EFFECT OF CARBON NANOTUBE STRUCTURE ON ENHANCING THERMAL PROPERTIES OF NANOFLUIDS
SYAZWANI BINTI ZAINAL ABIDIN
IMRAN SYAKIR
UNIVERSITI TEKNIKAL MALAYSIA MELAKA
SUPERVISOR DECLARATION
“I hereby declare that I have read this thesis and in my opinion this report is sufficient in terms of scope and quality for the award of the degree of Bachelor of Mechanical Engineering (Thermal-Fluids) with honours”
IMRAN SYAKIR Signature
: ........................................
Supervisor
: IMRAN SYAKIR BIN MOHAMAD
Date
: ........................................
EFFECT OF CARBON NANOTUBE STRUCTURE ON ENHANCING THERMAL PROPERTIES OF NANOFLUIDS
SYAZWANI BINTI ZAINAL ABIDIN
IMRAN SYAKIR This thesis is submitted in partial fulfillment of requirement for the completion of Bachelor of Mechanical Engineering (Thermal-Fluids) with honours
Faculty of Mechanical Engineering Universiti Teknikal Malaysia Melaka
JUNE 2015
ii
DECLARATION
“I hereby declare that the work in this thesis is my own except for summaries and quotations which have been duly acknowledged.”
IMRAN SYAKIR Signature
: ................................................
Author
: SYAZWANI BINTI ZAINAL ABIDIN
Date
: .................................................
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DEDICATION
To my beloved parents Emak dan Abah, Abang Long, Leen, Jinggo, dan Yana.
IMRAN SYAKIR Thank you for your love, care and support.
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ACKNOWLEDGEMENT
The special gratitude goes to my helpful supervisor, Mr Imran Syakir Bin Mohamad. The supervision and support that he gave truly help the progression and smoothness of this research. The co-operation is much indeed appreciated. I also want to express my deepest gratitude to my co-supervisor, Dr Norli Abdullah (UPNM) for her guidance and invested a full effort to help me to complete this final year project.
IMRAN SYAKIR My grateful thanks also go to my team mates. A big contribution and hard
worked from both of them during this research is very great indeed. The research
would be nothing without the enthusiasm and imagination from both of them. Besides, this research makes me realized the value of working together as a team and as a new experience in working environment. Great deals appreciated go to the contribution of my faculty - Faculty of Mechanical Engineering (FKM). Last but not least, I also would like to thankful to my parents for the support that truly motivated me. I hope this research will give a positive impact to students and help next researchers when doing the research regarding this topic.
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ABSTRACT
The low thermal conductivities of conventional heat transfer fluids limit the cooling performance in many industrial applications. The addition of the small amount of nanocarbon in heat transfer nanofluids contributes to the enhancement of thermal conductivities of the fluids. However, the different in nanocarbon structure may results in different thermal conductivity of the nanofluids. In order to design heat transfer fluids that suit industrial applications, the understanding about the
IMRAN SYAKIR behaviour of the difference types of nanocarbon structure is very important. The characterization testing for the nanocarbon materials was conducted to study the
surface properties of carbon nanotube to suggest the best CNT which can enhance a
good thermal and heat transfer properties for industrial cooling application. Three carbon nanotube were characterized in this research that is commercial MWCNT, functionalized MWCNT and carbon nanofiber. All three CNT were characterized using Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and Nitrogen gas (N2) adsorption. The characterization testing examination provides an overview of nanostructures of the selected CNT. Then, the thermal conductivity was conducted to all the sample tested. The suspension of nanofluid-based carbon nanofiber had a better thermal conductivity enhancement compare to nanofluid carbon nanotube. This result reveal that the carbon nanofiber proves to be a great alternative for heat transfer fluid in industrial cooling application.
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ABSTRAK
Keberaliran haba yang rendah dalam cecair pemindahan haba konvensional mengehadkan kadar prestasi penyejukan dalam pelbagai aplikasi industri. Penambahan karbon nano dalam cecair pemindahan haba menyumbang kepada peningkatan keberaliran haba di dalam sesuatu cecair. Walau bagaimanapun, perbezaan dalam struktur karbon nano boleh menyebabkan kekonduksian termal yang berbeza dalam bendalir nano. Dalam usaha untuk mereka bentuk cecair
IMRAN SYAKIR pemindahan haba yang sesuai dengan aplikasi industri, pemahaman tentang ciri-ciri dan jenis- jenis perbezaan struktur karbon nano adalah sangat penting. Ujian untuk
pencirian bahan karbon nano telah dijalankan untuk mengkaji sifat-sifat permukaan tiub karbon nano yang boleh meningkatkan kadar pemindahan haba. Tiga jenis
karbon nano telah dikaji di dalam kajian ini iaitu komersial MWCNT, MWCNT berfungsi (functionalized MWCNT) dan karbon nanofiber. Ketiga-tiga karbon nano tersebut telah dikaji morfologinya menggunakan Mikroskop Elektron Pengimbas (SEM), Fourier Transform Infrared (FTIR) spektroskopi dan penjerapan gas Nitrogen. Kemudian, ujian kekonduksian termal dijalankan untuk semua sampel yang diuji. Kajian yang dijalankan menunjukkan bahawa bendalir nano yang ditambah dengan diameter terkecil karbon nanofiber menghasilkan kekonduksian termal yang tertinggi apabila diukur pada tiga suhu yang berbeza iaitu 6 oC, 25 oC dan 45 oC. Daripada kajian ini, dapat disimpulkan bahawa karbon nanofiber boleh digunakan sebagai medium dalam meningkatkan hubungan kealiran haba dalam aplikasi industri.
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TABLE OF CONTENT
CHAPTER
TITLE
PAGE
DECLARATION
ii
DEDICATION
iii
ACKNOWLEDGEMENT
iv
ABSTRACT
v
ABSTRAK
vi
TABLE OF CONTENTS
vii
LIST OF TABLES
x
LIST OF FIGURES
xi
IMRAN SYAKIR CHAPTER I
LIST OF SYMBOL AND ABBREVIATION
xiii
LIST OF APPENDIX
xiv
INTRODUCTION
1
1.0
Introduction
1
1.1
Background Research
2
1.2
Problem Statement
2
1.3
Objective of Research
3
1.4
Scope
3
1.5
Rationale And Significant Of
3
Research
CHAPTER II
LITERATURE REVIEW
4
2.0
Introduction
4
2.1
Carbon
5
2.2
Nanocarbon
5
2.2.1 Types of Carbon Nanotube
6
viii
CHAPTER
TITLE
PAGE 2.2.1.1 Single Walled Carbon
6
Nanotube (SWCNT) 2.2.1.2 Multi walled carbon
7
Nanotube (MWCNT) 2.2.2 Properties of Carbon Nanotube
9
2.2.2.1 Functionalization of CNT’s
10
2.2.2.2 Structure and Morphology of
11
CNT 2.3
Synthesis and Characterization
11
2.3.1 Scanning Electron Microscopy (SEM)
12
2.3.2 Fourier Transform Infrared (FTIR)
13
2.3.3 Nitrogen gas (N2) Adsorption
15
Analysis 2.4
Thermal Conductivity
19
2.4.1 Effective parameters on thermal
20
IMRAN SYAKIR conductivity
CHAPTER III
2.4.1.1 Morphology
20
2.4.1.2 Temperature
21
2.4.1.3 Concentration
21
METHODOLOGY 3.0
18
Introduction
3.1 Flowchart of PSM 1
19
3.2 Parameter Used
20
3.2.1 Properties of carbon nanotube 3.3 Characterization Testing
20 21
3.3.1 Scanning Electron Microscopy (SEM)
22
3.3.2 Nitrogen gas (N2) Adsorption Analysis
24
3.3.3 Fourier Transform Infrared (FTIR)
26
3.4 Thermal Conductivity Test
28
ix
CHAPTER
TITLE
PAGE
CHAPTER IV
RESULT AND DISCUSSION
35
4.0
Introduction
35
4.1
Result and Discussion
31
4.1.1 Scanning Electron Microscope
36
(SEM) 4.1.2 Nitrogen gas (N2) Adsorption
40
Analysis 4.1.3 Fourier Transform Infrared (FTIR)
44
4.1.4 Thermal Conductivity Test
47
4.1.4.1 Percentage of Enhancement of
48
Thermal Conductivity 4.1.4.2 Thermal Conductivity Analysis
CHAPTER V
49
CONCLUSION AND RECOMMENDATION
50
5.1
51
Conclusion
IMRAN SYAKIR 5.2
Recommendation
51
REFERENCES
53
BIBLIOGRAPHY
57
APPENDICES
58
x
LIST OF TABLE
NO.
TITLE
PAGE
2.1
Comparison between SWCNT and MWCNT
2.2
Pore Type Diameter
17
3.1
Properties of CNT
26
9
IMRAN SYAKIR 4.1
BET Surface Area
44
4.2
FTIR Spectra Evaluation
46
4.3
Thermal conductivity of CNT Nanoamor, functionalized MWCNT and
47
CNF HHT-24 at 1.0 wt% of CNT 4.4
Thermal Conductivity of Deionized Water
48
4.5
Percentage Enhancement of Thermal Conductivity
48
xi
LIST OF FIGURE
NO.
TITLE
PAGE
2.1
Structure of Carbon Nanotube
5
2.2
Single Walled Carbon Nanotube
7
2.3
Multi Walled Carbon Nanotube
8
IMRAN SYAKIR 2.4
Functional Group of Organic Compound
10
2.5
SEM Image of the Multiwall Carbon Nanotube after Purification
12
2.6
FTIR Spectrum Evaluation
2.7
FTIR spectra of (a) TiO2-ionic liquid nanofluid and (b) pure TiO2
14
2.8
CNT-IR Absorbance Spectrum
15
2.9
Adsorption Isotherm
17
2.10
Hysteresis Loop
19
2.11
Thermal Conductivity Enhancement of Nanofluid with Increase of Nanoparticles Size
3.1
Flowchart for Whole Workflow
24
3.2
Diagram of SEM Column and Specimen Chamber
28
3.3
Autosorb 6-B
24
xii
NO.
TITLE
PAGE
3.4
FTIR Schematic Diagram
31
3.5
FTIR Spectrum
32
3.6
KD2-Pro Thermal Properties Analyser
33
3.7
Refrigerated Water Bath Schematic Diagram
34
4.1
SEM Images at 10000X and 50000x Magnification for CNT Nanoamor
37
(a, b), functionalized MWCNT (c, d) and CNF HHT-24 (e, f) 4.2
Diameter Distribution for (a) CNT Nanoamor, (b) functionalized
39
MWCNT, (c) CNF HHT-24 4.3
Isotherm Comparison
41
4.4
DFT Pore Size Distribution Comparison
43
IMRAN SYAKIR 4.5
FTIR Spectra of CNTs
45
xiii
LIST OF SYMBOL AND ABBREVIATION
BET
-
Brunauer Emmet Teller
CNT
-
Carbon Nanotube
CNF
-
Carbon Nanofiber
EBSD
-
Electron Backscatter Diffraction
IMRAN SYAKIR EDS
-
Energy-Dispersive Spectrometer
FESEM
-
Field Emission Scanning Electron Microscopy
FTIR
-
Fourier Transform Infrared
MWCNT
-
Multi-Walled Carbon Nanotube
N2
-
Nitrogen Gas
SEM
-
Scanning Electron Microscopy
SWCNT
-
Single Walled Carbon Nanotube
xiv
LIST OF APPENDIX
APPENDIX TITLE
PAGE
A
PSM I Gantt Chart
58
B
PSM II Gantt Chart
59
C
CNT Nanoamor Testing Data Sheet
60
D
Functionalized MWCNT Testing Data Sheet
69
E
CNF HHT-24 Testing Data Sheet
79
F
MERD’S 2015 Paper
88
IMRAN SYAKIR
1
CHAPTER I
INTRODUCTION
1.0
INTRODUCTION
Nanofluids are widely used as heat transfer media for many applications such as microelectronics, pharmaceuticals, vehicle thermal management and others. However, nanofluids are commonly used as a coolant in heat transfer equipment such
IMRAN SYAKIR as electronic cooling system. The recent research has demonstrated that nanofluids have provided significantly better heat transfer properties than the base fluids
because of its novel properties. The nanofluids proved to have a much higher and
strongly temperature-dependent thermal conductivity at very low particle concentrations than conventional radiator coolants without the nanoparticles. For this reason, the thermal conductivity is very important in the development of efficient heat transfer fluid. The great intrinsic electronic and mechanical properties of nanocarbons such as carbon nanotube and carbon nanofibre has gained attention among the researchers as the addition of the small amount of suspending nanoparticles has the potential to enhance the thermo physical, transport and radiative properties of the base fluid. These nanoparticles which have high surface area and high thermal conductivity are potentially to be used as superior medium for a heat transfer media. Thus, this shows that nanofluids are promising future coolants for industrial applications and the development of the nanofluids should be enhanced in a wide platform in nanotechnologies area.
2
1.1
BACKGROUND RESEARCH
Carbon nanotubes (CNT) which has a nanometer sized diameter and specifically has a molecularly smooth surfaces, offers an interesting framework for molecular transport in nanofluidics. Since the discovery of the carbon nanotube, CNT has received a considerable attention around of the world because of its interesting electronic characteristic which exhibit excellent mechanical and thermal properties. Apart from the excellent thermal and mechanical properties that been possess, carbon nanotube prove to have a physiochemical properties that makes carbon nanotube suitable as a conventional heat transfer fluids in industrial cooling application.
Recent studies conducted by many researcher reveal that the CNT have unusually high thermal conductivity which contribute to the enhancement of heat transfer. The suspension of fluids which contain CNT particle would enhance a great thermal conductivity and improved thermal performance. Overall, recent studies
IMRAN SYAKIR regarding CNT have shown a very promising glimpse of what lies ahead in the future of nanotechnology as well as in industrial cooling application.
1.2
PROBLEM STATEMENT
Low thermal conductivities of conventional heat transfer fluids limit the cooling performance in many industrial applications. The addition of a small amount of nanocarbon in heat transfer fluids contributes to the enhancement of thermal conductivities of the fluids. However, the different nanocarbon structure may result in different thermal conductivities. In order to design heat transfer fluids for specific industrial applications, the understanding about the behavior of different types of nanocarbon structure is very important. Thus, the characterization of selected carbon nanotube were conducted to study the behavior of CNT structure which can enhance a good thermal and heat transfer properties.
3
1.3
OBJECTIVE OF RESEARCH
The objectives of research studies are; i.
To study the surface properties of carbon nanotube which contribute to the thermal conductivity enhancement for nanofluids.
ii.
To analyze the effect of CNT structure on enhancing thermal properties of nanofluids.
1.4
SCOPE
i.
Selected carbon nanotube (Functionalized MWCNT, Commercial MWCNT and Commercial CNF) were characterized using Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) and Nitrogen gas (N2) adsorption analysis.
ii.
The morphology and surface species of the CNT are studied.
IMRAN SYAKIR iii.
The behavior of CNT structure which can enhance a good thermal and
heat transfer properties were analyzed in terms of thermal conductivity.
1.5
RATIONALE AND SIGNIFICANT OF RESEARCH
The study of nanofluids is very important to ensure the continuity of research in the field of nanotechnology due to the progressive use of nanofluids as a coolant for industrial applications. The use of nanocarbon in nanofluids contributes to the enhancement of thermal conductivity of the nanofluids. The understanding about the behavior of different types of nanocarbon structure is very important, in order to design heat transfer fluids for specific industrial applications. This research suggested the best CNT that can be used as thermal interface materials to enhance contact thermal conductance for electronic packaging applications. Thus, this finding generated a great interest in nanofluids and their potential for heat transfer enhancement.
4
CHAPTER II
LITERATURE REVIEW
2.0
INTRODUCTION
A decade ago, nanotechnology was an experimental technology, which using molecular or individual’s atom as a very small part of the machine, and was measured using nanometer. In other words, nanotechnology is the science of
IMRAN SYAKIR materials, systems, structures and components as well as it improves the characteristics of the fluids in terms of scientific branch, physics, chemistry, and
biology. This technology was geared towards research about the possibility exists for preparing the atom, which led to the creation of a smaller machine compared to living cells and makes the material stronger and lighter. Through nanotechnology, better equipment can be produced such as advanced space craft and medical equipment which can move within the blood vessels and thus improve the damaged living cells by cure the various diseases. The principal of nanotechnology lies in the way that properties of the material change significantly when size decreased to the nanometer scale (Raliya and Tarafdar, 2012).
5
2.1
CARBON
Carbon is the most abundant element in universe. Carbon does exists in a pure or nearly pure forms such as in diamonds and graphite but can also combine with other elements to form molecules. Carbon atoms arranged in a honeycomb-like lattice constitute the common building blocks of not only graphite but also other carbon nanomaterials including fullerene, carbon nanotubes (CNTs), and grapheme. Carbon materials suitable to be used as adsorbents when adsorption of traces of gases or vapours is considered (E Diaz, 1991a).
2.2
NANOCARBON
Carbon nanotubes (CNTs) can be defined as allotropes of carbon which has a cylindrical nanostructure having a diameter measuring on the nanometer scale. The carbon nanotube structure have unusual and unique properties which make them
IMRAN SYAKIR potentially useful in a wide range of nanotechnology and material science applications. Figure 2.1 shows the structure of carbon nanotube.
Figure 2.1: Structure of carbon nanotubes (Source: Hirlekar et al. 2009)
Carbon nanotubes with rolled-up graphene sheets has high thermal conductivity and has an ability to remain in stable suspension for a long period of time. The carbon nanotubes were discovered by Ijima in 1991 and since that, carbon nanotubes have received a much attention. The diameters and arrangement of the hexagon rings along the tube length determined the metal properties of the carbon nanotubes, metallic or semi-conductive.
6
The consistent arrangement of the hexagon rings without any loose bonds make the carbon nanotube walls to become unreactive (Lin, 2003). Compared carbon nanotubes with C60 fullerene, the fullerene is more reactive than the cylindrical nanotube (Ajayan et al. 1993) and certain reagents can more readily react with the fullerene.
Research conducted by Hummer et al. in 2001 observed the movement of water molecules through the CNT and found that the water molecules do not enter the narrow hydrophobic channel spontaneously, but can also move very fast through it. The research was conducted with the used of equilibrium molecular dynamics (MD) simulation. However, Hummer et al. (2001) counted the water molecules that passing through CNT on a computational domain to backing the following experimental.
The intrinsic mechanical and transport properties of CNT make them an ultimate carbon fiber. By and large, CNT demonstrate an exceptional blend of
IMRAN SYAKIR stiffness, strength, and tenacity contrasted with other fiber materials which generally fail to offer one or a greater amount of these properties.
2.2.1
Types of Carbon Nanotube
2.2.1.1 Single Walled Carbon Nanotube (SWCNT)
A single walled carbon nanotube was formed by enveloping a single sheet of graphite (Prabhakar, 2007) that are normally capped at the ends. The structure of SWCNT can be featured as a single cylindrical wall. The layer of graphite formed SWCNT from a single atom thick, which is called graphene. Typically, SWCNT has a diameter of within the range 0.4 nm to 2 nm. Figure 2.2 shows the structure of SWCNT.
7
Figure 2.2: Single walled carbon nanotube
The researcher has high interest on SWCNT because of the reason that slight changes in the diameter of the tube and the angle wrapping (Avouris et al. 2007) are characterized by the chirality indices will change its electrical conductivity from one properties of metallic to semi-conducting state. The SWCNT can be produced using a metal catalyst by the techniques arc-discharge method.
IMRAN SYAKIR SWCNT are more malleable yet harder to make compared to multi walled
carbon nanotube (MWCNT). SWCNT can be turned, straightened, and bowed into little loops or around sharp curves without breaking. SWCNT has remarkable
electronic and mechanical properties which can be utilized as a part of various applications. SWCNT is the materials that are on the main edge of electronic creation, and are required to assume a significant part in the up and coming era of scale down gadgets.
2.2.1.2 Multi-Walled Carbon Nanotube (MWCNT)
Multi-walled nanotubes (MWCNT) comprise concentric tubes of graphene with multiple rolled layers. One of the techniques to produce SWCNT and MWCNT is called arc-discharge method. This method produced a high quality SWCNT and MWCNT. Yacaman et al. is the first person who proposed catalytic growth of MWCNT by chemical vapor deposition (CVD) method in years 1993. Even though the arc-discharge method produces high quality of SWCNT and MWCNT, however the MWCNT does not need a catalyst for growth compared to SWCNT which can
8
only be grown with the presence of catalyst. Figure 2.3 shows the structure of MWCNT.
Figure 2.3: Multi walled carbon nanotube
IMRAN SYAKIR The MWCNT arrangement are perfect for applications where high quality to
weight proportion is essential, for example, the car and aviation commercial
ventures. In the plastics business, multi-walled carbon nanotubes can be utilized as added substances to enhance the properties of the final products. In games gear such
as tennis racquets and hockey stick, MWCNT can upgrade the materials execution without expanding final weight. Generally, MWCNT can be utilized as added substances as a part of cement and other building materials for rendering expanded mechanical properties. Table 2.1 shows summarize general properties for both SWCNT and MWCNT.
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Table 2.1: Comparison between SWCNT and MWCNT (Source: Hirlekar et al. 2009) SWCNT
MWCNT
Single layer of graphene
Multiple layer of grapheme
Catalyst is required for synthesis
Can be produced without catalyst
Poor purity
High purity
Difficult bulk synthesis as it requires
Easy bulk synthesis
proper control over growth and atmospheric condition Less accumulation in body
More accumulation in body
Easy characterization and evaluation
Has very complex structure
Can be easily twisted
Cannot be easily twisted
2.2.2
Properties of Carbon Nanotube
IMRAN SYAKIR A carbon nanotube is a tube-molded material, made of carbon, having a
measurement measuring on the nanometer scale. A nanometer is one-billionth of a meter, or around one ten-thousandth of the thickness of a human hair. The graphite
layer shows up to some degree like a moved up chicken wire with a consistent unbroken hexagonal cross section and carbon particles at the summits of the hexagons. Carbon nanotubes which has a long and a thin barrels of carbon, were found in 1991 by S. Iijima.
Carbon Nanotubes have numerous structures, contrasting long, thickness, and in the sort of helicity and number of layers. Despite the fact that they are framed from basically the same graphite sheet, their electrical attributes contrast relying upon these varieties, acting either as metals or as semiconductors (Thomas A. Adams II, 2006).
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2.2.2.1 Functionalization of CNT’s
In certain applications, the major technical barrier is the lack of solubility of carbon nanotubes in aqueous media. The functionalization is done to the surface of CNT to solve this problem (Yang et al. 2007). With diverse particles, functionalization is accomplished by adsorption, electrostatic interaction or covalent bonding of different molecules and chemistries that render the molecules to become more hydrophilic. Through such adjustments, the water solvency of CNT is enhanced and their biocompatibility profile is totally changed. Besides, the aggregation of individual tubes through Van der Waals forces are likewise decreased by the functionalization of the surface (Lacerda et al. 2006).
The recent development in methods to chemically modify and functionalize CNT has made it possible to solubilize and disperse CNT in water, thus opening the path for their facile manipulation and processing in physiological environments. The functionalization usually been done by oxidation process by refluxing in the mixture
IMRAN SYAKIR of HNO3 and H2SO4 and generally the defects and the ends of CNTs are thus
functionalized by carboxyl group. Figure 2.4 shows the common functional group of organic compound in functionalization.
Figure 2.4: Functional group of organic compound
11
2.2.2.2 Structure and Morphology of CNT
Each atom in carbon nanotubes joined to three neighbours as in graphite and forms sp2 bonding. The tubes were considered as rolled-up individual graphite layer sheets. The bonding structure is stronger than the sp3 bonds and can be found in diamond. The tubes structure provides the CNT molecules the unique strength. Nanotubes can merge together under high pressure and trading some sp² bonds for sp³ bonds, giving the possibility to produce strong and unlimited length wires through high-pressure nanotube linking.
The morphology of nanoparticles, such as shape and size can effect on viscosity and pumping power of the cooling system. The investigation on nanoparticles morphology would geared the nanofluids towards more effective and economical cooling media. Prasher et al. (2006) suggested that the nanoparticles diameter may not contribute to the viscosity change generally. Nguyen et al. in his studies in 2007 proved that 47 nm of Aluminium Oxide (Al2O3) nanoparticle sizes
IMRAN SYAKIR has a higher viscosity comparing to 29 nm of CuO particles sizes. Lu and Fan (2008) investigated on particle size theoretically and experimentally. Their studies on water
and ethylene glycol based Al2O3 found that the increases of particle size decreases the viscosity.
2.3
SYNTHESIS AND CHARACTERIZATION
The specific atomic structure of carbon nanotube make carbon nanotube an interesting chemical and physical properties according to those of graphite and diamond (Belin and Epron, 2005). The characterization testing were performed to study the surface species of the materials which including morphology and specific surface area (pore type, pore volume, surface area). The characterization method of carbon nanotube which are most employed today is Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR), and Nitrogen gas adsorption analysis
12
2.3.1
Scanning Electron Microscopy (SEM)
The development of the electron-beam technology in 1960 has led to the advancement of the electron microprobe. The development of this technology has helped a much the way for geologists research the rocks by obtain the nondestructive analyses of micron-sized samples. Nowadays, recent studies more focused on the development of the variable-pressure scanning electron microscopes (SEM) that can be equipped with an energy-dispersive spectrometer (EDS) to analyse the chemistry, or an electron backscatter diffraction (EBSD) system to investigate and observe the crystalline structures and orientations of the materials being tested (Rachel, 2004).
IMRAN SYAKIR Figure 2.5: SEM image of the multiwall carbon nanotube after purification (Source: Yu Hsun Nien, 2011)
Figure 2.5 shows the SEM images of the MWCNT after being treated with purification process. The electron microscopes utilized a beam of highly energetic electrons to probe objects on a very fine scale (Wang, 2000). The electrons are mostly generated by the heating of the tungsten filament (electron gun) and occur mostly in standard electron microscopes. Besides, the electrons were also produced by a crystal of LaB6. The utilization of the LaB6 will impact in a higher electron density in the beam and a better resolution compared to conventional device.
13
2.3.2
Fourier Transform Infrared (FTIR)
The Fourier Transform Infrared (FTIR) is the one of the best and useful analytical tool for non-destructive analysis. The utilization of the FTIR for analytical chemists to investigate the chemical substances that making up the materials is not a trivial task to be performed nowadays. The complexity of the FTIR to conduct characterization comes mainly from the high degree of infrared absorption bands overlapping, that are difficult to be accurately assigned, and despite of the fact that development of software technology which enhance the spectrum processing data is currently available. Figure 2.6 shows the FTIR spectrum evaluation.
IMRAN SYAKIR Figure 2.6: FTIR spectrum evaluation
Peiyang et al. conducted a studies regarding characterizations of TiO2 nanofluids in 2011 to observe the structure using FTIR spectrometer analysis. The FTIR spectra are shown in Figure 2.7. The result reveal that all the spectrum data have peak at 450 cm-1 to 700 cm-1 which is the location of characteristic peaks of titania. The TiO2 nanofluids also have many new absorption peaks of organic groups compared to the pure TiO2 nanoparticles.
14
Figure 2.7: FTIR spectra of (a) TiO2-ionic liquid nanofluid and (b) pure TiO2
Kouklin et al. conducted a studies in 2004 regarding infrared absorption
IMRAN SYAKIR properties of carbon nanotubes synthesized by chemical vapor deposition. The studies were conducted by studies the infrared optical absorbance of highly uniform
nanotubes grown by chemical vapor deposition in the self-assembled porous matrix
in alumina. The infrared absorbance properties of highly uniform with 60 nm diameter, purified and mono-dispersed carbon nanotubes were investigated in the studies. Figure 2.8 represent the FTIR spectra produced from the studies.
15
Figure 2.8: CNT-IR absorbance spectrum
The spectra clearly shows the presence of an onset in the absorption
IMRAN SYAKIR indicative of the semiconducting character of the studied multi-walled nanotubes. The highest prime intensity peak was seen at 1584 cm−1. In general, the presence of C-H groups (evidenced in the IR active bands in the range of 3000 cm−1) and non-
conjugated carboxylic carbonyl groups (peak around 1725 cm−1) can benefit a number of bio-sensing applications by offering a simple route to nanotube functionalization.
2.3.3
Nitrogen gas (N2) Adsorption Analysis
The characterization of the porous materials commonly used gas adsorption as a major technique. Compared to the other gases and vapours available in this earth, nitrogen gas has become a universally pre-eminent gas to be used because of its availability and could be used as adsorptive. It is now possible to use nitrogen adsorption at a temperature 77 K for routine quality control and research of the new materials with the aid of new modern technology equipment which faster the corresponding data processing.
16
Dewar and Ramsay are the one of the earliest researchers that studies the adsorption nitrogen and other gases at liquid air temperature approximately to 88 K in 1905 by investigating the composition of the atmosphere and the separation of the noble gas. Then, the research regarding adsorption of nitrogen gas and other gases was conducted followed by other researcher but at a low-temperature studies by charcoal, including an extensive series of measurements over varies temperature by Ida Homfray in 1910.
The interpretation of adsorption data was idealised by Langmuir in 1916 as he introduced his work on monolayer adsorption. Langmuir (1916) revealed that the amount adsorbed at plateau of a Type I isotherm corresponds to the complete monolayer coverage.
However, it was realised that the multilayer adsorption of the nitrogen gas can takes place at the liquid nitrogen temperature 77 K. To adopt gas adsorption for the determination of the surface area, Benton and White (1932) have prompt
IMRAN SYAKIR Brunauer and Emmet (1937) on their studies. They reveal that the adsorption isotherms of nitrogen and other gases on an iron synthetic ammonia catalyst were all
the same sigmoidal shape (isotherm Type III). This studies was support by the
empirical theory that indicated the change from monolayer to multilayer adsorption occurred at the beginning of the middle which are nearly linear section of the isotherm. The Brunauer Emmet Teller (BET) theory then was published in 1938 to support this hypothesis and to provide theoretical support (Sing, 2001). Figure 2.9 shows the classification for adsorption isotherm.
17
Figure 2.9: Adsorption isotherm
Type I refers to adsorption on micro porous adsorbent. Type II and Type III show the adsorption on macro porous adsorbent with strong and weak adsorbateadsorbent interactions. Type IV and Type V show the adsorption with hysteresis.
IMRAN SYAKIR Type VI has steps.
The isotherm plot indicates the distribution of different type of pore which
consists of micro, meso and macropores from an adsorption isotherm. The micropore diameter size is between 0 nm to 2 nm, mesopore is between 2 nm to 50 nm and macropore size is more than 50 nm. Table 2.2 shows the pore diameter of different type of pores.
Table 2.2: Pore type diameter Pore Type
Pore Diameter (nm)
Micropore
0 - 20
Mesopore
20 - 50
Macropore
More than 50
18
Micro-sized pores shows the strong interactions among the narrow pore walls with material adsorbed on the relative pressure which cause the volume of material adsorbed in the pores increases. Pore with meso-sized shows an increase in the volume of the adsorption due to the effect of the occurrence of capillary condensation turn through the establishment of a hysteresis loop. Macro-sized pores indicate the formation of a monolayer on relatively at low pressure and the adsorption layers at relatively high pressure.
Hysteresis loop occurred when the condensation phenomena happen where the Nitrogen state deep into the mesopores in liquid form at a very low temperature during adsorption. The size or shape of hysteresis loop depends on type or shape of presence mesopores.
Type H1 can be classified as regular even pores without interconnecting channels. Type H2 can be classified as pores with narrow and wide section and also possible interconnecting channels. Type H3 represent slit-like pores that would yield
IMRAN SYAKIR Type II isotherm without pores. Type H4 represent slit-like pores that would yield Type I adsorbent-adsorbate pair. The hysteresis loop can be recognized based on the Figure 2.10.
19
Figure 2.10: Hysteresis Loop
IMRAN SYAKIR 2.4
THERMAL CONDUCTIVITY
In material science, morphology would be characterized as investigation of shape, size, composition and stage conveyance of physical items. Concerning kind of investigation of nanoparticles, the impact of the size of nanoparticles has been examined by a few scientists, for example, Chon et al. (2005) who have announced high impact of nanoparticle estimate on thermal conductivity of nanofluid. This can be seen in Figure 2.11 which shows the thermal conductivity enhancement of nanofluid with increase of nanoparticles size. Then, Chopkar et al. (2006) conducted a study on ethylene glycol based nanofluids containing Al70Cu30 nanoparticle and found that thermal conductivity firmly relies on upon the sizes of nanoparticles.
20
Figure 2.11: Thermal conductivity enhancement of nanofluid with increase of nanoparticles size (Source: Chon et al. 2005)
In 2009, Minsta et al. tried two distinctive sizes of Al2O3 nanoparticles with diameter of 36 nm and 47 nm and found that nanofluids with smaller nanoparticles
IMRAN SYAKIR indicated higher enhancement in thermal conductivity. The first analysts who have
reported impacts of nanoparticle shape such as spherical and cylinder on the enhancement of thermal conductivity of SiC nanofluid were Xie et al. in 2002. Later, Murshed et al. (2005) researched the impacts of molecular shape on thermal
conductivity of nanofluids. Then, Liu et al. (2006) also done a few tests on Cu nanoparticles with the diameter measurement range of 50 nm to 250 nm with needle and square shape, dispersed in water to observe the impact of these two parameters on thermal conductivity.
2.4.1
Effective Parameters on Thermal Conductivity
In nanofluid, nanoparticle can be considered as the key element of nanofluid which can affect the thermal conductivity of the nanofluid. Some parameters may influence on thermal conductivity of nanofluids such as particles size, temperature, concentration and particle motions. However, only several important features that will affect the thermal conductivity.
21
2.4.1.1 Morphology
The term morphology can be defined as study of shape, size, texture and phase distribution of physical objects. The study of nanoparticles has been investigated by some researchers such as Chon et al. (2005) which reveal that the nanoparticle size give the effect to the thermal conductivity of the nanofluid. Minsta et al. in 2009 reported that nanofluids with smaller nanoparticles showed higher enhancement in thermal conductivity. The experiment was conducted by two different sizes of Al2O3 with respective diameter 36 nm and 47 nm.
Xie et al. (2002a) was the first person who studies the effect of nanoparticle shape including spherical or cylindrical on the thermal conductivity enhancement of SiC nanofluid. A few years later, Murshed et al. (2005) investigated the effects of particle shape on thermal conductivity of nanofluids. The studies were carried out on spherical and rod-shaped TiO2 nanoparticles with respective diameter of 15 nm and 10 nm. The studies reveal that the higher thermal conductivity was gained by rod-
IMRAN SYAKIR shaped nanoparticles.
Other factors which effect the thermal conductivity enhancement is the
specific surface area of the nanoparticle. Decrement in the particle volume and increasing particle surface area will increase specific surface area and resulting to the increasing of thermal conductivity due to more contact surface. Xie et al. (2002b) proved in their research that increasing specific surface area can leads to the enhancement of thermal conductivity.
2.4.1.2 Temperature
The thermal conductivity of nanofluids is strongly depends on temperature. The research regarding temperature dependent on thermal conductivity has been investigated by Das et al. (2003). The experiment was carried out on water-based nanofluids including CuO and Al2O3 between temperatures range from 20 to 50 °C.
22
The result revealed the temperature dependency of nanofluids and suggest the reason due to the effect of particles motion. If the nanofluid particle move faster inside the basefluid with higher temperature, the nanofluid will have higher thermal conductivity. Besides, Ding et al. (2006) also conducted some studies on CNT water nanofluids and the result showed that the thermal conductivity is strongly depends on temperature.
Recently, the research conducted by some researcher suggest that the temperature and thermal conductivity have a direct relationship as the temperature increases, thermal conductivity will also increase. This was proved by Yu et al. in his studies in 2011.
2.4.1.3 Concentration
Concentration of nanoparticles inside the basefluid is one of the parameter
IMRAN SYAKIR which can highly affect thermal conductivity of nanofluid. Some researcher suggest
that the term concentration include volume as well as weight percentage. The research conducted by Choi and Eastman (1995) showed nonlinear relationship between nanofluid concentration and thermal conductivity. In addition, nonlinear relationship of these two properties, thermal conductivity and concentration has been investigated within studies accomplished by Hong et al. (2005) with Fe-ethylene glycol nanofluids.
23
CHAPTER III
METHODOLOGY
3.0
INTRODUCTION
This section represents detailed information of systematic and theoretical analysis of the method applied during the research for gathering of information and for analysis. This methodology section described the process and procedures for
IMRAN SYAKIR selecting materials, collecting and interpreting data. The flow chart in Figure 3.1 described the whole process of characterization of carbon nanotube (CNT) by using
Scanning Electron Microscopy (SEM), Nitrogen gas (N2) adsorption analysis and Fourier Transform Infrared (FTIR). The main objectives of the characterization
testing being conducted for the selected CNT is to find the best CNT, which can enhance and possess a good thermal properties based on the structural analysis. Then, thermal conductivity testing were conducted to find the best CNT, which has a good thermal conductivity.
24
3.1
FLOWCHART OF PSM 1
Start
Problem Statement
Literature Review
Selection of Carbon Nanotube
Characterization testing using Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) and Nitrogen gas (N2) absorption analysis
IMRAN SYAKIR Thermal Conductivity Test
Result and Discussion
Thesis Writing and Report Submission
End
Figure 3.1: Flowchart for whole workflow
25
The flow chart in the Figure 3.1 shows the whole process of project research. The research begin by discovering the problem statement of the research including the background of research, objective, scope and also rationale and significant of studies. Then, literature review on various aspects of studies and parameter concern for this research have been determined in early stage of workflow. The selection and preparation of materials which is carbon nanotube must be conducted before the characterization testing is perform. The further description of the parameter and material been used will be explained more details in next section.
3.2
PARAMETER USED
The parameter utilized to study the effect of the carbon nanotube structure on enhancing the thermal properties of CNT is the thermal conductivity and heat transfer efficiency of nanofluids. The CNT used for this research is Nanoamor CNT, functionalized multi walled carbon nanotube (fMWCNT) and HHT24 CNF. The
IMRAN SYAKIR material properties for each CNT is being described in materials properties section.
3.2.1
Properties of carbon nanotube
The characterization testing were performed on these selected carbon nanotube and carbon nanofiber (CNF) which are CNT Nanoamor, functionalized MWCNT and CNF HHT-24. CNT Nanoamor was founded in September 2001 produced by Nanostructured & Amorphous Materials, Inc. (Nanoamor) in Los Alamos, New Mexico, USA. Since that, Nanoamor becomes a leading nanomaterials company in all aspects of business such as manufacturing, processing, supplying and marketing of nanostructured materials and their dispersions. The functionalized MWCNT used in this research is from the industrial grade multi-walled CNT that has been functionalized with –OH. Table 3.1 describe the properties of the three CNT.
26
Table 3.1: Properties of CNT
Properties
CNT Nanoamor
Functionalized
CNF HHT-24
MWCNT Nanostructured
Nanostructured
Pyrograf
& Amorphous
& Amorphous
Products, Inc
Materials, Inc
Materials, Inc
90
95
98
Form
Powder
Fine Powder
Powder
Colour
Black
Black
Black
Odour
Odourless
Odourless
Odourless
Condition/Materials
Oxidizing agents,
Oxidizing agents,
Strong oxidizers
to avoid
acids, halogens
acids, halogens
and interhalogens
and interhalogens
Manufacturer
Weight Percentage, %
IMRAN SYAKIR and alkali metal
3.3
and alkali metal
CHARACTERIZATION TESTING EQUIPMENT
Carbon nanotube structure possess the most determinant properties for revolutionary applications. Proprieties exhibited by CNT are in general given qualitatively by electron microscopies which is Scanning Electron Microscopy (SEM) and this characterization testing examination provides an overview of nanostructures of the selected CNT. All these microscopies very often, mask some observations of CNT arrangements in structure. The characterization testing is also done qualitatively by a very few other techniques, which is often used to more deeply investigate the morphology and the structure of the nanocarbon using Fourier Transform Infrared (FTIR) and Nitrogen gas adsorption analysis.
27
3.3.1
Scanning Electron Microscopy (SEM)
The Scanning Electron Microscopy (SEM) utilizes a focused beam of high energy electrons to create a mixed bag of signs on the surface of solid specimens. The signals that formed from the electron-sample correlations will produce the specimen or sample data that is the morphology (surface), composition of chemical, crystalline structure and also material content that make up the specimen observed under SEM.
In many applications, information is gathered over a chose region of the surface of the sample and a two dimensional image is produced that shows spatial varieties in these properties. The SEM is likewise equipped for performing investigations of choosing point areas on the specimen or sample as this methodology is particularly valuable in qualitative or semi-quantitatively to determine the chemical compositions, crystalline structure and also the crystal orientations.
IMRAN SYAKIR As indicated in the Figure 3.2, the electron gun at the top enlightens the
sample and beam angle were controlled by the condenser lens in the transmission of the electron microscope. The lenses beneath the sample are utilized to magnify the image of the sample which is viewed on the final screen at numerous thousand times magnification.
28
Figure 3.2: Diagram of SEM column and specimen chamber (Source: Dunlap et al. 1997)
IMRAN SYAKIR The second electron source will be decreased in size by the same amount that
the sample image is magnified if a second electron gun is placed below the fluorescent screen at the bottom of the column. In the meantime, this impact can be seen when both electron guns on and exhibits the reversibility of beams through electron viewpoint frameworks. Thus, the determined point in the specimen image on the fluorescent screen or on the photographic plate is equivalent to the focused electron probe in the plane of the sample.
With a specific end goal to get a two-dimensional image, thus it is very important to move probe over the sample and collect the transmitted or reflected electrons. The coinciding between the two sorts of instruments is very important to understanding both the probe forming system and in the image that formed when the scanning microscope is utilized as a part of the transmission.
29
For this research, SEM was used to characterize the CNT to generate highresolution images with 10000x and 50000x magnification of shapes of objects and to observe the spatial variations in chemical compositions. The characterization testing using SEM will reveal the morphology, structure, texture, chemical composition, crystalline structure and material orientation of the sample be tested.
3.3.2
Nitrogen gas (N2) Adsorption Analysis
The characterization of carbon nanotube using adsorption analysis will reveal the properties of their surface area such as pore diameter, porosity and type of pores. The method to be use is the Brunauer, Emmet and Teller (BET) testing using Nitrogen Adsorption analysis. For this research, Autosorb 6-B surface area and pore size analyser machine manufactured by Quantachrome Instruments of USA were used as shown in Figure 3.5.
IMRAN SYAKIR
Figure 3.3: Autosorb 6-B (Source: Quantachrome Instruments)
30
The samples must first be treated to avoid any traces of moisture and vapour before the sample being tested. The procedure for pre-treatment sample start with the sample being degassed at 120 oC with estimation time approximately for 5 hours. The samples were weighed after the pre-treatment process before it was transferred to BET Testing Machine for performance analysis. The samples are commonly prepared by heating it up in BET performance analysis. Meanwhile, to remove the liberated impurities, the gases are evacuated over the sample. Then, liquid nitrogen were used to cool the prepared samples. The analysis for this characterization testing were made by measuring the volume of Nitrogen gas adsorbed at the specific pressures.
3.3.3
Fourier Transform Infrared (FTIR)
Infrared spectroscopy has been a workhorse method for materials structure examination in the lab for over seventy years. An infrared spectrum represents a
IMRAN SYAKIR fingerprint of a specimen with absorption peaks which correlate to the frequencies of vibrations between the obligations of the atom that making up the material. Since
every different material is a unique combination of atoms, thus no two compounds produces literally the same infrared spectrum. Therefore, infrared spectroscopy can
bring about a positive identification (qualitative analysis) of each distinctive sort of material. Furthermore, the size of the peaks in the spectrum is an immediate sign of the measure of material present.
For this research, the FTIR that has been used for characterization of CNT is PerkinElmer Spectrum 100 FTIR Spectrometer. This model offers the mid-infrared range and near infrared range for accurate measurement of optical filter and high refractive index materials. The use of this model has an advantages as it remove common sources of ordinate error and achieve higher levels of photometric accuracy. Figure 3.4 shows a FTIR schematic diagram for apparatus set up.
31
Figure 3.4: FTIR schematic diagram
The main aim of Fourier Transform Infrared (FTIR) spectrometry was developed is to overcome the limitations experienced with dispersive instruments. The main trouble that contributes to the development of the FTIR instruments is the
IMRAN SYAKIR moderate or slow scanning methodology. A technique for measuring the infrared
frequencies all the while and simultaneously, as opposed to separately, was required.
The best solution for this problem was created which utilized an exceptionally a very simple optical device which is called an interferometer.
The interferometer delivers a remarkable kind of signal which has all the infrared frequencies “encoded” into it. The signal can be measured rapidly, generally in one second only. Therefore, the time element per sample is decreased to a matter of a couple of seconds instead of a few minutes.
Most interferometers utilize a beam splitter which takes the approaching infrared beam and partitions it into two optical beams. One beam reflects off of a flat mirror which is fixed in place. The other beam reflects off of a flat mirror which is on a mechanism which permits this mirror to move a short distance (commonly a couple millimeters) far from the beam splitter. The two beams reflect off of their separate mirrors and are recombined when they meet back at the beam splitter. The ensuing sign is called an interferogram which has the unique property that each data
32
point (a function of the moving mirror position) which makes up the signal has data information about every infrared frequency which originates from the source.
When the interferogram is being measured, all frequencies are being measured simultaneously. In order to make an identification and requires a frequency spectrum, as the measured interferogram signal cannot be interpreted, a means of decoding the individual frequencies is required. This can be solved only through the well-known mathematical method called the Fourier transform. This transformation will be performed and solved by the computer which then presents the user with desired spectral information for analysis.
IMRAN SYAKIR Figure 3.5: FTIR spectrum
Figure 3.5 shows the spectrum produced by FTIR. Characterization of CNT using FTIR will reveal the organic compound of the CNT. The size of peaks in the spectrum produced is a direct indication of material present.
33
3.4
THERMAL CONDUCTIVITY TEST
KD2-Pro Thermal Properties Analyser is a handheld device manufactured by Decagon Devices Inc. used to measure thermal properties of materials which is shown in Figure 3.6. This device consists of several controllers and sensors that can be inserted to any materials to check the thermal conductivity. Single needle sensors that measure thermal conductivity and resistivity is the most suitable to be used in fluids while the dual-needle sensor is suitable to measures thermal conductivity, resistivity, volumetric specific heat capacity and diffusivity.
IMRAN SYAKIR Figure 3.6: KD2-Pro thermal properties analyser
The sensor of the KD2-Pro with single needle or known as KS-1 sensor is specifically designed to test the liquid sample or which provides a very small heat pulse. The KS-1 sensor were attached to the sensor slot at KD2-Pro. Before the thermal conductivity test is run, the samples must be transferred to the specimen container with the attachment of silicon cap so that the needle of KS-1 sensor will remain static during the testing process. Then, turn the KD2-Pro in automatic mode and take the measurement in one minute. The thermal conductivity test of the nanofluid were taken at different temperature which is at 6 °C, 25 °C and 40 °C.
34
To obtain such temperature of the nanofluid, those three samples were immersed in the water bath so that the temperature of the samples were maintain at desired temperature. The schematic diagram of the refrigerated water bath were shown in Figure 3.7.
IMRAN SYAKIR Figure 3.7: Refrigerated water bath schematic diagram
35
CHAPTER IV
RESULT AND DISCUSSION
4.0
INTRODUCTION
This chapter represent all the experimental results that was obtained from the characterization testing using Scanning Electron Microscopy (SEM), Nitrogen gas (N2)
adsorption
analysis
and
Fourier
Transform
Infrared
(FTIR).
The
IMRAN SYAKIR characterization testing examination provides an overview of nanostructures of the
selected CNT. The thermal conductivity test was performed to the CNT and the data
were gathered and shown in graphical and tabulation chart. Based on thermal conductivity analysis data, for all CNT, CNF HHT-24 shows the highest thermal conductivity when nanofluids were added with 1.0 wt% of nanocarbon.
The nanofluids added with the smallest diameter CNF enhanced the highest thermal conductivity when measured at three different temperature of 6 °C, 25 °C and 40 °C. The data obtained was discussed in further explanation in order to analyse the result expectation.
36
4.1
RESULT AND DISCUSSION
4.1.1
Scanning Electron Microscopy (SEM)
The characterization testing method were enhanced for carbon nanomaterials. However, the standard acquisition procedure conveyed with the commercial software were commonly favoured for easy analysis and comparison with the gained data. For morphological examinations of the CNT, a FEI Quanta 200F Field Emission Scanning Electron Microscopy (FESEM) was utilized.
The CNT sample were approximately scattered on conductive carbon tape to preserve the arranged morphology as much as could reasonably be expected. The images were gained at different magnifications to show both the agglomeration of the tubes and the surface structure of the individual tubes.
IMRAN SYAKIR All the resolution images were obtained utilizing an acceleration voltage of 2
kv and 5 kv for better determination of surface features. The SEM images produced
reveal the morphology (surface), composition of chemical, crystalline structure and also material content that make up the specimen observed under SEM.
37
a
b
c
d
IMRAN SYAKIR e
f
Figure 4.1: SEM images at 10000x and 50000x magnification for CNT Nanoamor (a, b), functionalized MWCNT (c, d) and CNF HHT-24 (e, f)
SEM analysis is valuable for visualising and measuring macroscopic features up to the nanoscale dimension. Figure 4.1 shows the morphology of the three different nanocarbons. From the SEM images shown in Figure 4.1, the morphology of the three different nanocarbons are clearly distinguished between each other.
For the CNT Nanoamor, the SEM images shown in Figure 4.1(a) and Figure 4.1(b) demonstrates that the morphology are quite similar when compared to
38
functionalized MWCNT. The images presence signify a non-uniform type of fibre nanocarbons with smallest size of nanocarbons with an average diameter of 10 nm to 30 nm. The nanocarbon structures for commercial CNT are well graphitized with 10 to 20 concentric layers where the outer layers are smooth (Verdejo et al. 2007).
The morphology images of functionalized MWCNT shown in Figure 4.1(c) and Figure 4.1(d) illustrate the presence of agglomerate nanocarbon with an average diameter from 30 nm to 50 nm. The images shows a tubular fibre structure with a polygonal cross section (Tessonnier et al. 2009). The SEM images clearly reveal that the functionalized MWCNT mainly have a well graphitized tubular fibers structure with polygonal cross section of CNT. The nanoparticles can be clearly seen from the morphology images which indicate the higher potential of thermal conductivity enhancement of the nanofluid and act predominantly in suspension because of its greater surface area.
Figures 4.1(e) and Figure 4.1(f) show images of CNF HHT-24. The
IMRAN SYAKIR morphology shows the fully graphitized tubular structure of carbon nanofiber.
From the Figure 4.1, the nanotubes morphology are randomly entangled and
highly interconnected, probably due to the Van der Waal’s force interaction. All the SEM images illustrated agglomerate carbon nanotube and nanofibers, primarily with non-uniform tubular structure.
The diameter distribution for the tube in CNT Nanoamor and functionalized MWCNT and fiber in CNF HHT-24 were gained from the SEM images. The diameter were scaled based on the SEM images scaling. Figure 4.2 shows the diameter distribution for all the nanocarbon. From the Figure 4.2, it can be seen that the diameter distribution for CNT Nanoamor mostly lies in between 16 nm to 20 nm. This shows the tally with the actual average diameter which is between the range of 10 nm to 30 nm. The same goes to functionalized MWCNT which shows the higher diameter distribution at 26 nm to 30 nm. The CNF HHT-24 shows the largest diameter distribution at 61 nm to 70 nm.
39
(a) CNT Nanoamor 30 25
No
20 15 10 5 0
11-15
16-20
21-25
26-30
41-45
55-60
Diameter Distribution (nm)
(b) Functionalized MWCNT 30 25
No
20 15 10
IMRAN SYAKIR 5 0
16-20 21-25 26-30 31-35 45-50 51-55
Diameter Distribution (nm)
(c) CNF HHT-24 25
No
20 15 10 5 0
41-50 51-60 61-70 71-80 81-90 91-100 101-110 130-140
Diameter Distribution (nm)
Figure 4.2: Diameter distribution for (a) CNT Nanoamor, (b) functionalized MWCNT, (c) CNF HHT-24
40
From previous SEM result, the diameter of the nanocarbon increases from carbon nanotubes to carbon nanofibers (CNT Nanoamor < functionalized MWCNT < CNF HHT-24). The increase in diameter results in reducing the surface area of nanocarbon.
CNF HHT-24 has a bigger diameter comparing to other CNT and has lowest specific surface area. However, the thermal conductivity test conducted shows that CNF HHT-24 conduct high thermal conductivity better compared to other CNT. The reason which explain this is the dispersion of CNF HHT-24 in nanofluids. When all the CNT is dispersed in nanofluids, the solution might look well because of the black solution. However, CNF HHT-24 might has a better dispersion compared to others. The better dispersion is obtained from the aggregates formed in nanofluids. The ultrasonication process break the aggregates into a smaller aggregates. The high heat treated of CNF HHT-24 converts the fiber to a fully graphitized form and creates a highly conductive carbon nanofiber.
IMRAN SYAKIR Generally, the surface areas contribute to the enhancement of physical and
chemical properties of nanofluids. The properties that found to influence surface area
were number of walls or diameter, impurities, and surface functionalization with
hydroxyl and carboxyl groups. Higher surface areas are expected to provide a better media for thermal transport in nanofluids. Even though CNT Nanoamor had the smallest diameter of all nanocarbons, which should provide the highest surface area, the larger sizes of the activated carbons, as a nanocarbon support are expected to reduce thermal conductivity performance.
4.1.2
Nitrogen gas (N2) Adsorption Analysis
The Nitrogen gas (N2) adsorption analysis were performed generally focused on ability of absorbent features for characterization properties influenced by porosity and texture development of nanomaterial. The porosity existence is analysed by using BET method through the adsorption and desorption techniques by applying gas or steam as an adsorbate. A graph of Volume against Relative Pressure for each sample were plotted to visualize the adsorption isotherm.
41
CNT Nanoamor (adsorption) CNT Nanoamor (Desorption) CNF HHT-24 (adsorption) CNF HHT-24 (desorption) Functionalized MWCNT (adsorption) Functionalized MWCNT (desorption)
300
volume, cc/g
250 200 150 100 50 0 0
0.2
0.4
0.6
0.8
1
1.2
Relative Pressure, P/Po
Figure 4.3: Isotherm comparison for CNT Nanoamor, functionalized MWCNT and CNF HHT-24
The isotherm plot explaining the porosity information especially related to the shape, porosity type and depth of existed pores. Basically, the isotherm is divided
IMRAN SYAKIR to three regions indication. First region is derived from 0 - 0.3 P/P0 relative pressure, second are 0.3 - 0.75 P/P0 and third region in range of 0.75 - 1.0 P/P0.
According to Figure 4.3, for CNT Nanoamor, the isotherm can be classified as Type II and Type III. Type II isotherm is produced by the non-porous or solid macro pore. Isotherm is not limited to a monolayer adsorption at adsorbent surface, on otherwise it is also can occur on adsorption multilayer. Type III isotherms showed non-porous solid characteristics. The presence of hysteresis in this isotherm shows a presence of a macropore or non-porous with mesopore solid. The presence of hysteresis type H3 yield the Type II isotherm with slit-like pores.
For functionalized MWCNT, the isotherm can be classified as Type II and Type IV. From here, it is assumed that the sample used is macroporous and has hysteresis with different value of adsorbed and desorbed. Isotherm Type IV is characterized by hysteresis loop showing the presence of capillary condensation turned in a mesoporous materials. The presence of hysteresis type H3 can be seen from the isotherm plot which represent slit-like pores that yield in Type II isotherm.
42
The CNF HHT-24 can be classified as Type I and Type IV isotherm which means that the sample is mostly microporous with hysteresis loops. The hysteresis type H4 would yield isotherm Type I (adsorbent-adsorbate pair) which represent slitlike pores.
Materials with micro-sized pores shows the strong interactions among the narrow pore walls with material adsorbed on the relative pressure which cause the volume of material adsorbed in the pores increases. Pore with meso-sized shows an increase in the volume of the adsorption due to the effect of the occurrence of capillary condensation turn through the establishment of a hysteresis loop. Macrosized pores indicate the formation of a monolayer on relatively at low pressure and the adsorption layers at relatively high pressure. Material which have bigger pore will result in a weak interaction between materials adsorbed and the adsorbent which causing difficult adsorption.
The isotherm were figured out from curve slope and adsorption point
IMRAN SYAKIR placement. Therefore, the acquisition surface area reading is supportive from
isotherm assessment and further evaluation were proven by Figure 4.4 of DFT plot which covering all type of pores of tested sample features. Density Functional
Theory (DFT) is the best evidence to clarify an existence of porosity type and elucidating the distribution of porosity population.
Generally, DFT pore size distribution method calculates the distribution of micro, meso and macropores from an adsorption isotherm. The micropore diameter size is between 0 nm to 2 nm, mesopore is between 2 nm to 50 nm and macropore size is more than 50 nm. For each samples, a graph of Pore Volume against Pore Width were plotted to visualize the pore size distribution.
43
0.0045
micropore
mesopore CNT Nanoamor
0.004
Functionalized MWCNT
pore volume, cc/A/g
0.0035
CNF HHT-24
0.003 0.0025 0.002 0.0015 0.001 0.0005 0 0
10
20
30
40
50
60
70
pore width, A
Figure 4.4: DFT pore size distribution comparison
Referring to the Figure 4.4, the plot for CNT Nanoamor shows that the high peak is representing range of micropore type with diameter 1.4 nm and depth
IMRAN SYAKIR 2.15x10-2 cc/g. This shows that the CNT Nanoamor has a high distribution of micropores and average distribution of mesopores. High distribution of micropores
contribute to the high surface area. For functionalized MWCNT, the plot shows that
high peak is representing range of mesopore type with diameter 3.1 nm and depth 5.25x10-3 cc/g. Whilst, CNF HHT-24 shows the high peak with high distribution of micropores which have 0.39 nm and depth 2.07x10-4 cc/g and moderate distribution of mesopores.
Surface area is measured from diameter and depth of existed pores whether it is coming from micro, meso or macro types influencing on surface area reading based on volume of gas adsorbed. Table 4.1 shows the BET surface area for all sample tested.
44
Table 4.1: BET surface area CNT
BET Surface Area (m2/s)
CNT Nanoamor
1.610x102
Functionalized MWCNT
1.261x101
CNF HHT-24
3.241x101
The BET surface area obtained shows that CNT Nanoamor has the largest surface area (CNT Nanoamor > CNF HHT-24 > Functionalized MWCNT) compared to other CNT. This is due to the high distribution of micropores in the sample. The functionalized MWCNT has the smallest surface area due to the high distribution of mesopores in the sample. This contribute to the lower surface area.
From the SEM result, CNF HHT-24 has a bigger diameter which should has smallest surface area compared to others. However, the BET surface area shows that functionalized MWCNT has the smallest surface area. The brief explanation which
IMRAN SYAKIR can explain this is in term of agglomeration. The more the agglomeration between
CNT or CNF, the more the void space in the materials. The void space contribute to the large surface area. The more the void space, the higher the surface area. Functionalized MWCNT may contain less agglomeration and has a straight tube structure, thus no void space which gives lower surface area.
4.1.3
Fourier Transform Infrared (FTIR)
FTIR spectra was gained utilizing a PerkinElmer Spectrum 100 FTIR spectrometer. All the spectra recorded were processed with the computer software program Spectra for Windows (Perkin-Elmer). The descriptive example of CNT FTIR spectrum is presented in Figure 4.5.
Transmittance [a.u]
1026
1383
3437
1624
45
CNT Nanoamor Nanoamor MWCNT
Functionalized MWCNT HHT24 CNF HHT-24 4000
3500
3000
2500
2000
1500
1000
500
-1
Wavenumber [cm ]
Figure 4.5: FTIR spectra of CNTs
On the horizontal axis is the infrared wavelengths expressed in term of a unit
IMRAN SYAKIR called wavenumber (cm-1) which represent the number of waves fit into one
centimeter. The size of peaks in the spectrum represent a direct indication of material present which is the content of the organic compound in CNT.
The peaks in the COOH spectrum represent the functional groups that are present in the molecule. FTIR spectra of the CNTs reveal that the functionalized MWCNT gives the highest carboxyl group –COOH (3437 cm-1) peak followed by CNT Nanoamor and CNF HHT-24. Table 4.2 shows the FTIR spectra evaluation based on the peaks produced.
46
Table 4.2: FTIR spectra evaluation Bond
Compound Type
Frequency Range
-COOH
Carboxylic Acid
3000 – 3640 cm-1
C=C
Aromatic Rings
1600, 1500 cm-1
C-O
Alcohol, Ethers,
1000 – 1260 cm-1
Carboxylic Acid, Esthers The functionalized MWCNT has the highest –COOH peak due to the functionalization of the molecule with –COOH group. The CNT which has carboxyl group contributes to the easy dispersion of the CNT in nanofluids. The contribution of carboxyl group on the nanocarbon surface will increase the hydrophilicity and thus enable a good dispersion of CNT particles in nanofluids, hence improve its stability.
IMRAN SYAKIR From the Figure 4.5 it can be seen that CNF HHT-24 still have –COOH
group even though has been treated with higher temperature.
In generally, FTIR Spectroscopy is a technique based on the determination of the interaction between an infrared radiation and a sample that can be solid, liquid or gaseous. It measures the frequencies at which the sample absorbs, and also the intensities of these absorptions. The frequencies are very helpful for the identification of the sample chemical and organic compound make-up due to the fact that chemical functional groups are responsible for the absorption of radiation at different frequencies.
47
4.1.4
Thermal Conductivity Test
The thermal conductivity testing were performed experimentally at various temperatures ranging from 6 °C to 40 °C to analyse the heat transfer performance. To obtain such temperature of the nanofluid, those three samples was immersed in the water bath so that the temperature of the samples were maintain at desired temperature. The stable nanofluid was tested using KD2-Pro device after the observation and validation of the stability of the nanofluid in order to obtain thermal conductivity of nanofluid. The nanofluid was prepared by mixed together CNT in the deionized water with 1.0 wt% of CNT. The addition of nanoparticles in nanofluid is to enhance the thermal conductivity of the nanofluids. Table 4.2 shows the thermal conductivity reading for all the CNTs at 1.0 wt% at different temperature.
Table 4.3: Thermal conductivity of CNT Nanoamor, functionalized MWCNT and CNF HHT-24 at 1.0 wt% of CNT Thermal Conductivity (W/m.K) at Temperature
IMRAN SYAKIR CNT
(°C)
6
25
40
CNT Nanoamor
0.582
0.600
0.676
Functionalized MWCNT
0.577
0.579
0.633
CNF HHT-24
0.610
0.656
0.681
Based on thermal conductivity data in Table 4.3, for all CNT, CNF HHT-24 shows the highest thermal conductivity at all measured temperature when nanofluids were added with 1.0 wt% of nanocarbon. The highest thermal conductivity was gained at temperature 40 °C with 0.681 W/m.K.
48
4.1.4.1 Percentage of Enhancement of Thermal Conductivity
In order to determine the percentage of enhancement of thermal conductivity, the thermal conductivity result from the addition of the CNT has been compared with the normal rate of deionized water. Table 4.4 shows the reading of thermal conductivity of deionized water at 6 °C, 25 °C and 40 °C.
Table 4.4: Thermal conductivity of deionized water Temperature (°C)
Thermal Conductivity (W/m.K)
6
0.570
25
0.595
40
0.615
IMRAN SYAKIR Table 4.5: Percentage enhancement of thermal conductivity
Percentage of Enhancement (%) at Temperature
CNT
(°C)
6
25
40
CNT Nanoamor
2.11%
-0.16%
9.92%
functionalized MWCNT
1.23%
-2.69%
2.93%
CNF HHT-24
7.02%
10.25%
10.73%
The percentage of the enhancement of thermal conductivity is shown in the Table 4.5. From the Table 4.5, the thermal conductivity testing at 40°C, the nanofluids containing 1.0 wt% of CNF HHT-24 nanocarbon showed the best enhancement with 10.73 %. The negative value show in the Table 4.3 signify there is no improvement on the thermal conductivity of the nanofluid and the value of thermal conductivity obtained is lower than deionized water. Overall, nanofluid based CNF HHT-24 nanocarbon loading of 1.0 wt% gave the best enhancement of all temperatures tested.
49
4.1.4.2 Thermal Conductivity Analysis
The nanofluids added with the CNF HHT-24 enhance the highest thermal conductivity when measured at three different temperature of 6 °C, 25 °C and 40 °C. Focusing on the enhancement of thermal conductivity and convective heat transfer experimentally, the past research done by some researcher reveal that the carbon nanofiber proves to be great alternative for carbon nanotube. This was supported by the studies conducted by K.J Lee et al. in 2007 which showed that suspension of nanofluid-based CNF had a better thermal conductivity enhancement compare to nanofluid CNT.
From the Table 4.1, it can be seen that the thermal conductivity increase with increase of the temperature of the nanofluids. When the temperature increase, the average kinetic energy of the nanoparticles also increases and cause the nanoparticles to move more energetically. Thus, the thermal conductivity is higher as temperature increase. This was supported by the research conducted by Murshed et al. in 2007,
IMRAN SYAKIR the thermal conductivity increase with the increment of temperature being investigated.
Even though CNT Nanoamor had the smallest diameter of all nanocarbons, which should provide the highest surface area, the larger sizes of the activated carbons, as a nanocarbon support are expected to reduce thermal conductivity performance. These characteristics of the nanocarbon are expected to provide the best features for improving the thermal conductivity of nanofluids to be a medium for a heat transfer fluid. This result reveal that the carbon nanofiber proves to be a great alternative for carbon nanotube.
50
CHAPTER V
CONCLUSION AND RECOMMENDATION
5.1
CONCLUSION
The characterization testing for the nanocarbon materials was conducted to study the surface properties of carbon nanotube to analyse the thermal and heat transfer properties for industrial cooling application. Three carbon nanotube were
IMRAN SYAKIR characterized in this research that is CNT Nanoamor, functionalized MWCNT and CNF HHT 24. All three CNT were characterized using Scanning Electron
Microscopy (SEM), Fourier Transform Infrared (FTIR) and Nitrogen gas (N2) adsorption. Then, the thermal conductivity was conducted to all the sample tested. The morphology structure of the three sample tested using SEM shows that the nanotubes are randomly entangled and highly interconnected, probably due to the Van der Waals force interaction. All the SEM images illustrated agglomerate carbon nanotube and nanofibers, primarily with non-uniform tubular structure.
From FTIR result, the spectra reveal that the functionalized MWCNT gives the highest carboxyl group –COOH with 3437 cm-1 peak followed by CNT Nanoamor and CNF HHT-24. The contribution of carboxyl group on the nanocarbon surface will increase the hydrophilicity and thus enable a good dispersion of CNT particles in nanofluids and improve stability. Characterization using Nitrogen gas (N2) adsorption analysis reveal the pore type of the material tested. According to Figure 4.3, for CNT Nanoamor, the isotherm can be classified as Type II and Type III which shows that it have a non-porous or solid macro pore. For functionalized MWCNT, the isotherm can be classified as Type II and Type IV. From here, it is
51
assumed that the sample used is macroporous and has hysteresis loop showing the presence of capillary condensation turned in a mesoporous materials.
The CNF HHT-24 can be classified as Type I and Type IV isotherm which means that the sample is mostly microporous with hysteresis loops. In conclusion, the BET characterization technique encompasses external area and pore area evaluations to determine the total specific surface area in order to yield important information in studying the effects of surface porosity and particle size in nanofluids applications.
Focusing on the enhancement of thermal conductivity and convective heat transfer experimentally, the result reveal that the suspension of nanofluid-based CNF had a better thermal conductivity enhancement compare to nanofluid CNT. The research conducted shows that the nanofluids added with the smallest diameter CNF will enhance the highest thermal conductivity when measured at three different temperature of 6 oC, 25 oC and 45 oC. This can be proved from the result in Table 4.3
IMRAN SYAKIR which shows CNF HHT-24 conduct the highest thermal conductivity at 45 oC with 0.681 W/m.k. This result reveal that the carbon nanofiber proves to be a great alternative for carbon nanotube.
5.2
RECOMMENDATION
In future research with regard to the nanofluids, the investigation can be improve by considering other characterization testing methods which employed nowadays such as Inverse Gas Chromatoghraphy (IGC), Scanning Tunnelling Microscopy (STM) and High Resolution Transmission Electron Microscopy (HRTEM). IGC can be a versatile and powerful fast technique for characterizing the physicochemical properties of material due to its applicability in determining the surface properties of solids in any form such as films, fibres and powders of both crystalline and amorphous structures. For STM method, it is a type of electron microscope that shows three-dimensional images of a sample. In the STM, the structure of a surface is studied using a stylus that scans the surface at a fixed distance from it. HRTEM is an instrument for high-magnification studies of
52
nanomaterials. High resolution of HRTEM makes it perfect for imaging materials on the atomic scale.
These characterization method allows the advance research of the sample tested by quantify the graphitic content of the nanocarbon and characterize the local atomic structure such as lattice defects which cannot be studies in conventional method. Besides, the sample used also can be improved by studies a large variety of commercial nanocarbon that has in the market nowadays. Each nanocarbon might be has a different characteristics as it was produced from a different company. Thus, a more result would yield if more sample is been investigated. The investigation of the textural properties could also be revised by broadening the scope of research by investigating the thermal properties of nanofluids in terms of heat capacity, viscosity, and heat transfer.
IMRAN SYAKIR
53
REFERENCES
Ali, F., Yunus, W. and Talib, Z. (2013). “Study of the Effect of Particles Size and Volume Fraction Concentration on the Thermal Conductivity and Thermal Diffusivity of Al2O3 Nanofluids”. International Journal of Physical Sciences. 8(28). pp 1442-1457. Buongiorno, J. (2006). “Convective Transport in Nanofluids”. Journal of Heat Transfer. 128(3). pp 240-250. Chen L., Xie H., Li Y. and Yu W. (2008). “Nanofluids Containing Carbon
IMRAN SYAKIR Nanotubes Treated by Mechanochemical Reaction”. Thermochimica Acta. 477. 1. pp 21–24. Choi,
J.,
Alexandrova,
M.
and
Park,
H.
(2011).
“Carbon
Nanotube
Nanofluidics”. Carbon nanotubes applications on electron devices. InTech Education and Publishing, Open Access Publication. Choi S. U. S and J. A. Eastman. (1995). “Enhancing Thermal Conductivity of Fluids with Nanoparticles”. ASME International Mechanical Engineering Congress and Exhibition. Califf. San Francisco, USA. Chopkar M., Das P. K. and Manna, I. (2006). “Synthesis and Characterization of Nanofluid for Advanced Heat Transfer Applications”. Scripta Materialia. 55. pp 549. Das, S.K, Putra, N. and Roetzel, W. (2003). “Pool Boiling Characteristics of Nanofluids”. International Journal of Heat and Mass Transfer. 46(5). pp 851-862.
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Eastman J. A., Choi S., Li S., Thompson L. J. and Lee S. (1997). “Enhanced Thermal Conductivity Through the Development of Nanofluids, in Nanophase and Nanocomposite Materials II”. 6. pp 457. Emmanuel, B., Thomas, S., Raghuvaran, G. and Sherwood, D., 2009. “Simulated XRD Profiles of Carbon Nanotubes (CNTs): An Efficient Algorithm and a Recurrence Relation for Characterising CNTs”. Journal of Alloys and Compounds. 479. pp 484-488. Hirlekar, R., Yamagar, M., Garse, H., Vij, M. and Kadam, V. (2009). “Carbon Nanotubes and Its Applications: A Review”. Asian Journal of Pharmaceutical and Clinical Research. 2(4). pp 17-27. Iijima.S. (2007). “Nano-Carbon Materials: Their Fundamentals and Various Applications Including Nano-Biotechnology”. University of Wien.
IMRAN SYAKIR Jang, S. and Choi, S. (2007). “Effects of Various Parameters on Nanofluid Thermal
Conductivity”. Journal of Heat Transfer. 129(5). pp 617-623.
Lee, S., Choi, S. U. S., Li, S., and Eastman, J. A., 1999, “Measuring Thermal Conductivity of Fluids Containing Oxide Nanoparticles”. ASME Journal of Heat Transfer. 121. pp 280–289. Lin, T., Bajpai, V., Ji, T. and Dai, L. (2003). “Chemistry of Carbon Nanotubes”. Australian journal of chemistry. 56(7). pp 635-651.
Mahmoodi, A., Ghoranneviss, M., Mojtahedzadeh, M., Hosseini, S. and Eshghabadi, M. (2012). “Various Temperature Effects on the Growth of Carbon Nanotubes (CNTs) By Thermal Chemical Vapor Deposition (TCVD) Method”. International Journal of Physical Sciences. 7(6). pp 949-952. McEuen, P., Fuhrer, M. and Park, H. (2002). “Single-Walled Carbon Nanotube Electronics”. IEEE Transactions on Nanotechnology. 1(1). pp 78-85. Meakin, P., 1992, “Aggregation Kinetics,” Phys. Scr. 46. pp 295–331.
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Minsta H.A., Roy G., Nguyen C.T., Doucet, D. (2009), “New Temperature Dependent Thermal Conductivity Data for Water-Based Nanofluids”. International Journal of Thermal Science. 48(2). pp 363-371.
Mohamad I. S., Hamid S. B. A., Chin W. M., Yau K. H. and Samsuri A. (2011). “Nanofluid-Based Nanocarbons: An Investigation of Thermal Conductivity Performance”. Journal of Mechanical Engineering and Technology. 3(1). pp 83. Murshed, S.M., Leong, K.C. and Yang, C. (2005). “Enhanced Thermal Conductivity of TiO2 - Water-based Nanofluids”. International Journal of Thermal Science. 44. pp 367-373 Nakhaei, F. and Bahari, A. (2009). “A Newly Defined Envelope Function for Nano Particles-Carbon Nano Tube”. Scientific Research and Essays. 4(12). pp 1496-1499. Nandkeolyar, R., Shaw, S., Sibanda, P. and Kameswaran, P. (2014). “Heat Transfer
IMRAN SYAKIR on Nanofluid Flow with Homogeneous-Heterogeneous Reactions and Internal Heat Generation”. Journal of Heat Transfer. 136(12).
Nguyen C. T., Roy G., Gauthier C. and Galanis N. (2007) “Heat Transfer Enhancement using Al2O3-Water Nanofluid for An Electronic Liquid Cooling System”. Applied Thermal Engineering. 27.
Singh, D., Timofeeva, E., Yu, W., Routbort, J., France, D., Smith, D., and LopezCepero, J. M., 2009, “An Investigation of Silicon Carbide-Water Nanofluid for Heat Transfer Applications”. Journal of Applied Physics. 105(6). Tarafdar, J., Sharma, S. and Raliya, R. (2013). “Nanotechnology: Interdisciplinary Science of Applications”. African Journal of Biotechnology. 12(3). pp 219-226. Wang, X., Xu, X., and Choi, S. U. S., 1999, “Thermal Conductivity of NanoparticleFluid Mixture,” Journal of Thermophysics Heat Transfer. 13. pp 474-480.
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Weitz, D. A., Huang, J. S., Lin, M. Y., and Sung, J., 1984, “Dynamics of DiffusionLimited Kinetic Aggregation,” Physic Review Letter. 53. pp 1657-1660. Weitz, D. A., Huang, J. S., Lin, M. Y., and Sung, J., 1985, “Limits of the Fractal Dimension for Irreversible Kinetic Aggregation of Gold Colloids”, Physics Review Letter. 54. pp 1416-1419. Xie, H., Lee, H., Youn, W. and Choi, M. (2003). “Nanofluids Containing Multiwalled Carbon Nanotubes and Their Enhanced Thermal Conductivities”. Journal of Applied Physics. 94(8). pp 4967-4971.
IMRAN SYAKIR
57
BIBLIOGRAPHY
Decagon Devices Inc. (2013). “KD2-Pro Thermal Properties Analyzer”. Pullman (Washington): Operator’s Manual.
Pyrografproducts.com. (2011). Pyrograf-III Carbon Nanofiber, Stacked-Cup Carbon Nanotubes. Retrieved 4 December 2014, from http://pyrografproducts.com/nanofiber
Industrial-grade MWNT-OH (90+%, O. Amorphous Products | Nanoscale Products Industrial-grade MWNT-OH (90+%, OD 10-30 nm). Nanoamor.com. Retrieved 2 December 2014, from http://www.nanoamor.com/inc/sdetail/27340
IMRAN SYAKIR Nanocyl.com,. (2014). Carbon Nanotubes: Technology, Properties and Definition:
Single wall and multiwall carbon nanotubes, Physical properties, Sinthesis, Electric Conductivity, Electrical, Electronics. Nanotube. Retrieved 4 December 2014, from http://www.nanocyl.com/jp/CNT-Expertise-Centre/Carbon-Nanotubes
FT-IR and FT-NIR Spectrometers. Retrieved 4 February 2015, from http://www.perkinelmer.com/Content/relatedmaterials/productnotes/prd_spectrum10 0opticaft-ir.pdf
58
APPENDIX A (i)
NO
Gantt chart for PSM I
TASK
PSM 1 (Week) 1
1
2
3
4
5
2
3
4
5
6
7
8
9
10
11
12
13
14
Title Selection
Literature Review
Methodology
Material Selection and Preparation Characterization Testing: Scanning Electron Microscopy (SEM) Characterization Testing: Fourier Transform Infrared (FTIR)
IMRAN SYAKIR 6
7
8
9
10
11
Characterization Testing: N2 adsorption analysis Thermal Conductivity Test
Presentation of PSM 1
Thesis Writing
Thesis Submission
Planning Ongoing
15
59
APPENDIX B (ii)
Gantt chart for PSM II
PSM 2 (Week) NO
TASK 1
1
PSM I Feedback
2
PSM II Planning
3
Material Selection and Preparation
4
5
2
3
4
5
6
7
8
9
10
11
12
13
14
15
Characterization Testing: Scanning Electron Microscopy (SEM) Characterization Testing: Fourier Transform Infrared (FTIR)
IMRAN SYAKIR 6
Characterization Testing: N2 adsorption analysis
7
Thermal Conductivity Test
8
Presentation of PSM II
9
Completion of Thesis
10
Thesis Submission
Planning Ongoing
60
APPENDIX C CNT Nanoamor Data Sheet Testing Date:
09/02/2015 Quantachrome Corporation Quantachrome Autosorb Automated Gas Sorption System Report Autosorb for Windows® for AS-3 and AS-6 Version 1.23
Sample ID Description Comments Sample Weight Adsorbate Cross-Sec Area NonIdeality 01:38 Molecular Wt Station #
CNT Nanoamor Powder 0.1992 g NITROGEN Outgas Temp 16.2 Ų/molec Outgas Time 6.580E-05 P/Po Toler
120 °C Operator 7.0 hrs Analysis Time 3 End of Run
28.0134 g/mol 4
2 77.35
Equil Time Bath Temp.
File Name
Rostam Omar 1519.2 min 04/02/2015 CNT.RAW
Isotherm P/Po 1.3963e-02 1.9874e-02 2.6106e-02 3.2265e-02 3.8048e-02 4.3559e-02 4.8924e-02 5.4193e-02 5.9406e-02 6.4488e-02 6.9640e-02 7.4758e-02 7.9827e-02 8.4867e-02 8.9962e-02 9.5039e-02 9.9970e-02 1.0512e-01
Volume [cc/g] STP 24.5272 26.4597 28.0379 29.2934 30.3337 31.2262 32.0103 32.7235 33.3754 33.9934 34.5766 35.1256 35.6565 36.1757 36.6714 37.1412 37.6189 38.0669
P/Po
Volume [cc/g] STP
1.1009e-01 1.4988e-01 2.0824e-01 2.5074e-01 2.9981e-01 3.4951e-01 3.9899e-01 4.4855e-01 4.9701e-01 6.0268e-01 6.9875e-01 7.9812e-01 8.9813e-01 9.4701e-01 9.5721e-01 9.6663e-01 9.7640e-01 9.9282e-01
P/Po
38.5151 41.5747 45.4854 48.1914 51.1059 54.0261 57.1074 60.1662 63.5060 71.4764 81.2520 96.5673 128.6682 171.0412 189.1019 213.2425 254.0532 626.4859
9.8229e-01 9.7272e-01 9.6091e-01 9.5187e-01 9.0336e-01 8.4889e-01 7.9909e-01 6.9637e-01 5.9547e-01 5.0135e-01 4.4937e-01 3.9857e-01 3.4762e-01 2.9691e-01 2.4620e-01 1.9575e-01 1.4667e-01 9.7948e-02
Volume [cc/g] STP 442.0722 316.4769 252.6360 219.0793 151.8855 122.5131 110.1797 91.7781 80.0351 71.3293 67.0863 63.0241 59.1998 55.4749 51.7520 48.1651 43.9979 39.2685
IMRAN SYAKIR MULTIPOINT BET P/Po 7.9827e-02 8.4867e-02 8.9962e-02 9.5039e-02 9.9970e-02 1.0512e-01 1.1009e-01 1.4988e-01 2.0824e-01 2.5074e-01 2.9981e-01
Volume [cc/g] STP
1/(W((Po/P)-1))
35.6565 36.1757 36.6714 37.1412 37.6189 38.0669 38.5151 41.5747 45.4854 48.1914 51.1059 BET Surface Area = Slope = Y - Intercept =
Correlation Coefficient = C =
1.947E+00 2.051E+00 2.157E+00 2.262E+00 2.362E+00 2.469E+00 2.570E+00 3.393E+00 4.627E+00 5.556E+00 6.704E+00 1.610E+02 m²/g 2.142E+01 2.179E-01 0.999811 9.927E+01
TOTAL PORE VOLUME Total pore volume = 2.925E-01 cc/g for pores smaller than 469.1 Å (Diameter),
61
at P/Po = 0.95721 AVERAGE PORE SIZE Average Pore Diameter = 7.269E+01 Å t-Method Micropore Analysis (de Boer) P/Po
Thickness Å
7.9827e-02 8.4867e-02 8.9962e-02 9.5039e-02 9.9970e-02 1.0512e-01 1.1009e-01 1.4988e-01 2.0824e-01 2.5074e-01 2.9981e-01
Volume [cc/g] STP
3.52 3.56 3.60 3.64 3.68 3.72 3.75 4.04 4.42 4.69 5.01
35.657 36.176 36.671 37.141 37.619 38.067 38.515 41.575 45.485 48.191 51.106
Slope =
1.037E+01
Y - Intercept = -5.736E-01 cc/g Micro-pore volume
=
-8.873E-04 cc/g
Micro-pore area
=
5.317E-01 m²/g
External Surface Area =
1.604E+02 m²/g
Correlation Coefficient
=
0.999437
BJH ADSORPTION PORE SIZE DISTRIBUTION
IMRAN SYAKIR Diameter Å
Pore Vol [cc/g]
10.23 10.84 11.37 11.83 12.24 12.60 12.94 13.27 13.58 13.87 14.16 14.45 14.72 14.99 15.26 15.52 15.78 16.04 17.15 19.57 22.10 24.53 27.36 30.50 34.03 38.05 46.37 61.50 87.85 154.66 292.95 425.47 532.78 715.79 1762.33
4.715E-03 8.372E-03 1.101E-02 1.321E-02 1.508E-02 1.665E-02 1.806E-02 1.929E-02 2.051E-02 2.162E-02 2.263E-02 2.363E-02 2.465E-02 2.558E-02 2.643E-02 2.741E-02 2.820E-02 2.909E-02 3.428E-02 4.064E-02 4.514E-02 4.961E-02 5.398E-02 5.885E-02 6.333E-02 6.858E-02 8.041E-02 9.572E-02 1.206E-01 1.745E-01 2.470E-01 2.780E-01 3.190E-01 3.873E-01 9.874E-01
Pore Surf Area Dv(d) [m²/g] [cc/Å/g] 1.843E+01 3.193E+01 4.121E+01 4.866E+01 5.477E+01 5.976E+01 6.410E+01 6.780E+01 7.142E+01 7.460E+01 7.745E+01 8.024E+01 8.301E+01 8.549E+01 8.770E+01 9.024E+01 9.225E+01 9.446E+01 1.066E+02 1.196E+02 1.277E+02 1.350E+02 1.414E+02 1.478E+02 1.530E+02 1.586E+02 1.688E+02 1.787E+02 1.900E+02 2.040E+02 2.139E+02 2.168E+02 2.199E+02 2.237E+02 2.373E+02
7.391E-03 6.429E-03 5.296E-03 5.148E-03 4.902E-03 4.460E-03 4.239E-03 3.890E-03 4.112E-03 3.731E-03 3.527E-03 3.624E-03 3.759E-03 3.438E-03 3.173E-03 3.859E-03 3.008E-03 3.510E-03 2.633E-03 2.208E-03 2.067E-03 1.666E-03 1.472E-03 1.473E-03 1.191E-03 1.228E-03 9.566E-04 8.561E-04 7.140E-04 5.454E-04 4.079E-04 3.552E-04 3.219E-04 2.865E-04 3.236E-04
Ds(d) [m²/Å/g]
2.889E+01 2.373E+01 1.864E+01 1.741E+01 1.603E+01 1.416E+01 1.310E+01 1.173E+01 1.211E+01 1.076E+01 9.961E+00 1.004E+01 1.021E+01 9.174E+00 8.317E+00 9.946E+00 7.624E+00 8.756E+00 6.142E+00 4.512E+00 3.742E+00 2.717E+00 2.152E+00 1.932E+00 1.400E+00 1.291E+00 8.253E-01 5.569E-01 3.251E-01 1.411E-01 5.570E-02 3.339E-02 2.417E-02 1.601E-02 7.344E-03
Dv(log d) [cc/g]
1.741E-01 1.604E-01 1.386E-01 1.402E-01 1.381E-01 1.294E-01 1.263E-01 1.188E-01 1.285E-01 1.192E-01 1.150E-01 1.205E-01 1.274E-01 1.187E-01 1.115E-01 1.379E-01 1.093E-01 1.296E-01 1.039E-01 9.934E-02 1.051E-01 9.402E-02 9.261E-02 1.033E-01 9.325E-02 1.075E-01 1.015E-01 1.204E-01 1.425E-01 1.874E-01 2.665E-01 3.467E-01 3.930E-01 4.678E-01 1.181E+00
Ds(log d) [m²/g]
6.805E+02 5.920E+02 4.877E+02 4.741E+02 4.515E+02 4.108E+02 3.904E+02 3.583E+02 3.787E+02 3.436E+02 3.249E+02 3.338E+02 3.462E+02 3.167E+02 2.922E+02 3.554E+02 2.770E+02 3.233E+02 2.423E+02 2.030E+02 1.903E+02 1.533E+02 1.354E+02 1.355E+02 1.096E+02 1.130E+02 8.759E+01 7.829E+01 6.489E+01 4.848E+01 3.639E+01 3.260E+01 2.950E+01 2.614E+01 2.681E+01
62 DR Method Micro-Pore Analysis log^2.00(Po/P)
Weight Adsorbed [grams]
1.41734E+00 1.33898E+00 1.26865E+00 1.20528E+00 1.14760E+00 1.09399E+00 1.04469E+00 1.00026E+00 9.57132E-01 9.18255E-01
8.463E-03 8.608E-03 8.745E-03 8.877E-03 9.006E-03 9.130E-03 9.247E-03 9.366E-03 9.477E-03 9.589E-03 Slope = -1.087E-01
Y - Intercept (anti-log) = Correlation Coefficient = Average Pore Width = Adsorption Energy (Eo) =
1.203E-02 0.998782 5.430E+00 nm 4.788E+00 kJ/mol
Micro Pore Volume =
7.473E-02 cc/g
Micro Pore Surface Area =
2.103E+02 m²/g
HK Method Pore Size Distribution Pore Width [Å]
Dv(w) [cc/Å/g]
Pore Width [Å]
Dv(w) [cc/Å/g]
Pore Width [Å]
Dv(w) [cc/Å/g]
3.1250 3.1750 3.2250 3.2750 3.3250 3.3750 3.4250 3.4750 3.5250 3.5750 3.6250 3.6750 3.7250 3.7750 3.8250 3.8750 3.9250 3.9750 4.0250 4.0750 4.1250 4.1750 4.2250 4.2750 4.3250 4.3750 4.4250 4.4750 4.5250 4.5750 4.6250 4.6750 4.7250 4.7750 4.8250 4.8750 4.9250 4.9750 5.0250 5.0750 5.1250 5.1750
0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001
8.5750 8.6250 8.6750 8.7250 8.7750 8.8250 8.8750 8.9250 8.9750 9.0250 9.0750 9.1250 9.1750 9.2250 9.2750 9.3250 9.3750 9.4250 9.4750 9.5250 9.5750 9.6250 9.6750 9.7250 9.7750 9.8250 9.8750 9.9250 9.9750 10.0250 10.0750 10.1250 10.1750 10.2250 10.2750 10.3250 10.3750 10.4250 10.4750 10.5250 10.5750 10.6250
0.00174 0.00182 0.00190 0.00198 0.00207 0.00216 0.00225 0.00234 0.00243 0.00252 0.00261 0.00270 0.00280 0.00289 0.00298 0.00308 0.00317 0.00326 0.00335 0.00343 0.00352 0.00360 0.00368 0.00376 0.00383 0.00390 0.00396 0.00402 0.00407 0.00412 0.00416 0.00419 0.00422 0.00424 0.00426 0.00427 0.00427 0.00427 0.00427 0.00425 0.00424 0.00422
14.0250 14.0750 14.1250 14.1750 14.2250 14.2750 14.3250 14.3750 14.4250 14.4750 14.5250 14.5750 14.6250 14.6750 14.7250 14.7750 14.8250 14.8750 14.9250 14.9750 15.0250 15.0750 15.1250 15.1750 15.2250 15.2750 15.3250 15.3750 15.4250 15.4750 15.5250 15.5750 15.6250 15.6750 15.7250 15.7750 15.8250 15.8750 15.9250 15.9750 16.0250 16.0750
0.00280 0.00278 0.00277 0.00276 0.00275 0.00274 0.00273 0.00273 0.00272 0.00271 0.00269 0.00268 0.00267 0.00266 0.00265 0.00265 0.00264 0.00263 0.00262 0.00261 0.00260 0.00259 0.00258 0.00257 0.00256 0.00255 0.00254 0.00254 0.00253 0.00253 0.00253 0.00253 0.00252 0.00251 0.00250 0.00249 0.00247 0.00246 0.00244 0.00243 0.00242 0.00242
IMRAN SYAKIR
63 5.2250 5.2750 5.3250 5.3750 5.4250 5.4750 5.5250 5.5750 5.6250 5.6750 5.7250 5.7750 5.8250 5.8750 5.9250 5.9750 6.0250 6.0750 6.1250 6.1750 6.2250 6.2750 6.3250 6.3750 6.4250 6.4750 6.5250 6.5750 6.6250 6.6750 6.7250 6.7750 6.8250 6.8750 6.9250 6.9750 7.0250 7.0750 7.1250 7.1750 7.2250 7.2750 7.3250 7.3750 7.4250 7.4750 7.5250 7.5750 7.6250 7.6750 7.7250 7.7750 7.8250 7.8750 7.9250 7.9750 8.0250 8.0750 8.1250 8.1750 8.2250 8.2750 8.3250 8.3750 8.4250 8.4750 8.5250
0.00001 0.00001 0.00001 0.00002 0.00002 0.00002 0.00002 0.00002 0.00003 0.00003 0.00003 0.00004 0.00004 0.00004 0.00005 0.00005 0.00006 0.00006 0.00007 0.00007 0.00008 0.00009 0.00009 0.00010 0.00011 0.00012 0.00013 0.00014 0.00015 0.00016 0.00018 0.00019 0.00020 0.00022 0.00024 0.00025 0.00027 0.00029 0.00031 0.00034 0.00036 0.00039 0.00041 0.00044 0.00047 0.00051 0.00054 0.00058 0.00061 0.00065 0.00070 0.00074 0.00078 0.00083 0.00088 0.00093 0.00099 0.00105 0.00110 0.00117 0.00123 0.00130 0.00136 0.00143 0.00151 0.00158 0.00166
10.6750 10.7250 10.7750 10.8250 10.8750 10.9250 10.9750 11.0250 11.0750 11.1250 11.1750 11.2250 11.2750 11.3250 11.3750 11.4250 11.4750 11.5250 11.5750 11.6250 11.6750 11.7250 11.7750 11.8250 11.8750 11.9250 11.9750 12.0250 12.0750 12.1250 12.1750 12.2250 12.2750 12.3250 12.3750 12.4250 12.4750 12.5250 12.5750 12.6250 12.6750 12.7250 12.7750 12.8250 12.8750 12.9250 12.9750 13.0250 13.0750 13.1250 13.1750 13.2250 13.2750 13.3250 13.3750 13.4250 13.4750 13.5250 13.5750 13.6250 13.6750 13.7250 13.7750 13.8250 13.8750 13.9250 13.9750
0.00420 0.00417 0.00414 0.00411 0.00408 0.00404 0.00401 0.00397 0.00393 0.00389 0.00386 0.00382 0.00378 0.00375 0.00372 0.00369 0.00367 0.00364 0.00362 0.00360 0.00357 0.00355 0.00354 0.00352 0.00350 0.00348 0.00346 0.00345 0.00343 0.00341 0.00339 0.00338 0.00336 0.00334 0.00332 0.00331 0.00329 0.00327 0.00325 0.00324 0.00322 0.00320 0.00318 0.00316 0.00314 0.00312 0.00310 0.00308 0.00306 0.00304 0.00303 0.00301 0.00300 0.00299 0.00297 0.00296 0.00295 0.00294 0.00292 0.00291 0.00290 0.00288 0.00287 0.00285 0.00284 0.00282 0.00281
16.1250 16.1750 16.2250 16.2750 16.3250 16.3750 16.4250 16.4750 16.5250 16.5750 16.6250 16.6750 16.7250 16.7750 16.8250 16.8750 16.9250 16.9750 17.0250 17.0750 17.1250 17.1750 17.2250 17.2750 17.3250 17.3750 17.4250 17.4750 17.5250 17.5750 17.6250 17.6750 17.7250 17.7750 17.8250 17.8750 17.9250 17.9750 18.0250 18.0750 18.1250 18.1750 18.2250 18.2750 18.3250 18.3750 18.4250 18.4750 18.5250 18.5750 18.6250 18.6750 18.7250 18.7750 18.8250 18.8750 18.9250 18.9750 19.0250 19.0750 19.1250 19.1750 19.2250 19.2750 19.3250
0.00241 0.00241 0.00241 0.00241 0.00240 0.00240 0.00240 0.00240 0.00240 0.00239 0.00238 0.00237 0.00236 0.00234 0.00233 0.00231 0.00230 0.00230 0.00229 0.00228 0.00228 0.00227 0.00226 0.00225 0.00224 0.00222 0.00221 0.00219 0.00217 0.00216 0.00214 0.00213 0.00211 0.00210 0.00209 0.00207 0.00206 0.00205 0.00204 0.00202 0.00201 0.00200 0.00199 0.00198 0.00197 0.00196 0.00195 0.00195 0.00194 0.00193 0.00192 0.00192 0.00191 0.00190 0.00190 0.00189 0.00189 0.00188 0.00188 0.00187 0.00187 0.00186 0.00186 0.00186 0.00185
IMRAN SYAKIR
AREA-VOLUME-PORE SIZE SUMMARY SURFACE AREA DATA Multipoint BET.............................................. Langmuir Surface Area....................................... BJH Method Cumulative Adsorption Surface Area............... DH Method Cumulative Adsorption Surface Area................ t-Method External Surface Area..............................
1.610E+02 2.339E+02 2.373E+02 2.400E+02 1.604E+02
m²/g m²/g m²/g m²/g m²/g
64 t-Method Micro Pore Surface Area............................ DR Method Micro Pore Area...................................
5.317E-01 2.103E+02
m²/g m²/g
Total Pore Volume for pores with Diameter less than 469.1 Å at P/Po = 0.95721......................... 2.925E-01 BJH Method Cumulative Adsorption Pore Volume................ 9.874E-01 DH Method Cumulative Adsorption Pore Volume................. 9.576E-01 t-Method Micro Pore Volume.................................. -8.873E-04 DR Method Micro Pore Volume................................. 7.473E-02 HK Method Cumulative Pore Volume............................ 6.457E-02 SF Method Cumulative Pore Volume............................ 6.612E-02
cc/g cc/g cc/g cc/g cc/g cc/g cc/g
PORE VOLUME DATA
PORE SIZE DATA Average Pore Diameter....................................... BJH Method Adsorption Pore Diameter (Mode).................. DH Method Adsorption Pore Diameter (Mode).................. DR Method Micro Pore Width .............................. DA Method Pore Diameter (Mode)............................. HK Method Pore Width (Mode)............................. SF Method Pore Diameter (Mode).............................
7.269E+01 1.023E+01 1.023E+01 1.086E+02 1.840E+01 1.038E+01 1.901E+01
Å Å Å Å Å Å Å
IMRAN SYAKIR DFT Method Pore Size Distribution
Pore Width [Å]
3.98620 4.17027 4.36282 4.56423 4.77491 4.99529 5.22581 5.46694 5.71917 5.98301 6.25899 6.54768 6.84965 7.16552 7.49593 7.84156 8.20308 8.58125 8.97682 9.39061 9.82344 10.27619 10.74977 11.24516 11.76335 12.30539 12.87238 13.46547 14.08585 14.73479 15.41360 16.12366 16.86639 17.64331 18.45600
Cumul. Pore Volume [cc/g]
Cumul. Surface Area [m²/g]
3.76247E-05 1.89911E-04 3.52815E-04 5.29675E-04 7.25629E-04 9.45249E-04 1.19447E-03 1.47857E-03 1.80231E-03 2.17222E-03 2.58863E-03 3.05127E-03 3.55583E-03 4.08906E-03 4.64643E-03 5.23092E-03 5.85946E-03 6.56163E-03 7.35902E-03 8.26150E-03 9.27094E-03 1.03777E-02 1.15571E-02 1.27922E-02 1.41046E-02 1.55686E-02 1.72426E-02 1.92217E-02 2.15478E-02 2.43186E-02 2.70436E-02 2.95640E-02 3.20968E-02 3.46607E-02 3.70254E-02
1.88775E-01 9.19115E-01 1.66590E+00 2.44088E+00 3.26165E+00 4.14096E+00 5.09475E+00 6.13411E+00 7.26624E+00 8.50276E+00 9.83336E+00 1.12465E+01 1.27197E+01 1.42081E+01 1.56952E+01 1.71859E+01 1.87184E+01 2.03549E+01 2.21315E+01 2.40536E+01 2.61087E+01 2.82627E+01 3.04570E+01 3.26536E+01 3.48851E+01 3.72645E+01 3.98655E+01 4.28049E+01 4.61076E+01 4.98686E+01 5.34044E+01 5.65308E+01 5.95341E+01 6.24404E+01 6.50030E+01
dV(w) [cc/Å/g]
4.08793E-04 8.08691E-04 8.27025E-04 8.58357E-04 9.09171E-04 9.74149E-04 1.05679E-03 1.15171E-03 1.25465E-03 1.37047E-03 1.47488E-03 1.56653E-03 1.63328E-03 1.65015E-03 1.64893E-03 1.65309E-03 1.69947E-03 1.81499E-03 1.97044E-03 2.13198E-03 2.27971E-03 2.38949E-03 2.43441E-03 2.43700E-03 2.47578E-03 2.64017E-03 2.88604E-03 3.26177E-03 3.66510E-03 4.17381E-03 3.92403E-03 3.46972E-03 3.33333E-03 3.22582E-03 2.84430E-03
dS(w) [m²/Å/g]
2.05104E+00 3.87836E+00 3.79124E+00 3.76124E+00 3.80812E+00 3.90027E+00 4.04451E+00 4.21337E+00 4.38751E+00 4.58121E+00 4.71284E+00 4.78499E+00 4.76894E+00 4.60580E+00 4.39952E+00 4.21624E+00 4.14349E+00 4.23012E+00 4.39005E+00 4.54067E+00 4.64136E+00 4.65054E+00 4.52924E+00 4.33431E+00 4.20932E+00 4.29108E+00 4.48409E+00 4.84464E+00 5.20394E+00 5.66525E+00 5.09164E+00 4.30389E+00 3.95263E+00 3.65670E+00 3.08225E+00
65 19.30608 20.19530 21.12544 22.09840 23.11614 24.18073 25.29431 26.45915 27.67761 28.95215 30.28536 31.67992 33.13868 34.66458 36.26072 37.93032 39.67677 41.50360 43.41452 45.41339 47.50428 49.69139 51.97918 54.37227 56.87551 59.49397
3.88351E-02 4.02035E-02 4.03823E-02 4.04495E-02 4.17740E-02 4.38339E-02 4.65730E-02 4.99961E-02 5.36676E-02 5.73381E-02 6.07449E-02 6.42154E-02 6.78674E-02 7.11057E-02 7.41840E-02 7.70050E-02 7.97513E-02 8.38118E-02 8.80418E-02 9.24258E-02 9.70235E-02 1.01764E-01 1.06548E-01 1.11186E-01 1.15050E-01 1.16069E-01
6.68777E+01 6.82329E+01 6.84022E+01 6.84630E+01 6.96090E+01 7.13127E+01 7.34785E+01 7.60660E+01 7.87190E+01 8.12546E+01 8.35044E+01 8.56954E+01 8.78995E+01 8.97678E+01 9.14657E+01 9.29531E+01 9.43375E+01 9.62942E+01 9.82428E+01 1.00174E+02 1.02109E+02 1.04017E+02 1.05858E+02 1.07564E+02 1.08923E+02 1.09265E+02
2.08094E-03 1.50432E-03 1.87884E-04 6.74866E-05 1.27218E-03 1.89135E-03 2.40442E-03 2.87257E-03 2.94548E-03 2.81504E-03 2.49790E-03 2.43258E-03 2.44720E-03 2.07448E-03 1.88521E-03 1.65159E-03 1.53716E-03 2.17267E-03 2.16382E-03 2.14386E-03 2.14946E-03 2.11859E-03 2.04405E-03 1.89460E-03 1.50892E-03 7.78512E-04
2.15574E+00 1.48977E+00 1.77875E-01 6.10783E-02 1.10069E+00 1.56435E+00 1.90116E+00 2.17133E+00 2.12842E+00 1.94462E+00 1.64957E+00 1.53572E+00 1.47695E+00 1.19689E+00 1.03981E+00 8.70853E-01 7.74841E-01 1.04698E+00 9.96817E-01 9.44155E-01 9.04956E-01 8.52700E-01 7.86489E-01 6.96899E-01 5.30606E-01 2.61711E-01
DFT Kernel File : N2_carb.gai Micro Pore Volume = 0.1161 cc/g Lower Confidence Limit
= 12.872 Å
Actual Fitting Error = 0.913 % Best Value of Regularization Parameter = 0
IMRAN SYAKIR Min. Relative Pressure = 1.4554E-02 Max. Relative Pressure = 6.8914E-01 Pore Width (Mode) = 1.4735E+01
Å
66
IMRAN SYAKIR
67
IMRAN SYAKIR
68
IMRAN SYAKIR
69
APPENDIX D Functionalized MWCNT Data Sheet Testing Date:
09/02/2015 Quantachrome Corporation Quantachrome Autosorb Automated Gas Sorption System Report Autosorb for Windows® for AS-3 and AS-6 Version 1.23
Sample ID Description Comments Sample Weight Adsorbate Cross-Sec Area NonIdeality 16:12 Molecular Wt Station #
FMWCNT (Functionalized MWCNT) Fine Powder Carbon 0.1488 g NITROGEN Outgas Temp 120°C Operator 16.2 Ų/molec Outgas Time 7.0 hrs Analysis Time 6.580E-05 P/Po Toler 3 End of Run 28.0134 g/mol 1
Equil Time Bath Temp.
2 77.35
File Name
Rostam Omar 341.1 min 05/02/2015 FMWCNT.RAW
Isotherm P/Po 9.9399e-03 2.5090e-02 3.1184e-02 3.6379e-02 4.1469e-02 4.6511e-02 5.1515e-02 5.6341e-02 6.1523e-02 6.6561e-02 7.1606e-02 7.6328e-02 8.1546e-02 8.6609e-02 9.1630e-02 9.6632e-02 1.0140e-01 1.0656e-01
Volume [cc/g] STP 2.0034 2.2829 2.3671 2.4228 2.4694 2.5087 2.5441 2.5975 2.6321 2.6611 2.6857 2.7392 2.7686 2.7950 2.8177 2.8405 2.8983 2.9270
P/Po
Volume [cc/g] STP
1.1163e-01 1.6008e-01 2.0941e-01 2.5982e-01 3.0975e-01 3.5985e-01 4.0851e-01 4.5928e-01 5.0932e-01 6.0595e-01 7.0150e-01 8.0856e-01 9.0125e-01 9.5058e-01 9.5677e-01 9.6629e-01 9.7670e-01 9.9261e-01
P/Po
2.9518 3.2133 3.5227 3.7967 4.0637 4.3184 4.6906 4.9899 5.2835 5.9624 7.0919 8.8736 12.6126 17.1977 18.7889 20.4673 23.6843 30.5137
9.8275e-01 9.7086e-01 9.6287e-01 9.4778e-01 9.0256e-01 8.4261e-01 7.9323e-01 6.9193e-01 6.0109e-01 4.9157e-01 4.4817e-01 4.0075e-01 3.5154e-01 3.0331e-01 2.3888e-01 1.9019e-01 1.4175e-01 5.3516e-02
Volume [cc/g] STP 27.3994 24.6737 23.0097 20.8557 15.9955 12.9306 11.1969 9.0168 7.8733 6.5242 5.6473 5.2352 5.0086 4.6775 4.2231 3.9180 3.5768 3.1956
IMRAN SYAKIR MULTIPOINT BET P/Po 6.6561e-02 7.1606e-02 7.6328e-02 8.1546e-02 8.6609e-02 9.1630e-02 9.6632e-02 1.0140e-01 1.0656e-01 1.1163e-01 1.6008e-01 2.0941e-01 2.5982e-01 3.0975e-01
Volume [cc/g] STP
1/(W((Po/P)-1))
2.6611 2.6857 2.7392 2.7686 2.7950 2.8177 2.8405 2.8983 2.9270 2.9518 3.2133 3.5227 3.7967 4.0637
BET Surface Area = Slope =
2.144E+01 2.298E+01 2.414E+01 2.566E+01 2.714E+01 2.864E+01 3.013E+01 3.115E+01 3.260E+01 3.406E+01 4.746E+01 6.016E+01 7.397E+01 8.836E+01
1.261E+01 m²/g 2.728E+02
70 Y - Intercept = Correlation Coefficient =
3.491E+00 0.999930
C =
7.914E+01
TOTAL PORE VOLUME Total pore volume = 2.906E-02 cc/g for pores smaller than 464.5 Å (Diameter), at P/Po = 0.95677 AVERAGE PORE SIZE Average Pore Diameter = 9.222E+01 Å t-Method Micropore Analysis (de Boer) P/Po
Thickness Å
9.9399e-03 2.5090e-02 3.1184e-02 3.6379e-02 4.1469e-02 4.6511e-02 5.1515e-02 5.6341e-02 6.1523e-02 6.6561e-02 7.1606e-02 7.6328e-02 8.1546e-02 8.6609e-02 9.1630e-02 9.6632e-02 1.0140e-01 1.0656e-01 1.1163e-01 1.6008e-01 2.0941e-01 2.5982e-01 3.0975e-01
Volume [cc/g] STP
2.62 2.93 3.01 3.08 3.14 3.20 3.25 3.30 3.35 3.40 3.44 3.49 3.53 3.57 3.61 3.65 3.69 3.73 3.77 4.11 4.43 4.75 5.08
2.003 2.283 2.367 2.423 2.469 2.509 2.544 2.598 2.632 2.661 2.686 2.739 2.769 2.795 2.818 2.841 2.898 2.927 2.952 3.213 3.523 3.797 4.064
IMRAN SYAKIR Slope =
8.250E-01
Y - Intercept = -1.414E-01 cc/g Micro-pore volume
=
0.000E+00 cc/g
Micro-pore area
=
0.000E+00 m²/g
External Surface Area =
1.261E+01 m²/g
Correlation Coefficient
=
0.999400
BJH ADSORPTION PORE SIZE DISTRIBUTION Diameter Å
Pore Vol [cc/g]
10.21 11.28 11.73 12.10 12.45 12.78 13.09 13.40
2.798E-04 3.973E-04 4.315E-04 4.385E-04 4.385E-04 4.385E-04 5.487E-04 5.487E-04
Pore Surf Area Dv(d) [m²/g] [cc/Å/g] 1.097E+00 1.513E+00 1.630E+00 1.653E+00 1.653E+00 1.653E+00 1.989E+00 1.989E+00
1.696E-04 2.343E-04 8.717E-05 1.966E-05 0.000E+00 0.000E+00 3.692E-04 0.000E+00
Ds(d) [m²/Å/g] 6.648E-01 8.306E-01 2.973E-01 6.498E-02 0.000E+00 0.000E+00 1.128E+00 0.000E+00
Dv(log d) [cc/g] 3.978E-03 6.086E-03 2.354E-03 5.480E-04 0.000E+00 0.000E+00 1.113E-02 0.000E+00
Ds(log d) [m²/g] 1.559E+01 2.158E+01 8.028E+00 1.811E+00 0.000E+00 0.000E+00 3.401E+01 0.000E+00
71 13.70 13.99 14.26 14.54 14.81 15.08 15.34 15.60 15.85 16.11 17.44 19.85 22.37 25.06 27.97 31.17 34.82 39.09 47.20 62.07 91.00 160.56 309.26 436.39 527.55 718.01 1728.95
5.487E-04 5.487E-04 6.903E-04 6.903E-04 6.903E-04 6.903E-04 6.903E-04 8.692E-04 8.804E-04 8.804E-04 1.069E-03 1.583E-03 1.963E-03 2.335E-03 2.648E-03 3.418E-03 3.869E-03 4.271E-03 5.259E-03 7.330E-03 1.051E-02 1.744E-02 2.563E-02 2.846E-02 3.136E-02 3.682E-02 4.783E-02
1.989E+00 1.989E+00 2.387E+00 2.387E+00 2.387E+00 2.387E+00 2.387E+00 2.845E+00 2.874E+00 2.874E+00 3.307E+00 4.341E+00 5.022E+00 5.615E+00 6.063E+00 7.051E+00 7.569E+00 7.980E+00 8.818E+00 1.015E+01 1.155E+01 1.328E+01 1.434E+01 1.460E+01 1.482E+01 1.512E+01 1.537E+01
0.000E+00 0.000E+00 5.400E-04 0.000E+00 0.000E+00 0.000E+00 0.000E+00 7.279E-04 4.230E-05 0.000E+00 7.892E-05 2.107E-04 1.463E-04 1.342E-04 1.023E-04 2.311E-04 1.136E-04 8.773E-05 8.489E-05 1.145E-04 7.987E-05 6.982E-05 4.135E-05 5.030E-05 2.302E-05 2.142E-05 6.232E-06
0.000E+00 0.000E+00 1.515E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 1.867E+00 1.067E-01 0.000E+00 1.810E-01 4.245E-01 2.617E-01 2.142E-01 1.464E-01 2.966E-01 1.305E-01 8.976E-02 7.193E-02 7.379E-02 3.511E-02 1.739E-02 5.348E-03 4.610E-03 1.746E-03 1.193E-03 1.442E-04
0.000E+00 0.000E+00 1.773E-02 0.000E+00 0.000E+00 0.000E+00 0.000E+00 2.614E-02 1.544E-03 0.000E+00 3.164E-03 9.620E-03 7.530E-03 7.733E-03 6.586E-03 1.657E-02 9.097E-03 7.888E-03 9.180E-03 1.625E-02 1.647E-02 2.497E-02 2.841E-02 5.047E-02 2.783E-02 3.503E-02 2.247E-02
0.000E+00 0.000E+00 4.974E+01 0.000E+00 0.000E+00 0.000E+00 0.000E+00 6.704E+01 3.896E+00 0.000E+00 7.257E+00 1.938E+01 1.346E+01 1.234E+01 9.417E+00 2.127E+01 1.045E+01 8.071E+00 7.779E+00 1.047E+01 7.238E+00 6.220E+00 3.675E+00 4.626E+00 2.110E+00 1.952E+00 5.199E-01
DR Method Micro-Pore Analysis log^2.00(Po/P)
Weight Adsorbed [grams]
1.31114E+00 1.24840E+00 1.18504E+00 9.87978E-01 9.45549E-01 9.06751E-01
8.351E-04 8.518E-04 8.609E-04 9.012E-04 9.102E-04 9.179E-04
IMRAN SYAKIR Slope = -9.947E-02
Y - Intercept (anti-log) = Correlation Coefficient =
Average Pore Width = Adsorption Energy (Eo) =
1.130E-03
0.999014 5.193E+00 nm 5.006E+00 kJ/mol
Micro Pore Volume =
5.622E-03 cc/g
Micro Pore Surface Area =
1.582E+01 m²/g
HK Method Pore Size Distribution Pore Width [Å]
Dv(w) [cc/Å/g]
Pore Width [Å]
Dv(w) [cc/Å/g]
Pore Width [Å]
Dv(w) [cc/Å/g]
3.1250 3.1750 3.2250 3.2750 3.3250 3.3750 3.4250 3.4750 3.5250 3.5750 3.6250 3.6750 3.7250 3.7750 3.8250 3.8750 3.9250
0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000
8.5750 8.6250 8.6750 8.7250 8.7750 8.8250 8.8750 8.9250 8.9750 9.0250 9.0750 9.1250 9.1750 9.2250 9.2750 9.3250 9.3750
0.00014 0.00014 0.00014 0.00015 0.00015 0.00016 0.00016 0.00016 0.00017 0.00017 0.00017 0.00018 0.00018 0.00019 0.00019 0.00019 0.00020
14.0250 14.0750 14.1250 14.1750 14.2250 14.2750 14.3250 14.3750 14.4250 14.4750 14.5250 14.5750 14.6250 14.6750 14.7250 14.7750 14.8250
0.00016 0.00016 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00016 0.00016 0.00017
72 3.9750 4.0250 4.0750 4.1250 4.1750 4.2250 4.2750 4.3250 4.3750 4.4250 4.4750 4.5250 4.5750 4.6250 4.6750 4.7250 4.7750 4.8250 4.8750 4.9250 4.9750 5.0250 5.0750 5.1250 5.1750 5.2250 5.2750 5.3250 5.3750 5.4250 5.4750 5.5250 5.5750 5.6250 5.6750 5.7250 5.7750 5.8250 5.8750 5.9250 5.9750 6.0250 6.0750 6.1250 6.1750 6.2250 6.2750 6.3250 6.3750 6.4250 6.4750 6.5250 6.5750 6.6250 6.6750 6.7250 6.7750 6.8250 6.8750 6.9250 6.9750 7.0250 7.0750 7.1250 7.1750 7.2250 7.2750 7.3250 7.3750 7.4250 7.4750 7.5250 7.5750 7.6250 7.6750 7.7250 7.7750
0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00002 0.00002 0.00002 0.00002 0.00002 0.00002 0.00002 0.00002 0.00003 0.00003 0.00003 0.00003 0.00003 0.00003 0.00004 0.00004 0.00004 0.00004 0.00004 0.00005 0.00005 0.00005 0.00005 0.00006 0.00006 0.00006 0.00006 0.00007 0.00007 0.00007 0.00007 0.00008 0.00008
9.4250 9.4750 9.5250 9.5750 9.6250 9.6750 9.7250 9.7750 9.8250 9.8750 9.9250 9.9750 10.0250 10.0750 10.1250 10.1750 10.2250 10.2750 10.3250 10.3750 10.4250 10.4750 10.5250 10.5750 10.6250 10.6750 10.7250 10.7750 10.8250 10.8750 10.9250 10.9750 11.0250 11.0750 11.1250 11.1750 11.2250 11.2750 11.3250 11.3750 11.4250 11.4750 11.5250 11.5750 11.6250 11.6750 11.7250 11.7750 11.8250 11.8750 11.9250 11.9750 12.0250 12.0750 12.1250 12.1750 12.2250 12.2750 12.3250 12.3750 12.4250 12.4750 12.5250 12.5750 12.6250 12.6750 12.7250 12.7750 12.8250 12.8750 12.9250 12.9750 13.0250 13.0750 13.1250 13.1750 13.2250
0.00020 0.00021 0.00021 0.00021 0.00022 0.00022 0.00022 0.00023 0.00023 0.00023 0.00023 0.00024 0.00024 0.00024 0.00025 0.00025 0.00025 0.00025 0.00025 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00025 0.00025 0.00025 0.00025 0.00025 0.00024 0.00024 0.00024 0.00023 0.00023 0.00023 0.00022 0.00022 0.00022 0.00022 0.00021 0.00021 0.00021 0.00020 0.00020 0.00020 0.00019 0.00019 0.00019 0.00018 0.00018 0.00018 0.00018 0.00017 0.00017 0.00017 0.00017 0.00017 0.00018 0.00018 0.00018 0.00018 0.00019 0.00019 0.00019 0.00019 0.00019 0.00018 0.00018
14.8750 14.9250 14.9750 15.0250 15.0750 15.1250 15.1750 15.2250 15.2750 15.3250 15.3750 15.4250 15.4750 15.5250 15.5750 15.6250 15.6750 15.7250 15.7750 15.8250 15.8750 15.9250 15.9750 16.0250 16.0750 16.1250 16.1750 16.2250 16.2750 16.3250 16.3750 16.4250 16.4750 16.5250 16.5750 16.6250 16.6750 16.7250 16.7750 16.8250 16.8750 16.9250 16.9750 17.0250 17.0750 17.1250 17.1750 17.2250 17.2750 17.3250 17.3750 17.4250 17.4750 17.5250 17.5750 17.6250 17.6750 17.7250 17.7750 17.8250 17.8750 17.9250 17.9750 18.0250 18.0750 18.1250 18.1750 18.2250 18.2750 18.3250 18.3750 18.4250 18.4750 18.5250 18.5750 18.6250 18.6750
0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00016 0.00015 0.00014 0.00014 0.00013 0.00013 0.00013 0.00014 0.00015 0.00016 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00017 0.00018 0.00018 0.00018 0.00018 0.00018 0.00018 0.00018 0.00017 0.00016 0.00015 0.00015 0.00014 0.00014 0.00013 0.00013 0.00013 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00014 0.00015
IMRAN SYAKIR
73 7.8250 7.8750 7.9250 7.9750 8.0250 8.0750 8.1250 8.1750 8.2250 8.2750 8.3250 8.3750 8.4250 8.4750 8.5250
0.00008 0.00009 0.00009 0.00009 0.00010 0.00010 0.00010 0.00011 0.00011 0.00011 0.00012 0.00012 0.00013 0.00013 0.00013
13.2750 13.3250 13.3750 13.4250 13.4750 13.5250 13.5750 13.6250 13.6750 13.7250 13.7750 13.8250 13.8750 13.9250 13.9750
0.00018 0.00018 0.00018 0.00018 0.00018 0.00018 0.00018 0.00018 0.00017 0.00017 0.00017 0.00017 0.00016 0.00016 0.00016
18.7250 18.7750 18.8250 18.8750 18.9250 18.9750 19.0250 19.0750 19.1250 19.1750 19.2250 19.2750 19.3250
0.00015 0.00015 0.00015 0.00015 0.00015 0.00015 0.00015 0.00015 0.00015 0.00015 0.00015 0.00015 0.00015
AREA-VOLUME-PORE SIZE SUMMARY SURFACE AREA DATA Multipoint BET.............................................. Langmuir Surface Area....................................... BJH Method Cumulative Adsorption Surface Area............... DH Method Cumulative Adsorption Surface Area................ t-Method External Surface Area.............................. t-Method Micro Pore Surface Area............................ DR Method Micro Pore Area...................................
1.261E+01 1.834E+01 1.537E+01 1.589E+01 1.261E+01 0.000E+00 1.582E+01
m²/g m²/g m²/g m²/g m²/g m²/g m²/g
2.906E-02 4.783E-02 4.680E-02 0.000E+00 5.622E-03 4.903E-03 5.036E-03
cc/g cc/g cc/g cc/g cc/g cc/g cc/g
9.222E+01 1.560E+01 1.560E+01 1.039E+02 1.840E+01 1.073E+01 1.975E+01
Å Å Å Å Å Å Å
PORE VOLUME DATA Total Pore Volume for pores with Diameter less than 464.5 Å at P/Po = 0.95677......................... BJH Method Cumulative Adsorption Pore Volume................ DH Method Cumulative Adsorption Pore Volume................. t-Method Micro Pore Volume.................................. DR Method Micro Pore Volume................................. HK Method Cumulative Pore Volume............................ SF Method Cumulative Pore Volume............................
IMRAN SYAKIR PORE SIZE DATA
Average Pore Diameter....................................... BJH Method Adsorption Pore Diameter (Mode).................. DH Method Adsorption Pore Diameter (Mode).................. DR Method Micro Pore Width .............................. DA Method Pore Diameter (Mode)............................. HK Method Pore Width (Mode)............................. SF Method Pore Diameter (Mode)............................. DFT Method Pore Size Distribution Pore Width [Å] 3.98620 4.17027 4.36282 4.56423 4.77491 4.99529 5.22581 5.46694 5.71917 5.98301 6.25899 6.54768 6.84965 7.16552 7.49593 7.84156 8.20308 8.58125 8.97682 9.39061 9.82344 10.27619 10.74977
Cumul. Pore Volume [cc/g]
Cumul. Surface Area [m²/g]
3.58865E-06 1.80899E-05 3.35613E-05 5.02993E-05 6.87569E-05 8.93738E-05 1.12719E-04 1.39274E-04 1.69549E-04 2.04157E-04 2.43209E-04 2.86744E-04 3.34392E-04 3.84818E-04 4.37464E-04 4.92410E-04 5.50838E-04 6.15182E-04 6.87897E-04 7.70458E-04 8.63325E-04 9.65688E-04 1.07502E-03
1.80054E-02 8.75514E-02 1.58475E-01 2.31819E-01 3.09130E-01 3.91676E-01 4.81023E-01 5.78170E-01 6.84040E-01 7.99729E-01 9.24517E-01 1.05750E+00 1.19662E+00 1.33736E+00 1.47783E+00 1.61797E+00 1.76043E+00 1.91039E+00 2.07240E+00 2.24823E+00 2.43731E+00 2.63653E+00 2.83994E+00
dV(w) [cc/Å/g] 3.89908E-05 7.70069E-05 7.85444E-05 8.12344E-05 8.56384E-05 9.14485E-05 9.89952E-05 1.07650E-04 1.17327E-04 1.28222E-04 1.38319E-04 1.47411E-04 1.54237E-04 1.56048E-04 1.55750E-04 1.55403E-04 1.57980E-04 1.66317E-04 1.79688E-04 1.95038E-04 2.09731E-04 2.21006E-04 2.25665E-04
dS(w) [m²/Å/g] 1.95629E-01 3.69313E-01 3.60062E-01 3.55961E-01 3.58702E-01 3.66139E-01 3.78870E-01 3.93821E-01 4.10293E-01 4.28620E-01 4.41985E-01 4.50269E-01 4.50351E-01 4.35553E-01 4.15559E-01 3.96356E-01 3.85172E-01 3.87630E-01 4.00337E-01 4.15389E-01 4.27000E-01 4.30133E-01 4.19850E-01
74 11.24516 11.76335 12.30539 12.87238 13.46547 14.08585 14.73479 15.41360 16.12366 16.86639 17.64331 18.45600 19.30608 20.19530 21.12544 22.09840 23.11614 24.18073 25.29431 26.45915 27.67761 28.95215 30.28536 31.67992 33.13868 34.66458 36.26072 37.93032 39.67677 41.50360 43.41452 45.41339 47.50428 49.69139
1.18900E-03 1.30813E-03 1.43695E-03 1.57979E-03 1.73588E-03 1.90575E-03 2.07950E-03 2.23628E-03 2.37871E-03 2.52011E-03 2.65750E-03 2.78416E-03 2.88242E-03 2.95546E-03 2.96529E-03 2.98560E-03 3.11555E-03 3.30909E-03 3.55600E-03 3.86035E-03 4.19633E-03 4.53924E-03 4.87569E-03 5.24745E-03 5.68286E-03 6.05747E-03 6.39608E-03 6.69866E-03 7.00666E-03 7.41210E-03 7.82786E-03 8.23614E-03 8.54510E-03 8.62216E-03
3.04266E+00 3.24521E+00 3.45457E+00 3.67651E+00 3.90834E+00 4.14954E+00 4.38538E+00 4.58880E+00 4.76547E+00 4.93315E+00 5.08889E+00 5.22615E+00 5.32794E+00 5.40028E+00 5.40958E+00 5.42796E+00 5.54039E+00 5.70047E+00 5.89570E+00 6.12575E+00 6.36853E+00 6.60542E+00 6.82760E+00 7.06230E+00 7.32508E+00 7.54121E+00 7.72798E+00 7.88752E+00 8.04278E+00 8.23815E+00 8.42968E+00 8.60949E+00 8.73957E+00 8.77058E+00
2.24907E-04 2.24726E-04 2.32308E-04 2.46258E-04 2.57260E-04 2.67657E-04 2.61730E-04 2.25759E-04 1.96073E-04 1.86102E-04 1.72864E-04 1.52347E-04 1.12986E-04 8.02971E-05 1.03292E-05 2.03962E-05 1.24813E-04 1.77712E-04 2.16740E-04 2.55396E-04 2.69540E-04 2.62998E-04 2.46683E-04 2.60581E-04 2.91765E-04 2.39978E-04 2.07371E-04 1.77147E-04 1.72394E-04 2.16944E-04 2.12677E-04 1.99660E-04 1.44440E-04 7.04636E-05
4.00006E-01 3.82078E-01 3.77571E-01 3.82615E-01 3.82103E-01 3.80037E-01 3.55254E-01 2.92935E-01 2.43211E-01 2.20678E-01 1.95954E-01 1.65092E-01 1.17048E-01 7.95206E-02 9.77893E-03 1.84594E-02 1.07988E-01 1.46987E-01 1.71375E-01 1.93049E-01 1.94771E-01 1.81678E-01 1.62906E-01 1.64509E-01 1.76088E-01 1.38457E-01 1.14378E-01 9.34067E-02 8.68993E-02 1.04542E-01 9.79752E-02 8.79300E-02 6.08115E-02 2.83605E-02
DFT Kernel File : N2_carb.gai
IMRAN SYAKIR Micro Pore Volume = 0.0086 cc/g
Lower Confidence Limit
= 12.305 Å
Actual Fitting Error = 1.182 %
Best Value of Regularization Parameter = 0 Min. Relative Pressure = 1.1455E-02 Max. Relative Pressure = 5.9629E-01 Pore Width (Mode) = 3.3139E+01
Å
75
IMRAN SYAKIR
76
IMRAN SYAKIR
77
IMRAN SYAKIR
78
IMRAN SYAKIR
79
APPENDIX E CNF HHT-24 Data Sheet Testing Date:
09/02/2015 Quantachrome Corporation Quantachrome Autosorb Automated Gas Sorption System Report Autosorb for Windows® for AS-3 and AS-6 Version 1.23
Sample ID Description Comments Sample Weight Adsorbate Cross-Sec Area NonIdeality 19:37 Molecular Wt Station #
CNF HHT-24 Powder 0.1533 g NITROGEN Outgas Temp 16.2 Ų/molec Outgas Time 6.580E-05 P/Po Toler
120 °C Operator 7.0 hrs Analysis Time 3 End of Run
Rostam Omar 661.2 min 03/02/2015
28.0134 g/mol 2
2 77.35
CNF.RAW
Equil Time Bath Temp.
File Name
Isotherm P/Po 6.9146e-03 2.5301e-02 3.1643e-02 3.6627e-02 4.1693e-02 4.6684e-02 5.1599e-02 5.6697e-02 6.1735e-02 6.6686e-02 7.1643e-02 7.6734e-02 8.1743e-02 8.6582e-02 9.1732e-02 9.6756e-02 1.0152e-01 1.0672e-01
Volume [cc/g] STP 6.2878 6.9444 7.0204 7.0957 7.1513 7.2017 7.2772 7.3266 7.3658 7.4176 7.4884 7.5299 7.5662 7.6545 7.6975 7.7339 7.8408 7.8942
P/Po
Volume [cc/g] STP
1.1197e-01 1.5999e-01 2.0979e-01 2.5918e-01 3.0796e-01 3.5826e-01 4.0861e-01 4.5794e-01 5.0852e-01 6.0496e-01 7.0264e-01 8.1006e-01 9.0540e-01 9.5184e-01 9.5839e-01 9.6798e-01 9.7864e-01 9.9164e-01
P/Po
7.9252 8.5368 9.2213 10.1150 11.3536 12.4601 13.3809 14.4305 15.2695 16.8827 19.1051 23.1432 30.2289 43.3883 48.0348 57.4627 72.1451 104.7553
9.8025e-01 9.7270e-01 9.5948e-01 9.5362e-01 8.9920e-01 8.5077e-01 7.9586e-01 6.8733e-01 5.9292e-01 4.9819e-01 4.3839e-01 3.8967e-01 3.4001e-01 2.9004e-01 2.3967e-01 1.8831e-01 1.3906e-01 5.8991e-02
Volume [cc/g] STP 82.8596 71.0475 59.9329 55.1559 36.3295 30.4198 26.6771 23.2024 20.3640 17.6998 16.8809 15.6291 14.2168 12.6799 11.2608 10.3638 9.3247 8.3597
IMRAN SYAKIR MULTIPOINT BET P/Po 7.6734e-02 8.1743e-02 8.6582e-02 9.1732e-02 9.6756e-02 1.0152e-01 1.0672e-01 1.1197e-01 1.5999e-01 2.0979e-01
Volume [cc/g] STP
1/(W((Po/P)-1))
7.5299 7.5662 7.6545 7.6975 7.7339 7.8408 7.8942 7.9252 8.5368 9.2213 BET Surface Area =
8.831E+00 9.414E+00 9.908E+00 1.050E+01 1.108E+01 1.153E+01 1.211E+01 1.273E+01 1.785E+01 2.304E+01 3.241E+01 m²/g
Slope =
1.068E+02
Y - Intercept =
7.046E-01
Correlation Coefficient = C =
0.999936 1.525E+02
TOTAL PORE VOLUME Total pore volume = 7.430E-02 cc/g for pores smaller than 481.9 Å (Diameter),
80
at P/Po = 0.95839 AVERAGE PORE SIZE Average Pore Diameter = 9.171E+01 Å t-Method Micropore Analysis (de Boer) P/Po
Thickness Å
7.6734e-02 8.1743e-02 8.6582e-02 9.1732e-02 9.6756e-02 1.0152e-01 1.0672e-01 1.1197e-01 1.5999e-01 2.0979e-01
Volume [cc/g] STP
3.49 3.53 3.57 3.61 3.65 3.69 3.73 3.77 4.11 4.43 Slope = Y - Intercept =
7.530 7.566 7.654 7.697 7.734 7.841 7.894 7.925 8.537 9.221 1.795E+00 1.213E+00 cc/g
Micro-pore volume
=
1.876E-03 cc/g
Micro-pore area
=
4.641E+00 m²/g
External Surface Area =
2.777E+01 m²/g
Correlation Coefficient
=
0.997358
BJH ADSORPTION PORE SIZE DISTRIBUTION
IMRAN SYAKIR Diameter Å
Pore Vol [cc/g]
9.97 11.31 11.76 12.12 12.47 12.79 13.11 13.41 13.71 13.99 14.27 14.55 14.82 15.08 15.35 15.60 15.86 16.12 17.44 19.86 22.36 24.99 27.87 31.12 34.77 39.00 47.09 62.14 91.57 165.41 318.82 450.25 551.33 770.53 1616.32
0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 5.635E-05 5.635E-05 5.635E-05 2.522E-04 2.522E-04 2.522E-04 2.522E-04 6.387E-04 2.149E-03 5.259E-03 7.805E-03 9.609E-03 1.186E-02 1.326E-02 1.560E-02 1.904E-02 2.574E-02 3.746E-02 6.050E-02 6.863E-02 8.491E-02 1.096E-01 1.624E-01
Pore Surf Area Dv(d) [m²/g] [cc/Å/g] 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 1.521E-01 1.521E-01 1.521E-01 6.542E-01 6.542E-01 6.542E-01 6.542E-01 1.433E+00 4.134E+00 9.113E+00 1.277E+01 1.509E+01 1.768E+01 1.911E+01 2.110E+01 2.331E+01 2.624E+01 2.907E+01 3.196E+01 3.269E+01 3.387E+01 3.515E+01 3.646E+01
0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 2.174E-04 0.000E+00 0.000E+00 7.980E-04 0.000E+00 0.000E+00 0.000E+00 1.570E-04 5.929E-04 1.151E-03 8.318E-04 5.246E-04 5.844E-04 3.036E-04 2.019E-04 1.859E-04 1.659E-04 1.093E-04 1.155E-04 1.284E-04 1.173E-04 8.256E-05 3.790E-05
Ds(d) [m²/Å/g]
0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 5.868E-01 0.000E+00 0.000E+00 2.046E+00 0.000E+00 0.000E+00 0.000E+00 3.163E-01 1.060E+00 1.843E+00 1.194E+00 6.743E-01 6.724E-01 3.114E-01 1.715E-01 1.197E-01 7.248E-02 2.642E-02 1.449E-02 1.140E-02 8.507E-03 4.286E-03 9.380E-04
DR Method Micro-Pore Analysis
Dv(log d) [cc/g]
0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 7.416E-03 0.000E+00 0.000E+00 2.867E-02 0.000E+00 0.000E+00 0.000E+00 7.172E-03 3.050E-02 6.619E-02 5.333E-02 3.755E-02 4.673E-02 2.723E-02 2.178E-02 2.640E-02 3.441E-02 4.011E-02 8.193E-02 1.329E-01 1.481E-01 1.446E-01 1.319E-01
Ds(log d) [m²/g]
0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 0.000E+00 2.002E+01 0.000E+00 0.000E+00 7.350E+01 0.000E+00 0.000E+00 0.000E+00 1.445E+01 5.455E+01 1.059E+02 7.654E+01 4.827E+01 5.377E+01 2.793E+01 1.850E+01 1.700E+01 1.503E+01 9.699E+00 1.028E+01 1.180E+01 1.074E+01 7.507E+00 3.263E+00
81
log^2.00(Po/P)
Weight Adsorbed [grams]
1.24325E+00 1.18277E+00 1.12906E+00 1.07636E+00 1.02885E+00 9.86965E-01 9.44330E-01 9.04244E-01
1.408E-03 1.415E-03 1.431E-03 1.439E-03 1.446E-03 1.466E-03 1.476E-03 1.482E-03 Slope = -6.919E-02
Y - Intercept (anti-log) = Correlation Coefficient = Average Pore Width = Adsorption Energy (Eo) =
1.712E-03 0.990193 4.331E+00 nm 6.002E+00 kJ/mol
Micro Pore Volume =
1.416E-02 cc/g
Micro Pore Surface Area =
3.984E+01 m²/g
HK Method Pore Size Distribution Pore Width [Å]
Dv(w) [cc/Å/g]
Pore Width [Å]
Dv(w) [cc/Å/g]
Pore Width [Å]
Dv(w) [cc/Å/g]
3.1250 3.1750 3.2250 3.2750 3.3250 3.3750 3.4250 3.4750 3.5250 3.5750 3.6250 3.6750 3.7250 3.7750 3.8250 3.8750 3.9250 3.9750 4.0250 4.0750 4.1250 4.1750 4.2250 4.2750 4.3250 4.3750 4.4250 4.4750 4.5250 4.5750 4.6250 4.6750 4.7250 4.7750 4.8250 4.8750 4.9250 4.9750 5.0250 5.0750 5.1250 5.1750 5.2250 5.2750 5.3250
0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00000 0.00001 0.00001 0.00001 0.00001 0.00001
8.5750 8.6250 8.6750 8.7250 8.7750 8.8250 8.8750 8.9250 8.9750 9.0250 9.0750 9.1250 9.1750 9.2250 9.2750 9.3250 9.3750 9.4250 9.4750 9.5250 9.5750 9.6250 9.6750 9.7250 9.7750 9.8250 9.8750 9.9250 9.9750 10.0250 10.0750 10.1250 10.1750 10.2250 10.2750 10.3250 10.3750 10.4250 10.4750 10.5250 10.5750 10.6250 10.6750 10.7250 10.7750
0.00031 0.00032 0.00033 0.00034 0.00035 0.00036 0.00036 0.00037 0.00038 0.00039 0.00040 0.00040 0.00041 0.00042 0.00043 0.00043 0.00044 0.00045 0.00045 0.00046 0.00046 0.00047 0.00047 0.00048 0.00048 0.00048 0.00048 0.00049 0.00049 0.00049 0.00049 0.00049 0.00048 0.00048 0.00048 0.00047 0.00047 0.00046 0.00046 0.00045 0.00044 0.00043 0.00042 0.00041 0.00039
14.0250 14.0750 14.1250 14.1750 14.2250 14.2750 14.3250 14.3750 14.4250 14.4750 14.5250 14.5750 14.6250 14.6750 14.7250 14.7750 14.8250 14.8750 14.9250 14.9750 15.0250 15.0750 15.1250 15.1750 15.2250 15.2750 15.3250 15.3750 15.4250 15.4750 15.5250 15.5750 15.6250 15.6750 15.7250 15.7750 15.8250 15.8750 15.9250 15.9750 16.0250 16.0750 16.1250 16.1750 16.2250
0.00025 0.00025 0.00025 0.00025 0.00025 0.00025 0.00024 0.00024 0.00024 0.00024 0.00024 0.00025 0.00026 0.00027 0.00028 0.00029 0.00030 0.00030 0.00030 0.00029 0.00029 0.00028 0.00027 0.00026 0.00025 0.00025 0.00024 0.00024 0.00025 0.00026 0.00028 0.00030 0.00032 0.00034 0.00035 0.00036 0.00036 0.00036 0.00035 0.00033 0.00032 0.00031 0.00030 0.00029 0.00029
IMRAN SYAKIR
82 5.3750 5.4250 5.4750 5.5250 5.5750 5.6250 5.6750 5.7250 5.7750 5.8250 5.8750 5.9250 5.9750 6.0250 6.0750 6.1250 6.1750 6.2250 6.2750 6.3250 6.3750 6.4250 6.4750 6.5250 6.5750 6.6250 6.6750 6.7250 6.7750 6.8250 6.8750 6.9250 6.9750 7.0250 7.0750 7.1250 7.1750 7.2250 7.2750 7.3250 7.3750 7.4250 7.4750 7.5250 7.5750 7.6250 7.6750 7.7250 7.7750 7.8250 7.8750 7.9250 7.9750 8.0250 8.0750 8.1250 8.1750 8.2250 8.2750 8.3250 8.3750 8.4250 8.4750 8.5250
0.00001 0.00001 0.00001 0.00001 0.00001 0.00001 0.00002 0.00002 0.00002 0.00002 0.00002 0.00002 0.00003 0.00003 0.00003 0.00003 0.00003 0.00004 0.00004 0.00004 0.00005 0.00005 0.00005 0.00006 0.00006 0.00006 0.00007 0.00007 0.00007 0.00008 0.00008 0.00009 0.00009 0.00010 0.00010 0.00011 0.00011 0.00012 0.00012 0.00013 0.00014 0.00014 0.00015 0.00015 0.00016 0.00017 0.00017 0.00018 0.00019 0.00019 0.00020 0.00021 0.00022 0.00022 0.00023 0.00024 0.00025 0.00026 0.00026 0.00027 0.00028 0.00029 0.00030 0.00031
10.8250 10.8750 10.9250 10.9750 11.0250 11.0750 11.1250 11.1750 11.2250 11.2750 11.3250 11.3750 11.4250 11.4750 11.5250 11.5750 11.6250 11.6750 11.7250 11.7750 11.8250 11.8750 11.9250 11.9750 12.0250 12.0750 12.1250 12.1750 12.2250 12.2750 12.3250 12.3750 12.4250 12.4750 12.5250 12.5750 12.6250 12.6750 12.7250 12.7750 12.8250 12.8750 12.9250 12.9750 13.0250 13.0750 13.1250 13.1750 13.2250 13.2750 13.3250 13.3750 13.4250 13.4750 13.5250 13.5750 13.6250 13.6750 13.7250 13.7750 13.8250 13.8750 13.9250 13.9750
0.00038 0.00037 0.00035 0.00034 0.00033 0.00032 0.00031 0.00030 0.00029 0.00029 0.00028 0.00028 0.00027 0.00027 0.00026 0.00026 0.00025 0.00025 0.00024 0.00024 0.00024 0.00024 0.00023 0.00023 0.00023 0.00023 0.00023 0.00024 0.00024 0.00024 0.00024 0.00025 0.00025 0.00026 0.00026 0.00026 0.00026 0.00026 0.00026 0.00025 0.00025 0.00025 0.00025 0.00025 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00024 0.00025 0.00025
16.2750 16.3250 16.3750 16.4250 16.4750 16.5250 16.5750 16.6250 16.6750 16.7250 16.7750 16.8250 16.8750 16.9250 16.9750 17.0250 17.0750 17.1250 17.1750 17.2250 17.2750 17.3250 17.3750 17.4250 17.4750 17.5250 17.5750 17.6250 17.6750 17.7250 17.7750 17.8250 17.8750 17.9250 17.9750 18.0250 18.0750 18.1250 18.1750 18.2250 18.2750 18.3250 18.3750 18.4250 18.4750 18.5250 18.5750 18.6250 18.6750 18.7250 18.7750 18.8250 18.8750 18.9250 18.9750 19.0250 19.0750 19.1250 19.1750 19.2250 19.2750 19.3250
0.00029 0.00029 0.00029 0.00029 0.00030 0.00030 0.00030 0.00030 0.00030 0.00029 0.00028 0.00027 0.00025 0.00024 0.00023 0.00022 0.00022 0.00022 0.00022 0.00022 0.00023 0.00024 0.00025 0.00025 0.00026 0.00027 0.00028 0.00028 0.00029 0.00030 0.00030 0.00031 0.00032 0.00032 0.00033 0.00033 0.00034 0.00035 0.00035 0.00035 0.00036 0.00036 0.00037 0.00037 0.00037 0.00038 0.00038 0.00038 0.00039 0.00039 0.00039 0.00039 0.00039 0.00040 0.00040 0.00040 0.00040 0.00040 0.00040 0.00040 0.00040 0.00040
IMRAN SYAKIR
AREA-VOLUME-PORE SIZE SUMMARY SURFACE AREA DATA Multipoint BET.............................................. Langmuir Surface Area....................................... BJH Method Cumulative Adsorption Surface Area............... DH Method Cumulative Adsorption Surface Area................ t-Method External Surface Area.............................. t-Method Micro Pore Surface Area............................ DR Method Micro Pore Area...................................
3.241E+01 4.864E+01 3.646E+01 3.721E+01 2.777E+01 4.641E+00 3.984E+01
m²/g m²/g m²/g m²/g m²/g m²/g m²/g
83 PORE VOLUME DATA Total Pore Volume for pores with Diameter less than 481.9 Å at P/Po = 0.95839......................... BJH Method Cumulative Adsorption Pore Volume................ DH Method Cumulative Adsorption Pore Volume................. t-Method Micro Pore Volume.................................. DR Method Micro Pore Volume................................. HK Method Cumulative Pore Volume............................ SF Method Cumulative Pore Volume............................
7.430E-02 1.624E-01 1.580E-01 1.876E-03 1.416E-02 1.303E-02 1.336E-02
cc/g cc/g cc/g cc/g cc/g cc/g cc/g
9.171E+01 2.499E+01 2.499E+01 8.663E+01 1.620E+01 1.002E+01 1.836E+01
Å Å Å Å Å Å Å
PORE SIZE DATA Average Pore Diameter....................................... BJH Method Adsorption Pore Diameter (Mode).................. DH Method Adsorption Pore Diameter (Mode).................. DR Method Micro Pore Width .............................. DA Method Pore Diameter (Mode)............................. HK Method Pore Width (Mode)............................. SF Method Pore Diameter (Mode).............................
IMRAN SYAKIR DFT Method Pore Size Distribution
Pore Width [Å]
3.98620 4.17027 4.36282 4.56423 4.77491 4.99529 5.22581 5.46694 5.71917 5.98301 6.25899 6.54768 6.84965 7.16552 7.49593 7.84156 8.20308 8.58125 8.97682 9.39061 9.82344 10.27619 10.74977 11.24516 11.76335 12.30539 12.87238 13.46547 14.08585 14.73479 15.41360 16.12366 16.86639 17.64331 18.45600
Cumul. Pore Volume [cc/g]
Cumul. Surface Area [m²/g]
2.07874E-04 4.10146E-04 6.10480E-04 8.12398E-04 1.02067E-03 1.23601E-03 1.46018E-03 1.69472E-03 1.93793E-03 2.19067E-03 2.44834E-03 2.70663E-03 2.96081E-03 3.20540E-03 3.44034E-03 3.67036E-03 3.90613E-03 4.15106E-03 4.40286E-03 4.66008E-03 4.91943E-03 5.17586E-03 5.42390E-03 5.66347E-03 5.90703E-03 6.15895E-03 6.39605E-03 6.61913E-03 6.83113E-03 7.00863E-03 7.16041E-03 7.30097E-03 7.41753E-03 7.51345E-03 7.59708E-03
1.04297E+00 2.01303E+00 2.93140E+00 3.81619E+00 4.68855E+00 5.55072E+00 6.40867E+00 7.26669E+00 8.11721E+00 8.96206E+00 9.78542E+00 1.05744E+01 1.13165E+01 1.19992E+01 1.26261E+01 1.32127E+01 1.37876E+01 1.43584E+01 1.49194E+01 1.54672E+01 1.59953E+01 1.64943E+01 1.69558E+01 1.73819E+01 1.77960E+01 1.82055E+01 1.85738E+01 1.89052E+01 1.92062E+01 1.94471E+01 1.96441E+01 1.98184E+01 1.99566E+01 2.00654E+01 2.01560E+01
dV(w) [cc/Å/g]
0.00000E+00 1.09885E-03 1.04045E-03 1.00254E-03 9.88556E-04 9.77147E-04 9.72467E-04 9.72658E-04 9.64254E-04 9.57920E-04 9.33644E-04 8.94707E-04 8.41734E-04 7.74327E-04 7.11051E-04 6.65523E-04 6.52147E-04 6.47668E-04 6.36549E-04 6.21632E-04 5.99206E-04 5.66376E-04 5.23741E-04 4.83613E-04 4.70015E-04 4.64765E-04 4.18171E-04 3.76138E-04 3.41718E-04 2.73524E-04 2.23604E-04 1.97949E-04 1.56937E-04 1.23459E-04 1.02908E-04
dS(w) [m²/Å/g]
0.00000E+00 5.26990E+00 4.76960E+00 4.39302E+00 4.14063E+00 3.91228E+00 3.72179E+00 3.55833E+00 3.37201E+00 3.20214E+00 2.98337E+00 2.73290E+00 2.45774E+00 2.16126E+00 1.89716E+00 1.69743E+00 1.59000E+00 1.50950E+00 1.41821E+00 1.32395E+00 1.21995E+00 1.10231E+00 9.74423E-01 8.60130E-01 7.99115E-01 7.55383E-01 6.49721E-01 5.58672E-01 4.85191E-01 3.71265E-01 2.90139E-01 2.45536E-01 1.86094E-01 1.39953E-01 1.11516E-01
84 19.30608 20.19530 21.12544 22.09840 23.11614 24.18073 25.29431 26.45915 27.67761 28.95215 30.28536 31.67992 33.13868 34.66458 36.26072 37.93032 39.67677 41.50360 43.41452 45.41339 47.50428 49.69139
7.67722E-03 7.73429E-03 7.73819E-03 7.82040E-03 8.18060E-03 8.73423E-03 9.47706E-03 1.04856E-02 1.17206E-02 1.30238E-02 1.43039E-02 1.55654E-02 1.67743E-02 1.79239E-02 1.90254E-02 2.00256E-02 2.09661E-02 2.18400E-02 2.25724E-02 2.31608E-02 2.34157E-02 2.36599E-02
2.02390E+01 2.02955E+01 2.02992E+01 2.03736E+01 2.06853E+01 2.11432E+01 2.17305E+01 2.24929E+01 2.33853E+01 2.42856E+01 2.51309E+01 2.59273E+01 2.66569E+01 2.73202E+01 2.79277E+01 2.84551E+01 2.89292E+01 2.93503E+01 2.96877E+01 2.99468E+01 3.00542E+01 3.01524E+01
9.42732E-05 6.41799E-05 4.19482E-06 8.44926E-05 3.53924E-04 5.20041E-04 6.67058E-04 8.65846E-04 1.01357E-03 1.02251E-03 9.60096E-04 9.04634E-04 8.28681E-04 7.53440E-04 6.90063E-04 5.99100E-04 5.38497E-04 4.78359E-04 3.83282E-04 2.94358E-04 1.21932E-04 1.11657E-04
9.76605E-02 6.35597E-02 3.97201E-03 7.64677E-02 3.06215E-01 4.30128E-01 5.27438E-01 6.54477E-01 7.32411E-01 7.06343E-01 6.34033E-01 5.71109E-01 5.00129E-01 4.34702E-01 3.80612E-01 3.15895E-01 2.71442E-01 2.30515E-01 1.76568E-01 1.29635E-01 5.13351E-02 4.49403E-02
DFT Kernel File : N2_carb.gai Micro Pore Volume = 0.0237 cc/g Lower Confidence Limit
= 12.305 Å
Actual Fitting Error = 2.385 % Best Value of Regularization Parameter = 0
IMRAN SYAKIR Min. Relative Pressure = 8.7532E-03 Max. Relative Pressure = 5.9532E-01 Pore Width (Mode) = 4.1703E+00
Å
85
IMRAN SYAKIR
86
IMRAN SYAKIR
87
IMRAN SYAKIR
Mechanical Engineering Research Day 2015 31 March 2015 - Melaka, Malaysia, pp. 1-2 © Centre for Advanced research on Energy
APPENDIX F
The effect of nanocarbon characteristics on enhancing thermal properties of nanofluids S. Zainal Abidin1,*, I.S. Mohamad1, N. Abdullah2, A.Y. Bani Hashim3
1)
Faculty of Mechanical Engineering, Universiti Teknikal Malaysia Melaka, Hang Tuah Jaya, 76100 Durian Tunggal, Melaka, Malaysia. 2) Department of Chemistry, Centre for Foundation Studies, Universiti Pertahanan Nasional Malaysia, Kem Sungai Besi, 57000, Kuala Lumpur. 3) Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, Hang Tuah Jaya, 76100 Durian Tunggal, Melaka, Malaysia. *Coresponding e-mail:
[email protected],
[email protected],
[email protected],
[email protected] Keywords: Carbon nanotube; thermal properties; nanofluids ABSTRACT – The different in nanocarbon structure may result in thermal conductivities performance. In this research, the understanding about the behavior and characteristic of different types of nanocarbon are investigated. The morphology and functionalized-group attachment on the nanocarbon surface were characterized using Scanning Electron Microscopy (SEM) and Fourier Transform Infra-Red (FTIR). The thermal conductivity testing were performed to select the best CNT which can possess a good thermal properties. The result shows that the CNT3 (HHT24) has the higher thermal conductivity enhancement.
The intrinsic mechanical and transport properties of CNT make them an ultimate carbon fiber. By and large, CNT demonstrate an exceptional blend of stiffness, strength, and tenacity contrasted with other fiber materials which generally fail to offer one or a greater amount of these properties. 2.
METHODOLOGY
IMRAN SYAKIR
1.
INTRODUCTION
Nanofluids were formed by fine dispersion of nanosized solid particles in a liquid. Even in dilute concentrations, typical colloids form aggregates that are dependent on the solution chemistry, surface charges, and thermal Brownian motion of the nanoparticles [1]. The external fields such as gravity and temperature can support or destroy the formation of aggregates. Thus, the tested nanofluids in most experimental shows that there is a competition between the growth of fractal-like structures, coalescence into large clumps, sedimentation, and fragmentation [2]. In general, the viscosity and thermal conductivity are sensitive to geometrical configuration and the connectivity [3] of the formed aggregated structure. Carbon nanotubes with rolled-up graphene sheets have high thermal conductivity and has the ability to remain in stable suspension for a long period of time. The carbon nanotubes were discovered by Iijima in 1991 [4] and since that, carbon nanotubes have received much attention. The diameters and arrangement of the hexagon rings along the tube length determined the metal properties of the carbon nanotubes, metallic or semiconductive. The consistent arrangement of the hexagon rings without any loose bonds make the carbon nanotube walls to become unreactive [5].
The characterizations which being conducted for the selected nanocarbon such as Carbon Nanotube (Nanoamor-CNT), Multiwalled CNT and Carbon Nanofiber (Pyrograf-CNF). The objectives is to find the best nanocarbon, which can enhance and possess a good thermal properties based on the structural analysis. Thermal conductivity testing was conducted using KD2Pro Thermal properties Analyzer. The results were used to syncronized the performance of thermal conductivity with the surface characteristic of nanocarbons. Table 1 shows the properties of commercial carbon nanotubes used in this studies. Table 1 Properties of the commercial CNT Specific Outer Sample Surface Types Diameter coding Area (nm) (m2/g) CNT1 Multiwalled30-50 60 CNT CNT2 Nanoamor 10-30 100 CNT CNT3 Pyrograf 100 43 CNF 2.1 Scanning Electron Microscopy (S.E.M) The Scanning Electron Microscopy (SEM) utilizes a focused beam of high energy electrons to create a mixed bag of signs on the surface of solid specimens. The signals that formed from the electron-sample correlations will produce the specimen or sample data that is the
Zainal Abidin et al., 2015
Transmittance [a.u]
2.2 Fourier Transform Infrared (FTIR) An infrared spectrum represents a fingerprint of a specimen with absorption peaks which correlate to the frequencies of vibrations between the obligations of the atom that making up the material. In order to make an identification and requires a frequency spectrum, as the measured interferogram signal cannot be interpreted, a means of decoding the individual frequencies is required. This can be solved only through the well-known mathematical method called the Fourier transform. This transformation will be performed and solved by the computer which then presents the user with desired spectral information for analysis.
1026
1383
1624
The results reveal that the CNT1 (fMWNT) shows the higher COOH spectrum followed by CNT2 (Nanoamor), and CNT3 (HHT24). The higher in the peak spectrum will enable a good dispersion of CNT in nanofluids and improve the stability of nanofluids.
3437
morphology (surface), composition of chemical, crystalline structure and also material content that make up the specimen observed under SEM. SEM was used to characterize the nanocarbons to generate high-resolution images with 10000x, 30000x, 60000x and 120000x magnification of shapes of objects and to observe the spatial variations in chemical compositions.
CNT2 Nanoamor MWCNT CNT1 HHT24 CNT3
4000
3500
3000
2500
2000
1500
1000
500
-1
Wavenumber [cm ]
Figure 2 FTIR spectra of CNTs 2.3 Thermal Conductivity Testing The thermal conductivity test of the nanofluid will be taken at three different temperatures which are at 6°C, 25°C and 40°C. To obtain such temperature of the nanofluid, those three samples will be immersed in the water bath so that the temperature of the samples will maintain at desired temperature.
Table 2 Thermal conductivity for CNT CNT Thermal Conductivity (W/m.K) at temperature (°C) 6 25 40 CNT1 0.553 0.592 0.598 CNT2 0.572 0.594 0.676 CNT3 0.584 0.628 0.693
IMRAN SYAKIR RESULTS AND DISCUSSION
3.
The morphology of three different types of carbon nanotubes is shown in Figure 1. The nanotubes morphology are randomly entangled and highly interconnected, probably due to the van der Waal’s. (a)
(b)
(c)
Table 2 shows the thermal conductivity analysis for the all CNT. CNT3 shows the higher thermal conductivity compared to others due to the decrement of diameter size in carbon nanofiber. The smallest diameter generates the best enhancement in thermal conductivity which contribute to the higher surface area. 4.
Figure 1 SEM images of a) CNT1, b) CNT2, c) CNT3 The surface areas contribute to the enhancement of physical and chemical properties of nanofluids. The properties that found to influence surface area were number of walls or diameter, impurities, and surface functionalization with hydroxyl and carboxyl groups. All images shown in Figure 1 illustrated agglomerate carbon nanotube and nanofibers, primarily with non-uniform tubular structure. The increase in diameter size will reduce the surface area. Higher surface areas are expected to provide a better media for thermal transport in nanofluid. Figure 2 shows the FTIR spectra of the CNTs. On the horizontal axis is the infrared wavelengths expressed in term of a unit called wavenumber (cm-1) which represent the number of waves fit into one centimeter. The peaks in the COOH spectrum represent the functional groups that are present in the molecule.
CONCLUSIONS
In conclusion, the study of surface area of the selected CNT nanocarbon shows that the decrement in diameter size will attributed to the highest surface area and possess a good thermal conductivity. The experimental studies shows that CNT3 (HHT24) generates the best enhancement in thermal conductivity. High surface area of the CNT3 (HHT24) offers a better media for thermal transport in nanofluids. 5.
REFERENCES
[1]
Weitz, D. A., Huang, J. S., Lin, M. Y., and Sung, J., “Dynamics of Diffusion-Limited Kinetic Aggregation,” Phys. Rev. Lett., vol. 53, pp. 1657– 1660, 1985. Meakin, P., “Aggregation Kinetics,” Phys. Scr., vol. 46, pp. 295–331, 1992. J. Eapen, R. Rusconi, R. Piazza and S. Yip, “The Classical Nature of Thermal Conduction in Nanofluids”, Journal of Heat Transfer, vol. 132, no. 10, pp. 1-14, 2010.
[2] [3]
Mechanical Engineering Research Day 2015 31 March 2015 - Melaka, Malaysia, pp. 1-2 © Centre for Advanced research on Energy
[4]
[5]
Iijima.S. (2007). “Nano-carbon materials: Their Fundamentals and Various Applications including Nano-Biotechnology”. University of Wien. Lin, T., Bajpai, V., Ji, T. and Dai, L., “Chemistry of Carbon Nanotubes”. Australian Journal of Chemistry, vol. 56, no. 7, pp. 635-651, 2003.
IMRAN SYAKIR
