Professional Documents
Culture Documents
COMPOSITE
Article M AT E R I A L S
Journal of Composite Materials
0(0) 1–19
! The Author(s) 2019
Short-beam shear of nanoprepreg/ Article reuse guidelines:
sagepub.com/journals-permissions
nanostitched three-dimensional DOI: 10.1177/0021998319863472
journals.sagepub.com/home/jcm
carbon/epoxy multiwall carbon
nanotube composites
Abstract
The effect of out-of-plane stitching and the addition of multiwalled carbon nanotubes on the short-beam shear proper-
ties of carbon/epoxy composites were investigated. Stitching influenced the short-beam strength of carbon satin and twill
fabric composites, where the stitched satin carbon/epoxy composites showed improved short-beam properties com-
pared with the unstitched satin carbon/epoxy composites. In general, stitching and MWCNTs addition enhanced the
short-beam strength of the composite. The fracture of the composites generally exhibited as a combination of lateral
total matrix cracking, warp fiber breakage and interlayer opening. In addition, all the structures experienced angularly
sheared catastrophic through-the-thickness layer breakage. It was also shown that delamination was largely restricted in
stitched and nano-added composites when compared to the unstitched samples. It can be concluded that nanostitching
could be considered for improving short-beam strength properties of the composite.
Keywords
Carbon nanotubes, nanoprepreg, nanostitching, short-beam test, interlaminar shear strength
applicable to obtain the interlayer shear strength of the mechanical and energy absorption characteristic of
composite, in which the support span to thickness ratio composites at the optimum stitch density. The damaged
was a critical parameter for shear stress and interlayer areas after the impact tests were considerably smaller in
matrix fracture was the main failure mode.13 Although the stitched composite than in the unstitched sample.29
comparatively uniform load distribution was achieved Mouritz exhibited that the KevlarÕ -49 stitching
in a four-point short-beam test, the pure interlaminar increased the damage tolerance of glass/vinyl ester com-
shear fracture was not obtained in the maximum posites against impact loading.30 Bilisik reported that
shear stress region because of low crack propagation the interlaminar shear strength of the 3D orthogonal
energy.14,15 woven composite was slightly higher (10%) compared
z-Pin-added advanced structural composite parts to the multiaxis 3D woven composites. The addition
demonstrated better fracture toughness due to bridging of bias yarns on both surfaces of the 3D orthogonal
effect, pull-out and friction. The critical parameters preform had no significant effect on interlaminar
were identified as z-pin density and length.16 Another shear strength by performing the short-beam shear
study showed that the carbon fiber-coated z-pin com- test.31 Another study showed that the short-beam
posite enhanced mode-I failure due to bonding between shear strength of the 3D layer-to-layer and through-
the z-pin and composite.17 the-thickness preforms was improved by directional
The short-beam shear fracture properties of 2D non- fiber hybridizations via various interlocking patterns.32
woven composite were studied via converted v-notched Failure mechanics of 2D and 3D woven composites
rail shear test. It was concluded that micro-crack, were also studied using the short-beam shear and
coupling crack and macro-crack were identified. The impact fatigue tests. The fracture in 2D woven compos-
micro-crack started during fiber micro-slippage in the ite was both shear and tensile mode, whereas it was
resin at the interlayer region of the composite and led to only tensile mode in 3D composite.33
the macro-cracks.18 It was identified that the interlayer Nanomaterials emerged as promising reinforcement
shear fracture of the E-glass/epoxy structure was fiber agents for composite applications.34–38 The epoxy
and matrix failures, interlaminar debonding and mul- sizing on the carbon fiber surface in carbon/epoxy com-
tiple macro-craking.19 posite improved the short-beam strength and toughness
The effect of stitching on the composite was investi- due to fiber and resin interfacial bonding strength.39–41
gated. Stitching improved the tensile and flexural Hosur et al. explained that the addition of different
strength of 2D composites because of a more efficient nanoparticles in epoxy led to noticeable enhancements
distribution of load in the out-of-plane direction due to in the viscoelastic and mechanical properties over the
the presence of z-fibers.20 The impact and short-beam pristine samples.42 It was realized that matrix modifica-
strength of fabric composites were improved by stitch- tion via multiwalled carbon nanotubes (MWCNTs)
ing.21 On the contrary, it was claimed that stitching and n-butyl glycidyl ether improved the interlayer
reduced the interlaminar shear and flexural strength strength of glass/epoxy composite.43 However,
of E-glass/vinyl ester composites after repeated MWCNTs (0.5%)-added glass/epoxy composite
impact. This was attributed to stitching-induced irregu- showed no significant improvement for interlaminar
larities and stitch holes, which acted as stress concen- shear strength.44 Nonetheless, it was demonstrated
tration sites in the structure.22,23 z-Stitching was shown that shear strength of the composite was enhanced
to improve fracture toughness (mode-I) behavior of due to the even MWCNTs dispersion in the matrix
biaxial fabric composites while degrading the in-plane and the MWCNTs bridging in the composite layers.45
properties.24 The number of fabric layers and yarn It was reported that the incorporation of nanosilica
orientation strongly influenced the flexural behavior increased the short-beam strength of E-glass/polyester
of E-glass/polyester composites where the composites composites. Stitch density, stitch yarn type and stitch
showed delamination under flexural load.25 Another pattern as well as the amount of nanomaterial influ-
study showed that cryogenic temperatures generally enced the interlaminar strength of the composite.46
decreased the interlaminar strength of carbon/epoxy Yong and Hahn investigated the feasibility of using
composites.26 Wei and Zhang characterized the stitch- silicon carbide (SiC) nanoparticles to produce SiC/
induced irregularities in fabric and composite structure vinyl ester nanocomposites. Improper dispersion of
using a fiber distortion model.27 Zhao et al. showed nanoparticles in the resin led to lower composite
that z-stitching noticeably increases the impact strength, whereas the composite strength and modulus
damage tolerance of glass/polypropylene (PP) compos- increased with the use of a dispersant.47 Patnaik et al.
ites without an adverse effect on tensile properties. demonstrated that the tensile strength of glass fiber/
There was a correlation between the fracture work of polyester composites were significantly reduced when
the stitch yarns and the energy absorption capability.28 aluminum oxide (Al2O3) and SiC particles were used
Kang and Lee reported that z-stitching improved the as filler material.48 Wichmann et al. noted that nano-
Bilisik et al. 3
Table 1. The suppliers and specifications of the carbon fibers, fabrics, epoxy resin and nanotubes.66
12K, A-42, no twist, (AKSACA, TR) 6.0 1.78 4.20 240 1.8 >1200
Epoxy resin
Araldite LZ 5021-resin – 1.0–1.2 0.78–0.82 3.3–3.4 5.0–8.5 110–119
Aradur 1571-hardener
Accelerator 1573-accelar
(Biesterfeld Spezialchemie GmbH, DE)
Carbon fabrics
Fabric
Fabric areal thickness
Supplier Weave Coating Warp Weft Warp Weft weight (g/m2) Warp Weft (mm)
(Spinteks Twill (2/2 Z) DO12, standard 800 800 38 38 590 0.30 0.22 0.81
A.S., TR) Satin (1/4) epoxy coating, 800 800 38 38 585 0.36 0.20 0.98
1.0–1.5%
Nanothinx, GR 15–35 10 1–2 12.01 >100 97 1.74 200 1.0 3550
(Nanothinx64) (Nanothinx64) (Lehman et al.65)
Stitched fibers
CS-TS-N and CT-TS-N, respectively. The CS-CS-N explanation to avoid repetition for readers. It was note-
and CT-CS-N were four-layer satin and twill fabrics, worthy that the MWCNTs ratio (0.03125%) and stir-
respectively. They were stitched with carbon nanos- ring time (120 min) used in this study was chosen after
titching fiber. The CS-TS and CT-TS were four-layer rigorous attempts to minimize the agglomeration of the
satin and twill fabrics, respectively. They were stitched MWCNTs. Stitching of the fabric layers was performed
with p-aramid nanostitching fiber. Some of the com- in the prepreg state. For this purpose, firstly the carbon
posites are exhibited in Figure 1. fabric prepreg and prepreg stitch yarns (nanostitching)
For manufacturing the composite samples, first, an were produced.67 Stitching was conducted manually on
epoxy and MWCNTs mixture was prepared. More the prepregs layered with a [0 /90 ]4 sequence using
information on the composite fabrication was pre- PAN carbon and Twaron-nanostitched yarn. The dens-
sented by Bilisik et al.66 In this paper, there is a short ity of stitching and the spacing of the stitch rows were
Bilisik et al. 5
Figure 1. (a) Twaron-stitched twill carbon fabric preform (left) and composite (CT-TS) (right); (b) carbon-stitched twill carbon fabric
preform (left) and composite (CT-CS) (right); (c) Twaron-stitched twill carbon fabric nano-preform (left) and composite (CT-TS-N)
(right); (d) schematic top view of the Twaron-stitched structure (CT-TS/CT-TS-N); (e) schematic sectional view of the Twaron-stitched
structure (CT-TS/CT-TS-N); (f) schematic top view of carbon-stitched structure (CT-CS/CT-CS-N).
1 step/cm and 1 cm, respectively. A mold which was (Figure 2(a) and (b)). The testing speed was
covered with Teflon film was employed for the curing 1.0 mm/min. The measured average actual sample
of the nanostitch prepreg material. A hot press was dimensions were 11.80 (width) 36.46 (length) 3.01
utilized to consolidate the prepreg material under (thickness) mm. The support span length to sample
0.6 MPa pressure at 150 C for 15 min. After curing thickness was 4.984/1. The short-beam test method
the 3D nanostitched prepreg preform, the mold was was near to have pure shear.71,72 The short-beam load
kept under pressure until the temperature decreased was conducted in the warp (0 , lengthwise) direction.
to 40 C. Then, the sample composites were removed The tests were executed at standard laboratory atmos-
from the mold. phere (temperature: 23 C 2 C, relative humidity:
50% 10%). The generated stresses during the flexure
load were compressive on the top surface of the sample
Fabric and composite testing
and tensile on the bottom surface of the sample during
The ISO 7211-3 standard was followed to determine the short-beam shear loading. It was assumed that the max-
directional crimp (%) by utilizing a Tautex digital imum interlaminar shear stress occurred on the neutral
instrument (James H. Heal Co., UK). The areal density plane of the sample.72 Thus, the stress state should be
of the fabric (g/m2) was identified based on the ISO pure shear on the neutral plane. The stresses during
6348 standard using an Ohaus AdventurerTM Pro flexure load were kept low (due to low span length/
AV812 (Ohaus Corp., USA). The weight measurement sample thickness ratio), promoting shear failures on
of the MWCNTs (g) was obtained using a Shimadzu the neutral plane. On the contrary, the stress concen-
AUX320 (Shimadzu Corp., JP) digital balance. The tration occurred around the applied load and support
PAN-based carbon fabric thickness (mm) was measured points.72 Therefore, the assumption of the maximum
by employing an EV07 digital measurement device stress distribution at the neutral plane was an approxi-
(Elastocon, SE). The ASTM D792-9168 standard was mation.72 The short-beam strength was calculated
followed to find the composite sample densities according to equation (1)
(g/cm3). The ASTM D3171-9969 and ASTM D2734-
9170 standards were followed to find the composite Pm
Fsbs ¼ 0:75 ð1Þ
volume fraction (%) and void content (%), respectively. bh
The ASTM D2344-1371 standard was followed to
conduct the short-beam shear test using a Shimadzu where Fsbs is the short-beam strength (MPa), Pm is the
AG-XD 50 (Shimadzu, JP) tester with a 5 kN maximum load (N), b is the specimen width (mm) and h
loading cell equipped with TrapeziumÕ software is the specimen thickness (mm).
6 Journal of Composite Materials 0(0)
Figure 2. (a) Short-beam fixture with sample; (b) failed sample under short-beam load; (c) damaged area measurements on
unstitched base composite (CSU); (d) unstitched nano (CSU-N); (e) stitched base (CS-CS); (f) stitched nanocomposite (CS-CS-N,
digital image).
Table 2. Physical characteristics of the composite samples for the short-beam test.
Short-beam Short-beam
Short-beam load displacement at strength Damaged
Label (maximum) (N) maximum load (mm) (MPa) area (mm2)
twill and satin fabrics, different stitch yarn densities and representative samples are illustrated in Figure 3(a)
the MWCNTs incorporation. The total fiber fractions, and (b). As exhibited in Figure 3, after the proportional
ranged between 60.09 and 70.76% with a mean value of limit was passed, the load attained its maximum value
64.20%. The variation in fiber fraction results can also and it abruptly fell due to major carbon warp/weft
be attributed to the aforementioned effects. The effect breakage. Then, a small increase was recorded in the
of the stitch yarns on the total fiber weight fraction was load value possibly due to crack arrest in the failed
considerably small with a value range of 1.17–1.70%. region. Eventually, the load was decreased sharply
The void content values were acceptable (0.42–1.30%) because of the complete fracture of the structure. As
for this kind of processing. shown in Figure 3(a), the highest load was obtained in
the CS-CS-N sample followed by the CS-CS, CSU-N
and CSU. In Figure 3(b), the highest load was from the
Short-beam strength
CTU-N sample followed by the CT-CS-N, CTU and
Table 3 demonstrates the short-beam test results of the CT-CS. Figure 4(a) and (b) shows some of the individ-
composite samples. Load–displacement graphs of some ual short-beam load–displacement curves. As seen in
8 Journal of Composite Materials 0(0)
Figure 4. Some of the individual load–displacement graphs of satin (1/4) and twill (2/2) carbon fabric composite samples: (a) load–
displacement curves of the CS-CS-N and CSU composite samples and (b) load–displacement curves of the CT-CS-N and CTU
composite samples.
Figure 4, each short-beam load–displacement curve for strength values of the CTU and the CSU structures
the CS-CS-N and CSU as well as the CT-CS-N and were almost the same. The interlaminar shear strength
CTU samples exhibited small standard deviation in of the CTU was approximately 11.93% higher than
both the proportional limits and around the maximum those of the stitched base (CT-CS and CT-TS) compos-
load regions. ites. Thus, stitching negatively influenced the short-
Figure 5 exhibits the short-beam load of all carbon/ beam strength of twill fabric composites for both the
epoxy MWCNT composites. It was understood that the carbon (CT-CS) and Twaron-stitched (CT-TS) yarns.
stitching and MWCNTs increased the short-beam load This result can be ascribed to the stitch-induced
of all the stitched base and stitched nanocomposites. unevenness in the structure as well as the minor fila-
The stitching yarn type also slightly effected the ment breakage and stitch holes which may act as stress
short-beam load of the stitched base and stitched nano- concentration points. The effect of the stitch yarn type
composites where the PAN carbon-stitched composite on these samples, i.e. carbon and Twaron stitching was
showed better performance compared to the para- negligible. The interlaminar shear strength of the CSU
aramid stitched composites. was approximately 14.20% lower than that of the
Figure 6 illustrates the short-beam strength values of carbon-stitched base (CS-CS) and was 19.26% higher
all composite samples. As depicted in Figure 6, the than that of the Twaron-stitched (CS-TS) composites.
interlaminar shear strength of unstitched base (CTU) Therefore, the effect of stitching was different in the
was insignificantly (1.54%) higher than that of the case of satin fabric composites. Stitching with carbon
unstitched base (CSU). Therefore, the short-beam yarns noticeably increased the short-beam strength of
Bilisik et al. 9
the satin fabric base composites (CS-CS) compared unstitched base (CSU) composite. Therefore, the
with the unstitched base samples (CSU). This can be MWCNTs addition on the unstitched CSU, carbon
attributed to the delamination suppression effect of and Twaron-stitched (CS-CS and CS-TS) satin fabric
stitching which generally increased the interlaminar composite samples considerably increased their short-
shear strength. The Twaron-stitched samples (CS-TS) beam strength.
showed smaller strength values compared with the Figure 7 illustrates the displacement values of the
unstitched base samples (CSU), probably due to both samples at maximum load. In Figure 7, carbon-
the toughness characteristic of the para-aramid fiber stitched twill carbon fabric composites (CT-CS) dis-
and bonding between the p-aramid fiber and epoxy. played a smaller displacement value compared with the
The interlaminar shear strength of the CTU was unstitched base sample (CTU), whereas the Twaron-
5.48% higher than that of the unstitched nano stitched samples (CT-TS) showed similar displacement
(CTU-N) composites and was approximately 11.81% values with the CTU sample. The carbon-stitched
higher than those of the stitched nano (CT-CS-N and satin fabric composites (CS-CS) displayed greater dis-
CT-TS-N) composites, probably partly due to agglom- placement when compared to the unstitched base satin
eration and the uneven dispersion of the MWCNTs in composites (CSU). Nano-addition increased the dis-
the resin and TOW fiber (filament bundles) surfaces. placement values in most of the cases probably due to
On the contrary, the interlaminar shear strength of the micro-level resin nanotube pull-out and friction.
the CSU-N was 15.21% higher than that of the Figure 8 exhibits the relative sizes of the damaged areas
unstitched base (CSU) composite. The stitched nano of the samples after the short-beam tests. The damaged
(CS-CS-N and CS-TS-N) composites were approxi- area of the unstitched base (CSU) composite was 36.47%
mately 15.42% and 7.47% higher than that of the lower than that of the unstitched base (CTU) composite,
10 Journal of Composite Materials 0(0)
Figure 8. Relative sizes of the damaged areas after the short-beam tests.
Figure 9. Warp directional short-beam failures in the composite samples. (a) Satin fabric unstitched base (CSU) top face; (b)
unstitched base (CSU) cross-section; (c) unstitched base (CSU) bottom face; (d) unstitched base nano (CSU-N) top face; (e)
unstitched base (CSU-N) cross-section and (f) unstitched base nano (CSU-N) bottom face (optical microscope, magnification 6.7).
probably due to the interlacement pattern. The damage well as it was 42.44% higher for stitched base (CS-CS)
size of the unstitched twill fabric composite (CTU) was composite. Additionally, the damaged area of the
similar to that of the carbon-stitched sample (CT-CS), carbon-stitched nano (CS-CS-N) was 28.21% higher for
whereas the Twaron-stitched sample (CT-TS) displayed p-aramid stitched nano (CS-TS-N) and was 71.11%
greater damage size compared with the unstitched base higher for the para-aramid stitched (CS-TS) samples. In
(CTU) sample. With regard to the satin fabric composites, addition, the unstitched nano (CSU-N) was 59.68%
the damaged area of the carbon-stitched nano (CS-CS-N) higher for the base (CSU) composite. Thus, the carbon-
composite was 37.78% higher for the unstitched nano stitched sample (CS-CS) exhibited greater damage size
(CSU-N) and was 74.92% higher for base (CSU) as compared with the unstitched (CSU) and Twaron-stitched
Bilisik et al. 11
Figure 10. Warp directional short-beam failures in the composite samples. (a) Carbon-stitched satin composite (CS-CS) top face;
(b) carbon-stitched satin composite (CS-CS) cross-section; (c) carbon-stitched satin composite (CS-CS) bottom face; (d) carbon-
stitched satin nanocomposite (CS-CS-N) top face; (e) carbon-stitched satin nanocomposite (CS-CS-N) cross-section and (f) carbon-
stitched satin nanocomposite (CS-CS-N) bottom face (optical microscope, magnification 6.7).
Figure 11. Warp directional short-beam failures in the cross-section of the composite samples. (a) Twill fabric unstitched base
(CTU); (b) twill fabric unstitched nano (CTU-N); (c) carbon-stitched twill base (CT-CS) and (d) carbon-stitched twill nanocomposite
(CT-CS-N) (optical microscope, magnification 6.7).
12 Journal of Composite Materials 0(0)
(CS-TS) sample. The twill fabric composites showed some especially the PAN carbon-stitched yarn on the base struc-
larger damage areas when compared to the satin fabric tures made the material slightly brittle.
composites. The MWCNTs addition increased the
damage size in short-beam tests for all the sample types.
This probably indicated that MWCNTs addition and
Figure 12. Warp directional short-beam failures in the composite samples. (a) Twaron-stitched satin base composite (CS-TS) cross-
section; (b) Twaron-stitching path in fractured satin base composite (CS-TS) cross-section and (c) Twaron-stitched satin nanocom-
posite (CS-TS-N) bottom face (optical microscope, magnification 6.7).
Figure 13. SEM images of warp directional short-beam failures in the composite samples. (a) Satin fabric unstitched base (CSU)
bottom face; (b) unstitched base (CSU) cross-section; (c) unstitched base nano (CSU-N) bottom face and (d) unstitched base (CSU-N)
cross-section.
Bilisik et al. 13
Failure analysis by optical micrograph to (f). Lateral total matrix cracking and warp yarn fail-
Post-failure micrographs of the satin fabric unstitched ures were identified on the compression side of the
base (CSU) and satin fabric unstitched nano (CSU-N) CS-CS and CS-CS-N composites (Figure 10(a) and
samples after the short-beam tests are shown in (d)). On the tension side of the structures, lateral
Figure 9(a) to (f). Lateral major matrix cracking and matrix cracking and warp yarn failures as well as
warp fiber failures were detected on the compression carbon-stitched yarn breakage were obtained. A limited
side of both the base and nano-added structures intralayer opening between the warp and weft TOWs
(Figure 9(a) and (d)). On the tension side of the struc- were found (Figure 10(c) and (f)). In cross-section of
tures, lateral multiple warp failures and TOW opening the CS-CS structure, catastrophic through-the-
between the warp and weft TOWs were observed thickness layer failures were observed and the layers
(Figure 9(c) and (f)). In cross-section of the CSU were angularly sheared in a large inward opening hori-
sample, catastrophic through-the-thickness layer break- zontal v-shape in the out-of-plane direction on both
age was found. Layers were angularly sheared in an the compression and tension sides as shown in
outward horizontal v-shape in the out-of-plane direc- Figure 10(b). However, sharp through-the-thickness
tion on both the compression and tension sides as layer failures were identified in the CS-CS-N composite
shown in Figure 9(b). In cross-section of the CSU-N (Figure 10(e)).
sample, total layer failures in the out-of-plane direction Post-failure cross-sectional micrographs of the twill
were observed. The layers were sheared in a large unstitched base (CTU), twill unstitched nano (CTU-N),
inward opening horizontal v-shape on both the com- twill carbon-stitched base (CT-CS) and twill carbon-
pression and tension sides where local layer delamin- stitched nano (CT-CS-N) composites after the short-
ation and crack opening was identified (Figure 9(e)). beam tests are demonstrated in Figure 11(a) to (d). In
Post-failure micrographs of the carbon-stitched base cross-section of the failed CTU and CTU-N structures,
(CS-CS) and carbon nanostitched (CS-CS-N) compos- two-line major catastrophic multiple layer failures were
ites after the short-beam tests are shown in Figure 10(a) identified and the layers were slightly angularly sheared
Figure 14. SEM images of warp directional short-beam failures in the composite samples. (a) Carbon-stitched satin composite
(CS-CS) bottom face; (b) carbon-stitched satin composite (CS-CS) cross-section; (c) carbon-stitched satin nanocomposite (CS-CS-N)
bottom face and (d) carbon-stitched satin nanocomposite (CS-CS-N) cross-section.
14 Journal of Composite Materials 0(0)
(Figure 11(a)), whereas severe interlayer failure in the zone (Figure 11(c)), whereas severe angular interlayer
form of inward horizontal v-shape cracks extending failure in the form of inward vertical v-shape (bulge
through the structure thickness from the compression zone) cracks extending through the sample thickness
to tension side was observed for the unstitched nanos- were observed for the stitched nanocomposite. In add-
tructure (Figure 11(b)). The cross-sectional views of the ition, indentation was observed on the compression side
twill carbon-stitched (CT-CS) and twill carbon nanos- and slight tensile failure was detected on the tension
titched (CT-CS-N) samples showed catastrophic side of the CT-CS-N structure (Figure 11(d)).
through-the-thickness tensile layer failures. The crack Post-failure micrographs of the satin fabric Twaron-
propagation was largely restricted around the failure stitched base (CS-TS) and satin fabric Twaron-stitched
Figure 15. SEM images of warp directional short-beam failures in the composite samples. (a) Twaron-stitched satin composite
(CS-TS) cross-section; (b) Twaron-stitched satin composite (CS-TS) cross-section; (c) Twaron-stitched satin nanocomposite
(CS-TS-N) cross-section; (d) Twaron-stitched satin nanocomposite (CS-TS-N) cross-section; (e) p-aramid stitching fiber in composite
(CS-TS) cross-section and (f) close view of through-the-thickness stitching zone in composite (CS-TS) cross-section.
Bilisik et al. 15
nano (CS-TS-N) samples after the short-beam tests are beam tests are shown in Figure 13(a) to (d). Lateral
shown in Figure 12(a) to (c). In the cross-section of the catastrophic tensile warp fiber failures and a weft
CS-TS, an inelastic deformation failure mode was found. TOW opening were found on the tensile side of the
Angularly oriented interlaminar shear failures on the CSU structure (Figure 13(a)). Bended warp TOW and
compression side were also observed (Figure 12(a)). warp-weft delamination near the tension side of the
Figure 12(b) shows layer-to-layer multiple yarn breakage CSU composite were identified. A weft TOW opening
as well as local delamination around the broken loop and complete warp TOW failures in the shear band
part of the p-aramid stitching yarn. The stitched yarn were also observed (Figure 13(b)). On the tension side
served as a delamination suppressor around the region. of the CSU-N structure, matrix-filament debonding
On the tension side of the stitched nano (CS-TS-N) and multiple matrix breakage as well as tensile filament
sample, catastrophic layer-to-layer breakage and partial fracture were seen. Shear hackle in the matrix was also
p-aramid stitch yarn failure at the loop section occurred. found due to subsequent shear flow during short-beam
Thus, delamination and layer failures in the fractured loading (Figure 13(c)). In the cross-section of the CSU-
region of the CS-TS-N were outwardly arrested N structure, a large weft TOW opening, kinked warp
(Figure 12(c)). TOW breakage as well as warp-weft delamination in
the shear zone were obtained (Figure 13(d)).
Failure analysis by scanning electron microscope SEM images of the carbon-stitched base (CS-CS)
and carbon-nanostitched (CS-CS-N) composites after
images the short-beam tests are shown in Figure 14(a) to (d).
Scanning electron microscope (SEM) images of the Lateral matrix cracking in the shear zone and filament
satin fabric unstitched base (CSU) and satin fabric pull-out marks on the matrix of the CS-CS structure
unstitched nano (CSU-N) composites after the short- were found on the tension side of base structure
Figure 16. SEM images of warp directional short-beam failures in the composite samples. (a) Twaron-stitched twill composite
(CT-TS) cross-section; (b) Twaron-stitched twill composite (CT-TS) cross-section; (c) Twaron-stitched twill nanocomposite (CT-TS-N)
bottom face and (d) Twaron-stitched twill nanocomposite (CT-TS-N) cross-section.
16 Journal of Composite Materials 0(0)
(Figure 14(a)). Matrix-TOW breakage and filament- Unstitched base (without MWCNTs) satin and twill
filament delamination in the bending region were iden- carbon/epoxy composites displayed similar short-beam
tified (Figure 14(b)). strength values. Stitching slightly reduced the short-
Multiple matrix failure lines in the shear zone and beam strength of twill fabric composites for both
multiple filament pull-out marks of the CS-CS-N com- carbon and Twaron-stitched yarns possibly due to stitch-
posite were also identified (Figure 14(c)). Multiple ten- ing based unevenness in the structure. The effect of the
sile failures in the single filament axis as well as in the stitching yarn types on twill carbon/epoxy composites
filament bundles were observed (Figure 14(d)). was negligible. Carbon-stitched yarns noticeably
SEM graphs of the satin fabric Twaron-stitched increased the short-beam strength of satin fabric stitched
base (CS-TS) and satin fabric Twaron-stitched nano base composites compared with the unstitched base
(CS-TS-N) structures after the short-beam tests are composite. However, the para-aramid stitched satin
shown in Figure 15(a) to (f). Kinked warp failure carbon/epoxy composite showed lower short-beam
(inelastic deformation failure) in the shear zone of strength values compared with the unstitched base com-
the CS-TS sample was seen (Figure 15(a)). Around posite. In general, stitching and MWCNTs addition
the shear zone, partial tensile filament failure enhanced the short-beam strength of the base composite.
and total catastrophic filament failure were found. Stitched composite samples generally showed
Local layer-to-layer delamination was also identified. increased damage size compared with the unstitched
Multiple tensile failures in the single filament axis composite samples. The addition of the MWCNTs
as well as in the filament bundles were observed increased the damage size in short-beam tests for all
(Figure 15(b)). Some kinked warp failures and a large the sample types. The failure of unstitched samples
weft TOW opening in the shear zone of the CS-TS-N occurred as a combination of lateral major matrix
sample were found (Figure 15(c)). Multiple tensile fila- cracking, warp fiber failures and catastrophic
ments in the kinked warp TOW were also identified and through-the-thickness layer breakage, whereas the
are shown in Figure 15(d). p-Aramid stitched Twaron stitched samples experienced lateral total matrix crack-
in the CS-TS composite made a slight curve path and ing, warp yarn failures and stitch yarn breakage. The
some of the filaments were frayed from the stitching delamination was arrested severely in the stitched sam-
bundle (Figure 15(e)). Next to the stitched fiber region, ples, as can be inferred from the local delamination
a sharp crack tip was identified. It was considered that around the stitch loops. Thus, the stitch yarn served
the stitching fiber acted as a crack barrier (Figure 15(e)). as a delamination suppressor around the region. It
In a closer view of the p-aramid stitching yarn, fibrillar can be concluded that both stitching and nano-addition
splitting and some fraying filaments were observed and can be used to improve the short-beam shear properties
are shown in Figure 15(f). of base composites.
SEM graphs of the twill Twaron-stitched (CT-TS)
and twill Twaron-stitched nano (CT-CS-N) samples Acknowledgements
after the short-beam tests are shown in Figure 16(a) The authors would like to thank Dr G Erdogan for helping to
to (d). Multiple weft TOW fractures and weft TOW make the composite samples and Dr S Gungor for some
crack propagation near the tension side of the CT-TS useful discussions on carbon nanotube processing. They
sample was found (Figure 16(a)). Multiple tensile also thank the Erciyes University Technology Research and
filament fractures were identified and the crack path Implementation Center (TAUM) for some scanning electron
followed directly to the out-of-plane direction of the microscope images.
sample. Later, it turned to the warp-weft TOW inter-
face and this led to local TOW to TOW delamination Declaration of Conflicting Interests
(Figure 16(b)). Intra filament-matrix peeling and shear- The author(s) declared no potential conflicts of interest with
based matrix breakage along the filament axis were respect to the research, authorship, and/or publication of this
found on the tensile side of the CT-TS-N sample article.
(Figure 16(c)). Large and small weft TOW shear
cracks and a kinked warp TOW fracture were observed Funding
in the shear zone of the compression side of the CT-TS- The author(s) disclosed receipt of the following financial sup-
N sample as shown in Figure 16(d). port for the research, authorship, and/or publication of this
article: This research received a grant from Roketsan
Industries Incorporations, Grant No. RS/ERCIYES _ DSM-
Conclusions 76301-14-01N/R.
In this study, the effects of stitching and carbon
nanotube addition on the short-beam shear properties ORCID iD
of carbon/epoxy composites were investigated. Kadir Bilisik https://orcid.org/0000-0002-0592-980X
Bilisik et al. 17
36. Thostenson ET, Ren ZF and Chou TW. Advances in the two-dimensional carbon fiber reinforced silicon carbide
science and technology of carbon nanotube and their composites. Mater Des 2016; 98: 120–127.
composites: a review. Compos Sci Technol 2001; 61: 52. Yip MC, Lin YC and Wu CL. Effect of multi-walled
1899–1912. carbon nanotubes addition on mechanical properties of
37. Shen L and Li J. Transversely isotropic elastic properties polymer composites laminate. Polym Polym Compos
of multiwalled carbon nanotubes. Phys Rev B 2005; 71: 2011; 19: 131–139.
035412. 53. Davis DC, Wilkerson JW, Zhu J, et al. A strategy for
38. Saravanan N, Rajasekar R, Mahalakshmi S, et al. improving mechanical properties of a fiber reinforced
Graphene and modified graphene-based polymer nano- epoxy composite using functionalized carbon nanotubes.
composites – a review. J Reinf Plast Compos 2014; 33: Compos Sci Technol 2011; 71: 1089–1097.
1158–1170. 54. Zhu J, Imam A, Crane R, et al. Processing a glass fiber
39. Fernández B, Arbelaiz A, Valea A, et al. A comparative reinforced vinyl ester composite with nanotube enhance-
study on the influence of epoxy sizings on the mechanical ment of interlaminar shear strength. Compos Sci Technol
performance of woven carbon fiber-epoxy composites. 2007; 67: 1509–1517.
Poly Compos 2004; 25: 319–330. 55. Fan Z and Advani SG. Characterization of orientation
40. Varma DS, Needles HL, Kourtides DA, et al. lnterlami- state of carbon nanotubes in shear flow. Polymer 2005;
nar shear properties of graphite fiber, high-performance 46: 5232–5240.
resin composites. Poly Compos 1983; 4: 98–103. 56. Fan Z, Santare MH and Advani SG. Interlaminar shear
41. Blackketter DM, Upadhyaya D, King TR, et al. strength of glass fiber reinforced epoxy composites
Evaluation of fiber surface treatment and sizing on the enhanced with multi-walled carbon nanotubes. Compos
shear and transverse tensile strengths of carbon fiber- Part A Appl Sci Manuf 2008; 39: 540–554.
reinforced thermoset and thermoplastic matrix compos- 57. Kim MT, Rhee KY, Park SJ, et al. Effects of silane-mod-
ites. Poly Compos 1993; 14: 430–436. ified carbon nanotubes on flexural and fracture behaviors
42. Hosur M, Mahdi TH, Islam ME, et al. Mechanical and of carbon nanotube-modified epoxy/basalt composites.
viscoelastic properties of epoxy nanocomposites rein- Compos Part B Eng 2012; 43: 2298–2302.
forced with carbon nanotubes, nanoclay, and binary 58. Ma PC, Kim JK and Tang BZ. Effects of silane functio-
nanoparticles. J Reinf Plast Compos 2017; 36: 667–684. nalization on the properties of carbon nanotube/epoxy
43. Liu Y, Yang JP, Xiao HM, et al. Role of matrix modifi- nanocomposites. Compos Sci Technol 2007; 67:
cation on interlaminar shear strength of glass fibre/epoxy 2965–2972.
composites. Compos Part B Eng 2012; 43: 95–98. 59. Yu B, Jiang Z, Tang XZ, et al. Enhanced interphase
44. Chandrasekaran VCS, Advani SG and Santare MH. Role between epoxy matrix and carbon fiber with carbon
of processing on interlaminar shear strength enhance- nanotube-modified silane coating. Compos Sci Technol
ment of epoxy/glass fiber/multi-walled carbon nanotube 2014; 99: 131–140.
hybrid composites. Carbon 2010; 48: 3692–3699. 60. Salam MBA, Hosur MV, Jahan N, et al. Improvement in
45. Gurkan I and Cebeci H. An approach to identify complex mechanical and thermo-mechanical properties of carbon
CNT reinforcement effect on the interlaminar shear fibre/epoxy composites using carboxyl functionalized
strength of prepreg composites by Taguchi method. multi-walled carbon nanotubes. Polym Polym Compos
Compos Struct 2016; 141: 172–178. 2013; 21: 495–507.
46. Bilisik K and Yolacan G. Short beam strength properties 61. Hu YF, Wang B, Zhang XN, et al. Development of mul-
of multistitched biaxial woven E-glass/polyester nano tiwalled carbon nanotube welded carbon fibers and
composites. J Ind Text 2015; 45: 199–221. evaluation of the interfacial strength in epoxy composites.
47. Yong V and Hahn HT. Processing and properties of J Appl Polym Sci 2017; 134: 45027–45033.
SiC/vinyl ester nanocomposites. Nanotech 2004; 15: 62. Wang Y, Pillai SKR, Che J, et al. High interlaminar shear
1338–1343. strength enhancement of carbon fiber/epoxy composite
48. Patnaik A, Satapathy A, Mahapatra SS, et al. through fiber-and matrix-anchored carbon nanotube net-
A comparative study on different ceramic fillers affecting works. ACS Appl Mater Interfaces 2017; 9: 89608966.
mechanical properties of glass-polyester composites. 63. Beylergil B, Tanoglu M and Aktas E. Enhancement of
J Reinf Plast Compos 2009; 28: 1305–1318. interlaminar fracture toughness of carbon fiber–epoxy
49. Wichmann MHG, Sumfleth J, Gojny FH, et al. Glass– composites using polyamide-6,6 electrospun nanofibers.
fibre-reinforced composites with enhanced mechanical J Appl Polym Sci 2017; 134: 45244–45256.
and electrical properties–benefits and limitations of a 64. www.nanothinx.com/raw-cnts-in-powder-form/; 2017
nanoparticle modified matrix. Eng Fract Mech 2006; 73: (accessed 10 March 2018).
2346–2359. 65. Lehman JH, Terrones M, Mansfield E, et al. Evaluating
50. Zhang Y, Zhang L, Liu Y, et al. Oxidation effects on the characteristics of multiwall carbon nanotubes: review.
in-plane and interlaminar shear strengths of two- Carbon 2011; 49: 2581–2602.
dimensional carbon fiber reinforced silicon carbide com- 66. Bilisik K, Karaduman NS and Sapanci E. Flexural
posite. Carbon 2016; 98: 144–156. characterization of 3D prepreg/stitched carbon/epoxy/
51. Zhang Y, Zhang L, Yin X, et al. Effects of porosity multiwall carbon nanotube preforms and composites.
on in-plane and interlaminar shear strengths of J Compos Mater 2019; 53: 563–577.
Bilisik et al. 19
67. Bilisik K, Karaduman NS, Erdogan G, et al. In-plane 70. ASTM D 2734-91:1991. Standard test methods for void
shear of nanoprepreg/nanostitched three dimensional content of reinforced plastics.
carbon/epoxy multiwall carbon nanotubes composites. 71. ASTM D2344-13:2013. Standard test method for short-
J Compos Mater. Epub ahead of print 5 April 2019. beam strength of polymer matrix composite materials
DOI: 10.1177/0021998319841671. and their laminates.
68. ASTM D792-91:1991. Standard test method for density 72. Adams DF, Carlsson LA and Pipes RB. Experimental
and specific gravity (relative density) of plastics by characterization of advanced composite materials.
displacement. New York: CRC Press, 2003.
69. ASTM D3171-99:1999. Standard test methods for con-
stituent content of composite materials.