Synthesis of Carbon Nanotubes

Diamond & Related Materials 50 (2014) 135150
Contents lists available at ScienceDirect
Diamond & Related Materials

journal homepage: www.elsevier.com/locate/diamond
Arc discharge synthesis of carbon nanotubes: Comprehensive review

Neha Arora , N.N. Sharma
Department of Mechanical Engineering, Birla Institute of Technology and Science, Pilani, India
a r t i c l e
i n f o
Article history:
Received 2 June 2014
Received in revised form 24 September 2014
Accepted 3 October 2014
Available online 13 October 2014
Keywords:
Arc discharge
Carbon nanotube synthesis
a b s t r a c t
In quest to synthesize high quality carbon nanotubes in bulk, different routes have been proposed and
established over the last two decades. Arc discharge is the oldest and among the best techniques to produce
high quality carbon nanotubes. Though this synthesis technique has been explored for a long time, the nanotube
growth mechanism is still unclear and the growth conditions lack strong correlation with the synthesized product. In this review, we attempt to present the mechanism of nanotube growth in arc discharge and the factors affecting its formation. In order to understand the physics of this mechanism, the effect of experimental parameters
such as setup modication, power supply, arc current, catalyst, pressure, grain size, electrode geometry and temperature on size and yield of the nanotubes has been detailed. The variation in synthesis parameters employed in
literature has been presented along with challenges and gaps that persist in the technique.
2014 Elsevier B.V. All rights reserved.
Contents
1.
2.
Introduction . . . . . . . . . . . . . . . . . . . . . . . .
Nanotube growth in arc discharge . . . . . . . . . . . . . .
2.1.
Arc discharge setup . . . . . . . . . . . . . . . . .
2.2.
Growth mechanism of carbon nanotubes in arc discharge
2.2.1.
Vapour phase growth . . . . . . . . . . . .
2.2.2.
Liquid phase growth . . . . . . . . . . . . .
2.2.3.
Solid phase growth . . . . . . . . . . . . .
3.
Physics of nanotube growth in arc discharge . . . . . . . . . .
3.1.
Effect of power supply . . . . . . . . . . . . . . . .
3.1.1.
Type of power supply . . . . . . . . . . . .
3.1.2.
Effect of voltage . . . . . . . . . . . . . . .
3.1.3.
Effect of arc current . . . . . . . . . . . . .
3.1.4.
Frequency . . . . . . . . . . . . . . . . .
3.2.
Carbon precursors in arc discharge . . . . . . . . . .
3.3.
Effect of grain size . . . . . . . . . . . . . . . . . .
3.4.
Role of catalyst . . . . . . . . . . . . . . . . . . .
3.5.
Role of atmosphere . . . . . . . . . . . . . . . . .
3.6.
Effect of pressure . . . . . . . . . . . . . . . . . .
3.7.
Role of temperature . . . . . . . . . . . . . . . . .
3.8.
Effect of setup modication . . . . . . . . . . . . .
3.9.
Effect of cathode shape . . . . . . . . . . . . . . .
3.10.
Size and yield of CNT in arc discharge . . . . . . . .
4.
Conclusion . . . . . . . . . . . . . . . . . . . . . . . . .
Appendix A.
. . . . . . . . . . . . . . . . . . . . . . . . .
Appendix B.
. . . . . . . . . . . . . . . . . . . . . . . . .
References . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Corresponding author.
E-mail address: neha.arora@pilani.bits-pilani.ac.in (N. Arora).
http://dx.doi.org/10.1016/j.diamond.2014.10.001
0925-9635/ 2014 Elsevier B.V. All rights reserved.
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N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150
1. Introduction
Carbon nanotubes (CNTs) possess excellent mechanical, electronic,
thermal, optical and chemical properties which have revolutionized the
state-of-the-art in nanotechnology. CNTs have been broadly classied
as Single-Walled Nanotubes (SWNTs), Double-Walled Nanotubes
(DWNTs) and Multi-walled Nanotubes (MWNTs). Researchers have devised different routes to synthesize CNTs from various carbon precursors.
The most popular and widely used nanotube synthesis techniques are:
Arc Discharge, Chemical Vapour Deposition and Laser Ablation [116].
Apart from these methods, Hydro-thermal synthesis [17], Electrolysis
[18,19], and Ball milling [20,21] methods have also been used.
CNTs were rst synthesized by Iijima [22] in 1991 using arc discharge method. Over the last two decades, researchers have demonstrated a successful use of this technique in the production of high
quality CNTs. A bar graph shown in Fig. A.1(a) (Appendix A) depicts
the number of papers published year wise on CNT synthesis using arc
discharge. We gained some insights of nanotube growth process and
understood the fundamental role of few arc discharge parameters.
However, the literature lacks comprehensive study on the mechanism
of nanotube formation and needs strong correlation between growth
conditions and synthesized nanotubes. The requiem to understand the
role of growth conditions lays in selective growth of nanotubes using
arc discharge, which remains largely unexplored.
For researchers taking up the nanotube synthesis using arc discharge, the availability of comprehensive review on the process is quintessential. Previously, Ando and Zhao [7] discussed the synthesis of
SWNTs and MWNTs using arc discharge. In 2007, Harris [8] investigated
the models of nanotube growth in arc discharge and laser ablation processes. In 2010, Ando [10] presented the chronological aspect of arc
grown nanotubes in hydrogen atmosphere. In 2011, Tessonnier and
Su [12] briey discussed the nucleation and growth process of nanotube
in arc grown CNTs. In 2011, Prasek et al. [13] reviewed the different
routes of nanotube synthesis. In 2012, Journet et al. [16] discussed low
or medium temperature techniques to synthesize CNTs.
The present review updates and details on experimental attempts to
manufacture carbon nanotubes using this technique. The growth mechanism of nanotubes, as explored in literature has been briefed. It further
discusses the role of synthesis parameters like setup modication,
power supplies, arc current, catalyst, pressure, grain size, electrode geometry and temperature on the nanotube production. Few parameters like
pressure and catalyst have been investigated quantitatively in literature
but the exact role of the growth conditions still requires extensive investigation. The review has been divided into four sections. Section 2
discusses the nanotube growth in arc discharge. Section 3 outlines the

physics of CNT growth in arc discharge process and the role of growth
conditions on nanotube formation, which is followed by the conclusion.
2. Nanotube growth in arc discharge
2.1. Arc discharge setup
Arc discharge is the electrical breakdown of a gas to generate plasma.
This old technique of generating arc using electric current was rst used
to produce CNTs by Iijima [22] in 1991. A schematic of an arc discharge
chamber is shown in Fig. 1. The chamber consists of two electrodes
which are mounted horizontally or vertically; one of which (anode) is
lled with powdered carbon precursor along with the catalyst and the
other electrode (cathode) is usually a pure graphite rod. The chamber is
lled with a gas or submerged inside a liquid environment. After
switching on the power supply (AC or DC), the electrodes are brought
in contact to generate an arc and are kept at an intermittent gap of
12 mm to attain a steady discharge. A constant current is maintained
through the electrodes to obtain a non-uctuating arc for which closed
loop automation is employed to adjust the gap automatically. A uctuating arc results in unstable plasma and the quality of the synthesized product is affected. The arc current generates plasma of very high temperature
~40006000 K, which sublimes the carbon precursor lled inside the
anode. The carbon vapours aggregate in the gas phase and drift towards
the cathode where it cools down due to the temperature gradient. After
an arc application time of few minutes the discharge is stopped and cathodic deposit which contains CNTs along with the soot is collected
from the walls of chamber. The deposit is further puried and observed
under an electron microscope to investigate their morphology.
2.2. Growth mechanism of carbon nanotubes in arc discharge
Over the last two decades, researchers have investigated and suggested growth conditions for nanotube formation based on their experimental observations. Despite seminal studies, no clear understanding
of the growth mechanism has been developed and a critical study lies
in understanding the physics of this mechanism which certainly helps
in predicting the optimum growth conditions of nanotubes. In this section, we present an outline of the synthesis mechanism in the growth of
CNTs in arc discharge.
The two electrodes are brought in contact and upon application of
voltage, constant current ows through them. The electric current results in resistive heating and raises the temperature of the electrodes.
Glass window
Gas Inlet
Gas Outlet
Deposition
Cathode
Anode
Precursor +
Catalyst
Closed Chamber
Base
Power Supply
Fig. 1. Schematic of an arc discharge setup.
The anode is moved back to maintain a desired gap (~1 mm) between
the electrodes for continuous deposition of carbon vapours. Meanwhile,
the high temperature ~ 40006000 K facilitates the breakdown of the
surrounding gas lled inside the chamber. The gas ionizes into electrons
and ions and results in hot plasma formation between the electrodes.
Stable plasma grows uniformly over the electrode surface corresponding to stable anode and cathode voltage. The collisions of ions and electrons in the plasma emit photons responsible for the glow in plasma.
The electrons are ejected from cathode hit the anode at high velocity
and sputter the carbon precursor lled at the centre of the anode. The
high temperature resulting from resistive heating results in sublimation
of carbon precursor and converts them into carbon vapours. The carbon
vapours are decomposed in carbon ions. The decomposition occurs due
to high heat ux or thermal energy of the plasma. The carbon vapours
aggregate to form viscous carbon clusters and drift towards the cathode,
which is cooler as compared to anode. The carbon vapours undergo a
phase change and get converted into liquid carbon. The temperature
gradient at cathode and quenching effect of atmosphere solidies and
crystallizes the liquid carbon to form cylindrical deposits that grow
steadily on cathode. The cathodic deposit is composed of a grey outer
shell and a dark inner core. The grey deposit consists of the rolls of
graphene sheets known as carbon nanotubes. The addition of hexagonal
carbon atom clusters lead to the growth of nanotube. However, instability in plasma leads to capping of nanotubes. The diameter of the nanotubes is governed by the density of carbon vapours in the plasma.
Variation in temperature gradients strongly affects the diameter distribution of CNTs produced and nanotubes are formed in bundles due to
van der Waals interaction.
In reported literature, mechanism of nanotube synthesis has been
explained by few researchers [2342] but the exact growth mechanism
is still debatable due to different theories of nanotube growth in vapour
phase [34], liquid phase [33], solid phase [35] and crystal phase [43].
2.2.1. Vapour phase growth

Gamaly and Ebbesen [34] detailed the vapour phase growth of
MWNTs and suggested that the carbon vapours condense and nucleate
to form nanotubes. They proposed a model for the velocity distribution
of carbon vapours and divided the carbon vapours in two groups depending upon their velocity distributions. One group of carbon vapours
will have the isotropic (Maxwellian) velocity distribution. The other
group of carbon particles has higher velocities than the rst group
which is due to the acceleration of carbon vapours between the electrodes. According to Gamaly and Ebbesen, the nanotube growth occurs
in three steps seed formation, tube growth and termination. The
seeds are formed as a result of the two velocity distributions. In the beginning, the carbon vapours possess Maxwellian distributions which result in nanoparticle formation. Upon increasing the current, the other
group of directed carbon vapours results in open structures or seeds.
Once the current reaches a stable value, the carbon ions ow perpendicular to the cathode surface resulting in the nanotube growth. Finally the
nanotube growth is terminated due to instabilities in the plasma. A similar theory has also been validated by other researchers [4447].
2.2.2. Liquid phase growth

The liquid phase growth model was suggested by Heer [33] in 2005.
He proposed that the liquid carbon solidies to result in nanotubes.
They found beads of amorphous carbon within the nanotubes which result during solidication of liquid drops. According to them, when the
electric arc is applied to heat the carbon precursor, the electrons
bombarding the surface result in localized heating, which causes the
surface to liquefy. The liquid droplets are ejected from the anode and
are drifted towards cathode. These globules of liquid carbon tend to
cool at the cathode surface. The cooling propagates from outer layer towards the centre, resulting in multilayered tubular structures.
137
2.2.3. Solid phase growth

Solid phase growth of nanotubes was proposed by Harris et al. [48]
in 1994. They found that nanotubes are synthesized by high temperature heat treatment of fullerene soot. Based on their observations,
they proposed that initially carbon vapours in the gas phase condense
onto the cathode to form fullerene soot. Since the temperature of cathode is high due to continuous arc, the fullerene soot is converted to
MWNTs via the seed-growth-termination process. The requiem for
this process is rapid heating of fullerene soot since slow heating of fullerene results in nanoparticle formation [35]. In order to improve
upon the existing theories, experimental investigations are necessary
to develop a strong correlation between the synthesized product and
input parameters. In literature, large number of experimental reports
has been published on arc discharge synthesis of nanotubes which has
been discussed in the next section.
3. Physics of nanotube growth in arc discharge
The arc discharge process is dependent on several parameters like
type of power supply, environment, pressure, electrode geometry, catalyst and temperature that inuence the quality and quantity of the synthesized product. Researchers have studied the variation of these
parameters and have attempted to establish an optimal range for
improving quality and quantity of CNTs using arc discharge. In order
to develop the physics of nanotube growth in arc discharge, we rst
need to understand the role of various synthesis parameters on the
product. The implication of these parameters and their corresponding
physics is detailed in the next subsections respectively.
3.1. Effect of power supply
The power supply controls the arc current and voltage which govern
the energy distribution of electron discharge. This affects the plasma temperature that plays decisive role in the product of arc discharge. In this
section we have detailed the affect of type of power supply, voltage, arc
current and frequency on quality and yield of synthesized nanotubes.
3.1.1. Type of power supply
The type of power supply plays a vital role in nanotube formation.
When DC arc current is applied across the electrodes, as shown in
Fig. 2(a), continuous emission of electrons from cathode bombards the
anode at high velocity. The cathode diameter is usually larger than the
anode diameter, which results in lower current density of cathode than
anode. Thus, a high temperature gradient across the electrodes is observed which sublimes the carbon precursor lled inside the anode and
results in the formation of CNTs. In AC arc discharge, the current alters periodically across the electrodes and no deposition is observed at either
side of the electrodes. The carbon vapours y out of the plasma due to
thermal effects which results in CNT formation at the walls of the chamber as shown in Fig. 2(b). In pulsed arc method as shown in Fig. 2(c),
CNT formation takes place with some short range and long range pulses,
normally of the millisecond width. Pulse strikes the anode surface and it
begins to vaporize and deposition takes place on the cathode.
In case of DC supply, the ionized gas drifts towards cathode and hinders the continuous deposition of carbon ions on cathode. In order to remove the gas ions, the cathode should not be negatively charged. This
problem may be overcome by using an AC or pulsed power supply.
The disadvantage of using AC supply is that the formation of nanotubes
occurs only in positive cycle and thus the yield is reduced. Thus, pulsed
arc discharge is the most favourable for nanotube formation.
Ashraf et al. [49] compared the continuous and pulsed arc discharges
and their effect on nanotube formation. They observed variation in type
and quantity of atomic carbon species on using different power supply.
According to them, the continuous arc discharge results in higher
amount of C2 which is the precursor for nanotube formation. The pulsed
discharge contained additional amount of C1 due to disintegration of C2,
138
Fig. 2. Schematics showing the formation of CNTs using different power supplies.
which does not form closed carbon structures. However, pulsed arc is
advantageous as it provides more control over the process.
The pulsed arc is found to be more energetic than a continuous arc.
The energy of an electron is higher at the time of ejection and it takes
microseconds for the electron to attain the Maxwellian energy distribution. Thus, continuous bombardment of anode with pulses of width
shorter than this time results in higher electron energy which increases
the yield [50]. On contrary to this, continuous power supply has lesser
electron energy distribution. We have categorized the existing literature based on the type of power supply used in the synthesis of CNTs.
Pie charts showing the percentage of papers published in these categories are shown in Fig. A.2 (Appendix A). It can be clearly seen from
Fig. A.2(a) that the DC power supply is most widely used to synthesize
CNT using arc discharge method.
The rst attempts to synthesize MWNTs [22] and SWNTs [51,52]
using DC power supply were reported in 1991 and 1993 respectively.
Some of the early insightful works include large scale synthesis of
CNTs in helium atmosphere by Ebbesen and Ajayan [53] in 1992. In
1995, Wang et al. [54] produced MWNTs in hydrogen atmosphere
using arc discharge. In 1997, Journet et al. [55] demonstrated large
scale synthesis of SWNTs in helium atmosphere. Shi et al. [56] in 1999
demonstrated bulk synthesis of SWNTs in high pressure helium atmosphere. High yields of 6.5 g/h CNTs have been demonstrated by Zhao
[57]. In 2004, Itkis et al. [58] produced 515 g CNTs using DC arc discharge. Chronological attempts using DC power supply have been listed
in Table B.1 (Appendix B).
Researchers have also used AC power supply of constant frequency
to generate arc between the electrodes. The advantage of using AC arc
discharge is the formation of deposits on the wall of chamber. Very
few experimental attempts have been made to synthesize CNTs using
AC arc discharge. In 1992, Ebbesen and Ajayan [53] reported CNTs
using AC arc discharge. In 1997, Zeng et al. [59] reported MWNTs at
700 A arc current. In 1999, Ohkohchi [60] rst reported SWNTs using
AC arc discharge. In 2007, Matsuura et al. [61] reported poor quality of
CNT synthesized by AC arc discharge. CNT yield in AC is found to be
smaller than that of DC as it is produced during one part of cycle [53].
Chronological attempts using AC power supply have been listed in
Table B.2 (Appendix B).
Few researchers have synthesized carbon nanotubes using pulsed
DC power supply. Parkansky et al. [62] suggested that the pulsed arc is
advantageous over other power supply as no pressure chamber is required and can be performed in open air. Yield is found to be increased
in case of pulsed as compared to DC supply [63,64]. Sugai et al. [65] have
found yield of SWNT increases as pulse width increases. Cathode is also
found to be consumed by pulsed arc method [66]. One observation from
pulsed discharge is that the CNT formation is reported at low current
levels. Chronological attempts using pulsed power supply have been

listed in Table B.3 (Appendix B).
3.1.2. Effect of voltage
In arc discharge, voltage is applied across the electrodes to generate
electrical breakdown of the dielectric gas. The voltage across the electrodes for CNT synthesis ranges between 15 and 30 V. This voltage
must be kept constant for stable plasma. The sudden change in arc voltage results in the formation of bamboo like structures as observed by
[67]. Scalese et al. [68] suggested that the major effect of voltage variation was found to be the spatial distribution and sharpness of CNT pillars
in the deposit. Jahanshahi et al. [69] observed fullerenes at 10 V and
observed CNTs upon increasing the voltage to 30 V. Antisari et al. [70]
observed deposits of amorphous carbon with few nanotubes for voltages less than 22 V and found no cathodic deposits for voltages higher
than 27 V. They have also reported an increase in quality of nanotubes
when the voltage is increased from 15 V to 20 V. However synthesis at
high voltages (~700 V) has also been reported [25,61,71-74].
Besides voltage, the synthesis time has also been investigated in literature for CNT formation. Generally, the voltage across the electrodes is
maintained for 30120 s. However CNTs have been synthesized at time
ranging from milliseconds [75,76,77] to high synthesis time of 15 min
[78,79], 20 min [80,81,82], 40 min [83], 30150 min [84], 60 min [85],
6090 min [58], 12 h [86], and 330 h arc run time [65]. This is an interesting parameter and raises a question of impact of arc application
time in the formation of carbon nanotubes.
3.1.3. Effect of arc current
One of the signicant parameters in arc discharge method is the arc
current. It affects the quality, yield and size of synthesized nanotubes. In
an arc discharge apparatus, arc current results in emission of electrons
from cathode which travel at high velocity towards anode. These electrons hit the anode surface which results in sputtering of carbon precursors. Upon increasing the arc current, the number of electrons striking
the anode surface increases, thereby sputtering more carbon precursor
from the anode. The applied current produces resistive heating which
results in high temperature. Due to high temperature, the carbon precursor lled in anode sublimes to form carbon vapours and nucleates
at cathode resulting in nanotube formation. There also exists a minimum discharge current called as chopping current at which the plasma
production is insufcient and leads to arc extinction.
During the synthesis, non-uctuating current of an order of 50100
A is maintained to ablate the anode. Ebbesen and Gamaly [34] suggested
that the current density for synthesis of CNTs should be around 165
195 A/cm2. Cadek et al. [87] studied the dependence of arc current on
the yield of nanotubes and concluded that the yield increases as current
density is varied from 165 A/cm2 to 195 A/cm2. Nishizaka et al. [88]
found the optimal current density for SWNT formation as 250270 A/
cm2. Matsuura et al. [89] observed better yields of SWNT at a current density of ~450 A/cm2. In literature, vast variations have been reported in arc
current, from 2.5 A to 900 A, which creates an ambiguity of the optimum
arc current rating. A comparative view of the current ratings used in literature has been shown above in Fig. A.1(b) (Appendix A). We have not
included the experiments where ranges of current values were used. It
can be observed from the graph that majority of the experiments have
been conducted between the range of 50 and 100 A.
Effect of variation of current has been investigated in the literature
[87,88,89]. It has been observed that at currents below 30 A, the arc is
unstable and lower yields are obtained. The anomalies in the current
levels corresponding to CNT formation are noteworthy. Okada et al.
[90] have reported a low current synthesis of 120 A whereas Delong
He et al. [91] suggested that the nanotube formation takes place at current levels beyond 100 A. Takizawa et al. [92] found the highest nanotube yield at 100 A. Researchers have produced CNTs at low arc
current of 210 A [77,78,93,94,95]. However, high arc currents of
700 A [59] and 900 A [96] have also been employed to produce CNTs.
139
It has been observed that as current increases, the yield increases [74,
89,97] however increasing the arc current does not improve the structure of CNT [68]. He et al. [91] observed that the increase in arc current
reduces the amount of SWNTs and favours the formation of amorphous
carbon particles. Zhao et al. [98] studied the variation of pressure along
with the variation in arc current. Tang et al. [99] investigated reduction
in the arc current by changing the shape of cathode. Lange et al. [75] observed that a carbon precursor with smaller grain size requires lesser arc
current for nanotube formation. However, it raises an interesting debate
on the optimum current requirements for nanotube formation. Thus,
there is a critical need to develop a strong correlation between
optimum current levels and formation of nanotubes.
3.1.4. Frequency
The frequency of the power supply has been found to affect the quality of the deposits produced in arc discharge. First reported by Ohkohchi
et al. [60] in 1999, AC arc discharge has been found to produce high
quality SWNTs. In literature, the effect of variation in frequency has
not been explored. Kia and Bonabi [78] found that at low frequencies
of 50 Hz, better growth is observed at anode, however at high frequencies of 400 Hz, the cathode soot and production rate increase. This can
be an interesting area for investigation and may lead to value addition
to existing growth mechanism of CNTs.
3.2. Carbon precursors in arc discharge
The synthesis of CNTs is carried out by sublimation of a carbon
precursor using an external power source; in case of arc discharge, the
applied current ablates the carbon precursor to form carbon vapours,
which nucleates to form a nanotube. A pie chart in Fig. A.2(b) shows
the percentage of papers published on CNT synthesis using various carbon precursors. It can be observed from the gure that most of the arc
discharge synthesis of CNTs has been carried out using graphite as precursor. It is an excellent conductor of heat and electricity and is commercially available in high purity. When graphite is subjected to high
current, the lattice structure breaks and releases C1 or C2 carbon species
that vaporize due to high temperature.
Some groups have used carbon black as a raw material to produce
CNTs [31,88,100,101,102,103]. Carbon black is amorphous in nature,
easily available material on earth and can be a potential precursor to synthesize CNT due to techno-economic reasons. The synthesis of CNTs from
carbon black will require larger current value than graphite. Carbon black
upon application of current gets rst converted to graphite and then
forms tubular structures of CNTs. Lange et al. [75] have used carbon
black as starting material to synthesize SWNT. Chen et al. [104] have
utilized carbon black as a dot carbon source for the production of DWNT.
Some researchers have used coal as a starting material to synthesize
CNTs. Coal is a mixture of aromatic and aliphatic hydrocarbon molecules,
which are highly reactive in nature. Qiu et al. [105] have discussed coal as
an ideal starting material for large synthesis of DWNTs. When high arc
current passes through coal, the weak linkages between the polymeric
aryl structures get broken down into alkyne and aromatic species that further form DWNTs. Coal contains sulphur, which favours the growth of
DWNTs and affects the diameter distribution of the nanotubes produced.
Other carbon sources like fullerene waste soot [106], toluene [90], tire
powder [107], poly-vinyl-alcohol [108], MWNT/carbon nanobers [109]
and other hydrocarbons [32,86] have been utilized to produce CNTs by
arc discharge method. Whereas graphite is the mostly investigated precursor, the other precursor materials need further understanding and
investigations.
3.3. Effect of grain size
One of the less explored aspects of arc discharge is the effect of grain
size on current requirement and nanotube production. It seems logical
that a smaller particle requires lesser energy to vaporize. Solid state
140
properties namely cohesive energy of cathode and anode play vital role
in the quality of the nanotubes formed. The cohesive energy [110] is
found to depend upon the size of nanoparticle [111].
Lange et al. [75] used carbon precursors with different grain sizes
and found that the current requirement reduces drastically by changing
the grain size. Labedz et al. [103] investigated the effect of particle size
and the carbon density of the electrode. They found that the anode
with smallest particle size and more electrode density yields lesser
CNTs and more carbonaceous particles. Also, the particle size may affect
the diameter of the synthesized nanotubes. It was observed that larger
grain size results in smaller diameter CNT [103]. This may be a potential
area for investigation and validations are required to develop an association with formation of nanotubes.
3.4. Role of catalyst
The catalyst used in arc discharge synthesis of CNTs is usually a
metal, which is powdered and lled in either side of the electrode
along with a carbon precursor. The metal should have low boiling temperature and high evaporation rate to act as a good catalyst in nanotube
formation [23]. On application of arc current, the metal atoms vaporize
along with the carbon precursor. The metal particles agglomerate with
carbon vapours and nucleate at arc reactor walls. There is no established
reason for deposition of SWNTs on walls of chamber instead of cathode
and is an open area for investigation. A probable reason for this
behaviour may be that the carbon vapours along with the liquid metal
move towards cathode in the plasma. Since metal particles do not
stick to the surface of the cathode, they y away due to their momentum and form SWNTs at the walls. A graphical representation of the suggested mechanism is shown in Fig. 3.
The catalyst favours the growth of SWNTs than MWNTs. Lin et al.
[112] experimentally conrmed that the presence of metal catalyst in
gas phase and on the surface of the cathode alters the temperature distribution and prevents the growth of MWNTs on cathode. The most
commonly used catalysts are Ni, Fe, and Co along with Y, S, and Cr
added as a promoter. Mostly, SWNTs are observed in the presence of
catalyst, whereas MWNTs are produced in its absence. However some
reports on MWNT formation in the presence of catalyst have been reported in literature [23,69,76,108,113,114,115,116]. The interesting observation among these reports is that MWNT synthesis occurs upon the
use a binary catalyst. Zhao et al. [117] reported that no CNT formation
occurs without the use of catalyst.
Few researchers have investigated the role of various catalysts on the
quality of the CNTs formed. Among the metals, Ni and Fe have been most
widely used catalyst for the growth of high quality CNTs. Both Ni and Fe
increase the yield and quality of CNTs. Nickel is found to produce more
crystalline nanotubes. Ni is mixed with elements like Y, Mo, Fe, Co, Cr to
improve the synthesized product. Fe is generally added with sulphur or
W to facilitate growth of SWNTs. The drawback of using Fe as catalyst is
the formation of its oxides (Fe2O3) which doesn't act as catalyst and
Fig. 3. Role of catalyst in growth of CNTs.
retards the growth of SWNTs. Li et al. [118] suggested that the Fe promotes the length of the nanotubes. Zhao et al. [81] suggested that the addition of sulphur to Fe catalyst results in the development of a core/shell
at the cathode due to different melting points. This core/shell promotes
the growth of DWNTs. Zhao et al. [117] observed a more uniform distribution of ACNT diameter upon using FeS catalyst as compared to Ni/Co alloy.
Wang et al. [119] suggested that sulphur plays a major role in the formation of branched CNTs. It forms an active site on the surface of the catalyst
where nucleation of carbon vapours takes place. Ando et al. [120] observed that sulphur promotes the growth of CNTs by removal of the terminating species at the nanotube ends. The catalyst may also control
the wall number of synthesized CNTs. Yang et al. [121] observed a control
on wall number of CNTs on addition of KCl to NiCo mixture. Montoro
et al. [80] observed that VO groups also promote nucleation of carbon vapours in the synthesis of CNTs. Qiu et al. [122] observed that KCl also promotes the formation of DWNTs.
The size of nanotubes can be readily controlled by using appropriate
size of metal catalyst particles. The carbon vapours move along with the
metal particles and nucleate on these to form nanotubes. Thus, the size
of metal particles plays a vital role in nanotube diameter distribution.
The concentration of metal particles is found to affect the yield of nanotubes produced. The composition of catalyst also plays a major role in
the existence of CNTs. Wang et al. [108] reported that the maximum
concentration of iron particles in the anode composition must not exceed 10% for CNT formation. One reason for this maybe that larger concentration of catalyst particles restricts the motion of carbon vapours
towards cathode. Keidar [27] suggested that SWNT synthesis is
governed by catalyst carbon phase diagram. The effect of various catalysts on CNT formation as reported in literature is tabulated in Table 1.
3.5. Role of atmosphere
The atmosphere plays an important role in thermo-ionic effects, plasma formation, and provides the thermal growth of CNT and the necessary
annealing effects. When the arc current ows through the electrodes, the
gas gets ionized due to high temperatures and plasma is formed. The ionized gas acts as a highly conducting medium which provides transfer of
mass on either side. The ions in the plasma are thermally agitated and
provide the necessary energy for movement of carbon vapours. The atmosphere also plays a signicant role in the thermal growth of CNTs. The
Table 1
Effect of catalyst on CNT formation.
Base
catalyst
Mixture
used
Comments
Ni
Ni
NiY
Promotes the growth of SWNT [23]

Y alone cannot synthesize CNT formation [58]
Addition of Y to Ni reduces the yield [123]
Y promotes the growth of SWNT [55]
Mo does not affect CNT formation [90]
MoFe favours CNT formation [90]
Results in SWNT formation [121]
Results in DWNT formation [121]
Results in MWNT formation [113]
Increases yield and purity [60]
Diameter of SWNT increases with sulphur [124,125]
Affects yield and diameter of MWNT [108]
Addition of sulphur promotes growth of DWNT and
increases the yield [81]
Retards the growth of CNT [126]
Increases the yield of SWNT [127]
Tungsten reduces the diameter and increases
yield of SWNT [128]
Improves yield of SWNT [115]
Produces smaller diameter CNT than Ni [129,56]
Increases the yield [130]
Superior catalyst for DWNT production [109]
Increases the mean diameter of DWNT [66]
Addition of sulphur promotes CNT production [104]
Fe
NiMo
NiMoFe
NiCo
NiCo + KCl
NiCr
NiHo
NiCoFeS
Fe
FeFeS
FeFe2O3
FeFe3O4
FeW
Ca
RhPt
Co
FeFe(C5H5)2
Ca
RhPt
Co
CoCoS
141
thermal conductivity of the atmosphere provides annealing effects at

the cathode which is essential for nanotube formation. The atmosphere
also regulates the temperature of plasma depending on its ionization potential. The gas with higher ionization potential will require large arc current for breakdown. Thus, the choice of atmosphere depends on its
ionization potential and thermal and electrical conductivity.
The arc chamber is pressurized with a gas like nitrogen, hydrogen,
helium or argon or immersed in a liquid environment. Hydrogen has
the highest thermal conductivity and is regarded as the most efcient
quencher in nanotube growth. Zhao and Ando [131] suggested that hydrogen promotes the growth of CNTs and reduces the carbonaceous
materials by forming hydrocarbons with them. Li et al. [132] found
that hydrogen results in a cleaner CNT surface as it selectively etches
the amorphous carbon impurities. However, Zhao [133] suggested
that pure hydrogen is unfavourable for mass production of SWNT due
to the instability of arc discharge plasma. Tang et al. [134] observed
that rapid introduction of hydrogen prevents the ends of nanotube
from closing. Due to this problem, hydrogen is generally mixed with a
noble gas like argon or helium to stabilize the plasma. Liu et al. [135]
found that changing of gas from hydrogen to helium promotes the
growth of SWNT. Shi et al. [129] observed that helium atmosphere
strongly affects the yield of SWNTs. Farhat et al. [28] controlled the diameter of nanotubes by changing the composition of argonhelium
gas ratio. Su et al. [136] investigated the effect of CO concentration on
the amount of impurities present in SWNTs. They suggested that
lower concentration of CO should be preferred for better SWNT yield.
Ando et al. [79] observed the increase in yield upon addition of nitrogen
to hydrogen when compared to H2Ar mixture. The H2N2 has more enthalpy than H2Ar which promotes the evaporation of CFe mixture.
Apart from the gaseous atmosphere, liquid environments have also
been used to produce CNTs. In case of liquid environments the CNTs
are found to be oating on the surface of the liquid. The most popular
choice of the liquid environment in the literature is deionised water.
Few works [116,126] have synthesized CNTs in NaCl solution owing to
its good electrical conductivity, better cooling ability than deionised
water, cheaper than liquid nitrogen and helium. NaCl dissociates into
Na+ and Cl ions which provide better ionic conductivity to the plasma.
The concentration of Na+ ions is a critical parameter for better yields.
The excess of Na+ ions hinders the locomotion of carbon vapours
from anode and reduces the yield of the SWNTs [126]. Other solutions
like LiCl [69], H3PO4 aqueous solution [80], and beer froth [137] have
been used as atmosphere in synthesizing CNTs using arc discharge.
Kim et al. [137] suggested that the agglomerating effect of both beer
froth and carbon nanotubes helps in obtaining a cleaner product. The
CNTs stick to beer froth and the other carbonaceous materials get separated out. The effects of different atmosphere in arc discharge chamber
on yield, quality and size of nanotubes are listed in Table 2.
3.6. Effect of pressure
In arc discharge method, the role of pressure is to provide energy to
the gas molecules and to act as a wall for a steady ow of ions between
the electrodes. The optimum range of pressure for CNT synthesis has
been found ranging from 300 to 700 Torr. At pressure below 300 Torr,
the yield is found to be very low as the density of ions is low resulting
in unstable plasma. Whereas at high pressure, more number of ions
participate in the plasma thereby restricting the motion of carbon vapours
from anode to cathode and decreases the yield. That is why high pressure
is unfavourable for the synthesis of CNTs and very less number of researchers has used pressure beyond 700 Torr as shown in Fig. A.1(c).
In literature the effects of pressure on yield and quality of synthesized
nanotubes have been vastly explored. Cui et al. [142] found that the nanotube yield decreases for low and high pressures of nitrogen. Grebenyukov
et al. [141] found that the efcient pressure for nitrogen is 350 Torr. In
case of air, 4590 Torr has been found to be the optimum pressure
[143]. However, yield is reduced upon increasing the air pressure from
142
Table 2
Effects of different environments on CNT formation.
Type of atmosphere
Effect on yield and quality of nanotubes
Effect on size of nanotubes
Comments
Hydrogen
Formation of MWNT is highly graphitized

and has crystalline perfection [120]
H2 discharge is better compared to He as it

produces twice aspect ratio nanotubes [120]
H2He produces in growth of CNT with small
diameter [138] as compared to H2Ar.
Hydrogen is more effective for

MWNT formation [97]
Diameter of synthesized CNT in air atmosphere

is smaller than in He [97]
Argon produces smaller diameter CNT compared
to He [27,28]
Diameter of MWNTs decreases with the increase
of the N2 [141]
Diameter distribution can be controlled by varying
the mixture ratio of H2 and N2 gas [79].
He results in uniform cathode deposit [67]
Hydrogenhelium
Hydrogenargon
Helium
H2 added to argon increases the yield [139,83]

Yield of SWNT increases in He [130]
Argon
Nitrogen
N2 at low pressure yield more SWNT

[140] and MWNTs [70]
Hydrogennitrogen
Open air
CO
Better yield in open air than He [29]
Krypton
NaCl solution
Yield of SWNT is more in Kr compared to Ar [65]
Nitrogen atom incorporated for

closure of CNT [142]
CO plays requisite role for selective diameter

growth of SWNT [136]
Observed short CNTs in NaCl solution [126]
40 to 300 Torr [82]. Kim and Kim [97] observed MWNTs in air and helium
at 300 Torr and 500 Torr respectively. The pressure versus yield trend for
helium has been studied by few groups [28,73,129,144] and pressure
ranging from 500 to 700 Torr has been found to be optimum. However reversal in trend has been shown by Park et al. in 2002 [124] who observed
a decrease in yield on increasing the pressure from 100 to 500 Torr. Also,
Shi et al. [56] reported high yield of 2.5 g/h for helium pressure of
1520 Torr. Optimum hydrogen pressure is found to be 500 Torr [57].
The yield increases from 100 to 700 Torr but decreases beyond 700 Torr
[122]. Farhat et al. [28] have reported that the optimum argon pressure
is 100 Torr. It may be concluded from the reports in literature that the optimum pressure condition for high yield of CNTs has been found to be
~500 Torr. However, some variations that have been reported need to
be investigated for better understanding of the growth mechanism.
3.7. Role of temperature

The temperature ionizes the gas and forms the plasma. It simultaneously sublimes the carbon precursor and provides thermal ux for
decomposition of carbon vapours into ions. It is responsible for
thermo-ionic emission of carbon ions and nally helps in nucleation of
carbon vapours at cathode to form CNTs. Temperature variation in plasma signicantly affects the quality and size of the CNTs. Temperature required for growth and nucleation in arc discharge synthesis is achieved
by the electric arc. The temperature increases as the current density is
increased, thereby subliming the anode at a faster rate. Higher temperature results in more crystalline CNTs. The temperature of the plasma is
regulated by the thermal properties of atmosphere. Hydrogen plasma
generates higher temperature of 36003800 K, whereas Argon plasma
restricts the plasma temperature to 22002400 K. The temperature gradient across the two electrodes is dependent on the diameter of the
electrodes. A smaller diameter anode has higher current density and
has high temperature which is favourable for sublimation of carbon precursor, whereas cathode with larger diameter has less current density
and is cooler than anode and facilitates nucleation of CNTs. This is why
cathode diameter is selected to be greater than anode diameter.
In literature, the effect of temperature on nanotube formation has not
been vastly explored and is a potential area of investigation for better understanding of the growth of CNTs. Among few published reports, Kim
et al. [42] have discussed that nanotube growth occurs below 2000 C
even though inter-electrode temperature approaches more than
4000 C. Matsuura et al. [61] have suggested optimum range for CNT formation of 10001250 C. Keidar [27] observed nanotube formation in region of low plasma temperature of 13001800 K, where carbon reacts to
form large molecules or clusters. Lange et al. [145] have found an average
plasma temperature ranging from 4000 to 6500 C in water. Joshi et al.
[29] have found that temperature requirement for MWNT is the least
followed by DWNT and SWNT for nucleation and growth. Sugai et al.
[65] suggested that SWNT formation takes place in strong annealing condition. Doherty and Chang [100] observed a decrease in yield of MWNT on
an increase in temperature. Nishio et al. [146] observed high yield at high
plasma temperature. Liu et al. [135] found that an increase in temperature
increases the yield of CNT. However Zhao and Liu [147] suggested that
SWNT diameter reduces with an increase in temperature but yield increases. Zhao et al. [117] suggested that optimum temperature for CNT
formation is 600 C beyond which diameter decreases.
3.8. Effect of setup modication
The basic arc discharge apparatus described above and shown in Fig. 1
has been modied by the researchers over the passage of time to improve
the quality, size and yield of CNTs. Zhao and Liu [147] reported an increase
in yield of SWNTs by using six anodes. Researchers [29,4042] have used
a rotating carbon cathode for a homogeneous micro-discharge resulting
in good quality nanotubes. Joshi et al. [29] found a 5055% increase in
yield at lower electrode disk rotation speed compared to higher disk
speeds. Lee et al. [40] suggested that rotating electrodes result in continuous growth of nanotubes as the carbon vapours move out due to centrifugal force resulting in uniformly distributed plasma.
Kanai et al. [148] have proposed a gravity free discharge for high
yields. Ando et al. [149] inclined the cathode and anode at an angle of
30 to improve the yield of the process. Horvath et al. [86] also investigated the effect of angle between two electrodes immersed in water and
found that highest yield is obtained at 90 inclination. Upon inclination
of the electrodes, a majority of the product does not get deposited on
the cathode and the deposition mostly ies away to the walls, thereby
increasing the yield of SWNTs.
3.9. Effect of cathode shape
The geometry of the electrodes is also a potential area of research and
greatly affects the quality of the product. Usually the anode is chosen to be
of smaller diameter than cathode which results in increased current density at anode, thereby subliming the precursor at lower current levels.
Cathode being larger in diameter will be at low temperature due to less
current density and allows the liquid carbon to nucleate. Thus, ow of carbon ions is achieved from anode to cathode. The relative size of electrodes
affects the plasma temperature distribution which directly affects the
synthesized product. However, upon using similar electrodes the deposition is not found on cathode but on the chamber walls [59].
The effect of change in electrode shape and size has been studied in literature by few groups. Researchers [150,151] have observed deposition
on anode for cathode diameter less than anode diameter. Joshi et al.
[29] suggested that the cathode surface topography may play a decisive
role in nanotube formation. Raniszewski et al. [152] have suggested that
anode tip diameter should be lower than 10 mm. Fetterman et al. [153]
have found an increase in yield for smaller diameter anode. Wang et al.
[154] suggest a reduction in cathode area in order to increase SWNT production which is formed at the walls of chamber. Tang et al. [99] have
found a reduction in current requirement by using a cupped cathode
and outer diameter of synthesized MWNT increases. Nishio et al. [146]
and Shi et al. [56] found the yield decreases upon using a sharp cathode.
Kia and Bonabi [78] concluded that the shape of electrodes affects the
yield of CNTs.
3.10. Size and yield of CNT in arc discharge

The major concern of arc discharge CNT synthesis is to improve the
yield of the product. However, arc discharge technique has not been successful in producing pure CNTs at large scale due to difculty in controlling the experimental parameters. The yields of nanotubes depend on
the arc current, catalyst composition and its particle size, atmospheric effects and electrode shape and composition. Nishio et al. [146] suggested
that the yield of nanotube depends on the cooling rate. However, cooling
rate is dependent on arc current, cathode size, and thermal conductivity
of gas and temperature gradient. Typical yields are of the order of few milligrams for a synthesis that runs several minutes and thus makes this
technique less preferred over CVD. However researchers have improved
the yield through this technique by controlling the synthesis parameters.
Few studies related to modied setups have been already been discussed
above. Some reports on variations in current and pressure values, electrode diameters, catalyst composition and atmosphere have been suggested to optimize the arc discharge. The typical yield of nanotubes
obtained in arc discharge is ~2050 mg/min per synthesis. However
few attempts to produce CNT through semi-continuous and continuous
arc discharge have been made and yields of 2 g/h [155] and 6.5 g/h [57]
have been achieved. The control of size and diameter in nanotubes is
still unanswerable. The size of SWNTs may be controlled by using the desired size of catalyst particles [28]. SWNT diameter increases by 0.2
143
upon increasing the argon helium ratio by 10%. The effect of various
parameters on size and yield of nanotubes has been tabulated in Table 3.
4. Conclusion
We have reviewed the arc discharge method for synthesis of carbon
nanotubes and have tabulated the synthesis conditions reported in
literature for CNT formation. We have discussed the growth mechanism of nanotube formation and have presented discussions on
physics of the individual effect of the critical parameters on the
quality and yield of the product as explored in literature. Some of
the observations are:
The most signicant parameter of arc discharge synthesis is the arc
current. Large variations in current ratings corresponding to nanotube
formation have been reported creating an ambiguity. Thus, there is a
critical need to further investigate and study its effect to develop an
optimum arc discharge.
The role of atmosphere has been studied vastly and similar observations between pressure and nanotube formation have been reported.
Temperature effects in nucleation and growth of nanotubes in arc discharge technique are largely unexplored and considerable studies are
required to understand the vital role of temperature in arc discharge
synthesis of CNT.
Electrode geometry is a decisive parameter in the production of CNT.
Further explorations are necessary to understand the exact role of geometry and shape of electrodes in carbon nanotube formation.
DC power supply has been commonly employed for arc discharge.
However, effect of use of different types of power supply (AC and
pulsed) has not been reported in large numbers.
Most of the synthesis has been done using graphite as a precursor,
whereas other carbon materials like carbon black, and coal have not
been utilized and are a potential area of investigation.
Mass production of carbon nanotubes is also a concern. Few attempts
to manufacture bulk synthesis have been reported; there is lot of
scope for improvisation by modifying the arc discharge parameters
for better yield.
There is a strong need for theoretical investigations and mathematical
models to approximate arc discharge synthesis and develop the
growth mechanism of CNT in arc discharge.
Though a large number of experimental reports have been published
in the last two decades, this eld still needs experimental and
Table 3
Effect of different growth parameters on size and yield of CNT.
Parameter
Effect on size of nanotube
Effect on yield
Catalyst
Yield of 4 g/h obtained by optimizing the composition

of catalyst [109]
Increase in yield with catalyst [127]
Temperature
Electrodes
Atmosphere
Grain size
Current
Setup modication
Pressure
Diameter of SWNT increases with sulphur [124,125]

Diameter increases by using Co [66]
Tungsten reduces the diameter of SWNT [128]
Observed smaller diameter SWNT when CaNi catalyst [56]
Increase in temperature reduces the diameter [147,117].
Diameter of MWNT increases with an increase in temperature [114]
Electrode has signicant effect on diameter and purity of SWNT [152]
Increasing the cathode diameter from 0.8 to 2 cm; length of SWNT
increases from 1.2 to 1.8 m [156]
Observed short CNT in NaCl solution [126]
When atmosphere changes from H2Ar to H2He, it results in smaller diameter CNT [138],
Ar affects the diameter of SWNT in HeAr mixture [28,27]
Diameter distribution of SWNT changes by varying the kind of inert gas [157]
Diameter of synthesized CNT in air atmosphere is smaller than in He [97].
Smaller diameter CNTs were formed with larger grain size [103]
Increasing the current increases the diameter [158]
Diameter under 0G condition is 3.7 times larger than 1G [148]

Growth of SWNT with small diameter can be suppressed when
pressure of CO greater than 4 kPa [136]
SWNT diameter was independent of pressure in pure He environment [119]
Smaller anode diameters increase the yield [153]

Adjusted the angle between two electrodes and found
that 90 angle produces the best yield [149,86].
Krypton increases the yield [65]
Increase in current increases the yield [74]

Maximum yield at 8 A [32]
Increase in yield by rotating electrodes [29,82]
Yield increases as pressure increases from 250 to
400 Torr [159]
Low yield for pressure below 100 Torr [144]
144
Appendix A
Fig. A.1. (a): Bar graph showing papers published on arc discharge synthesis of CNT. (b): Variation in current values used in literature to synthesize CNTs using arc discharge. (c): Bar graph
showing number of papers published at different range of pressure.
(a)
(b)
(c)
Fig. A.2. Pie chart showing percentage of papers published on arc discharge synthesis of CNT (a) using different power supplies, (b) various carbon precursors (c) under different atmosphere.
Appendix B
Table B.1
Arc discharge synthesis of CNT using DC power supply.
Yearauthor
1991Iijima [22]
1992Ebbesen and Ajayan [53]
1993Iijima et al. [51]
1993Bethune et al. [52]
1994Lin et al. [112]
Arc current, synthesis

time
100 A
95105 A
Precursor
Catalyst
Graphite
Graphite
Graphite
Graphite
Co
Environment, pressure
Type of CNTs,
diameter, yield
Argon, 100 Torr

Helium, 500 Torr
MWNT, 520 nm
CNT, 220 nm
Helium, 100500 Torr
SWCNT, 20 nm
145
Table B.1 (continued)

Yearauthor

time
Precursor
1994Guerret-Plecourt et al. [160]

1995Wang et al. [54]
1995Zhou and Seraphin [161]
1996Loiseau and Pascard [162]
1997Lange et al. [72]
1997Journet et al. [55]
1997Zhao et al. [98]
1998Saito et al. [130]
1998Chang et al. [163]
1998Zhao and Ando [131]
1999Takizawa et al. [92]
1999Yudasaka et al. [123]
1999Shi et al. [164]
1999Zhao et al. [165]
1999Shi et al. [56]
1999Kiselev et al. [166]
1999Liu et al. [41]
2000Ishigami et al. [167]
2000Tang et al. [134]
2000Shi et al. [129]
2000Ando et al. [168]
100110 A, 3060 min

90 A
220 A/cm2
100110 A, 3045 min
6070 A, 4 min
100 A, 2 min
20100 A
70 A & 100 A, 13 min
5565 A
50 A, 3060 s
100 A, 10 s
100 A, 10 s
40100 A
50 A, 3060 s
40 A, ~120 min
80 A, 60 s
150 A, 3 min
60 A
58 A
4060 A, ~120 min
50100 A, ~3 min
Type of CNTs,
diameter, yield
Graphite
Graphite
Helium, 0.6 bar

Hydrogen, 50700 Torr
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Helium, 0.6 bar

Helium, 500 Torr
Helium, 500 Torr
Helium, 1520 Torr
Helium, 500 Torr
Hydrogen, 60 Torr
Helium, 500 Torr
Helium, 500 Torr
Helium, 100700 Torr
Hydrogen, 60 Torr
Helium, 1520 Torr
Helium, 100 Torr
Hydrogen, 200 Torr
Liquid nitrogen
Helium, 400 Torr
Helium, 500700 Torr
Helium, 400700 Torr
CNT
MWNT
Branched CNT
CNT
2000Ando et al. [169]

2000Cheng et al. [155]
2001Ando et al. [149]
2001Srivastav et al. [170]
2001Farhat et al. [28]
2001Hutchison et al. [83]
2001Kanai et al. [148]
2001Shimotani et al. [171]
2001Li et al. [172]
2001Ando et al. [120]
2001Lai et al. [173]
50 A, 3060 s
150 A, 3 min
50100 A, 3 min
200 A, 3 min
100 A
7580 A, 40 min
2040 A, 30 min
100 A, 2 min
30 A, 5 min
50 A, 3060 s
6090 A
2002Osvath et al. [174]

2002Jain et al. [96]
2002Tang et al. [99]
2002Li et al. [132]
2002Jong Lee et al. [40]
2002Soo et al. [124]
2002Ando et al. [67]
2002Sheng et al. [175]
2002Cadek et al. [87]
2002Zhen-Hua et al. [144]
2002Doherty and Chang [100]
2003Antisari et al. [70]
2003Doherty et al. [101]
2003Saito et al. [125]
2003Qiu et al. [176]
2003Jung et al. [177]
2003Zhao et al. [133]
2003Cui et al. [142]
2003Osvath et al. [178]
2003Tarasov et al. [179]
2004Liu et al. [135]
2004Waldorff et al. [73]
2004Nishio et al. [146]
2004Wang et al. [108]
100 A, 2 min
900 A, 1520 min
7585 A
50 A, 1 min
80120 A
6080 A, 5 min
60 A, 10 min
8595 A
~57 A
5080 A,10 min
100 A, 1 min
3070 A, 1 min
100 A, 1 min
50 A
5070 A, 20 min
80 A
3070 A, 3 min
3040 A, 10 min
3544 A, 3 min
100 A, 2 min
50130 A
100 A, 10 min
78.5 A, 180 s
60 A, 28 s
60450 A
80 A, 5 min
2004Bera et al. [150]

2004Cui et al. [180]
2004Zhao and Liu [147]
2004Jinno et al. [181]
2004Keidar and Waas [182]
2004Itkis et al. [58]
2004Qiu et al. [183]
2004Sano et al. [184]
2005Murr et al. [107]
2005Hahn et al. [185]
2005Shang et al. [186]
2005de Heer et al. [33]
2005Ando et al. [79]
35 A
3544 A, 50120 s
60 A, 5 min
50 A, 3060s
Graphite
Graphite
Graphite
Graphite
90 A, 6090 min
5070 A
60 A, 45 s
50100 A
60 A
50 A
100 A
4070 A, 15 min
Graphite
Coal
Graphite
Tire Powder
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Hydrocarbon
(xylene, pyrene)
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Carbon black
Graphite
Carbon black
Graphite
Coal
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Polyvinyl alcohol
Graphite
Catalyst
NiCoY
Ru/Pd/Rh/Pt
NiY2O3
NiY
NiY
NiY
NiY
NiFeCoFeS
NiY
NiY
NiY
NiCoFeS
NiY
FeSNiSCoS
Fe
Fe
NiY
NiCo + YNi2
NiY
Fe
NiCo

Hydrogen, 200 Torr
Helium, 400700 Torr
Helium, 500 Torr
Helium & argon, 495 Torr
Hydrogenargon, 350 Torr
Helium, 600 Torr
Heliumhydrocarbons, 150500 Torr
Helium, 15 kPa
Hydrogen, 8 kPa
Helium, 300600 Torr
Helium, 660 mbar
Helium, 800 Torr
Helium, 400 Torr
HydrogenCO
Helium, 500 Torr
Helium, 100500 Torr
Hydrogen, 13 kPa
Helium, 375 Torr
Helium, 500 Torr
Helium, 100200 Torr
Helium, 100 Torr
Liquid nitrogen, deionised water
Helium, 100 Torr
Hydrogenhelium, 300 Torr
Helium, 490 Torr
Liquid nitrogen
Deionised water
Nitrogen, 0.02900 Torr
Helium, 500 Torr
Helium, 400800 Torr
Hydrogen, 50 kPa
Helium, 500700 Torr
Helium, 760 Torr
Helium, 260 Torr
Hydrogen, 500 Torr
PdCl2
Nitrogen, 0900 Torr
Helium, 400 Torr
Hydrogennitrogen, 70 Torr
NiY
Ni
Fe
Helium, 680 Torr

Helium, 250570 Torr
Liquid nitrogen
Helium, 250 Torr
Hydrogen, 13 kPa
Helium, 30120 Torr
Helium, 375 Torr
Hydrogennitrogen, 200 Torr
SWNT, 520 nm
MWNT, 1 nm
SWNT, 1.28 nm
CNTs, 1040 nm
MWNT, 120 nm
SWNT
SWNT
SWNT, 1.3 nm, 1.5 g
MWNT
SWNT, 5 g
MWNT, 115 mg/min
SWNT, 20 nm, 100 mg
MWNT, 44 mg/min/cm2
CNT
SWNT, 5 g
SWNT, 1.281.52 nm,
1.24 g/min
MWNT
SWNT, 100 mg
SWNT, 1.341.53 nm
CNT
SWNT
DWNT, 2.74.7 nm
SWNT
MWNT
MWNT/SWNT, 0.34 nm
MWNT
CNT, 1050 m
Branched CNT, 10 & 20 nm
MWNT
MWNT
MWNT, 1020 nm
CNT
SWNT, 1020 nm
MWNT
CNT
MWNT
SWNT, 1020 nm
MWNT
MWNT
MWNT
DWNT, 25 nm
SWNT, 1020 nm
MWNT, 2050 nm
SWNT
Nanocarbon/CNT
MWNT
Branched CNT, 10 nm
SWNT
Amorphous CNT
SWNT, 2 nm
CNT
MWNT
Amorphous CNT,
720 nm, 6.5 g/h
CNT
MWNT/SWNT
SWNT
MWNT, 1 nm
CNT
SWNT, 515 g
MWNT
SWNT
MWNT, 550 nm
MWNT
MWNT, 1.1 nm
MWNT, 320 nm
SWNT
(continued on next page)
146

Yearauthor

time
Precursor
Catalyst
Type of CNTs,
diameter, yield
2005Yang et al. [121]

2005Guo et al. [139]
2005Li et al. [109]
2005Wang et al. [126]
100120 A
3070 A
120 A, 3 min
50 A, 60 s
Graphite
Graphite
Graphite
Graphite
Fe
NiCoFeS
Hydrogenargon, 70 Torr H2, 50 Torr argon

Hydrogen, 240 Torr
NaCl
2005Xin Lv et al. [84]

2005Makita et al. [140]
2005Yao et al. [187]
2005Montoro et al. [80]
2005Zhao et al. [117]
2005Tang et al. [188]
2005Wang et al. [189]
2006Doherty et al. [102]
2006Wang et al. [154]
2006Chen et al. [104]
2006Qiu et al. [122]
2006Wang et al. [190]
90120 A, 30150 min

5060 A
90 A, 510 min
65 A, 20 min
80 A
8595 A
50 A, 60 s
100 A, 1 min
70 A
120 A
70 A, 15 min
70 A, 15 min
25 A & 55 A
Graphite
Graphite
Graphite
Helium, 530550 Torr

Helium, argon, nitrogen 501000 Torr
Helium, 600 Torr
H3VO4 aqueous solution
Hydrogen, 500 Torr
Helium, 400 Torr
Deionised water, open air
Helium, 100 Torr
Helium, 120 Torr
Hydrogenargon
Hydrogen, 350 Torr
Argon, 8090 kPa
DWNT
SWNT
DWNT, 4 g/h
SWNT, 0.89 nm
MWNT, 8.9 nm
SWNT
SWNT
SWNT, 1030 nm, 0.61 g
SWNT/MWNT, 2030 nm
Amorphous CNT, 720 nm
CNT
CNT
CNT
SWNT, 10 g
DWNT
DWNT
CNT, 3080 nm
SWNT
2006Zhao et al. [157]

2006Suzuki et al. [191]
2006Yusoff et al. [25]
2006HH Kim and HJ Kim [97]
2006Wang et al. [119]
2007Cazzanelli et al. [113]
2007Okada et al. [90]
2007Mathur et al. [192]
50 A, 320 min
60A, 10 min
16 A
4080 A
7080 A, 10 min
40100 A
60 A, 100 s
120 A, 30s
100120 A
Hydrogen-inert gases, 50500 Torr

Nitrogen, 760 Torr
Air, 100760 Torr
Helium, 5060 kPa
Helium, 500 Torr
Helium, 375 Torr
Toluene
Helium, 600 Torr
SWNT
MWNT, 900 mg
CNT
MWNT
Branched CNT
MWNT/SWNT
MWNT
CNT
MWNT/SWNT
2007Song et al. [114]

2007Guo et al. [193]
2007Duncan et al. [194]
2007Qiu et al. [105]
2007Sun et al. [127]
2007Delong He et al. [91]
2007Xing et al. [195]
2008Grebenyukov et al. [141]
2008Li et al. [196]
2008Fetterman et al. [153]
2008Joshi et al. [29]
2008Keidar et al. [197]
2008Keidar et al. [198]
2008Kim et al. [137]
2009Kim et al. [199]
2009Charinpanitkul et al. [158]
2009Ha et al. [200]
2009Labedz et al. [103]
100 A, 58 min
1070 A
50 A
80 A & 100 A, 5 min
5060 A, 10 min
70100 A, 10 min
80280 A
3075 A
65 A
90 A
4070 A, 12480 s
150 A/cm2
7080 A
180 s
10 A, 2 min
15 A
50250 A
3070 A, 20 min
4060 A
Hydrogen, 300 Torr

Xylene ferrocene, 30500 Torr
Deionised water
Heliumargon, 500700 mbar
Helium, 375525 Torr
Helium, 500 Torr
Deionised water
Nitrogen, 50760 Torr
Helium, 300 Torr
Helium, 600 Torr
Open air, helium, 500 Torr
Helium, 500700 Torr
Helium, 500700 Torr
Beer foam
Beer foam
Liquid nitrogen
Hydrogenargon, 30 kPa
MWNT
MWNT/SWNT
MWNT, 520 nm
MWNT
DWNT, 15 nm
SWNT, 0.8 g
SWNT
MWNT, 1020 nm
SWNT
SWNT
CNT
MWNT
SWNT
SWNT
MWNT
MWNT
MWNT, 825 nm
SWNT
SWNT
2009Hoa et al. [201]

2009Jahanshahi et al. [69]
2010Jahanshahi et al. [116]
2010Scalese et al. [30]
2010Scalese et al. [68]
2010J Qiu et al. [106]
85 A/cm2, 1 min
100 A, 60 s
80 A, 60 s
80 A, 30 s
85110 A
Hydrogen, 400 Torr

LiCl
NaCl
Liquid nitrogen
Liquid nitrogen
SWNT
MWNT/SWNT, 7.7 mg/min
MWNT
MWNT
CNT
DWNT, 1.081.44 nm
2011Nishizaka et al. [88]
10 min
Helium, 100 Torr
SWNT
2011Ding et al. [202]

2011Hou et al. [203]
2011Zhang et al. [204]
2011Su et al. [136]
2012Tripathi et al. [205]
2012Kim et al. [42]
2012Zhao et al. [206]
2012Wu et al. [26]
2012Su et al. [156]
2012Liang et al. [24]
2012Zhang [138]
2012Cai et al. [151]
2013Mohammad et al. [159]
2013Fang et al. [128]
120 A
150 A, 3 min
120 A
100 A
105 A, 58 min
100 A
80 A
120 A
90 A
80 A, 100 A, 150 A, 8 min
50 A
80 A, 20 min
210 A, 4 min
80 A, 20 min
7595 A, 5 min
80 A, 10 min

Hydrogen, 200 Torr
Hydrogen, 240 Torr
HeliumCO, 225 Torr
CNTs
SWNT, 1 g
MWNT
SWNT
CNT
MWNT
MWNT
SWNT
SWNT
MWNT
Few-walled CNT,110 nm
MWNT
CNT, 4060 nm
DWNT
CNTs, 3444 mg
SWNT, 1030 nm,
100200 mg
Graphite
Graphite
Graphite
Carbon Black
Graphite
Carbon black
Graphite
Coal
Graphite/carbon
black
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Toluene
Graphite + coke
powder
Graphite
Xylene
Graphite
Coal
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite/carbon
black
Graphite
Graphite
Graphite
Graphite
Graphite
Fullerene
waste soot
Graphite +
coal + carbon
black
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
NiCo
NiHO2O3
Fe
NiY
CoCoS
FeSKCl
Fe
Fe
NiCoTi
NiCr
NiMoFe
CoSPt
Ferrocene
Fe
Fe3O4
NiCo
NiY2O3
NiOY2O3
NiY
NiY
Fe
FeNiMo
NiMo
NiMo
NiFeCo
NiY
NiY2O3
NiY
FeRh
NiY2O3
FeW
Argon
Air, 60 Torr
Helium, 375 Torr
Helium, 760 Torr
Air, 40300 Torr
Hydrogen, 50 Torr
Air, 50 Torr
147

Yearauthor

time
Precursor
Catalyst
Type of CNTs,
diameter, yield
2013Su et al. [143]

2014Chaudhary et al. [207]
90 A
90 A
Graphite
Graphite
FeS
Air, 0.75135 Torr

Methane, 100, 300 and 500 Torr
Few-walled CNT, 1.66 nm

MWCNT, 1020 nm
Table B.2
Arc discharge synthesis of CNT using AC power supply.
Yearauthor
Arc current, synthesis time
Precursor
Type of CNTs, diameter, yield
1992Ebbesen and Ajayan [53]

1997Zeng et al. [59]
1999Ohkohchi M [60]
2003Biro et al. [74]
2006Horvath et al. [86]
2007Matsuura et al. [61]
2010Matsuura et al. [89]
2012Jia-Shiang Su [93]
2013Yousef et al. [208]
2013Kia and Bonabi [71]
100 A
700 A
85 A, 12 min
4585 A
40 A, 12 h
70100 A
110120 A
620 A
2.5 A, 1.4 ms
75 A
50 A, 510 min
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Benzene
Graphite
Graphite
Hydrocarbon
Helium, 500 Torr

Helium, 140 Torr
Helium, 400 Torr
Deionised water
Deionised water
Helium, 600 Torr
CNT, 220 nm
MWNT
SWNT
MWNT, 510 mg/min
MWNT, 1035 nm
MWNT
CNT
MWNT
CNT
MWNT, 0.6g/h
MWNT, 50100 nm
Argon, 760 Torr

Air
Deionised water
Argon, 525 Torr
Table B.3
Arc discharge synthesis of CNT using pulsed DC power supply.
Yearauthor
Arc current, synthesis time
Precursor
Catalyst
Type of CNTs, diameter, yield
2000Sugai et al. [65]

2001Murooka et al. [94]
2003Sugai et al. [209]
2004Parkansky et al. [62]
2006Imasaka et al. [63]
2007Roch et al. [64]
2008Tsai et al. [95]
2008Yoshida et al. [66]
2009Tsai et al. [76]
2010Jia-Shiang Su [77]
2012Kia and Bonabi [78]
2012Takekosh et al. [85]
22 A, 330 h
12 A, 13 s
4060 A
7100 A
30A, 4 h
100 A
22.5 A, 8001300 s
50 A
2.5 A, 1 ms
35 A, 1.2 ms
10 A, 15 min
20 A, 60 min
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Graphite
Acetone
Graphite
NiCo
Argon, 500 Torr

Argon, 250500 Torr
Argon
Open air
De-ionized water
Argon, 75 Torr
Open air
Argon, 760 Torr
Open air, 760 Torr
Open air
Argon, 525 Torr
De-ionized water
SWNT, 210 mg
Nanoparticles
DWNT
MWNT
MWNT
SWNT
MWNT
DWNT
MWNT
MWNT
MWNT
CNT, 5 nm
theoretical investigations to establish a correlation between the synthesis parameters and nucleation of carbon nanotubes and help us better
understand the growth mechanism of carbon nanotubes.
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Synthesis of Carbon Nanotubes

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Diamond & Related Materials 50 (2014) 135150

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Diamond & Related Materials

Arc discharge synthesis of carbon nanotubes: Comprehensive review

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

discusses the nanotube growth in arc discharge. Section 3 outlines the

Fig. 1. Schematic of an arc discharge setup.

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

2.2.1. Vapour phase growth

2.2.2. Liquid phase growth

2.2.3. Solid phase growth

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

levels. Chronological attempts using pulsed power supply have been

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

Fig. 3. Role of catalyst in growth of CNTs.

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

Promotes the growth of SWNT [23]

thermal conductivity of the atmosphere provides annealing effects at

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

Effect on yield and quality of nanotubes

Effect on size of nanotubes

Formation of MWNT is highly graphitized

H2 discharge is better compared to He as it

Hydrogen is more effective for

Diameter of synthesized CNT in air atmosphere

He results in uniform cathode deposit [67]

H2 added to argon increases the yield [139,83]

N2 at low pressure yield more SWNT

Better yield in open air than He [29]

Yield of SWNT is more in Kr compared to Ar [65]

Nitrogen atom incorporated for

CO plays requisite role for selective diameter

3.7. Role of temperature

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

3.10. Size and yield of CNT in arc discharge

Effect on size of nanotube

Yield of 4 g/h obtained by optimizing the composition

Diameter of SWNT increases with sulphur [124,125]

Diameter under 0G condition is 3.7 times larger than 1G [148]

Smaller anode diameters increase the yield [153]

Increase in current increases the yield [74]

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

Arc current, synthesis

Argon, 100 Torr

Helium, 100500 Torr

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

Table B.1 (continued)

Arc current, synthesis

1994Guerret-Plecourt et al. [160]

100110 A, 3060 min

Helium, 0.6 bar

Helium, 0.6 bar

2000Ando et al. [169]

2002Osvath et al. [174]

2004Bera et al. [150]

Hydrogen, 30120 Torr

Helium, 680 Torr

N. Arora, N.N. Sharma / Diamond & Related Materials 50 (2014) 135150

Table B.1 (continued)

Arc current, synthesis

2005Yang et al. [121]

Hydrogenargon, 70 Torr H2, 50 Torr argon