FE-SEM micrographs of the fracture surfaces of (a) control composite (b) hybrid after complete deposition of the nanofibers (1 g m−2 deposition of
composite containing SAN nanofibers. nanofibers on the surfaces of carbon fabric) before composite pre-
paration. Fig. 3c shows the SAN nanofiber layers on the surfaces of the
Table 2
unidirectional carbon fibers. From this FE-SEM micrograph, the thick-
T-test results of flexural strength of the control and hybrid composites. ness of the nanofiber layers was determined to be 22 nm before com-
posite preparation. Chen et al. reported that the optimum thickness of
Flexural strength of the composites Control composite Hybrid composite nanofiber layer is approximately 20 μm and the thickness more than
Mean 472.07 592.32
this amount leads to decreasing diffusion of resin through the nanofi-
Variance 1939.28 0.19 bers and subsequently the mechanical properties of the obtained com-
Observations 5 5 posite will be decreased [40]. Therefore, it can be expected 1 g m−2 of
Significance level 0.05 the SAN nanofibers on the surfaces of carbon fibers can provide the
df 6
maximum of the fracture toughness improvement.
tStat −5.44
P(T ≤ t) 0.001
tCritical 2.45 3.2. Interfacial toughening assessments

As explained in Section 2.4.2, three-point bending, and short beam

scanning electron microscope (FE-SEM). The surfaces of the samples
were coated with a fine layer of gold prior to morphological studies.
2.4.2. Interfacial toughening evaluations
In order to investigate the effect of embedding SAN nanofibers on
interfacial toughening of the hybrid composite three-point bending, and
short beam shear tests were performed in accordance to the standards
ASTM D790, ASTM D2344, respectively to reveal the effect of in-
corporation SAN nanofibers on out-of-plane properties of the carbon/
epoxy composite. In addition, the Izod impact test was carried out ac-
cording to ASTM D256 to reveal the effect of SAN nanofibers in-
corporation on the impact energy absorption of the hybrid composite.
The aforementioned tests were conducted with the instruments and
procedures described in our previous work [37]. The bending test was
carried out with adjusting the cross-head speed at 1 mm min−1 and the
span-to-depth ratio at 40 by using a 5 kN load cell Shimadzu AG-25 TB
shear tests were carried out to evaluate the effect of incorporation
electrospun SAN nanofibers on out-of-plane properties of hybrid
carbon/epoxy composite. The obtained results of three-point bending
test are summarized in Table 1. The results in Table 1 shows that the
incorporation of the electrospun SAN nanofibers in the resin rich area of
the composite had a significant positive impact on the flexural strength
as well as work to fracture, resulting in enhancing of 26% and 37%,
respectively. Strong bonding of the electrospun SAN nanofibers to the
epoxy resin (matrix) can be assigned to the higher specific surface area
of electrospun SAN nanofibers on how their diameters (approximately
500 nm) are remarkably smaller than the diameter of carbon fiber
(approximately 5 μm). These results enhanced the interfacial bonding
strength, and consequently, the flexural strength of the hybrid com-
posite. Furthermore, during applying a load, the SAN nanofibers are
broken and/or be detached from the matrix (epoxy). These two phe-
nomena dissipate strain energy, delay the onset of fracture of the hybrid

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R.E. Neisiany et al.
Fig. 5. Load-displacement curves of short beam shear strength test of (a) control composite and (b) hybrid composite.
composite, and consequently lead to the higher work to fracture. Fig. 4
shows the delaminated interlaminar surfaces of control composite and
hybrid composite after three-point bending test. It can be discerned that
the fracture occurred in the resin rich area (interlaminar regions) for
both types of the composites. From Fig. 4a the control composite
fracture surfaces are relatively smooth (conforming for brittle fracture)
due to oriented fracture features. The features were created from the
extensions in the formed micro-cracks which initiated at the locations
of the stress concentration. In contrast, Fig. 4b revealed that the more
roughness in the fracture surface for the hybrid composite confirming
for tough fracture. These results reinforced that presence of the elec-
trospun SAN nanofibers could deflect the created microcracks, leading
to direct the microcracks along more tortuous paths, and consequently,
increasing the resistance of resin rich area to crack propagation. Hence
the microcracks break away from the SAN nanofibers; they induce
kinked fracture surfaces, which offer more strain energy will be dis-
sipated. Voids/holes were also discerned in the fracture surfaces of the
hybrid composite which can be attributed to deboning and pull-out of
the electrospun SAN nanofibers from the epoxy matrix. The nanofiber
breakage and nanofiber pull-out are possibly the two mechanisms
which are responsible for positive contributions to the enhancing of the
fracture toughness of hybrid composite enriched with the nanofibers
[37]. Similarly, this improvement was also reported for epoxy adhesive
by modified carbon nanotubes [41,42]. In addition, as mentioned in the
experimental section, the statistical analysis (t-test) was carried out to
confirm the significant difference between obtained mechanical prop-
erties. The t-test results are summarized in Table 1. Table 2 indicates
the T-test results of the flexural strength of the control and hybrid
composites. According to t-test results, incorporation of the SAN na-
nofibers between carbon layers significantly increased the flexural
strength and bending work to fracture of the hybrid composite com-
pared to control composite (due to |tstat | > tcritical ) [29].
To assess the effect of incorporating the electrospun SAN nanofibers
on the interlaminar shear strength of hybrid composite, short beam
shear test was performed. With using short beam shear test, the com-
posites are assessed for resistance to interlaminar shear fracture in-
cluding free edge delamination in the polymer matrix composites [43].
In this technique, the interlaminar shear strength is determined ac-
cording to Eq. (1):
τs = 0.75 × Pm /( b× h)
In this equation, τs (MPa) is the interlaminar shear strength of polymer
matrix composite, Pm (N) is the peak load, b (mm) is the width of the
specimens, and h (mm) is the sample thickness.
Fig. 5a and b indicate the load-displacement results of control and
hybrid composite, respectively obtained via short beam interlaminar
shear strength assessments. Short beam strength of the composites was
calculated according to Eq. (1), and the results were summarized in
Theoretical and Applied Fracture Mechanics 95 (2018) 242–247
Table 1. The results in Table 1 indicate that incorporating the SAN
nanofibers between carbon layers led to a 27% enhancement in the
short beam shear strength of the hybrid composite when compared to
the results acquired for control composite. The reason for this im-
provement is attributed to the strengthening effect of the SAN nanofiber
incorporation had on the resin rich area of the hybrid composite. In this
case, the electrospun SAN nanofibers exert their effect as nano-re-
inforcements in the interlaminar areas, by stress transfer from the resin
rich area (epoxy matrix) to the reinforcing phase (carbon fibers). They
act to damp the microcracks propagation in the resin rich area by acting
as a bridge in this layers hence the microcracks are created due to the
high-stress concentration [43]. In addition, statistical analysis confirms
that incorporation SAN nanofiber between carbon layers significantly
increased the interlaminar shear strength of the hybrid composite.
Izod impact test was also carried out to determine the fracture re-
sistance of the hybrid composite at high strain rates via evaluating the
absorbed energy during impact. The impact test results indicated in
Table 1 reveals that the impact absorption energy of the hybrid com-
posite was increased by 8% with the incorporation of the electrospun
SAN nanofibers. This enhancement is possibly assigned to the SAN
nanofibers hindering the propagation of the microcrack and also attri-
buting to distributing of the applied loads, consequently storing some
measure of impact energy, which allowed for more energy to be ab-
sorbed before the catastrophic fracture. However, statistical analysis (t-
test) suggests a negligible effect of incorporating SAN nanofibers on
impact absorption energy of the hybrid composite compared to control
composite.
4. Conclusions
The electrospun SAN nanofibers were used to improve the out-of-
plane properties of a conventional carbon/epoxy composite. The ap-
plication of electrospun SAN nanofibers prepared with this technique is
easily streamlined with the existing VARTM composite fabrication
method. This can be carried out by facile electrospinning of a nanofiber
layer onto the reinforcing phases via a scalable process. Morphological
investigations of the electrospun SAN indicated that the electrospun
SAN nanofibers are smooth without any signs of beads with diameter
size range of nano. The hybrid composite with SAN nanofibers gave a
(1) 26% gain in flexural strength, 37% improvement in flexural work to
fracture, 27% increase in short beam shear strength, and 8% en-
hancement in impact energy absorption in comparison with results
acquired for control composite. Furthermore, the statistical analysis (t-
test) confirmed significant enhancements in flexural strength, bending
work to fracture, and short beam interlaminar shear strength, but did
not significantly affect impact absorption energy of the hybrid com-
posite. These improvements confirmed great potential in overcoming
the shortcomings of the laminated polymer matrix composites even in
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the critical applications, especially for the terms of enhancing the out-
of-plane properties.
Acknowledgments
The authors express their sincere gratitude to the Iranian Ministry of
Science, Research and Technology (MSRT) for the monetary support of
research visit for the accomplishment of this work at National
University of Singapore. This work was also supported by a grant from
the Department of Mechanical Engineering, Faculty of Engineering,
National University of Singapore, Singapore, Lloyd’s Register
Foundation [Grant number R-265-000-553-597].
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