Composites: Part A 43 (2012) 1620–1627

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Composites: Part A
journal homepage: www.elsevier.com/locate/compositesa

Effect of CNT functionalization on crack resistance of a carbon/epoxy composite

at a cryogenic temperature
Myung-Gon Kim, Jin-Bum Moon, Chun-Gon Kim ⇑
Department of Aerospace Engineering, KAIST 373-1 Guseong-dong, Yuseong-gu, Daejeon 305-701, Republic of Korea

a r t i c l e i n f o a b s t r a c t

Article history: In this study, the authors attempted to enhance the crack resistance of a carbon/epoxy composite by add-
Received 4 January 2012 ing carbon nanotubes (CNTs) into the resin formulation. Prior to applying CNTs, a chemical surface treat-
Received in revised form 18 March 2012 ment, amino-functionalization, was conducted to enhance the interfacial bonding between CNTs and
Accepted 1 April 2012
epoxy resin. The resultant increase in tensile strength was attributed to good interfacial bonding quality.
Available online 6 April 2012
Two kinds of 3-phase carbon/CNT-epoxy unidirectional prepregs were fabricated via a hot-melting pro-
cess with the addition of CNTs. The CNT-reinforcing and -functionalizing effects were investigated
Keywords:
through DCB tests and measurement of the acoustic emission (AE) signal of a cross-ply specimen both
A. Polymer–matrix composites (PMCs)
B. Thermal properties
at RT and at 150 °C. The carbon/epoxy composite containing functionalized-CNTs showed improved
D. Acoustic emission interlaminar fracture toughness and transverse crack resistance at the cryogenic temperature.
D. Mechanical testing Ó 2012 Published by Elsevier Ltd.

1. Introduction
Epoxy resins have been widely used as polymer matrices for fi-
ber reinforced composites due to their excellent mechanical prop-
erties. Their brittle characteristics, however, may bring about low
fracture toughness against crack-induced fracture. For instance,
when the composites are used for spacecraft structures, i.e., satel-
lites or cryogenic tanks of launch vehicles, the toughness degrada-
tion induced by low temperatures can lead to structural damages
in the form of microcracks or delamination [1,2].
One promising technique to enhance the fracture toughness is
to apply nano-sized rigid fillers into polymer matrices, a potential
alternative to the use of toughened resin. The crack resistance
mechanism can be realized through nanofiller pull-out or breaking
as well as crack-deflection, -pining, or -blunting during crack
propagation.
Epoxy resins incorporated with alumina [3] and clay [4,5] nano-
particles have shown enhanced crack growth resistance when
applied in fiber reinforced composites. In particular, carbon nano-
tubes (CNTs), applied as a nanofiller, have exceptional mechanical
properties as well as a high aspect ratio with large specific surface
area, making them a promising reinforcing material for polymer
matrix composites [6]. Some previous works reported that CNTs
can be employed as an alternative reinforcing filler to enhance not
only mechanical properties but also crack growth resistance, as they
⇑ Corresponding author. Tel.: +82 42 869 3719; fax: +82 42 869 3710.
E-mail address: cgkim@kaist.ac.kr (C.-G. Kim).
can serve as bridges between crack surfaces and induce mechanical
interlocking with the matrix material [7–9]. Recently, it was also
proposed that a combination of a CNT-modified matrix together
with conventional fiber-reinforcements can lead to improved ma-
trix dominated properties such as interlaminar shear strength
[10]. Consequently, the use of CNTs as the second reinforcement
of carbon fiber composites is expected to provide enhanced tough-
ness at cryogenic temperatures.
In this study, an attempt to improve the crack resistance of a
carbon/epoxy composite is performed by adding CNTs into the
resin formulation. Prior to applying CNTs, a chemical surface treat-
ment, called amino-functionalization, is conducted to enhance the
interfacial bonding between CNTs and epoxy resin. As a conse-
quence, two kinds of 3-phase carbon/CNT-epoxy unidirectional
prepregs are fabricated. Investigations of the CNT-reinforcing and
functionalizing effects are conducted through DCB tests and mea-
surement of the AE signal of a cross-ply specimen both at RT and
at 150 °C has been done.
2. Chemical surface treatment of CNTs
2.1. Amino-functionalization process
Carbon nanotubes have inherently low bending stiffness and
weak interaction with polymer phases, which results in strong
intermolecular interaction between individual nanotubes. Thus,
this nature is attributed to excessive agglomeration. Therefore,
control over the surface polarity and the resulting interactive force

1359-835X/$ - see front matter Ó 2012 Published by Elsevier Ltd.

http://dx.doi.org/10.1016/j.compositesa.2012.04.001
 M.-G. Kim et al. / Composites: Part A 43 (2012) 1620–1627 1621

between CNTs and polymer phase is necessary. In this study, a
chemical surface treatment called amino-functionalization was
employed to enhance the interfacial bonding between CNTs and
an epoxy matrix as well as the dispersibility of CNTs. Amino-func-
tionalization is used to introduce reactive groups on the surface of
CNTs to form covalent bonds between the reactive groups and the
epoxides [9]. Carbon nanotubes synthesized via a chemical vapor
deposition method show a relatively high degree of purity, but
there are also impurities such as metal catalysts, and amorphous
carbon. Therefore, an acid treatment was adopted to remove the
impurities as well as to introduce chemical functional groups.
Multi-walled carbon nanotubes (CM-95, Iljin Nanotech Co., Kor-
ea) were immersed into a mixture of 3:1 sulfuric (H2SO4, 98%)/ni-
tric (HNO3, 68%) acids with a ratio of 1 g:250 ml, respectively, and
the solution was subsequently sonicated with a frequency of
40 kHz at 60 °C for 1 h. The above solution was then diluted with
de-ionized water under magnetic agitation for 12 h. Filtration
using PETE membrane filters having 0.47 lm hole-diameter was
conducted using a vacuum pump to filtrate CNTs out of the solu-
tion. Finally, subsequent to heat treatment in a 400 °C furnace,
CNT powders were obtained by pounding the CNT lumps. After
the acid treatment of the CNTs, amino-functionalization using tri-
ethylenetetramine (TETA) was conducted. TETA is expected to
form amide bonds with a carboxylic group generated after the acid
treatment [10,11]. The oxidized CNTs were immersed into TETA
with a ratio of 1 mg:1 ml and sonicated at 60 °C for 1 h. The solu-
tion was magnetically agitated at 120 °C for 24 h. After that, the
solution was mixed with excess acetone and filtrated using mem-
brane filters. Finally, subsequent to evaporation of the acetone in
an oven overnight, CNT powders were obtained by pounding the
functionalized CNT lumps.
The molecular structures of chemically treated CNTs were char-
acterized through FT-IR spectroscopy. As shown in Fig. 1a, the peak
at 1707 cm 1 is due to the C@O bond, which means that a ACOOH
functional group was generated on the CNT surface after the acid
treatment. Furthermore, amino-functionalization could be ex-
pected with an amide-I bond (CAN) and amide-II bond (C@O),
and the two peaks representing the amide bonds are observed after
only functionalized CNTs in Fig. 1b.
2.2. Tensile properties of CNT-epoxy nanocomposites
2.2.1. Specimen preparation
Tensile tests were performed in order to investigate the effect of
chemical treatment and the addition of CNTs on the tensile proper-
ties of epoxy specimens. The test procedure followed the ASTM
D638 test method. The fabrication process for the CNT-epoxy spec-
imens is as follows: first, the functionalized CNTs were immersed
into acetone solvent, and then sonicated with a frequency of
40 kHz at 40 °C for 3 h. The solution was subsequently mixed with
pre-heated bisphenol-A type epoxy resin (YD-128, Kukdo Chem.
Co., Korea) according to the weight percent of CNTs, and thereafter
sonicated at 60 °C for 1 h. The mixture was then placed in an oven
for 72 h to evaporate the solvent. After the evaporation process, the
epoxy resin containing CNTs was mixed with a pre-heated aro-
matic hardener (TH-431, Kukdo Chem. Co., Korea) through
mechanical stirring for 10 min. The mixing ratio of epoxy resin
and hardener was 5:3 in their weight percent, respectively. Finally,
the mixture was poured into a silicon-rubber casting mold and
subsequently cured in an autoclave at 80 °C under 7 atm for 4 h.

As-received 2.2.2. Tensile properties

(a) After Oxidization
Fig. 2 compares the tensile strength of the epoxy based speci-
After Functionalization
mens with the chemical treatment of CNTs. The specimens were
-1
1715Cm fabricated by adding CNTs in a quantity of 0.2% of the total weight
of epoxy and hardener. From the results, it is found that the tensile
Absorbance

-1
strength of the epoxy specimen increased when CNTs were added
1707Cm
but showed different values according to the chemical treatment.
The epoxy specimen with functionalized CNTs showed the highest
strength among the candidates, constituting an 18.5% and 8.6% in-
creases compared to pure epoxy and an as-received CNT added
specimen, respectively.
Fig. 3 shows SEM (20 k) and optical microscope (50) images
of the fracture surfaces of the specimens. From the microscopic
images, smooth rive marks are observed on the fractured surface
1680 1700 1720 1740 1760 1780 1800
-1
Frequency (cm )
80

(b) amide II bond amide I bond 70

-1
1572cm -1
Tensile Strength (MPa)

1669cm
60

50
Absorbance

As-received
After Oxidization 40
After Functionalization
30

20

10

0
Pure Oxidized Funtionalized As-recieved
Epoxy CNT-Epoxy CNT-Epoxy CNT-Epoxy
1500 1530 1560 1590 1620 1650 1680 1710
-1
Frequency (cm ) Fig. 2. Tensile strengths of the epoxy based specimens according to the chemical
treatment of CNTs. (For interpretation of the references to color in this figure
Fig. 1. FT-IR spectra of the chemically treated CNTs. legend, the reader is referred to the web version of this article.)
1622 M.-G. Kim et al. / Composites: Part A 43 (2012) 1620–1627

(a) Pure epoxy

(b) As-received CNT-epoxy

(c) Functionalized CNT-epoxy

Fig. 3. Microscope and SEM images of the fracture surfaces. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this
article.)

of the pure epoxy specimen where many microcracks with dim-
pled patterns can be seen on the CNT-added specimens. It can be
inferred that, during fracture, more energy absorbed by the gener-
ation of numerous microcracks dissipated in the CNT-added spec-
imens compared to the case of the pure epoxy specimen. In
addition, when comparing the SEM images of the CNT-added spec-
imens, it is found that the CNTs in the functionalized CNT-epoxy
specimen were broken instead of being pulled out of the epoxy ma-
trix. Consequently, it is confirmed that interfacial bonding quality
was enhanced through functionalization of CNTs.
Tensile strength and stiffness of the epoxy specimen were
investigated with the addition of functionalized CNTs, and the re-
sults are shown in Fig. 4. The highest strength and stiffness are
found when CNTs were loaded by 0.7 wt%, and the values of
strength and stiffness are increased by 18.5% and 9.2% relative to
the epoxy specimen, respectively.
3. Fracture characteristics of carbon/CNT-epoxy composites
3.1. Mode-I interlaminar fracture toughness
3.1.1. Fabrication of the prepregs
In this study, two kinds of unidirectional (UD) prepregs were
fabricated to investigate the CNT-reinforcing and -functionalizing
effects on fracture characteristics of composites at a cryogenic
temperature. A T700-carbon/epoxy UD prepreg (CU125NS, Hankuk
Fiber Glass Co., Korea) was designated as the controlled material.
Multi-walled carbon nanotubes were added into the resin mixture
in a quantity of 0.7 wt% of the total weight of epoxy and hardener.
The fabrication process for the CNT-added prepregs is as fol-
lows: first, the nanotubes were directly poured into an epoxy resin
composed of phenolic novolac and bisphenol-A type epoxy, and
the mixture was then stirred with a direct driven at 80 °C for 4 h.
A hardening agent, aliphatic polyamine dicyandiamide (DICY),
was subsequently mixed into the blend, and stirring was thereafter
conducted for 15 min. Finally, the CNT-added carbon/epoxy pre-
pregs were fabricated by way of a hot-melting process. Table 1
shows the fabricated prepreg systems and their designation in this
paper.
3.1.2. Test procedure
The toughness variation according to CNT addition was investi-
gated through a comparison of mode-I interlaminar fracture tough-
ness of the laminated composites using a double cantilever beam
(DCB) test. Fig. 5 shows the configuration of the DCB specimen
and cryogenic test setup. The specimen configuration and test pro-
cedure were in accordance with the ASTM D5528 test method. Each
laminate of the prepregs was stacked with [0]40T, respectively. In
 M.-G. Kim et al. / Composites: Part A 43 (2012) 1620–1627 1623

80 3.1.3. Results and discussion

Typical load–displacement curves were obtained from the DCB
70
tests at 150 °C, as shown in Fig. 6a. It is found that the load–dis-
Tensile Strength (MPa)

60 placement curves show many sudden load-drops in their history at

the cryogenic temperature, which results from unstable delamina-
50
tion growth [11]. The carbon/FCNT-epoxy containing chemically
40 treated CNTs shows the highest maximum load among the candi-
dates. Fig. 6b shows variations of strain energy release rates (GI)
30 calculated from the measured data, i.e., load, displacement, and
20 crack length [12]. The carbon/epoxy composite, the control, shows
unstable crack growth throughout the test. This behavior resulted
10 from a reduction of the fiber bridging effect and a decrease of the
0 process zone in the wake of the crack surfaces at cryogenic temper-
0.0 0.2 0.7 1.0 ature [11]. A stable resistance curve, however, can be observed in
CNT wt% the carbon/FCNT-epoxy composite, in contrast to the other mate-
rial systems. Consequently, it can be considered that nanotube
4.0 bridging was realized on the fracture surfaces when mode-I load
was applied.
3.5
Matrix-cracking or delamination may occur at cryogenic tem-
Tensile Stiffness (GPa)

3.0 perature even with a low-load level due to matrix embrittlement

and thermally induced stresses in a structure. Therefore, relaxation
2.5
of the crack propagation would be a more efficient means of apply-
2.0 ing composites for cryogenic use. In a point of this technical ap-
proach, in this study, mode-I interlaminar fracture toughness was
1.5
compared in terms of strain energy release rate in the unstable
1.0 crack propagation region. Fig. 7 shows the average strain energy
release rates of each material system. The CNT-added composites
0.5
generally show a higher strain energy release rate than that of
0.0 the control. Moreover, the carbon/FCNT-epoxy composite shows
0.0 0.2 0.7 1.0 the highest value, which is by 82% higher than that of the control
CNT wt% and 36% higher than that of the carbon/AsCNT-epoxy. Therefore,
it can be considered that employing CNTs as a nanofiller and utiliz-
Fig. 4. Tensile properties of CNT-epoxy as the weight percent of CNTs. (For
ing functionalized CNTs are effective strategies to obtain high frac-
interpretation of the references to color in this figure legend, the reader is referred
to the web version of this article.)
ture toughness at cryogenic temperature.

3.1.4. Fracture morphology

Table 1
Prepreg systems and their designation.
Fiber/resin type Nanofiller
T700/epoxy N/A
T700/epoxy As-received CNT
T700/epoxy Functionalized CNT
order to form an initiation site for delamination, a non-adhesive
insert (Teflon film A4000, Airtech International Inc.) having a thick-
ness of 25 lm was inserted in the mid-plane of the laminate during
the lay-up. In addition, white color paint was sprayed on the side
face of the DCB specimens, and then plotting paper was attached
to clearly observe the crack propagation during the test. Five or
more specimens are tested in each test.
In this study, an environmental test chamber was used to
simulate a cryogenic environment. The temperature of the envi-
ronmental chamber (Instron 3119-407) was lowered to 150 °C
by evaporating liquid nitrogen (LN2). The chamber was installed
on an Instron 4202 universal testing machine and sealed with an
insulating material. The DCB grips and loading bars of the appara-
tus were inserted into the chamber. The time needed to lower the
temperature generally depends on the pressure level of the vessel
containing the liquid medium. Accordingly, the use of a pressuriz-
ing device helped maintain an evaporating pressure of 1.5 atm
(22 psi) and kept the cooling time constant. In the DCB test, the
delamination growth length, which propagated during loading,
was monitored using a traveling optical microscope (magnification
of  40). In most cases, a resin rich area was found at the tip of the
insert of the DCB specimen, and therefore a pre-crack of 5 mm was
created before the test.
Fracture morphologies of the DCB specimens were observed by
scanning electron microscopy (SEM). Fig. 8a and b shows the frac-
Designation ture surfaces of a carbon/epoxy specimen and carbon/FCNT-epoxy
specimen after the cryogenic test, respectively. It is observed that
The control
Carbon/AsCNT-epoxy the controlled specimen shows smooth crack surfaces while the
Carbon/FCNT-epoxy carbon/FCNT-epoxy specimen displays a relatively rougher frac-
ture surface. In addition, CNTs are observed near the rough regions
in the carbon/FCNT-epoxy specimen. Therefore, it is considered
that the rough fracture surface was caused by nanotubes, which
is evidence that high fracture energy dissipation occurred during
crack propagation [5].
Fig. 8c and d shows CNTs embedded in the fracture surface of
the carbon/AsCNT-epoxy specimen and carbon/FCNT-epoxy speci-
men, respectively. It is observed that the CNTs in the carbon/FCNT-
epoxy specimen are shortened or broken while CNTs in the carbon/
AsCNT-epoxy specimen appear as relatively long and pulled-out
nanotubes. Therefore, it is concluded that good interfacial bonds
between functionalized CNTs and the epoxy matrix was realized
in the 3-phase carbon/FCNT-epoxy composite.
3.2. Evaluation of matrix-cracking using acoustic emission
3.2.1. Test procedure
Specimens with cross-ply layups were tested to examine matrix
cracking characteristics by measuring acoustic emission (AE) sig-
nals. Laminated cross-ply specimens of the candidate materials
were fabricated with a sequence of [02/906]S.
Fig. 9 shows the specimen configuration and experimental
apparatus for the tensile test. On the front surface of the specimen,
a PZT sensor (C6, Fuji Ceramics Co., Japan) was bonded and an
1624 M.-G. Kim et al. / Composites: Part A 43 (2012) 1620–1627

Fig. 5. Configuration of the DCB specimen and the test setup. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this
article.)

350
(a) 80
2

Carbon/epoxy
Strain energy release rate GI J/m

Carbon/epoxy Carbon/AsCNT-epoxy
300
70 Carbon/AsCNT-epoxy Carbon/FCNT-epoxy
Carbon/FCNT-Epoxy
60 250

200
Load, P (N)

50

40 150

30 100

20 50

10
0
0
0 2 4 6 8 10 12 Fig. 7. Strain energy releases rates during steady-state crack propagation at
150 °C.
Displacement, δ (mm

electric strain gage (CFLA, TML, Japan) was attached on the back-
(b) side in order to measure the mechanical strain.
500
Test coupons were installed on an Instron 4206 multipurpose
Strain energy release rate GI J/m 2

Carbon/epoxy
Carbon/AsCNT-epoxy test machine equipped with an environmental test chamber. An
400 Carbon/FCNT-epoxy electric strain gage was excited by a conditioning amplifier and
connected to a digital storage oscilloscope with a PZT sensor, and
the triggered data were transferred to a signal-processing com-
300
puter using a GPIB interface. For data acquisition, the sampling fre-
quency and trigger level were set at 1 MHz scan rate and 0.01 V,
200 respectively. Before the cryogenic tests, matrix cracking signals de-
tected by the PZT sensor were stored continuously from RT to
150 °C. The tensile load was applied through displacement con-
100
trol and the moving rate was set at 1.0 mm/min.

0
50 60 70 80 90 100 110 120 130 3.2.2. Results and discussion
Crack length, a (mm) Crack resistant effects by CNTs against transverse failure of 90°
plies in the cross-ply specimen are the main concerns of this
Fig. 6. Typical loading responses and strain energy release at 150 °C. experiment. Therefore, energy levels of the AE counts were inves-
 M.-G. Kim et al. / Composites: Part A 43 (2012) 1620–1627
Fig. 8. SEM images of fracture surface of DCB specimens.
25 125
ESG
2 verse crack propagation, as it showed smaller strain jumps than
PZT
22
175
unit: mm
Fig. 9. Configuration of the specimen and experimental setup of the tensile test.
(For interpretation of the references to color in this figure legend, the reader is
referred to the web version of this article.)
tigated in a region of 1.0% strain of the stress–strain curves. Fig. 10
shows typical stress–strain responses and energy levels of each AE
signal during the tensile tests, both at RT and at 150 °C, respec-
tively. In the stress–strain curves of all the graphs, several strain
jumps are observed. The strain jumps represent the occurrence of
transverse failure of the 90° plies in cross-ply specimens caused by
matrix cracks.
Notably, it is found that there were several small strain jumps in
the case of the carbon/FCNT-epoxy specimens, whereas one or two
large strain jumps were found in the controlled specimens at both
temperatures. This indicates that the larger strain jumps reflect
bigger transverse failure of the 90° plies. The carbon/FCNT-epoxy
1625
composite thus showed superior crack resistance against trans-
those of the control. Moreover, at the cryogenic temperature, the
dominant strain jumps in carbon/FCNT-epoxy were observed at
higher stress levels than those in the control. This indicates that
progressive transverse failures occurred in spite of the high load
level.
As shown in Fig. 10, it is found that all of the specimens showed
high AE energy levels just before the transverse failure of the 90°
plies. Furthermore, both composites showed similar AE energy lev-
els and the time of occurrence of transverse failure RT in Fig. 10a
and b. It shows that the CNT nanofillers have a little effect on trans-
verse facture behavior of laminated composites at room tempera-
ture. On the other hand, the composites showed different AE
energy level behaviors at the cryogenic temperature, as shown in
Fig. 10c and d. It is observed that AE signals of the carbon/FCNT-
epoxy specimen show higher AE energy levels than those of the
control just prior to the first transverse failure of the 90° plies. This
result can be explained as follows. Fiber reinforced composites
usually present high AE energy levels when the fibers fracture.
Therefore, it could be concluded that the CNT nanofillers played
a similar role as that fulfilled by fibers, resulting in large energy
dissipation during the transverse failure. As a result, it is obviously
concluded the CNT nanofiller have a large effect on transverse fac-
ture behavior of composites at cryogenic temperature.
Fig. 11 shows SEM images of transversely fractured 90° ply-
surface of the carbon/FCNT-epoxy specimen. Broken CNTs (a)
and a rough fracture surface (b) are observed in Fig. 11, respec-
tively. Therefore, there is evidence that higher strain energy
was released to break the nanotubes or to bifurcate crack propa-
gating paths.
Finally, the energy levels of each AE signal showed higher val-
ues at cryogenic temperature than at RT. This means there were
large strain energy releases before the final failure of specimens,
which coincides with the ultimate stresses of the cross-ply speci-
mens. The average ultimate stresses of carbon/epoxy and carbon/
FCNT-epoxy were measured to be 476 MPa and 553 MPa at
150 °C, respectively; these values are lower than those at RT
(i.e., 558 MPa and 651 MPa, respectively). The reason is that trans-
verse matrix cracks propagated rapidly at the cryogenic tempera-
ture, resulting in high energy dissipation at each crack count.
1626 M.-G. Kim et al. / Composites: Part A 43 (2012) 1620–1627

500 2.0 500 2.0

(a) Carbon/epoxy, (b) Carbon/ FCNT-epoxy,
400 at RT 1.6 400 at RT 1.6

Energy level (mVs)

Energy level (mVs)

Stress (MPa)
Stress (MPa)

300 1.2 300 1.2

200 0.8 200 0.8

100 0.4 100 0.4

0 0.0 0 0.0
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Strain (%) Strain (%)

350 2.0 350 2.0

300 (c) Carbon/epoxy, 300 (d) Carbon/ FCNT-epoxy,

1.6

Energy level (mVs)

1.6

Energy level (mVs)

at- 150oC at- 150oC
250 250

Stress (MPa)
Stress (MPa)

1.2 200 1.2

200

150 150
0.8 0.8
100 100
0.4 0.4
50 50

0 0.0 0 0.0
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Strain (%) Strain (%)

Fig. 10. Stress–strain responses and energy levels of the each AE signal during tensile tests.

(a) enhance the interfacial bonding between CNTs and the epoxy ma-
trix. The functionalized CNT-epoxy specimen showed higher
strength than as-received CNT-epoxy specimen. It was thus con-
cluded that the strength increase mainly arises from greater energy
dissipation to break CNTs rather than pull-out during loading. Two
kinds of UD prepregs were fabricated to investigate the CNT-rein-
forcing and -functionalizing effects on fracture characteristics of
composites at a cryogenic temperature. From the results of DCBs
test at cryogenic temperature, the carbon/FCNT-epoxy composite
showed the highest fracture toughness among the candidates. It
Transverse direction was also found that AE signals of the carbon/FCNT-epoxy specimen
showed higher energy levels than those of the control just prior
to the first transverse failure of the 90° plies. This was attributed
to the release of higher strain energy to break the nanotubes or
(b) to bifurcate crack propagating paths.

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