52897_Chap-9 CNTs & Composites_Veena,BPSingh,RBMathur

Chapter 9
Carbon Nanotubes and Their Composites
Veena Choudhary, B.P. Singh and R.B. Mathur
Additional information is available at the end of the chapter
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1. Introduction
Carbon nanotubes (CNTs), a fascinating material with outstanding properties has inspired
the scientist, engineer and technologist for wide range of potential applications in many
areas [1]. Since all these properties are concerned directly to the atomic structure of nano‐
tubes, it is quite necessary to have a thorough understanding of the phenomenon to control
nanotube size, the number of shells (walls), the helicities and the structure during growth.
The full potential of nanotubes for applications will not be realized until the structure of
nanotubes during their growth is optimized and well controlled. For utilization of CNTs
properties in real world applications, like composite preparation, it is desired to obtain high
quality and in bulk quantity using growth methods that are simple, efficient and inexpen‐
sive. Significant work has been carried out in this field and various methods have been stud‐
ied to synthesize CNTs by several researchers.
2. Properties
Carbon nanotubes are endowed with exceptionally high material properties, very close to
their theoretical limits, such as electrical and thermal conductivity, strength, stiffness, tough‐
ness and low density.
2.1. Mechanical properties of CNTs
The strength of C-C bond gives a large interest in mechanical properties of nanotubes. Theoreti‐
cally, these should be stiffer than any other known substance. Young's modulus of the single
walled carbon nanotubes (SWCNTs) can be as high as 2.8-3.6 TPa and 1.7-2.4 TPa for multiwal‐
led carbon nanotubes (MWCNTs) [2]which is approximately 10 times higher than steel, the
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194 Syntheses and Applications of Carbon Nanotubes and Their Composites
strongest metallic alloy known. Experimental values of Young’s modulus for SWCNTs are re‐
ported as high as to 1470 GPa and 950 GPa [3, 4] for MWCNTs, nearly 5 times of steel. There are no
direct mechanical testing experiments that can be done on individual nanotubes (nanoscopic
specimens) to determine directly their axial strength. However, the indirect experiments like
AFM provide a brief view of the mechanical properties as well as scanning probe techniques that
can manipulate individual nanotubes, have provide some basic answers to the mechanical be‐
havior of the nanotubes [5]. The analysis performed on several MWCNTs gave average Young’s
modulus values of 1.8 TPa, which is higher than the in – plane modulus for single crystal graph‐
ite. So the high stiffness and strength combined with low density implies that nanotubes could
serve as ideal reinforcement in composite materials and provide them great potential in applica‐
tions such as aerospace and other military applications.
2.2. Electrical properties of CNTs
The nanometer dimensions of CNTs, together with the unique electronic structure of a graphene
sheet, make the electronic properties of these one-dimensional (1D) structures extraordinary.
The one dimensional structure of CNTs helps them in making a good electric conductor. In a 3D
conductor the possibility of scattering of electrons is large as these can scatter at any angle. Espe‐
cially notable is the fact that SWCNTs can be metallic or semiconducting depending on their
structure and their band gap can vary from zero to about 2 eV, whereas MWCNTs are zero-gap
metals. Thus, some nanotubes have conductivities higher than that of copper, while others be‐
have more like silicon. Theoretically, metallic nanotubes having electrical conductivity of 105 to
106 S/m can carry an electric current density of 4 × 109 A/cm2 which is more than 1000 times great‐
er than copper metal and hence can be used as fine electron gun for low weight displays. Due to
the large diameter of MWCNTs, their transport properties approaches those of turbostatic
graphite. Theoretical study also shows that in case of MWCNTs the overall behavior is deter‐
mined by the electronic properties of the external shell. Conductivities of individual MWCNTs
have been reported to range between 20 and 2 × 107 S/m [6], depending on the helicities of the out‐
ermost shells or the presence of defects [7].The electronic properties of larger diameter
MWCNTs approach those of graphite. Nanotubes have been shown to be superconducting at
low temperatures. As probably CNTs are not perfect at ends and end defects like pentagons or
heptagons are found to modify the electronic properties of these nanosystems drastically. There
is great interest in the possibility of constructing nanoscale electronic devices from nanotubes
and some progress is being made in this area. SWCNTs have been recently used to form conduct‐
ing and semiconducting layers (source, drain and gate electrodes) in thin films transistors. So the
high electrical conductivity of CNTs makes them an excellent additive to impart electrical con‐
ductivity in otherwise insulating polymers. Their high aspect ratio means that a very low load‐
ing is needed to form a connecting network in a polymer compared to make them conducting.
2.3. Thermal properties of CNTs
CNTs are expected to be very good thermal conductors along the tube, but good insulators
laterally to the tube axis. Experiments on individual tubes are extremely difficult but meas‐
urements show that a SWCNT has a room-temperature thermal conductivity along its axis
Carbon Nanotubes and Their Composites 195
of about 3500 W m−1 K−1 and MWCNTs have a peak value of ~ 3000 W m−1 K−1 at 320 K; com‐
pare this to copper, a metal well-known for its good thermal conductivity, which transmits
385 W m−1 K−1 [8]. Although for bulk MWCNTs foils, thermal conductivity limits to 20 W m
−1 K−1 suggesting that thermally opaque junctions between tubes severely limit the large
scale diffusion of phonons. The thermal conductivity of CNTs across axis (in the radial di‐
rection) is about 1.52 W m−1 K−1, which is about as thermally conductive as soil. Both
SWCNT and MWCNT materials and composites are being actively studied for thermal man‐
agement applications, either as “heat pipes” or as an alternative to metallic addition to low
thermal conductive materials. In case of composites, the important limiting factors are quali‐
ty of dispersion and interphase thermal barriers.
3. Synthesis of CNTs
A variety of synthesis methods now exist to produce carbon nanotubes. The three main pro‐
duction methods used for synthesis of CNTs are d.c. arc discharge, laser ablation and chemi‐
cal vapor deposition (CVD).
3.1. d.c. arc discharge technique
The carbon arc discharge method, initially used for producing C60 fullerenes, is the most
common and perhaps easiest way to produce carbon nanotubes as it is rather simple to un‐
dertake. In this method two carbon rods placed end to end, separated by approximately
1mm, in an enclosure that is usually filled with inert gas (helium, argon) at low pressure (be‐
tween 50 and 700 mbar) as shown in Figure 1. Recent investigations have shown that it is
also possible to create nanotubes with the arc method in liquid nitrogen [9]. A direct current
of 50 to 100 A driven by approximately 20 V creates a high temperature (~4000K) discharge
between the two electrodes. The discharge vaporizes one of the carbon rods (anode) and
forms a small rod shaped deposit on the other rod (cathode). Large-scale synthesis of
MWCNTs by a variant of the standard arc-discharge technique was reported by Ebbesen
and Ajayan [10]. A potential of 18 V dc was applied between two thin graphite rods in heli‐
um atmosphere. At helium pressure of ~500 Torr, the yield of nanotubes was maximal of
75% relative to the starting graphitic material. The TEM analysis revealed that the samples
consisted of nanotubes of two or more concentric carbon shells. The nanotubes had diame‐
ters between 2 and 20 nm, and lengths of several micrometers. The tube tips were usually
capped with pentagons.
If SWCNT are preferable, the anode has to be filled with metal catalyst, such as Fe, Co, Ni, Y
or Mo. Experimental results show that the width and diameter distribution depends on the
composition of the catalyst, the growth temperature and the various other growth condi‐
tions. If both electrodes are graphite, the main product will be MWCNTs. Typical sizes for
MWCNTs are an inner diameter of 1-3nm and an outer diameter of approximately 10nm.
Because no catalyst is involved in this process, there is no need for a heavy acidic purifica‐
tion step. This means MWCNT can be synthesized with a low amount of defects.
Figure 1. Schematic diagram of dc-arc discharge set-up
In most of the studies, SWCNTs are synthesized using the dc-arc discharge process by filling
the catalyst powder into a hole drilled in a graphite elctrode act as an anode and arcing
takes place between this anode and a pure graphite based cathode in optimized chamber
conditions. In one of the study by Mathur et al. [11] SWCNTs and MWCNTs were synthe‐
sized simultaneously in a single experiment selectively. In their experiment, However, in‐
stead of filling the catalyst powder into a hole drilled in a graphite electrode; they prepared
a catalyst/graphite composite electrode. Coke powder, catalyst powder, natural graphite
powder and binder pitch were thoroughly mixed together in a ball mill in appropriate pro‐
portions and molded into green blocks using conventional compression molding technique.
A mixture of Ni and Co powders was used as catalyst. The green blocks were heated to
1200o C in an inert atmosphere to yield carbonized blocks with varying compositions of
coke, natural graphite powder, Ni and Co. These electrodes were used as the anodes in the
arcing process and a high density graphite block was used as the cathode. A uniform gap of
1– 2 mm was maintained between the electrodes during the arcing process with the help of a
stepper motor for a stable arc-discharge (dc voltage 20–25 V, current 100–120 A, 600 torr he‐
lium).The SWCNTs yield was found to be doubled in this case.
3.1.1. Characteristics of CNTs produced by d.c. arc discharge technique
Arc discharge is a technique that produces a mixture of components and requires separating
nanotubes from the soot and the catalytic metals present in the crude product. In this techni‐
que both SWCNT and MWCNT can be produced and it has been described by several re‐
searchers.
The scanning electron microscope (SEM) and transmission electron microscope (TEM) are
generally used to observe the physical appearance of any carbon based soot. Similarly, Ma‐
thur et al. [11] used SEM and TEM for the observation of SWCNT and MWCNT produced
from the arc discharge technique as shown in Figure 2. In this technique, the carbon material
deposits on the chamber and cathode. The arcing process resulted in the formation of web-
like deposits on the inner walls of the arc chamber. A typical SEM micrograph of such de‐
posit (Figure 2a) revealed the presence of SWNT bundles along with the amorphous carbon
and catalyst particles. Rod-like microstructures aligned preferentially along the length of the
cathode were also found at the tip of the cathode as shown in Figure 2b. The inset in Figure
2b shows the presence of graphitized carbon and sharp needle-like nanostructure when
these rods are powdered. Upon detailed electron microscopic examination, these needles ex‐
hibited the MWCNT structure with an outer diameter of 20–25 nm (Figure 2c).
Figure 2. (a) SEM micrograph of the chamber deposit showing the presence of long and flexible carbon nanotubes.
(b) SEM micrograph of the cathode deposit showing the presence of rod-like microstructures. The inset figure shows
the presence of needle-like nanostructures present within each microstructure. (c) TEM micrograph of a single needle-
like nanostructure (Reprinted with permission from Elsevier (11))
The nature of the soot can be identified using Raman spectrometer and generally used for
confirmation of the quality of CNTs. The nature of these two deposits obtained using this
arc discharge process was confirmed from their respective Raman spectrum (Figure 3). The
Raman spectrum of the chamber deposit showed the characteristic radial breathing and tan‐
gential bands at 165–183 and 1591 cm-1, respectively. The strong G-band at 1580 cm-1 in the
Raman spectrum of the cathode deposit and its TEM image depicted in Figure 2c, confirmed
that the cathode deposit predominantly contained MWCNTs. The prominent D-band
around 1350 cm-1seen in both spectrum is attributed to the presence of disordered carbona‐
ceous material present in the as-prepared deposits. In their study, Mathur et al. [11] show
that SWCNTs deposit on the arc chamber and MWCNTs on cathode deposit.
Figure 3. Room temperature Raman spectrum of the chamber and cathode deposit (Reprinted with permission from
Elsevier (11))
3.2. Chemical vapor deposition
Pyrolysis of organometallic precursors such as metallocenes (e.g. ferrocene) in a furnace pro‐

vides a straight forward procedure to prepare CNT by CVD technique. Different hydrocar‐
bons, catalyst and inert gas combinations have been used by several researchers in the past
for the growth of CNT by CVD technique. In one of the study by Mathur et al. [12], CNTs
were grown inside the quartz reactor by thermal decomposition of hydrocarbons, e.g. tol‐
uene in presence of iron catalyst obtained by the decomposition of organometallic like ferro‐
cene. The furnace provided a constant temperature zone of 18 cm in the centre as shown in
Figure 4. The reaction zone was maintained at 750oC. Once the temperature was reached, the
solution containing a mixture of ferrocene and toluene in particular proportion (0.077 g fer‐
rocene in 1 ml toluene) was injected in the reactor at a point where the temperature was
200oC. Argon was also fed along with the charge as a carrier gas and its flow rate was ad‐
justed so that the maximum amount of precursor is consumed inside the desired zone.
Figure 4. Schematic diagram of the CVD reactor along with the temperature profile (Reprinted with permission from
Elsevier (12))
3.2.1. Characteristics of CNTs Produced by CVD Technique
CNTs are produced in the form of big bundles using CVD technique. The physical appear‐
ance of the as produced CNTs is shown in Figure 5a and Figure 5b for SEM and TEM re‐
spectively. Figure 5a shows a big CNT bundle of length >300µm and the inset image of
Figure 5a shows very good quality of uniform CNTs. Figure 5b shows the TEM image of as
produced CNTs confirming the presence of MWCNT with metallic catalytic impurites either
on the tip of the tube or in the cavity of of CNTs (inset of Figure 5b).
Further confirmation of the quality and type of CNTs can be obtained using Raman spec‐
trometer as shown in Figure 6. This shows the tangential band at 1580 cm-1 (G band) of high
intensity and the disorder-induced band at 1352 cm-1 (D band) as a perfect MWCNT nature
[13]. The ratio of intensity of G to D band gives the information regarding the quality of the
CNTs. The high value of intensity ratio of G/D band confirms the better quality of CNTs.
a b
Figure 5. (a) SEM image of aligned CNT bundle synthesized by CVD technique.The inset figure shows the very good
quality of uniform CNTs (b) TEM image of as grown MWCNT and inset image shows the MWCNTs with encapsulated
metallic impurities
Figure 6. Raman spectrum of CVD-grown MWCNTs.
3.3. Laser ablation
In the laser ablation process, a pulsed laser vaporizes a graphite target containing small
amounts of a metal catalyst [14] as shown in Figure 7. The target is placed in a furnace at
roughly 1200°C in an inert atmosphere. The nanotubes develop on the cooler surface of the
reactor, as the vaporized carbon condenses. The yield of nanotube synthesis by this process
is roughly 70%.
Figure 7. Schematic diagram of Laser ablation set-up for CNT synthesis
3.3.1. Characteristics of CNTs produced by laser ablation technique
The laser-ablation prepared samples usually contain >70% nearly endless, highly tangled
ropes of SWCNTs along with nanoscale impurities. The SWCNTs formed in this case are
bundled together by van der Waals forces. Laser vaporisation results in a higher yield for
SWCNT synthesis and a narrower size distribution than SWCNTs produced by arc-dis‐
charge [15]. The nanotubes generated by the laser ablation and arc discharge technique are
relatively impure, with presence of unwanted carbonaceous impurities and not operated at
higher scale; therefore, the overall production costs are high.
Compared to other methods for synthesis of CNTs, more parameters, including tempera‐
ture, feeding gases, flow rate, catalyst components and heating rate are accessible to control
the growth process in CVD. By changing the growth conditions, we can control the proper‐
ties of the produced CNTs such as length, orientation and diameter to some extent. It has
been observed that the gas phase processes produces CNTs with fewer impurities and are
most amenable to large scale processing. So the gas phase techniques such as CVD, for
nanotube growth offer the greatest potential for scaling up nanotube production for process‐
ing of composites.
4. Purification
During CNTs synthesis, impurities in the form of catalyst particles, amorphous carbon and
non tubular fullerenes are also produced. The most of the production methods involve the
use of catalysts which are normally transition metals (Fe, Co, Ni or Y), these remains in the
resulting nanotubes as spherical or cylindrical particles after experiments. Through careful

control of process parameters one could minimize the formation of amorphous carbon parti‐
cles, so that the main impurities in CNTs are the remaining catalyst particles. However as
most of these catalytic particles may either hide in internal cavity or stick firmly to the walls
of CNTs, it is almost impossible to get rid of these effectively without damaging the nano‐
tubes. Several purification methods have been tried to overcome these impurities. In one of
the study by Mathur et al. [11], SWCNT soot prepared by dc arc discharge process was puri‐
fied by removing various forms of impurities, such as amorphous carbon, graphitic nano‐
shells and catalyst particles present in the chamber deposit by applying a judicious
combination of wet and dry chemical methods (acid treatment and oxidation). In this proc‐
ess, initially SWCNT soot were oxidized at 350 oC for 6h in air which remove the amorphous
carbon followed by refluxing in HCl for the removal of metallic impurities like Ni and Co
and again oxidation at 550oC for 30 min for the removal of graphitic nanoshell.The final
product gives 97% purified SWCNT. The MWCNTs produced by CVD technique contains
mainly ~10% metallic impruites which can be removed by heating it in the inert atmosphere
at 2500oC in graphitization furnace. This process gives >99% pure MWCNTs and also helps
in annealing out the defects in the tubes. This graphitization process at high temperature can
also be useful for removal of impurities in the arc discharge produced SWCNTs soots with
the combination of other purification steps.
5. Nanocomposites
Because of the high strength and stiffness of CNTs, they are ideal candidates for structural
applications. For example, they may be used as reinforcements in high strength, low weight
and high performance composites. Presently there is a great interest in exploiting the excit‐
ing properties of these CNTs by incorporating them into some form of polymer matrix.
5.1. Composite fabrication techniques
A large number of techniques have been used for the fabrication of CNT-polymer nanocom‐
posites based on the type of polymer used.
5.1.1. Solvent casting
The solution casting is most valuable technique to form CNTs/polymer nanocomposites.

However, its use is restricted to polymers that are soluble. Solvent casting facilitates nano‐
tube dispersion and involves preparing a suspension of CNTs in the desirable polymer solu‐
tion via energetic agitation (magnetic stirring or sonication) and then allowing the solvent to
evaporate to produce CNT-polymer nanocomposites. A lot of study is available in open lit‐
erature for the formation of CNT nanocomposites by this method [16-18]. Mathur et al. [18]
cast the solutions of the MWCNT/polystyrene (PS)/toluene and MWCNT/ polymethyl meth‐
acrylate (PMMA)/toluene suspensions after sonication into a petry dish to produce nano‐
tubes composites with enhanced electrical and mechanical properties. Benoit et al. [19]
obtained electrically conductive nanocomposites by dispersing CNT and PMMA in toluene,

followed by the drop casting on substrate. The choice of solvent is generally made based on
the solubility of the polymer. The solvent selection for nanotube dispersion also had a signif‐
icant influence on the properties of the nanocomposites and studied by Lau and co-workers
[20].Their results demonstrates that, contrary to the general belief that small traces of CNTs
alone will serve to strengthen the epoxy composites, the choice of the solvent used in the
dispersion of CNTs also can have a significant impact. The change trend of the mechanical
properties was found to be related to the boiling point of respective solvent used. In the
samples observed in their study, only acetone-dispersed nanocomposites displayed im‐
provements in flexural strength over the pure epoxy, while ethanol and DMF used in CNTs
dispersion actually countered the benefits of CNTs in the resulting nanocomposites.It is rea‐
sonable that, easier the solvent can evaporate, less solvent will remain to affect the curing
reaction. Their results of thermogravimetric analysis (TGA) proved the existence of residual
solvent in the resulting nanocomposites. Further evidence of the solvent influence was ob‐
tained by Fourier transform infrared (FTIR) spectra, which displayed the difference in the
molecular structure of the final nanocomposites depending on the solvent used. The solvent
influence is attributed to the different amount of unreacted epoxide groups and the extent of
cure reaction in the manufacturing process. The presence of residual solvent may alter the
reaction mechanism by restricting the nucleophile–electrophile interaction between the
hardener and epoxy, henceforth, affect the cross-linking density and thus degrade the trans‐
port properties [21]and mechanical properties of the cured structures. The residual solvent
may absorb some heat energy from the composite systems in the pre-cured process, causing
a change in local temperature. Nanocomposites with other thermoplastic materials with en‐
hanced properties have been fabricated by solvent casting [16-18, 22]. The limitation of this
method is that during slow process of solvent evaporation, nanotubes may tend to agglom‐
erate, that leads to inhomogeneous nanotube distribution in polymer matrix. The evapora‐
tion time can be decreased by dropping the nanotube/polymer suspension on a hot substrate
(drop casting) [19]or by putting suspension on a rotating substrate (spin-casting) [23]. Du et
al. [24] developed a versatile coagulation method to avoid agglomeration of CNTs in
PMMA-CNT nanocompositses that involves pouring a nanotube/polymer suspension into
an excess of solvent. The precipitating polymer chains entrap the CNT, thereby preventing
the CNT from bundling.
5.1.2. Melt mixing method
The alternative and second most commonly used method is melt mixing, which is mostly
used for thermoplastics and most compatible with current industrial practices. This techni‐
que makes use of the fact that thermoplastic polymers softens when heated. Melt mixing
uses elevated temperatures to make substrate less viscous and high shear forces to disrupt
the nanotubes bundle. Samples of different shapes can then be fabricated by techniques such
as compression molding, injection molding or extrusion. Andrews and co-workers [25]
formed composites of commercial polymers such as high impact polystyrene, polypropy‐
lene and acrylonitrile–butadiene–styrene (ABS) with MWCNT by melt processing. Initially
these polymers were blended in a high shear mixer with nanotubes at high loading level to
form master batches that were thereafter diluted with pure polymer to form lower mass
fraction samples. Compression molding was used to form composite films. A similar combi‐
nation of shear mixing and compression molding is studied by many other groups dis‐
cussed elsewhere [16]. Also Meincke et al. [5] mixed polyamide-6, ABS and CVD-MWCNT
in a twin screw extruder at 260oC and used injection molding to make nanocomposites.
Tang et al. [26] used both compression and twin-screw extrusion to form CNT/polyethylene
composites. Although melt-processing technique has advantages of speed and simplicity, it
is not much effective in breaking of agglomeration of CNTs and their dispersion. Bhatta‐
charyya et al. [27] made 1 wt% CNT/polypropylene (PP) nanocomposites by melt mixing,
but found that melt mixing alone did not provide uniform nanotube dispersion. Niu et el.
[28] studied both methods to prepare polyvinylidene fluoride (PVDF)-CNT nanocomposites
to study electrical properties and found it better in composites formed by solution casting.
5.1.3. In-situ polymerization
In addition to solvent casting and melt mixing the other method which combines nanotubes
with high molecular weight polymers is in-situ polymerization starting with CNTs and mono‐
mers. In-situ polymerization has advantages over other composite fabrication methods. A
stronger interface can be obtained because it is easier to get intimate interactions between the
polymer and nanotube during the growth stage than afterwards [29, 30].The most common in
situ polymerization methods involve epoxy in which the monomer resins and hardeners are
combined with CNTs prior to polymerizing [31]. Pande and coworkers [32] performed the in-
situ polymerization of MWCNT/ PMMA composites for the enhancement in flexural strength
and modulus of composites. Li et al. [33] reported the fabrication and characterization of CNT/
polyaniline (PANI) composites. Xiao and Zhou [34]deposited polypyrrolre (PP) and poly(3-
methylthiophene) (PMet) on the surface of MWCNTs by in situ polymerization. Saini et al. [35]
reported fabrication process of highly conducting polyaniline (PANI)–(MWCNT) nanocompo‐
sites by in-situ polymerization. This material was used in polystyrene for the fabrication of
MWCNT-PANI-PS blend for microwave absorption [36]. Moniruzzaman [17] reported many
other studies of in-situ polymerization of CNTs with different polymers. Generally, in situ poly‐
merization can be used for the fabrication of almost any polymer composites containing CNT
that can be non-covalently or covalently bound to polymer matrix. This technique enables the
grafting of large polymer molecules onto the walls of CNT. This technique is particularly impor‐
tant for the preparation of insoluble and thermally unstable polymers, which cannot be process‐
ed by solution or melt processing.
Some studies have been also carried out using combined methods, such as solvent casting in
conjunction with sonication, followed by melt mixing. Haggenmueller et al. [37] observed
considerable nanotube dispersion in CNT-polymer nanocomposites using combination of
solvent casting and melt mixing. Pande et al. [32, 38] also prepared MWCNT bulk compo‐
sites with PMMA and PS using a two-step method of solvent casting followed by compres‐
sion molding and obtained better electrical and mechanical properties. Singh et al. [39] also
prepared MWCNT-LDPE composites using solvent casting followed by compression
moulding and obtained better electrical conductivity. Jindal et al. [29, 40] prepared
MWCNT-polycarbonate composite using solvent casting followed by compression mould‐

ing for the enhancement in the impact properties.
The other less commonly known methods for CNT- polymer nanocomposites formation are
twin screw pulverization [41], latex fabrication [42], coagulation spinning [43] and electro‐
phoretic deposition [44].
6. Challenges in MWCNT polymer composites fabrication and possible

solutions
Although these fabrication methods helped to enhance the properties of CNT reinforced
composites over neat polymer but there are several key challenges that hinders the excellent
CNT properties to be fruitful in polymer composite formation.
6.1. Dispersion
Disperion of nanoscale filler in a matrix is the key challenge for the formation of nanocomposite.
Dispersion involves separation and then stabilization of CNTs in a medium. The methods de‐
scribed above for the nanocomposites fabrication require CNTs to be well dispersed either in
solvent or in polymer for maximizing their contact surface area with polymer matrix. As CNTs
have diameters on nanoscale the entanglement during growth and the substantial van der
Waals interaction between them forces to agglomerate into bundles. The ability of bundle for‐
mation of CNTs with its inert chemical structure makes these high aspect ratio fibers dissolving
in common solvents to form solution quite impossible. The SEM of MWCNTs synthesized by
CVD technique seems to be highly entangled and the dimensions of nanotube bundles is hun‐
dreds of micrometer. This shows several thousands of MWCNTs in one bundle as shown in Fig‐
ure 5a. These bundles exhibits inferior mechanical and electrical properties as compared to
individual nanotube because of slippage of nanotubes inside bundles and lower aspect ratio as
compared to individual nanotube. The aggregated bundles tend to act as defect sites which ad‐
versely affect mechanical and electrical properties of nanocomposites. Effective separation re‐
quires the overcoming of the inter-tube van der Waal attraction, which is anomalously strong in
CNT case. To achieve large fractions of individual CNT several methods have been employed.
The most effective methods are by attaching several functional sites on the surface of CNTs
through some chemical treatment or by surrounding the nanotubes with dispersing agents such
as surfactant. Thereafter the difficulty of dispersion can be overcome by mechanical/physical
means such as ultrasonication, high shear mixing or melt blending. Another obstacle in dispers‐
ing the CNTs is the presence of various impurities including amorphous carbon, spherical full‐
erenes and other metal catalyst particles. These impurities are responsible for the poor
properties of CNTs reinforced composites [45].
6.2. Adhesion between CNTs and polymer

The second key challenge is in creating a good interface between nanotubes and the poly‐
mer matrix. From the research on microfiber based polymer composites over the past few
decades, it is well established that the structure and properties of filler-matrix interface
plays a major role in determining the structural integrity and mechanical performance of
composite materials. CNTs have atomically smooth non-reactive surfaces and as such there
is a lack of interfacial bonding between the CNT and the polymer chains that limits load
transfer. Hence the benefits of high mechanical properties of CNTs are not utilized properly.
The first experimental study focusing on interfacial interaction between MWCNT and poly‐
mer was carried out by Cooper et al. [46]. They investigated the detachment of MWCNTs
from an epoxy matrix using a pullout test for individual MWCNT and observed the interfa‐
cial shear stress varied from 35-376 MPa. This variation is attributed to difference in struc‐
ture and morphology of CNTs.
There are three main mechanisms for load transfer from matrix to filler. The first is weak
van der Waal interaction between filler and polymer. Using small size filler and close con‐
tact at the interface can increase it. The large specific surface area of CNTs is advantageous
for bonding with matrix in a composite, but is a major cause for agglomeration of CNTs.
Therefore, uniformally dispersed individual nanotubes in matrix is helpful. The second
mechanism of load transfer is micromechanical interlocking which is difficult in CNTs nano‐
composites due to their atomically smooth surface. Although local non uniformity along
length of CNTs i.e. varying diameter and bends due to non hexagonal defects contributes to
this micromechanical interlocking. This interlocking can increase by using long CNTs to
block the movement of polymer chains. The contribution of this mechanism may reach satu‐
ration at low CNT content. The third and best mechanism for better adhesion and hence
load transfer between CNTs and polymer is covalent or ionic bonding between them. The
chemical bonding between CNTs and polymer can be created and enhanced by the surface
treatment such as oxidation of CNTs with acids or other chemicals. This mode of mecha‐
nism have much importance as it provides strong interaction between polymer and CNT
and hence efficiently transfers the load from polymer matrix to nanotubes necessary for en‐
hanced mechanical response in high-performance polymers.
6.3. Chemical functionalization of CNTs
The best route to achieve individual CNT to ensure better dispersion is chemical modifica‐
tions of CNT surface. The chemical functionalization involves the attachment of chemical
bonds to CNT surface or on end caps. Nanotube functionalization typically starts with oxi‐
datative conditions, commonly by refluxing in nitric or sulfuric acid or combination of both
to attach carboxylic acid moieties to the defect sites. The end caps of nanotubes have extra
strain energy because of their high degree of curvature with pentagons and heptagonal car‐
bon atoms are most vulnerable to reaction with acid. The side walls also containing defects
like pentagon-heptagon pairs, sp3 hybridized defects and vacancies in nanotube lattice and
are easily supplemented by oxidative damage and can be stabilized by formation of func‐
tional groups mainly carboxylic acid and hydroxide group. These acid moieties and hydrox‐
ide groups can be further replaced to more reactive groups like –COCl or –CORNH2. The
addition of these functional groups on CNTs possesses intermolecular repulsion between
functional groups on surface that overcomes the otherwise weak van der Waal attraction be‐
tween CNTs. It is also vital to stabilize the dispersion to prevent reagglomeration of the
CNTs. Chemical functionalization can prevent reagglomeration of CNTs also. Sen et al. [47]
carried out chemical functionalization to form ester functionalized CNTs and found that it is
an effective approach to exfoliate the CNTs bundles and improve their processibility with
polymer matrix. Georgakilas et al. [48] observed that CNT covalently functionalized with
pyrrolidone by 1,3-dipolar cycloaddition of azomethine ylides show a solubility of 50
mg/mL in chloroform, even without sonication whereas the pristine CNT is completely in‐
soluble in this solvent. Liang et al. [49] performed reductive alkylation of CNTs using lithi‐
um and alkyl halides in liquid ammonia for sidewall functionalization of CNTs and
observed their extensive debundling by inspection of HRTEM images. Kinloch et al. [50]
studied the rheological behavior of oxidized CNTs and found that the composites filled with
functionalized CNTs had better dispersion. It has been observed by the researchers that
amine modified CNTs is very important for the enhancement in the mechanical properties
with epoxy. Garg et al. [31] shows the reaction mechanism for the formation of acid func‐
tionalized and amine functionalized CNT and their interaction with the epoxy resin as Fig‐
ure 8a and b respectively. Two different types of functional groups were attached on the
CNT surface. In the first case MWCNTs were refluxed for 48 h in HNO3 (400 ml, 60% con‐
centration) to achieve reasonable surface oxidation of the tubes. The mixture was then fil‐
tered and the residue (treated material) was washed several times with distilled water till
washings were neutral to pH paper. The treated MWCNT were dried in oven before use. In
a second step the oxidized nanotubes were dispersed in benzene by stirring, and then re‐
fluxed with excess SOCl2 along with a few drops of DMF used as catalyst for chlorination of
MWCNT surfaces. After the acyl chlorination, SOCl2 and DMF were removed through re‐
peatedly washing by tetrahydrofuran (THF). 100 ml of triethylene tetra-amine (TETA) was
added to react with acyl chlorinated MWCNT at 100 °C for 24 h reflux until no HCl gas
evolved. After cooling to room temperature, MWCNTs were washed with deionized water 5
times to remove excess TETA. Finally, the black solid was dried at room temperature over‐
night in vacuum and named as amine modified CNTs. These functionalized CNTs were
characterized by FTIR, TGA and HRTEM and clearly showed the presence of these types of
functional group. Gojny et al. [51]achieved surface modified MWCNTs by refluxing of oxi‐
dized MWCNTs with multifunctional amines and observed from TEM images that these
were completely covered by epoxy matrix that confirmed the bonding between them. Sin‐
nott [52]has provided an in depth review of chemical functionalization of CNTs where the
chemical bonds are used to tailor the interactions between nanotubes and polymers or sol‐
vent. The chemical functionalization of CNTs has also been accomplished through irradia‐
tion with electrons or ions [53]. In this manner one may hope to improve the binding of
CNTs by interdigitation of active sites on its sides into polymer matrix.
Covalent bond also benefits phonon transferring between nanotubes and polymer matrix,
which is a key factor for improving thermal conductivity of the nanocomposites. To ensure
the adhesion between polymer and nanotubes various surfactant and chemical modification
procedures have been adopted to modify the surface of otherwise inert surface of CNTs that
provides bonding sites to the polymer matrix.
Figure 8. Reaction mechanism for (a) acid modified-MWCNT (b) amine modified-MWCNT with epoxy resin (Reprinted
with permission from Springer(31))
So the surface modification of CNTs is the crucial factor that decides the effective dispersion
and improves the interactions between CNTs and matrix. However there are certain draw‐
backs of using chemically functionalized CNTs. Chemical functionalization normally em‐
ploys harsh techniques resulting in tube fragmentation and also disrupts the bonding
between graphene sheets and thereby reduces the properties of CNTs. Studies revealed that
different chemical treatments may decrease the maximum buckling force of nanotubes by
15% [16]. Also the chemical functionalized CNTs significantly decrease the electrical con‐
ductivity of CNTs nanocomposites due to unbalance polarization effect, shortening of
length and physical structure defects during acidic treatment [54]. But it is still necessary for
increased dispersion and strengthens the interfacial bonding of CNTs with polymer matrix
that is more important in structural applications.
The solubility or dispersion of CNTs in certain specified solvents or polymers can also in‐
crease by non covalent association which is more fragile. The non-ionic surfactant such as
sodium dodecylbenzene sulfonate (SDS) or polyoxyethylene-8-lauryl (PoEL) has two seg‐
ments. The hydrophobic segment of surfactant shows strong interactions with carbon of
CNTs via van der Waal force and the hydrophilic segment shows hydrogen bonding with
solvent or polymer used for dispersion. Islam et al. [55] reported that ~ 65% CNT bundles
exfoliated into individual nanotubes even with a very low of 20 mg (CNT)/ml of water con‐
taining SDS as surfactant. Barrau et al. [56] used palmitic acid as surfactant to disperse CNTs
into epoxy resin and observed that electrical percolation threshold decreases indicating bet‐
ter CNT dispersion. Gong et al. [57] added PoEL as surfactant in CNT/epoxy composite to
assist the dispersion of CNTs. The improvement in dispersion in chitosan with nitric acid
treated CNTs was also reported by Ozarkar et al. [58] and the stability of dispersion pre‐
pared by using functionalized CNTs was observed to be better. However, CNTs treated
with different surfactants are wrapped in it and hence contacts between CNTs decreases
thereby the transport properties (electrical and thermal conductivities) of CNTs/polymer
nanocomposites are adversely affected.
6.4. Dispersion of high loading of CNTs in polymer matrix
Dispersion of high loading of CNTs in any polymer is very difficult due to the formation of
agglomerates by the conventional techniques. To maximize the improvment in properties,
higher loading of CNTs is preferred [59]. However, polymer composites synthesized by us‐
ing the conventional methods generally have low CNT contents. It has been observed that
beyond 1 wt.-% of loading, CNTs tend to agglomerate [60] resulting in poor mechanical
properties of the composites. It is therefore important to develop a technique to incorporate
higher CNT loading in the polymer matrices without sacrificing their mechanical properties.
Recently, several methods have been developed for fabricating CNT/polymer composites
with high CNT loadings. One such technique is mechanical densification technique where
vertically aligned CNTs were densified by the capillary induced wetting with epoxy resin
[61]. By this technique dimensions of sample preparation are limited. In another technique, a
filtration system was used to impregnate the epoxy resin into CNT bucky paper [62, 63].
However, it was very difficult to completely impregnate the bucky paper with epoxy resin.
Recently, Feng et al., [64] reported a mixed curing assisted layer by layer method to synthe‐
size MWCNT/epoxy composite film with a high CNT loading from ~15 to ~36 wt.-%. The
mixed-curing-agent consists of two types of agents, one of which is responsible for the parti‐
al initial curing at room temperature to avoid agglomeration of the CNTs, and the other for
complete curing of epoxy resin at high temperature to synthesize epoxy composite films
with good CNT dispersion. In another study by Feng et al. [65] upto ~39.1 wt. % SWCNT-
epoxy composites were fabricated using same mixed curing layer by layer method and their
mechanical properties were enhanced significantly. Bradford et al. [66] reported a method to
quickly produce macroscopic CNT composites with a high volume fraction upto 27% of mil‐
limeter long, well aligned CNTs. Specifically, they used the novel method, shear pressing, to
process tall, vertically aligned CNT arrays into dense aligned CNT preforms, which are sub‐
sequently processed into composites. In another study by Ogasawara et al. [67] aligned
MWCNT/epoxy composites were processed using a hot-melt prepreg method. Vertically
aligned ultra-long CNT arrays (forest) were converted to horizontally aligned CNT sheets
by pulling them out. An aligned CNT/epoxy prepreg was fabricated using hot-melting with
B-stage cured epoxy resin film. The final composites contains 21.4 vol% of MWCNTs.
6.5. Alignment of CNTs in polymer matrix

The other key challenge is to understand the effect of nanotube alignment on nanocompo‐
sites properties because the nanotubes have asymmetric structure and properties. Like other
one-dimensional fiber fillers CNTs displays highest properties in the oriented reinforced di‐
rection and the mechanical, electrical, magnetic and optical performance of its composites
are linked directly to their alignment in the matrix. So to take the full advantage of excellent
properties of CNTs these should be aligned in a particular direction. For example, the align‐
ment of CNT increases the elastic modulus and electrical conductivity of nanocomposites
along the nanotube alignment direction.
Several methods like application of electric field during composite formation and carbon arc
discharge [68], composite slicing [69], film rubbing [70], chemical vapor deposition [71, 72],
mechanical stretching of CNT-polymer composites [73] and magnetic orientation [74] have
been reported for aligning nanotubes in composites. Electrospinning is also an effective
method for the alignment of CNTs in polymer matrix.
7. Properties of the nanocomposites
7.1. Mechanical properties of MWCNTs polymer nanocomposites

Different thermoplastic and thermoset polymer matrices have been tried to realize the supe‐
rior mechanical properties of CNTs for development of light weight strong material. NASA
scientists are considering CNT-polymer composite for space elevator. To date, a volume of
literature is available on the improvement of mechanical performance of polymers with ad‐
dition of CNTs. The first study for formation of CNT-polymer composites was carried out
by Ajayan et al. [69]. CNTs were aligned within the epoxy matrix by the shear forces in‐
duced by cutting with a diamond knife, however no quantitative mechanical measurements

were made. The first true study for tensile and compression properties of CNT polymer
composites was carried by Schadler et al. [75] with epoxy. On addition of 5-wt% MWCNTs
the tensile modulus increased from 3.1 GPa to 3.71 GPa. and compression modulus in‐
creased from 3.63 to 4.5 GPa. However, no significant increases in toughness values were
observed. Bai et al. [76] observed doubling of Young’s modulus from 1.2 to 2.4 GPa and sig‐
nificant increase in strength from 30 to 41 MPa on addition of 1 wt.% MWCNTs. Also excel‐
lent matrix–nanotube adhesion was confirmed by the observation of nanotube breakage
during fracture surface studies. Zhou et al. [77] reported steady increase of flexural modulus
in CNT-epoxy composite with higher CNT weight percentage and found an improvement of
11.7% in modulus with 0.4 wt% loading of CNTs and 28% enhancement in flexural strength
with 0.3 wt% loading. Garg et al. [31] reported an increment of 155 % in flexural strength of
epoxy with addition of merely 0.3% amine functionalized MWCNTs and an increment of
38% in flexural modulus. Mathur et al. [13] reported an increment of 158% in flexural
strength of phenolic with addition of 5 vol% of MWCNT. Colemann et al. [16] reviewed the
mechanical properties of a large number of CNT reinforced polymer (thermoplastic and
thermosetting) composites fabricated by various methods and reported enhancement in me‐
chanical properties. Du et al. [78] studied the experimental results for mechanical perform‐
ance of CNTs nanocomposites carried out by different research groups and observed that
the gains are modest and far below the simplest theoretical estimates. Haggenmueller [79]
applied the Halpen Tsai composite theory to CNT nanocomposites and observed that the ex‐
perimental elastic modulus is smaller than predicted by more than one order. It is attributed
to the lack of perfect load transfer from nanotubes to matrix due to non uniform dispersion
and small interfacial interaction. Although chemical functionalization of CNTs has sorted
out those problems to an extent yet the best results have to be achieved. Also aspect ratio is
other source of uncertainty in mechanical properties. Defects on the CNT surface also ex‐
pected to influence the mechanical properties significantly. The methods of handling nano‐
tubes, including acid treatments and sonication for long time are known to shorten
nanotubes results in decreasing aspect ratio and are detrimental to mechanical properties.
The mechanical properties of CNT based composites increased upto a certain loading of
CNTs and beyond which it starts decreasing. This may be because of increase in viscosity of
polymers at higher CNTs loading and also cause some surface of CNTs not to be completely
covered by polymers matrix due to the large specific surface area of CNTs.Therefore, few
studies have been carried out to disperse high loading of CNTs in polymer matrices with
improved mechanical properties. Bradford et al. [66] reported 400 MPa (tensile strength)
and 22.3 GPa (tensile modulus) for 27vol% of MWCNT–epoxy composites. Feng et al. [80]
also reported 183% and 408% improvement in tensile strength and tensile modulus respec‐
tively at 39.1 wt% SWCNTs loading compared with those of the neat epoxy. Ogasawara et
al. [67] found 50.6 GPa and 183 MPa modulus and ultimate tensile strength respectively of
CNT (21.4 vol.%)/epoxy composite. These values were 19 and 2.9 times those of the epoxy
resin respectively.
Andrews et al. [80] prepared aligned CNT/pitch composites and found the significant im‐
provement in the electrical and mechanical properties especially due to orientation of CNTs.
Du et al. [78] compared the mechanical performance of randomly oriented and aligned
CNTs polymer composites. Their study revealed that in aligned CNT polymer nanocompo‐
sites tensile strength and modulus even reached to 3600 MPa and 80 GPA respectively
which is much higher than the general value of 100 MPa and 6 GPa in case of randomly ori‐
ented CNT polymer nanocomposites. They also observed that the mechanical properties are
always higher for aligned CNTs composites with higher loading while the case is different
for isotropic CNT polymer composites.
7.2. Electrical properties of MWCNTs polymer nanocomposites
CNTs because of their extraordinary electrical conductivity are also excellent additive to im‐
part electrical conductivity to polymer. Many experimental results shows that the conduc‐
tive CNT composites can be constructed at low loading of CNTs due to low percolation
threshold originated from the high aspect ratio and conductivity of CNTs [70, 78]. Figure 9
shows the general trend of electrical conductivity of CNT- polymer nanocomposites. It can
be found from almost all the experimental results and also obvious from figure that CNT
nanocomposites exhibit a typical percolation behavior and CNT reinforcement to polymers
can increase the conductivity of resulting composites to several order of magnitude or even
some times higher than ten orders of magnitude.
According to percolation theory the conductivity follow the following power law close to
threshold percolation.
σ = σo ( p − po )t for p > po
where σ is the composite conductivity, σo is a constant, p the weight fraction of nanotubes, po

is the percolation threshold and t the critical exponent [81]. Theoretical and experimental re‐
sults have shown that percolation laws are applicable to CNT-based composites and that the
enhanced maximum conductivity and percolation can be achieved with significantly lower
filler concentrations than with other carbon and other conductive fillers. Depending on the
polymer matrix, the processing technology and the type of nanotubes used, recent experi‐
mental studies have achieved percolation thresholds between 0.0021 to 9.5% by weight and
critical exponents varying from 0.9 to 7.6 [78].
Sandler et al. [82] observed the percolation threshold of CNTs/epoxy nanocomposites be‐
tween 0.0225 and 0.04 wt %. They further observed very low percolation threshold at 0.0025
wt% for aligned CNT- epoxy composites [83]. The current voltage behavior measurements
exhibited non-ohmic behavior, which is most likely due to tunneling conduction mecha‐
nism. The main mechanism of conduction between adjacent nanotubes is probably electron
hopping when their separation distance is small. At concentration greater than percolation
threshold, conducting paths are formed through the whole nanocomposites, because the dis‐
tance between the conductive CNT filler (individual or bundles) is small enough to allow
efficient electron hopping.
The electrical conductivity of CNT/polymer composites also effected by dispersion and as‐
pect ratio of CNTs and was studied by Barrau et al. [56]. They used palmitic acid as surfac‐
tant to improve the nanotube dispersion and reduced the threshold concentration from 0.18
to 0.08 wt%. To study the effect of aspect ratio on electrical conductivity of CNT nanocom‐
posites Bai et al. [84] pretreated MWCNTs to alter their aspect ratios before preparing ep‐
oxy/MWCNTs composites and found that the threshold concentration varied from 0.5 to > 4
wt % with decreasing aspect ratio. The effect of alignment of CNTs in polymer composites
was also studied. Du et al. [24] found some contradictory results with respect to alignment
of rod like fillers and observed the lowest percolation threshold and maximum conductivity
with their random orientation. They found that the electrical conductivity of 2 wt% CNT/
PMMA nanocomposites decrease significantly (from ~10-4 to ~10-10 S/cm) when CNTs were
highly aligned. In contrast Choi et al. [85] observed that the nanotube alignment increased
the conductivity of a 3 wt% CNT/epoxy composites from ~10-7 to ~10-6S/cm. In most of the
cases the CNT nanocomposites with isotropic nanotubes orientation have greater electrical
conductivity than the nanocomposites with highly aligned CNTs especially at lower CNT
loadings. By alignment of CNTs in polymers, the percolation pathway is destroyed as
aligned CNTs seldomly intersects each other. At higher CNTs loading the conductivity is
more in case of aligned CNTs as compared to randomly oriented CNTs.
Figure 9. General trend of electrical conductivity of CNT polymer composites
The study carried out by different researchers also revealed that the composites with ther‐
moplastic polymers have higher conductivity as compared to that of thermosetting poly‐
mers above percolation threshold. Transport properties in CNT-PMMA composites have
been reported by Stephan et al. [86] and Benoit et al. [19] where low percolation threshold of
0.5 wt% and 0.33 wt% respectively were obtained. Singhai et al. [87] found that increase in
number of defects lead to a decrease in conductivity. However Lau et al. [88] concluded that
fuctionalization of CNTs can enhance the electrical conductivity of MWCNTs. The reason at‐
tributed to this phenomenon is electron transfer from the carbon atoms on MWCNTs to
functionalized groups attached to the surface favorably promoting conductivity. The study
carried out by Grimes et al. [89] revealed that the electrical response of as fabricated
MWCNTs is significantly influenced by the presence of residual catalyst metal particles.
7.3. EMI shielding proerties of MWCNTs polymer nanocomposites
The electrical conductivity of CNT reinforced polymer composites makes them a very suita‐
ble candidate to be employed for electromagnetic interference (EMI) shielding. EMI is the
process by which disruptive electromagnetic energy is transmitted from one electronic de‐
vice to another via radiation or conduction. As we all know that the electromagnetic waves
produced from some electronic instrument have an adverse effect on the performance of the
other equipments present nearby causing data loss, introduction of noise, degradation of
picture quality etc. The common example is the appearance of noise in television signal
when a telephone or mobile rings. Also recent reports of deterious effects of electromagnetic
radiations on electro medical devices have caused concern among health care providers. The
overlapping of signals transmitted in air traffic system with signals from other electronic
equipments became cause of several accidents in past. Also mobile phones and passing taxi
radios have been known to interfere with anti-skid braking system (ABS), airbags and other
electronic equipments causing drivers to lose control. In today’s scenario where rapid com‐
munication is required, there is an increase in electromagnetic radiations within the spec‐
trum in which the wireless, cordless and satellite system operates. So it a strong desire to
shield electronics equipments from the undesired signals. Problems with EMI can be mini‐
mized or sometime eliminated by ensuring that all electronic equipments are operated with
a good housing to keep away unwanted radio frequency from entering or leaving. The
shielding effectiveness (SE) of the shielding material is its ability to attenuate the propaga‐
tion of electromagnetic waves through it and measured in decibels (dB) given by
SE (dB) = − 10 log( Pt / P0),
where Pt and P0 are, respectively, the transmitted and incident electromagnetic power. A SE
of 10 dB means 90% of signal is blocked and 20 dB means 99% of signal is blocked.
One of the important criterion for a material to be used for EMI shielding material is that it
should be electrically conducting. Because of their high electrical conductivity metals have
been used for past several years as EMI shielding materials. But the shortcomings of metals
like heavy weight, physical rigidity and corrosion restricts their use. The most notable sub‐
stance that could overcome these shortcomings is the CNT-polymer composites. As dis‐
cussed in previous sections these are electrically conductive, having low density, corrosion
resistant and can be molded in any form. Due to easy processing and good flexibility, CNT–
polymer composites have been employed for application as promising EMI shielding mate‐
rials. The SE of the CNT-polymer composites depends on various factors like,type of CNTs
(either SWCNT or MWCNT), aspect ratio of CNTs, quality of CNTs, thickness and electrical
conductivity of the shielding material. Several studies have been reported on EMI shielding
properties of randomly oriented CNT based polymer composites. Mathur and co-workers
[18] have prepared MWNT-PMMA and MWNT-PS composites and observed 18dB and
17dB SE respectively with 10-wt % MWCNT loading. Singh et al. [90] reported a SE of 51 dB
by using MWCNT grown carbon fibre fabric based epoxy composites with improved me‐
chanical properties [91].The effect of the length (aspect ratio) of CNTs on EMI SE of compo‐
sites was also studied by few researchers. Huang et al. [92] reported EMI SE of 18 dB with 15
wt.-% small CNTs and 23-28 dB with 15 wt% long CNTs in X band (8-12.4 GHz). Li et al. [93]
also observed that SE with long length CNTs is more as compared to small length CNTs at
the same 15wt % loading composites. The residual catalyst metal particle in the cavity of
CNTs also effects the SE of the composites.
There are few additional advantages of using MWCNTs as EMI shielding material. The EMI
SE also depends on the source of origin of electromagnetic waves. Electrically conducting
material can effectively shield the electromagnetic waves generated from an electric source,
whereas magnetic materials effectively shield the electromagnetic waves generated from a
magnetic source. The MWCNTs exhibits electrical properties because of presence of pi elec‐
trons and magnetic properties because of the presence of catalytic iron particles in tubes. Al‐
so one common problem experienced with commonly used composite materials for EMI
shielding is build up of heat in the substance being shielded. The possible solution for this is
to add thermal conducting material. Composites with MWCNTs can easily overcome this
problem as it has high thermal conductivity.
7.4. Thermal properties of MWCNTs polymer nanocomposites
As discussed above that the CNTs have thermal conductivity as high as 6600W/mK predict‐
ed for SWCNTs [94] at room temperature and have experimental value 3000W/mK for iso‐
lated MWCNT. So it is quite expected that the reinforcement of CNTs can significantly
enhance the thermal properties of CNT-polymer nanocomposites. The improvement in ther‐
mal transport properties of CNT polymer composites leads their applications for usage as
printed circuit boards, connectors, thermal interface materials, heat sinks.
8. Conclusion
Synthesis of high quality and reproducible CNTs is still remain a very importnat issue.
Chemical vapor deposition has been found an efficient process for the synthseis of bulk
quantity of CNTs. The CNT-polymer composites have been developed with improved me‐
chanical properties but for actual structural applications, these have to compete with the ex‐
isting carbon fibre based composites. Dispersion of high loading of CNTs and their
alignment in any polymer matrix without sacrificing their mechanical properties is still a
challenge for using CNTs in high performance composites for specific applications such as
as automobile, defence, aerospace, sports etc. CNT- carbon fibres-polymer multiscale com‐
posites could be an alternative route for further improvement in the mechanical properties
of the composites over commercially available CF-polymer composites. Till then electrical
properties of CNT polymer composites provides exciting possibility as antistatic and electro‐
magnetic interference shielding material.
Author details
Veena Choudhary1, B.P. Singh2 and R.B. Mathur2
1 Centre for Polymer Science and Engineering, Indian Institute of Technology Delhi, India
2 Physics and Engineering of Carbon, Division of Materials Physics and Engineering, CSIR-
National Physical Laboratory, New Delhi, India
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Chapter 9

Carbon Nanotubes and Their Composites

Veena Choudhary, B.P. Singh and R.B. Mathur

Additional information is available at the end of the chapter

2.1. Mechanical properties of CNTs

2.2. Electrical properties of CNTs

2.3. Thermal properties of CNTs

3.1. d.c. arc discharge technique

Figure 1. Schematic diagram of dc-arc discharge set-up

3.1.1. Characteristics of CNTs produced by d.c. arc discharge technique

3.2. Chemical vapor deposition

Pyrolysis of organometallic precursors such as metallocenes (e.g. ferrocene) in a furnace pro‐

3.2.1. Characteristics of CNTs Produced by CVD Technique

Figure 6. Raman spectrum of CVD-grown MWCNTs.

3.3. Laser ablation

Figure 7. Schematic diagram of Laser ablation set-up for CNT synthesis

3.3.1. Characteristics of CNTs produced by laser ablation technique

resulting nanotubes as spherical or cylindrical particles after experiments. Through careful

5.1. Composite fabrication techniques

5.1.1. Solvent casting

The solution casting is most valuable technique to form CNTs/polymer nanocomposites.

obtained electrically conductive nanocomposites by dispersing CNT and PMMA in toluene,

5.1.2. Melt mixing method

5.1.3. In-situ polymerization

MWCNT-polycarbonate composite using solvent casting followed by compression mould‐

6. Challenges in MWCNT polymer composites fabrication and possible

6.2. Adhesion between CNTs and polymer

6.3. Chemical functionalization of CNTs

6.4. Dispersion of high loading of CNTs in polymer matrix

6.5. Alignment of CNTs in polymer matrix

7. Properties of the nanocomposites

7.1. Mechanical properties of MWCNTs polymer nanocomposites

duced by cutting with a diamond knife, however no quantitative mechanical measurements

7.2. Electrical properties of MWCNTs polymer nanocomposites

where σ is the composite conductivity, σo is a constant, p the weight fraction of nanotubes, po

Figure 9. General trend of electrical conductivity of CNT polymer composites

7.3. EMI shielding proerties of MWCNTs polymer nanocomposites

SE (dB) = − 10 log( Pt / P0),

7.4. Thermal properties of MWCNTs polymer nanocomposites

Veena Choudhary1, B.P. Singh2 and R.B. Mathur2

[5] Meincke O, Kaempfer D, Weickmann H, Friedrich C, Vathauer M, Warth H. Mechan‐

[8] Hone J. Dekker Encyclopedia of Nanoscience and Nanotechnology 2004.

[10] Ebbesen TW, Ajayan PM. LARGE-SCALE SYNTHESIS OF CARBON NANOTUBES.

[17] Moniruzzaman M, Winey KI. Polymer nanocomposites containing carbon nanotubes.

[67] Ogasawara T, Moon SY, Inoue Y, Shimamura Y. Mechanical properties of aligned

[87] Singjai P, Changsarn S, Thongtem S. Electrical resistivity of bulk multi-walled carbon

[92] Huang Y, Li N, Ma Y, Feng D, Li F, He X, et al. The influence of single-walled carbon

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