1. Synthesis and Characterization of Carbon Nanotube Fibers
(CNTFs) Using Horizontally Spinning Fibers in Chemical Vapor
Deposition (CVD) Technique
By
Prengki Pransisco
MSc By Research

2. OUT LINES

3. INTRODUCTION

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 Detection Hydrocarbon in deep water is using HED (horizontal
electric Dipole) made from Al (Aluminum) Rod with controlled
source electromagnetic.
 This technique is not effective to detection of hydrocarbon in
shallow waters, because of the limited strength of conventional
HED source.
 Due to the critical issue, the improvement HED is needed.
 One of way to improve the technique is to find the good material
to improvement the performance of design HED EM transmitter.
 Carbon nanotube Fibers (CNTFs) is proposing to use in Design
of EM transmitter because of CNTFs has a lot of superb
properties, such as remarkable mechanical stiffness, High
current capacity, high electrical conductivity, high thermal
conductivity and High tensile Strength(Rodney S Ruof et al,
1995).

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 To synthesis the CNTFs is another critical issue, various method
have been proved to synthesis the material.
 The most common method to synthesis carbon nanotubes (CNTs)
are:

 Which one will be going to use?
Arc Discharge Pulsed Laser Ablation Chemical Vapor Deposition

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 This Research will be use Chemical Vapor Deposition (CVD)
Method, why?
 Arc discharge, Pulsed laser ablation methods normally require
High amount of Energy for CNTs formation, the energy is
provided through laser or plasma arch discharge to organize the
Carbon atoms into CNTs and sometimes these methods require
high temperature about 300 C, so both of these method need high
cost.
 In order to get the fibers of CNTs, will be use Horizontally
Spinning technique. This technique is a new in term to get the
fibers of CNTs.
 There are so many challenges in this technique beside
parameters on CVD, including: gravitation force, turbulence of
carrier gas must be considered

7. Literature Review
What is CNTs ?
Carbon nanotubes is Nano-size cylinder of carbon atoms
Carbon nanotubes were discovered by sumio Iijima, in 1991, its
about 22 years ago by used Arc discharge synthesis method
Carbon nanotubes (CNTs) is a strongest and the most flexible
material, because it has modulus young’s of the order of terapascal,
hardest material known and its also has tensile strength about 200
GP, its 100 times stronger than steel

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 There are two type of CNTs :
 Single walled has a wall one atom thick and diameter typically 1.4
nm and 200+ nm in length (I. Kang et. Al, 2006)
 Multi walled has multiple wall and diameter typically 10 nm and 1-
20 micrometer Length. (I. Kang et. Al, 2006)
Single walled CNTs Multi walled CNTs

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 Another Shape of SWNTs if its Rolled into a tube

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 The “armchair” structures, with a = 30°, have metallic character
 The “zigzag” tubes, for which a = 0°, can be either semimetallic or
semiconducting, depending on the specific diameter.
 Nanotubes with chiral angles intermediate between 0 and 30°
include both semimetals and semiconductors. (“Armchair” and
“zigzag” refer to the pattern of carbon–carbon bonds along a
tube’s circumference.)
 So, by determining the structure of CNTs actually the electrical
conductivity can be shown.
 What kind of application that the CNTs can be used ?

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Application of CNTs :
1.Nano electronic Device
2.Electrochemical double layer capacitors
3.Field Emitters
4.Functional emitters
5.Hydrogen Storage
6.Sensors
7.Medical Application, etc
However, there is no one until now using CNTs for EM Transmitter
Application.

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What is CNTFs?
Actually Both of CNTs and CNTFs are almost same under the SEM,
Both are similar to a hollow cylinder.
The different is CNTs made up of unbroken graphene sheet,
otherwise CNTFs is made up from broken graphene sheet, means
that CNTFs is CNTs in form of fibers from CNTs. (Mukul kumar, 2010)
How to produce the Fibers?
The most direct technique for spinning of CNT Fibers was
developed by Windle’s group at University of Cambridge, this
method relies on drawing CNTFs directly and continuously from CVD
synthesis Zone.

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 (Koziol et al, 2009) were developed controlled method for
continuous spinning of fibers from CVD reactor with different
nanotube orientation based on liquid condensation and drawing
from CVD reactor.
 (Jiang Jia et al. 2010) were synthesis CNTFs using CVD and draw
and twist the fibers aligned CNTs arrays.
 The result is there are CNTFs with different structure because of
using two different CVD method

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 (Li song et al, 2012) were offer new technique to spin the fibers of
the CNTs, they were utilizing a motorized pulling or twisting
technique.
 In this Research will offer new technique to spin the fibers i.e.
using horizontally spinning fibers in CVD reactor, where the CNTs
will be deposited in CVD chamber and then direct pulled and twist
the fibers.

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What is CVD actually ?
CVD (Chemical Vapor Deposition) is a popular technique of
growing thin films of various materials, a large variety of crystalline
and amorphous materials can be grown by this method.
Even if CVD is establish deposition technique since early as 1950s,
But until now this method still in used because of relative ease of
creating material of wide range, tend to be low cost that other
method and high purity.
There are Various CVD:
1. PE CVD (Plasma enhanced CVD)
2. Thermal CVD
3. Vapor Phase Growth

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 This research will be used thermal chemical vapor deposition
because of this method tend to be more easy to conduct and to
get the fibers.
 There are parameters in growing CNTs in CVD method:
1. Carbon Source
2. Catalyst
3. Temperature
4. Flow rate
 All of the parameters have an important role in growing aligned of
CNTs

17. Problem Statement
To development high performance of EM Transmitter is needed
material with high remarkable properties, CNTFs is proposed to use
as the material. However, in order to get the Fibers of CNTs is
needed right technique to reduce Defect in the CNTFs.

18. Research Objective
1. To synthesize of carbon nanotube fibers (CNTFs) with
horizontally spinning technique chemical vapor deposition (CVD).
2. To Characterize the characteristic microstructure of CNTFs by
using SEM (Scanning Electronic Microscope)
3. To Investigate properties of the CNTFs in term of Electrical
Conductivity.

19. Scope Of Study
Scope of study in this research are synthesis and characterization of
carbon nanotube fibers (CNTFs) Horizontally Spinning Fibers in
Chemical Vapor Deposition Technique.

20. METHODOLOGY
 Preparation of the catalyst
Catalyst has a strong effect on nanotube diameters, growth rate,
wall thickness, morphology and micro structure of CNTs, In this
research Fe (Iron) will be used as a catalyst, it will be annealed in
vacuum (~10-8 Torr) at ~850oC for 10 minutes to promote the
formation of discrete Fe island. After that the specimen is placed
in a quartz boat the boat is positioned in a CVD reaction furnace.
 Growing Carbon nanotubes (CNTs) and Spinning into carbon
nanotube fibers (CNTFs)
Put sample in the boat Plug on the supply Set
Temperature (800-1200 C) Set voltage (200 V) Pass the
carrier gas (Ar) Pass the carbon source methane (CH4)
CNTs will be deposited on the substrate CNTs is ready to
pulled and twist (spinning).

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 Characterization Using SEM (Scanning Electron Microscope)
The aim of this stage is to investigate characteristic
microstructure of CNTFs, with high energy of beam electron in
raster scan pattern from the SEM, CNTFs will be viewed the
characteristic such as topography, morphology, shape, size and
other properties like electrical conductivity.

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 Research Flow Chart
EQUIPMENT SET UPEQUIPMENT SET UP
PREPARATION CARBON SOURCE AND
CATALYST
PREPARATION CARBON SOURCE AND
CATALYST
GROWING CARBON NANOTUBE FOREST
SPINNING CNTFs
GROWING CARBON NANOTUBE FOREST
SPINNING CNTFs
Analysis
Defect of
CNTFs
Analysis
Defect of
CNTFs
YES
NO
CHARACTERYZATION MICROSTRUCTURE OF
CNTFs USING SEM
CHARACTERYZATION MICROSTRUCTURE OF
CNTFs USING SEM
VALIDATION AND DISCUSSIONVALIDATION AND DISCUSSION

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 Gant Chart
Item
Research
Activities
2013 2014
3 4 5 6 7 8 9 10 11 12 1 2 3 4 5 6 7 8 9
1
Literature Review for carbon
nanotube fiber
2
Set up equipment,
preparation catalyst and
carbon source
3
Growing carbon nanotube
(CNTs) and spinning CNTFs
5
Characterization Carbon
Nanotube Fibers Using SEM
6
Analysis and
Validation
7
Conference
Submission
8
Thesis
Writing Up

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 Milestone
ITEM MILESTONE
DATE OF
COMPLETION
1 Literature review August 2013
2 Preparation Catalyst September 2013
3 Growing CNTs and spinning CNTFs November 2013
4 Characterization of the CNTFs January 2013
5 Analysis and Validation result March 2014
6 Final Report May 2014

25. References