Composites Part B 103 (2016) 113e121

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

Mechanical properties of carbon nanotubes based polymer composites

M. Tarfaoui a, K. Lafdi b, A. El Moumen a, *
a
b

ENSTA Bretagne, FRE CNRS 3744, IRDL, F-29200 Brest, France

University of Dayton Research Institute, Dayton, OH 45469-0168, United States

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 1 April 2016
Received in revised form
8 June 2016
Accepted 17 August 2016
Available online 19 August 2016

The objective of this paper was to understand the effect of carbon nanotubes (CNT) additives on the
elastic behaviors of textile based composites. The materials consist of three phases namely, carbon bers
fabric, Epoxy matrix and carbon nanotubes. Different volume fractions of CNTs were used (0% as reference, 0.5%, 1%, 2% and 4%). A set of mechanical tests as Open Hole Tension, shear Beam Test and Flatwise
Tension tests were performed. A damage initiation and cracks propagation in composite specimens were
controlled. The experimental results show an increase the mechanical performance of the composite up
to 2% of CNT additives. However, beyond this value, the material strength shows a signicant decay.
2016 Elsevier Ltd. All rights reserved.

Keywords:
Carbon-carbon composites
Polymer-matrix composites
Mechanical properties
Laminates
Carbon nanotubes

1. Introduction
Carbon nanotubes (CNTs) reinforced textile composites are a
promising new class of composite materials nding their use in
some military and aerospace applications. Consequently, the use of
CNTs in polymers has attracted wide attention [1,2], because their
excellent mechanical, electrical, thermal and structural properties.
Especially, it has been addressed that CNTs have outstanding a great
Young's modulus, thermal and electrical conductivity [3]. For mechanical properties, previous studies, see for example [4e7], show
that the Young's modulus ranging from 600 to 1.4 TPa and tensile
strength from 10 to 200 GPa. It should be mentioned that the
measured properties of CNTs depending on the size and structure of
nanotubes.
Studies on the mechanical properties of the composite based
CNTs were carried out [8e10]. A review paper has been published
on this subject [11]. Depending on the matrix class, a wide variety of
composite materials based CNTs have been manufactured and
characterized. For example, Peigney et al. [12] and Zhan et al. [13]
have fabricated some specimens of CNTs reinforced ceramic resin
and Milo et al. [14] and Qian et al. [15] have embedded CNTs in
polymer matrix. Others works have interested to metallic composites containing aligned and non-aligned CNTs.

* Corresponding author.
E-mail address: ahmed.el_moumen@ensta-bretagne.fr (A. El Moumen).
http://dx.doi.org/10.1016/j.compositesb.2016.08.016
1359-8368/ 2016 Elsevier Ltd. All rights reserved.

The experimental measurement of elastic moduli of composites

based CNTs shows that there is an increase in the composite
modulus over the pristine matrix modulus. Qian et al. [15] have
shown that the added of a few per cent of CNTs (about of 1 wt%) in a
matrix material, the stiffness of a resulting composite can increase
between 36% and 42% and the tensile strength by 25%. Schadeler
et al. [16] found a 40% increase in the effective stiffness of Epoxy
resin with 5 wt % of CNTs. The stress strain curve of Epoxy resin
with CNTs has been observed by Zhu et al. [17] for 1 and 4 wt%. For
these weight fractions, the authors found an increase of 30e70% in
the elastic moduli. Composites based CNTs is one of the most
promising applications have been studied. A review paper has been
published on the subject [18]. Recently, in a series of papers, Baretta
et al. [19e22] have been interested to modeling and characterization of nanobeams and nanorods materials and the CNTs based
polymer using a new gradient elasticity model. It is noted that there
is very little works related to CNTs reinforced laminate composites.
In this work, we develop experimental techniques to estimate
mechanical behavior of textile composites reinforced with CNTs,
and their effect on elastic properties. First, different specimens with
different volume fractions ranging from 0% to 4% were prepared
Second, using Open Hole Tension (OHT), Shear Bear Tension (SBT)
and Flatwise Tension Test (FTT), the elastic moduli of textile composites with and without CNTs are characterized.
This is the main contribution of the paper. Indeed, while most of
papers dealing only with the prediction of elastic properties and
damage propagation of CNTs/polymer, CNTs/metallic or CNTs/

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M. Tarfaoui et al. / Composites Part B 103 (2016) 113e121

ceramic composites. In the present work we investigate the case of

textile composites using experimental techniques. We will focus in
this paper to the mechanical performance of the composite
without/with CNT through an analysis of the mechanical response

in terms of the evolution of the maximum force and the equivalent

stiffness of the material for the different cases considered. Special
attention is given to the analysis of the development of damage in
these materials for these tests.

Table 1
Material properties.

2. Materials

Carbon ber
E11 (GPa)
E22 (GPa)
E33 (GPa)
v12
v13
v23
G12 (GPa)
G13 (GPa)
G23 (GPa)

Epoxy matrix
230
15
15
0,28
0,28
0,28
15
15
15

E11 (GPa)
E22 (GPa)
E33 (GPa)
v12
v13
v23
G12 (GPa)
G13 (GPa)
G23 (GPa)

CNT
2,72
2,72
2,72
0,3
0,3
0,3
1,18
1,18
1,18

E (GPa)
v

500
0,261

In this study composites consist of three phase materials: Epon

862 Epoxy Resin (phase 1), in which fraction of CNTs was added
between 0 and 4% by weight (phase 2). The composite resulting
from mixing of phases 1 and 2 went through a is considered as
second matrix reinforced with T300 6k carbon bers fabric (phase
3). All panels fabricated with 5-Harness satin weave fabric using
infusion process. Each panel consisted of 12 layers of carbon ber
fabric (satin) interleaved with 12 layers of epoxy lm with a target
ber volume of 50%. Panels were press cured according to

Fig. 1. Microscopic observation of a specimen, 4% CNT.

Fig. 2. Manufactured panels and specimens for mechanical testing.

M. Tarfaoui et al. / Composites Part B 103 (2016) 113e121

manufacturer's cure cycle under a pressure of 200 MPa. After the

panels had cooled, they were prepared for mechanical testing. Final
panel thickness is nominally 4 mm. The mechanical properties of
these materials are shown in Table 1.
The resin lm between plies ows into the ply during fabrication process. We have used, ASTM D5766 for Open Hole Tension at
room temperature, ASTM D7291 for interlaminar tension room
temperature and hot-wet (180
F and 100% Humidity) and ASTM
D2344 for interlaminar shear room temperature and hot-wet
(180
F and 100% Humidity). Fig. 1 gives an accurate SEM nanomorphologies of investigated panel composites. Therefore, it appears that the CNTs are randomly distributed in the matrix.
Specimen dimensions are prepared for testing as follows in
L  W  T format. Where L is the length, W the width and T is the
thickness of the specimen.
 Open Hole Tensile test (OHT): L 300 mm, W 38 mm,
T 4.1 mm
 Short Beam Shear (SBS): L 25,4 mm, W 8.128 mm,
T 4.1 mm
 Flatwise Tension (FWT): L 25,4 mm, W 25.4 mm, T 4.1 mm
An example of the manufactured panel and specimens for mechanical testing is presented on Fig. 2.

3. Tests procedure and experimental results

3.1. Open hole tension test (OHT)
An experimental study was carried out to determine the open
hole tension (OHT) characteristics of carbon ber-reinforced plastic

115

(CFRP) with different carbon nanotubes volume fraction (CNT).

Tests to failure and percentages of ultimate load were carried out
and CNTs volume fraction effects were evaluated. An experimental
test series was carried out to determine the ultimate strength and
stiffness of a CFRP/CNT.
The geometry of the tensile hole in plate specimen is shown in
Fig. 3. The specimen dimensions are the same as the standard
tensile test, but the specimen has a 6.25 mm hole drilled at the
middle, to act as a stress concentrator. Strain was measured using
an extensometer across a 220 mm gauge length of the specimen.
Specimens were tested at a displacement rate of 2 mm/min.
Specimens are placed in the grips of Instron test machine and
pulled until failure. Open Hole Tension ASTM D5766 is a mechanical
test that measures the force required to break a composite specimens with hole. All specimens (ASTM D5766) have a constant
rectangular cross section. Specimens that were bonded with Hysol
4800, conditioned at 180 F (82.22
C) and 95% Humidity for two
weeks, then dried for 2 weeks.
Specimens with ve volume fractions (0%, 0.5%, 1%, 2% and 4%) of
CNTs have been tested. For each volume fraction, three specimens
were considered and the mean values of the mechanical properties
were recorded. Fig. 4 shows a typical experimental loaddisplacement curves, of different specimens, obtained using Open
Hole test for each volume fractions. Good reproducibility of tests is
noted for the different CNT %. The general tendency is that the force
level is increased by the addition of minor amount of CNTs which
play the role of reinforcement and decrease in the case of 4% of CNTs.
However, at higher CNTs%, the CNT tends to agglomerate and behave
like an inclusion defect. Conversely, all curves of CNTs reinforced
composites have the same tendency and show reproducible results.
To deduce a better view of the effect of CNTs on the elastic

Fig. 3. Manufactured specimens for Open Hole Tension using Instron.

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M. Tarfaoui et al. / Composites Part B 103 (2016) 113e121

Fig. 4. Tensile hole in plate test results of Carbon/Epoxy-NTC composites.

M. Tarfaoui et al. / Composites Part B 103 (2016) 113e121

117

fraction. This decay was noticeable due to the presence of porosities

and CNTs aggregates.
We have also tried to highlight the inuence of the addition of
carbon nanotubes on the mechanical response of the material in
terms of maximum force and stiffness of the composite. Fig. 5
shows the average maximum force versus CNT volume fraction.
IT seems that adding CNTs does not seem to have any inuence
on the maximum force, we can still note that for 2% this is slightly
increased. A percentage of 0.5% leads to a drop of the effort, which
can be interpreted by the fact that the CNTs are seen as defects.
As shown in Fig. 6 that the slope of the curves, ie the elastic
portion is lower for samples containing carbon nanotubes that the
specimens without CNTs. In general, taking into account the standard deviation, the stiffness is almost constant for all specimens.
However, the stiffness decreases when the percentage of the CNTs
increases, which causes the decrease in mechanical performance.
Tables 2 and 3 give a summary of the results presented above.
Thus it is possible to conclude that from an experimental point
of view, in the case of Open Hole Tension tests, the contribution of
the CNT is not considerable.

Fig. 5. Maximum force vs. CNTs volume fraction, OHT.

3.2. Short Beam Shear (SBS)

Fig. 6. Stiffness vs. CNTs volume fraction, OHT.

Table 2
Stiffness versus CNTs volume fraction, OHT.
%CNT

0,5

Average Stiffness (kN/mm)

Standard deviation (kN/mm)

10,16
0,14

9,94
0,30

9,876
0,39

9,71
0,43

9,37
0,38

Table 3
Maximum load versus % CNTs volume fraction, OHT.
%CNT

0,5

Average Fmax (kN)

Standard deviation (kN)

67,30
1,12

62,10
0,96

66,72
1,24

69,45
3,15

66,14
1,19

moduli of the textile composites, the maximum force and the

specimen stiffness obtained at each volume fraction were determined. Histograms presented on Fig. 5 illustrate the evolution of
the maximum force and the director coefcient as a function of
CNTs volume fraction. It should be noted that the director coefcient represents the Young's modulus of the specimens. The
maximum value is obtained in the case of 1% of CNTs. However,
mechanical properties decay was observed at 4% of CNTs volume

The short-beam shear test has become a widely used method for
characterizing the interlaminar failure resistance of ber reinforced
composites. This test method involves loading a beam under threepoint bending with the dimensions such that an interlaminar shear
failure is inducted. The simplicity of the test method makes it very
popular materials screening tool.as pointed out in the title of ASTM
Standard D-2344, this method measures the apparent interlaminar
shear strength of composite materials.
As the ASTM D 2344 standard prescribes, a specimens with
L 25,4 mm, W 8.128 mm and T 4.1 mm has been used. The
schematic presentation of considered specimen dimensions and
machine tests were given on Fig. 7. The specimens were placed on
the two 3 mm diameter supports. Not that, span between supports
is xed for all the tests. The carbon ber of the specimen should be
aligned with the longitudinal axis of the specimen.
The indenter has a nominal outer diameter of 6 mm and is made
of steel. The specimen is placed on a horizontal shear test xture,
Fig. 7b. The loading is then used to ex the specimen at a speed of
1.2 mm/min until total fracture. Displacement of the specimen was
measured from the movement of the loading head through the use
of displacement gauge.
For reproducibility, tests were realized on 10 specimens for
each volume fraction. Then 50 samples were tested. For this test,
the evolution of experimental results as a function of the CNTs
volume fraction is presented on Fig. 8. The mean value of the
considered cases is also determined and presented on Figs. 9 and
10. It appears that, the curves of textile composites containing
CNTs demonstrate a good correspondence compared to the case
of baseline (0%-CNTs). Also the curves of same volume fractions
have same tendency. Fig. 10 shows that the adding of minor
CNTs amounts less than 2% improves the mechanical properties
of textile composites. However, at 4% of CNTs volume fraction
there is a considerable drop of properties. The average value of
maximum load and stiffness versus volume fractions is calculated and plotted, Figs. 9 and 10. Moreover, it appears the
important drop and degradation of the properties for 4% of CNTs.
The same phenomenon of OHT test was observed for this test.
The general tendency is that CNTs play the role of reinforcement
is some cases, lower volume fractions, but also a defect in other
cases.
Tables 4 and 5 summaries the results presented above.

Fig. 7. Schematic and experimental shear test rig.

Fig. 8. Short Beam Shear test results of Carbon/Epoxy-NTC.

M. Tarfaoui et al. / Composites Part B 103 (2016) 113e121

119

Fig. 11. Flatwise Tension conguration and dimensions using Instron machine.

Fig. 9. Stiffness vs. CNTs volume fraction, SBS.

Fig. 10. Maximum force vs. CNTs volume fraction, SBS.

Table 4
Average Stiffness versus CNTs volume fraction, SBS.
%CNT

0,5

Stiffness (kN/mm)
Standard deviation (kN/mm)

5,37
0,2506

5,52
0,1547

5,65
0,1279

5,29
0,1793

4,57
0,3904

Table 5
Average Fmax versus % CNT, SBS.
%CNT

0,5

Fmax (kN)
Standard deviation (kN)

1,72
0,0953

1,75
0,0735

1,91
0,0792

1,68
0,0592

1,04
0,1030

3.3. Flatwise tensile test (FWT)

The Flatwise Tension (FWT) Test is used to measure the out-ofplane strength of composite laminates. Typically, in this test, solid
tabs are bonded to opposite faces of a at sample from a composite
laminate and the sample is loaded in a direction normal to the
plane of the laminate, Fig. 11. In some cases, a thick specimen is
manufactured and machined in order to produce a tapered section,

ensuring that failure will occur in that region. Several different

sample geometries have been used with the Flatwise Tension Test
to characterize the out-of-plane strength of composite laminates
[23,24]. The purpose of this section is to evaluate the contribution
of CNT on out-of-plane strength of composite materials with
nanotubes of carbon. ASTM D7291 is a more standard test used for
Flatwise tensile test. The composite samples tested had a dimension of 25.4  25.4  4 mm. All of the specimens were bonded to
ends tabs with metal material. Tensile specimens were bonded to
grit blasted aluminum loading blocks with Loctite H4800 structural
adhesive. The bonded assembly is loaded under tension in the
thickness direction. Specimens are loaded under a constant crosshead displacement of 0.1 mm/min Fig. 11 shows a picture of used
materials and machine xture.
Five tests were realized for each volume fraction. Typical loaddisplacement curves obtained for each case are listed on Fig. 12.
Regarding the reproducibility of the tests, we can say that there is a
fairly good reproducibility especially for the linear part. It can be
seen that the samples containing 2% CNT may allow a greater
maximum force, 15 kN. A signicant drop in the maximum load is
denoted by 4% CNTs, 8.5 kN. We can also say that the failure
mechanism is fragile for all samples; it is indicated by a sudden
drop of the load.
The stiffness of the various categories of specimens increases
with increasing CNTs volume fraction up to 2% which was a signicant drop in this setting. The average maximum stiffness is
recorded for 1% of CNT, Fig. 13.
Regarding the average maximum effort, we have recorded an
increase with increasing CNT up to 2%, 15 kN, then a fall to 8,8 kN for
4%, Fig. 14.
It appears that the maximum effort is found in the case of
specimens with 2% of CNTs. The maximum force has increased
nearly 50% by the addition of 2% of CNTs. In order to determine the
real effect of CNTs embedded textile composites, the director coefcient (stiffness) and the maximum force of each curve are
determined, Figs. 13 and 14. However, CNTs embedded textile
composite samples, especially for 2% of volume fraction, failed at a
much higher level than the case of samples without or containing
much CNTs amounts. Compared to results of previous tests,
important amount of CNTs degrade mechanical properties.
Tables 6 and 7 summaries the results presented above.
From results of all tests, it can be seen that the reinforcement
role is much reduced in the case of 4% CNTs volume fraction.
The same phenomenon was observed for stiffness and maximum
force. This can be related to CNTs distributions and may be
also the existence of porosity is some specimens. We conclude
on the existence of CNT critical volume fraction threshold for
which properties and mechanical performance are greatly
reduced.

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M. Tarfaoui et al. / Composites Part B 103 (2016) 113e121

Fig. 12. Flatwise tension test results of Carbon/Epoxy-NTC composites.

M. Tarfaoui et al. / Composites Part B 103 (2016) 113e121

121

properties. The degree of CNT dispersion and agglomeration was

observed in the case 4% of CNTs volume fraction. At high CNT
concentration, the nanocomposites viscosity had increases drastically and during the composite fabrication process, air bubble tend
to get trapped leading to the formation of porosity which has a
major effect on mechanical properties reduction.
Acknowledgments
ne
rale de l'armeThis work was funded by DGA (Direction ge
ment - Ministry of Defense), MRIS project: Study of composites
reinforced by carbon nanotubes (CNT). The Authors of this paper
gratefully acknowledge the nancial support of the DGA, France.
Acknowledgments have also addressed to Pr. Bruno Mortaigne and
Dr. Nickerson William from DGA and Ofce of Naval Research,
respectively.
Fig. 13. Stiffness vs. CNTs volume fraction, FWT.

References

Fig. 14. Maximum force vs. CNTs volume fraction, FWT.

Table 6
Stiffness versus % CNT, FWT.
%CNT

0,5

Stiffness (kN/mm)
Standard deviation (kN/mm)

13,88
1,0526

14,24
1,2501

14,39
0,5212

11,84
0,8334

14,11
0,6794

Table 7
Maximum load versus % CNT, FWT.
%CNT

0,5

Fmax (kN)
Standard deviation (kN)

10,58
0,9076

10,01
0,9582

12,50
0,9435

15,30
1,2934

8,81
1,1069

4. Conclusions
In this paper, the effect CNTs added into traditional polymer mix
based composites studied. Small CNT concentration can alter
considerably the mechanical behavior of composites. Considerable
improvement has been obtained in the case of lower CNTs volume
fractions. The critical volume fractions threshold was estimated to
be between 0.5% and 2% of CNTs reinforced textile composites. The
decrease and degradation of the mechanical behavior for 4% can be
explained by the effect of CNTs distributions and the existence of an
upper limit which starts from 2%. CNT dispersion and close porosity
of the composite plays a central role for the ultimate mechanical

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