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Carbon nanotubes synthesis: an overview

Shashank Pardhikar, Shivdeep Singh, Varun Kansal, Daniel Aggarwal

14045085, 1405093, 14045109, 14045117

Before 1991, only 3 forms of carbon allotropes were known: diamond, graphite and
fullerene. It was in this year that Iijima discovered this very important form of
carbon allotrope known as Carbon Nanotubes. After a couple of years, he observed
Single Walled Nano Tubes (SWNTs) which opened the gates of immense research
possibilities in this field. Many applications have been developed since then and
the unique physical and chemical properties of Nanotubes have been unraveled.
In a SWNT a cylinder of graphene sheet is formed by rolling over to a diameter of
approximately 1.4 nm while in a Multi Walled Nano Tube (MWNT) there are
concentric cylinders having a separation of 0.34-0.36 nm. The force binding the
nanotubes together into bundles is strong Van Der Walls force therefore their
tensile strength is approximately a hundred times that of steel. The Youngs
modulus value is 1.2 TPa.

Arc Discharge method was initially used for the production of C 60 fullerenes. It is
most common and easy method to produce carbon nanotubes. This method
produces CNTs by arc vaporization of carbon rods as electrodes, separated by
distance of approximately 1 mm, in an enclosure of inert gas and low pressure. A
direct current of 50-100A and potential difference 20V is used. The disadvantage
of this method is that it produces a complex mixture of different components
which is difficult to separate and requires further purification.

Ball milling and annealing method i.e. a mechano-thermal process of carbon

nanotube synthesis is an easy but not very effective method of production of
carbon nanotubes. It produces multi-walled carbon nanotubes with dangling ends
or encapsulated with iron particles. The amorphization and nanocrystallization on
isothermal annealing isn't homogenous because of the nature of milling. Wet
milling produces no results.

Tiny-high quality nanotubes were prepared by HiPco continuously but the methods
of HiPco and CoMoCat are generally used only for scientific purposes.

Single and defect free SWNTs have not obtained in previous methods. For
nanotubes to be of any use, it should be defect free and it requires large scale
synthesis of nanotubes. CVD can be the solution for these problems. Carbon rich
gases are used as carbon feedstock in CVD. Efficiency of CVD is high compared to
other methods. By controlling different parameters in CVD experiments, it is
possible to obtain control over the formation of different types of nanotubes. On
supported transition-metal oxide catalysts, high quality SWNT were formed by
chemical vapor deposition of methane. Various factors are involved in
production of SWNT.

Nanotubes have a wide range of untapped potential applications in diverse

technological areas such as energy, aviation, automobile, pharmaceutics and
chemical industry, where theyre used as gas adsorbents, composite
reinforcements, reactors, catalyst supports, chemical sensors and probes.


Electric Arc method

In electric arc method, two graphite rods as electrodes at different potential are
placed in an enclosure filled with inert gas at low pressure(50-700 mbar).Anode
is moved closer to cathode until an arc appears and the electrodes are kept at
the distance of 1 mm for the whole duration of the process. After
depressurization and cooling of the chamber the nanotubes together with the
by-products are collected. Most nanotubes deposit on cathode. The efficiency
of this method is approximately 60%.

Ball Milling and Annealing -

In the milling and annealing method for the synthesis of carbon nanotubes, dry
milling of commercial graphite powder is done at 900 RPM and 78G centrifugal
force for 5 hours. The nucleation process was catalyzed by 4 wt.% Iron. The
crystalline hexagonal graphite gets converted to amorphous carbon powder
which is then annealed isothermally at 1600 degrees Celsius in presence of
inert Argon for 6 hours. Presence of multiwalled carbon nanotubes are reported
post annealing process.

HiPco and CoMoCat -

In the HiPco method, Fe(CO)5 catalyst was used with carbon-monoxide at high
pressure to obtain very thin single-walled carbon nanotubes. The nanotubes
obtained in this method had minimum structural defects and very high intrinsic
selectivity. Carbon nanotubes were produced at a high rate with minimum
wastage of carbon-monoxide.
The CoMoCat method gets its name from the catalyst mixture of cobalt and
molybdenum. The temperature required for this method was 700-950C for the
decomposition of CO into carbon and CO2 and this method produced no by-

Carbon Vapor Deposition (CVD)

For a methane CVD experiment, Fe2O3/alumina catalyst was prepared.

The Catalyst was kept in a quartz tube mounted in a tube furnace. Argon gas
was passed through the quartz tubes at 1000C. Methane (99%) replaced with
the Ar flow. Flow rate of methane was 6150 cm3/min at 1.25 atm. pressure. For
10 min methane flowed and it was replaced with Ar and furnace was cooled to
room temperature. Microscopic studies were done to evaluate the products.

Arc-discharge method suffers from disadvantage of being an economically
unfeasible method for large scale production of carbon nanotubes, in spite of
yielding high quality carbon nanotubes. Ball milling and annealing method
produces multiwalled nanotubes but is an easier method of generation of
nanotubes. Chemical Vapor Deposition is the most advantageous economic
method for large scale production of high-purity Single Walled Carbon
Nanotubes (SWNT). Different innovations and research in catalysts and carbon
feedstock bring in the scope of diverse possibilities. Alternatives of CVD
process such as CoMoCAT & HiPco can be replicated to large scale
processes with continuous process & high yield.

Remarkable opportunities have been brought by carbon nanotubes in the field

of basic science and nanotechnology. Growth of defect free carbon nanotubes
on a large scale is the main problem which needs to be addressed in future
work. Control over nanotube growth will open new possibilities in many real-
world applications. Carbon nanotubes are widely believed to bring ground-
breaking innovations to the developing world and shall be a huge force of
technological advancement in the twenty-first century.
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Physics Letters 292 (1998) 567574.

2. Guler and Evin, Carbon nanotubes formation by short-time ball milling and annealing of graphite,
February 2012, p. 183 187.

3. Shi, Lian, Zhou, Gu, Zhang, Iijima, Zhou, Yue and S. Zhang, Mass-production of single-wall carbon
nanotubes by arc discharge method, Carbon 37 (1999) 14491453.

4. Shifrina, Synthesis of Carbon Nanotubes.