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Potassium-promoted molybdenum catalysis higher alcohols from synthesis gas over MoC, Mo₂C and MoO₂ /Wright, James H. January 2006 (has links)
Thesis (M.S.)--West Virginia University, 2006. / Title from document title page. Document formatted into pages; contains xiii, 172 p. : ill. (some col.). Includes abstract. Includes bibliographical references (p. 123-125).
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Carbon Nanotube Synthesis for Microsystems ApplicationsSunden, Erik Oscar 23 June 2006 (has links)
Modern day engineering systems research presently lacks techniques to exploit the unique properties of many nanomaterials; coupled with this challenge exists the need to interface these nanomaterials with microscale and macroscale platforms. A nanomaterial of particular interest is the carbon nanotube (CNT), due to its enhanced physical properties. In addition to varied electrical properties, the CNT has demonstrated high thermal conductivity and tensile strength compared to conventional fiber materials. CNTs are beginning to see commercial applications in areas in which sufficient study has been dedicated. While a large part of the worldwide focus of CNT research has been in synthesis, an equally important area of research lies in CNT integration processes. The unique and useful properties of many nanostructured materials will never be realized in mainstream manufacturing processes and commercial applications without the proper exploration of integration methods such as those detailed in this thesis.
The primary motivation for the research detailed in this thesis has been to develop CNT synthesis processing techniques that allow for novel interfacing methods between carbon nanotubes and eventual applications. In this study, an investigation was performed to look at several approaches to integrating CNTs into micro-electromechanical systems (MEMS). Synthesis of CNTs was studied in two different settings. Synthesis was first performed, directly on the microsystem, via a global scale chemical vapor deposition (CVD) process. Secondly, synthesis was performed directly onto a microsystem device via localized resistive heating. Following synthesis, the application of atomically layered, protective coatings was then investigated. Integration methods were then investigated to allow for CNT transfer to microsystem applications incapable of withstanding synthesis temperatures. The developed integration methods were evaluated by creating functional microscale electrical circuits in flexible substrates via hot emboss imprint lithography. Lastly, post synthesis processing methods were used to create micropatterned cell guidance substrates as well as neuronal stimulating substrates.
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Formation and growth mechanisms of single-walled metal oxide nanotubesYucelen, Gulfem Ipek 04 June 2012 (has links)
Single-walled metal oxide nanotubes have emerged as an important class of 'building block' materials for molecular recognition-based applications in catalysis, separations, sensing, and molecular encapsulation due to their vast range of potentially accessible compositions and structures, and their unique properties such as well-defined wall structure and porosity, tunable dimensions, and chemically modifiable interior and exterior surfaces. However, their widespread application will depend on the development of synthesis processes that can yield structurally and compositionally well-controlled nanotubes. Moreover, such processes should be amenable to scale-up and preferably operate via benign chemistries under mild conditions. There is currently very little knowledge on the molecular-level 'design rules' underlying the engineering of such materials.
The capability to engineer single-walled tubular materials would lead to a range of structures, with novel properties relevant to diverse applications. In this thesis, main objectives are to discover the first molecular-level mechanistic framework governing the formation and growth of single-walled metal-oxide nanotubes, apply this framework to demonstrate the engineering of nanotubular materials of controlled dimensions, and to progress towards a quantitative multiscale understanding of nanotube formation. The class of aluminosilicate (AlSiOH)/germanate (AlGeOH) nanotubes are of particular interest to us, and serve as the exemplar materials for single-walled metal oxide nanotubes. They can be synthesized in pure form from inexpensive and easily accessible reactants at low temperatures (95 ˚C) from aqueous solutions. The synthesis of nanotubes occurs on a time-scale of hours to days, making them an ideal model system to study the nanotube formation mechanism.
In Chapter 2, the identification and elucidation of the mechanistic role of molecular precursors and nanoscale (1-3 nm) intermediates with intrinsic curvature, in the formation of single-walled aluminosilicate nanotubes is reported. The structural and compositional evolution of molecular and nanoscale species over a length scale of 0.1-100 nm, are characterized by electrospray ionization (ESI) mass spectrometry, and nuclear magnetic resonance (NMR) spectroscopy. DFT calculations revealed the intrinsic curvature of nanoscale intermediates with bonding environments similar to the structure of the final nanotube product. It is shown that curved nano-intermediates form in aqueous synthesis solutions immediately after initial hydrolysis of reactants at 25 ˚C, disappear from the solution upon heating to 95 ˚C due to condensation, and finally rearrange to form ordered single-walled aluminosilicate nanotubes. Integration of all results leads to the construction of the first molecular-level mechanism of single-walled metal oxide nanotube formation, incorporating the role of monomeric and polymeric aluminosilicate species as well as larger nanoparticles.
Then, in Chapter 3, new molecular-level concepts for constructing nanoscopic metal oxide objects are demonstrated. The diameters of metal oxide nanotubes are shaped with Ångstrom-level precision by controlling the shape of nanometer-scale precursors. The subtle relationships between precursor shape and structure and final nanotube curvature are measured (at the molecular level). Anionic ligands (both organic and inorganic) are used to exert fine control over precursor shapes, allowing assembly into nanotubes whose diameters relate directly to the curvatures of shaped precursors.
Having obtained considerable insight into aluminosilicate nanotube formation, in Chapter 4 the complex aqueous chemistry of nanotube-forming aluminogermanate solutions are examined. The aluminogermanate system is particularly interesting since it forms ultra-short nanotubes of lengths as small as ~20 nm. Insights into the underlying important mechanistic differences between aluminogermanate and aluminosilicate nanotube growth as well as structural differences in the final nanotube dimensions are provided. Furthermore, an experimental example of control over nanotube length is shown, using the understanding of the mechanistic differences, along with further suggestions for possible ways of controlling nanotube lengths.
Ultimately, it is desired to produce the single-walled aluminosilicate nanotubes on a larger scale (e.g., kilogram or ton scales) for technological application. However, a quantitative multiscale understanding of nanotube growth via a detailed growth model, is critical to be able to predict and control key properties such as the length distribution and concentration of the nanotubes. Such a model can then be used to design liquid-phase reactors for scale-up of nanotube synthesis. In Chapter 5, a generalized kinetic model is formulated to describe the reactions leading to formation and growth of single-walled metal oxide nanotubes. This model is capable of explaining and predicting the evolution of nanotube populations as a function of kinetic parameters. It also allows considerable insight into meso/microscale nanotube growth processes. For example, it shows that two different mechanisms operate during nanotube growth: (1) growth by precursor addition, and (2) by oriented attachment of nanotubes to each other.
In Chapter 6, a study of the structure of the nanotube walls is presented. It has usually been assumed in the literature that the nanotube wall is free of defects. A combination of 1H-29Si and 1H-27Al FSLG-HETCOR, 1H CRAMPS, and 1H-29Si CP/MAS NMR experiments were employed to evaluate the proton environments around Al and Si atoms during nanotube synthesis and in the final structure. The HETCOR experiments allowed to track the evolving Si and Al environments during the formation of the nanotubes from precursor species, and relate them to the Si and Al coordination environments found in the final nanotube structure. The 1H CRAMPS spectra of dehydrated aluminosilicate nanotubes revealed the proton environments in great detail. Integration of all the NMR results allows the structural assignment of all the chemical shifts and the identification of various types of defect structures in the aluminosilicate nanotube wall. In particular, five main types of defect structures are identified arising from specific atomic vacancies in the nanotube structure. It is estimated that ~16% of Si atoms in the nanotube inner wall are involved in a defect structure. The characterization of the detailed structure of the nanotube wall is expected to have significant implications for its chemical properties and applications.
Chapter 7 contains concluding remarks, as well as suggestions for future directions in the engineering of single-walled nanotube materials.
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The effect of catalyst properties on the synthesis of carbon nanotubes by plasma enhanced chemical vapor depositionCheemalapati, Surya Venkata Sekhar 08 November 2012 (has links)
A study of the effect of catalyst properties on the synthesis of carbon nanotubes (CNTs) is done in this thesis. Three different metal alloy catalysts, Fe/Ti, Ni/Ti, Co/Ti, have been studied. Various atomic concentrations and thicknesses were cosputter deposited on clean Si wafers using AJA Orion 4 RF Magnetron sputter deposition tool at 5mtorr and 17��C, and the films were characterized using a scanning electron microscope, Energy-dispersive X-ray spectroscopy. All the alloys have been annealed at 650��C and 3 torr in an argon atmosphere at 100 SCCM, followed by ammonia gas plasma etch at different powers at 3 torr and 50 SCCM NH��� flow in a modified parallel plate RF chemical vapor deposition tool for 1 minute. The influence of plasma power, thickness of catalyst and concentration of Ti the secondary metal in the alloy composition, on the surface morphology of the catalyst are investigated by characterizing them with atomic force microscopy. The study has shown that the surface roughness is affected by Ti concentration, thickness and plasma power. The 35 W power NH��� plasma produced rougher surfaces when compared to the 75 W NH��� plasma. The result is interpreted as follows: ion bombardment leads to greater etching of the catalyst surface. Thus, plasma power must be optimized for catalyst thin film and etch time. The study has provided an in depth analysis and understanding of the various factors that influence catalyst surface morphology which can be applied into further study for optimizing parameters for synthesis of single walled CNTs.
Following this, a study on catalysts for CNT synthesis was performed using Plasma enhanced chemical vapor deposition and characterized by scanning electron microscope. CNTs were synthesized on Ni, Ni-Ti, Co, Co-Ti and Fe catalyst. Ni, Ni-Ti catalyst produced forest like vertically aligned CNTs whereas Co, Co-Ti produced vertically aligned free standing CNTs. The growth was dense and uniform across the substrate. Initial growth runs on Fe, Fe-Ti alloy did not produce any CNTs until catalyst was restructured with a thicker Ti under layer after an investigation using Secondary ion mass spectrometry of suspected Fe catalyst poisoning due to reaction with Si substrate. A room temperature run was carried out on annealed and plasma etched Ni catalyst and no CNTs were produced indicating the importance of substrate temperature of CNTs. A deeper understanding of factors of influence on CNTs such as catalyst types, structure/morphology, and substrate temperature has been achieved with this study. / Graduation date: 2013
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Synthesis, Characterization, and Growth Mechanism of Single-Walled Metal Oxide NanotubesMukherjee, Sanjoy 03 July 2007 (has links)
Nanotubes have numerous potential applications in areas such as biotechnology, electronics, photonics, catalysis and separations. There are several challenges to be overcome in order to realize their potential, such as: (1) Synthesis of monodisperse (in diameter and in length) single-walled nanotubes; (2) Quantitative understanding of the mechanism of formation and growth of nanotubes; (3) Capability to engineer the nanotube size; (4) Low temperature synthesis process; and (5) Synthesis of impurity free nanotubes. Our investigation focuses on a class of metal oxide (aluminosilicate/germanate) nanotubes, which are; single walled nanotubes with monodisperse inner and outer diameters, can be synthesized in the laboratory by a low temperature (95ºC) process in mildly acidic aqueous solutions, and their formation timescales is hours, which makes it convenient as a model system to study the mechanisms of nanotube formation.
This work is focused on obtaining a qualitative and quantitative understanding of the mechanism of formation of aluminosilicate and aluminogermanate nanotubes. In order to achieve this overall objective, this thesis consists of the following aspects: (1) A systematic phenomenological study of the growth and structural properties of aluminosilicate and aluminogermanate nanotubes. The constant size and increasing nanotube concentration over the synthesis time strongly suggest that these nanotubular are assembled through self-assembly process. (II) Investigation of the mechanism of formation of single-walled aluminogermanate nanotubes provided the central phenomena underlying the formation of these nanostructures: (1) the generation (via pH control) of a precursor solution containing chemically bonded precursors, (2) the formation of amorphous nanoscale (~ 6 nm) condensates via temperature control, and (3) the self-assembly of short nanotubes from the amorphous nanoscale condensates. (III) Synthesis of mixed metal oxide (aluminosilicogermanate) nanotubes with precise control of elemental composition, diameter and length of the product nanotubes. (IV) Preliminary work towards generalization of the kinetic model developed for aluminogermanate nanotubes to a larger class of metal oxide nanotubes. It was found that the size of nanotubes is dependent on the amount of precursors that can be packed in a single ANP and in turn depends on the size of the ANP.
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From Synthesis To Applications Of Pristine And Nitrogen-Doped Carbon NanotubesGoswami, Gopal Krishna 07 1900 (has links) (PDF)
Carbon nanotubes (CNTs) are well known as excellent electrical conductors. However, their transport properties are limited by electrical breakdown in ambient. Moreover, the electronic properties can further be modulated by doping. Devices such as Schottky diodes, transistors and logic gates based on un-doped and doped CNT junctions have been realized. Recently, nitrogen doped CNTs show potential application in replacing platinum cathode catalyst in fuel cell technology.
We synthesize pristine, nitrogen-doped and nitrogen-doped:pristine CNT intratubular junctions by one-step co-pyrolysis and explore them for different applications. We show that the position of electrical breakdown can be predicted which is essential to know for high current applications. Among other applications, we show that individual CNT intratubular junction exhibits rectifying characteristics. Further investigation indicates the intratubular junction behaves like Schottky diode. Lastly, the potential replacement of platinum by nitrogen doped CNTs in direct methanol fuel cell has been explored.
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Synthesis, Characterization and Electrical Transport In Carbon NanotubesMahanandia, Pitamber 01 1900 (has links) (PDF)
In this thesis, synthesis, characterization and electrical transport of Carbon nanotubes (CNTs) have been discussed. The first chapter contains a brief introduction of various forms of carbon including CNT. The CNTs are currently the materials of intense research interest due to their remarkable mechanical and electrical properties. CNTs can be visualized as a graphene sheet that has been rolled into a seamless tube. CNTs are either single-walled carbon nanotubes (SWCNT) or multi-walled carbon nanotubes (MWCNT). SWCNT is a tube with only one wall and MWCNT has many coaxial tubes and weak Van der Waal forces hold them together. The properties depend on chirality, diameter and length of the tubes. Chirality is defined by the symmetry and the chiral angle formed between the carbon bonds. The atomic structure of CNTs is described in terms of the tube chirality, which is defined by the chiral vector Ch and the chiral angle . The chiral vector is Ch = na1 + ma2, where the integers (n, m) are the number of steps along the zig-zag carbon. Depending on the tube chirality the electrical properties of the CNTs differ; they can be metallic or semiconducting. When n-m = 3p, where p is an integer, the CNTs are metallic and when n-m 3p, the CNTs are semiconducting. Due to the high anisotropy and high aspect ratio, CNTs have many potential applications with great technological importance such as functionalized molecules, conductive wires, bearings of rotational motors, field emitters, hydrogen storage, sensors, polymer composites, nanotube yarn and nanotube filters, X-ray generator, electron sources for microscopy and lithography, gas discharge tubes and vacuum microwave amplifiers, etc.
The first chapter gives a brief introduction about various forms of carbon and their properties, particularly of CNTs. The nature of the CNTs depends on the method of production, which controls the degree of graphitization, the tube diameter and the chirality. Most synthesis methods originate from the idea of obtaining adequately active carbon atomic species or clusters from carbon sources and assembling them into CNTs without or with catalysts. The commonly used methods for the synthesis of carbon nanotubes are arc-discharge, Laser ablation, high-pressure catalytic decomposition of carbon monoxide (HiPCO), electrophoretic deposition (EPD), flame synthesis, pyrolysis, chemical vapour deposition (CVD), hot-filament CVD, plasma enhanced chemical vapour deposition (PECVD) using DC, RF, and micro wave power sources, hot-filament dc (HF-dc PECVD), inductively coupled plasma (ICPECVD) and electron cyclotron resonance (ECR PECVD). Although many efforts have been made to develop various synthesis methods, most of them require many steps. Moreover, the complicated and rigorous control of parameters and expensive materials are unavoidable that has put limitation in reproducing the same in large scale. In this chapter, a simple method for the synthesis of CNTs on a large scale that eliminates nearly the entire complex and expensive machinery associated with widely used growth techniques has been discussed.
In Chapter 2, the synthesis and characterization of entangled CNTs are discussed. It is shown that entangled CNTs can be synthesized in one step by using double stage furnace. Tetrahydrofuran as carbon source material and nickelocene as catalyst source material have been used to synthesize CNTs. With this method CNTs can be synthesized at a temperature as low as at 600 0C. In this technique the self-developed pressure carries the vapours to the hot zone of the furnace. This has led to think in modifying the double stage furnace. A single stage furnace having temperature gradient is made to synthesize CNTs. The vapours are carried from low temperature zone to hot zone where the carbon species and catalysts react to form CNTs. The advantage of this furnace is that it is one-step process. Using another carbon source material such as Diethyl Ether and nickelocene as catalyst source material CNTs are synthesized. The as synthesized and purified CNTs are characterized by X-ray diffraction (XRD), Scanning electron microscope (SEM), transmission electron microscope (TEM), high resolution TEM (HRTEM) and Raman spectroscopy. The CNTs are multi-walled in nature as observed by HRTEM.
In Chapter 3, the synthesis of aligned CNTs is discussed by using benzene as carbon source and ferrocene as catalyst source materials. Aligned MWCNTs were synthesized in the temperature range between 650 - 1100 0C in a single stage furnace without the need for carrier gas nor predeposited metal catalyst substrate. The essential need of CNTs are (1) to obtain aligned nanotubes with millimeter lengths to enable the formation of novel nanotube-polymer composites that incorporate continuous nanotubes throughout their thickness for highly anisotropic thermal and electrical conductivities; and (2) to provide samples for detailed physical characterization - tensile strength, thermal, electrical conductivity, field emission etc. SEM observation reveals the increase in length of nanotubes from 85 m to 1.4 mm with the increase of preparation temperature. The diameter as investigated by high-resolution transmission electron microscopy (HRTEM) remains almost constant 70-80 nm (75-85 layers). Once nanotube formation is established, the growth continues in the same direction and may well be reinforced by the presence of surrounding CNTs i.e. almost every particle produces a nanotube and bundling of neighboring tubes lead to collective vertical growth. The increase in length is due to the enhanced diffusion of active carbon with increasing preparation temperatures. The alignment of CNTs is also observed to the lateral side of the substrate.
In Chapter 4, the synthesis and characterization of carbon nanoribbon and singled crystal iron filled CNTs is discussed. Particularly interesting are those CNTs filled with magnetic nanowires, which can provide an effective barrier against oxidation and consequently ensure a long-term stability in the core. The filling of metals within carbon nanotubes has extended the potential application base of these materials to quantum memory elements, high density magnetic storage media, semiconducting devices, field electron emitters, high resolution magnetic atomic force microscopy tips, magnetic field sensors and scanning probe microscopes etc. Tetrahydrofuran as carbon source material and ferrocene as catalyst materials has been used to synthesize mixture of carbon nanoribbons and iron filled CNTs. The techniques used to characterize the materials are XRD, SEM, HRTEM and superconducting quantum interference device (SQUID). The powder XRD pattern shows that the bcc -Fe phase of iron is present. HRTEM studies reveal the presence of multi-walled carbon nanotubes and well-crystallized -Fe phase filled inside the core region. Closer inspection of the HRTEM images indicated that the bcc structure -Fe nanowires are monocrystalline and Fe (110) plane is indeed perpendicular to the G (002) plane. Large coercivity (i.e. 1037 Oe at 300 K and 2023 Oe at 10 K) in the iron filled CNTs and carbon nanoribbons have been observed. The high coercivity is mainly attributed to the following two factors. Firstly, it is known that due to the uniaxial magnetic anisotropy of the nano size iron in the core region of the carbon nanotubes. Secondly, ferromagnetic behavior exhibited by the localized states at the edges of the carbon nanoribbons.
The anisotropic electrical transport property of MWCNTs has been discussed in the chapter 5. The activated diffusive nature of transport along axial direction of CNT is explained. The transport perpendicular to the tube direction is explained in terms of a hopping mechanism. The anisotropic resistivity (N/P) value obtained is 3. The temperature dependent magnetoresistance (MR) is studied in magnetic fields up to 11 Tesla at low temperatures both in the parallel and perpendicular direction of an aligned MWCNT mat. In both cases a negative MR is observed.
Chapter 6 discusses the preparation of CNT-polymer composites. The temperature dependence of the conductivity and magnetoresistance (MR) has been studied making four-point contact method on the carbon nanotubes polymer composites as result of increasing CNT content. The conductivity increases with increasing carbon nanotube weight percentage. The increase in conductivity as a function of the CNT weight percent is attributed to the introduction of conducting CNT paths in the polymer matrix. With the increasing CNT content the number of interconnections present in a random system is found to vary. Electrical conduction in nanotube mat or nanotube composites is explained by a variable range hopping (VRH) conduction mechanism. The negative magnetoresistance has been observed for the polymer composites. It is consistent with the report on CNTs bundles and polymer composites.
Finally a brief summary of the work presented in this dissertation is discussed along with future directions in this research.
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Carbon Nanotubes: Chemical Vapor Deposition Synthesis and Application in Electrochemical Double Layer SupercapacitorsTurano, Stephan Parker 08 March 2005 (has links)
Carbon nanotubes (CNTs) have become a popular area of materials science research due to their outstanding material properties coupled with their small size. CNTs are expected to be included in a wide variety of applications and devices in the near future. Among these devices which are nearing mass production are electrochemical double layer (ECDL) supercapacitors. The current methods to produce CNTs are numerous, with each synthesis variable resulting in changes in the physical properties of the CNT.
A wide array of studies have focused on the effects of specific synthesis conditions. This research expands on earlier work done using bulk nickel catalyst, alumina supported iron catalyst, and standard chemical vapor deposition (CVD) synthesis methods. This work also investigates the effect of an applied voltage to the CVD chamber during synthesis on the physical nature of the CNTs produced. In addition, the work analyzes a novel nickel catalyst system, and the CNTs produced using this catalyst. The results of the effects of synthesis conditions on resultant CNTs are included. Additionally, CNT based ECDL supercapacitors were manufactured and tested.
Scanning electron microscope (SEM) analysis reveals that catalyst choice, catalyst thickness, synthesis temperature, and applied voltage have different results on CNT dimensions. Nanotube diameter distribution and average diameter data demonstrate the effect of each synthesis condition. Additionally, the concept of an alignment parameter is introduced in order to quantify the effect of an electric field on CNT alignment. CNT based ECDL supercapacitors testing reveals that CNTs work well as an active material when a higher purity is achieved. The molarity of the electrolyte also has an effect on the performance of CNT based ECDL supercapacitors.
On the basis of this research, we conclude that CNT physical dimensions can be moderately controlled based on the choice of synthesis conditions. Also, the novel nickel catalyst system investigated in this research has potential to produce bulk quantities of CNT under specific conditions. Finally, purified CNTs are recommended as a suitable active material for ECDL supercapacitors.
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Low Temperature Charge Transport And Magnetic Properties Of MWNTs/MWNT-Polystyrene CompositesBhatia, Ravi 12 1900 (has links) (PDF)
Carbon nanotubes (CNTs) have been recognized as potential candidates for mainstream device fabrication and technologies. CNTs have become a topic of interest worldwide due to their unique mechanical and electrical properties. In addition, CNTs possess high aspect ratio and low density that make them an important material for various technological applications. The field of carbon nanotube devices is rapidly evolving and attempts have been made to use CNTs in the fabrication of devices like field emitters, gas sensors, flow meters, batteries, CNT-field effect transistors etc. These molecular nanostructures are proposed to be an efficient hydrogen storage material. CNT cylindrical membranes are reported to be used as filters for the elimination of multiple components of heavy hydrocarbons from petroleum and for the filtration of bacterial contaminants of size less than 25 nm from water. Recently, CNT bundles have been proposed to be a good material for low-temperature sensing.
CNTs have also been considered as promising filler materials due to extraordinary characteristics mentioned above. Fabrication of nanocomposites using CNTs as reinforcing material has completely renewed the research interest in polymer composites. The conductive and absorptive properties of insulating polymer doped with conducting filler are sensitive to the exposure to gas vapors and hence they can be used in monitoring various gases. The application of fiibre reinforced polymer composites in aeronautic industry are well known due to their high mechanical strength and light weight. Also, the conductive composite materials can be used for electromagnetic shielding. Desired properties in CNT-composites can be attained by adding small amount of CNTs in comparison to traditional filler materials. Due to high aspect ratio and low density of CNTs, percolation threshold in CNT-polymer composites can be achieved at 0.1 vol % as compared to ~16 vol. % in case of carbon particles. The research work 0.1 vol. %, as compared to reported in this thesis includes the preparation of multiwall carbon nanotube (MWNTs) and MWNT-polystyrene composites, experimental investigations on low temperature charge transport, and magnetic properties in these systems.
This thesis contains 7 chapters.
Chapter 1 provides an overview of CNTs and CNT-polymer composites. This chapter briefly describes the methods for synthesizing CNTs and fabricating CNT-polymer composites, charge transport mechanisms in CNTs and composites, and their magnetic properties as well.
Chapter 2 deals with the concise introduction of various structural characterization tools and experimental techniques employed in the present work. An adequate knowledge of the strengths and limitations of experimental equipment can help in gathering necessary information about the sample, which helps in studying and interpreting its physical properties correctly.
Chapter 3 describes the synthesis of MWNTs and their use as filler material for the fabrication of composites with polystyrene (PS). The characterization results of as-prepared MWNT and composites show that MWNTs possess high aspect ratio (~4000), and are well dispersed in the composite samples (thickness ~50-70 µm). The composite samples are prepared by varying the MWNT concentration from 0.1 to 15 wt %. The as¬fabricated composites are electrically conductive and expected to display novel magnetic properties since MWNTs are embedded with iron (Fe) nanoparticles.
Chapter 4 presents the study of charge transport properties of aligned and random MWNTs in the temperature range 300-1.4 K. The low temperature electrical conductivity follows the weak localization (WL) and electron-electron (e-e) interaction model in both samples. The dominance of WL and e-e interaction is further verified by magneto-conductance (MC) measurements in the perpendicular magnetic field up to 11 T at low temperatures. The MC data of these samples consists of both positive and negative contributions, which originates from WL (at lower fields and higher temperatures) and e-e interaction (at higher fields and lower temperatures).
Chapter 5 contains the results of charge transport studies in MWNT-PS composite near the percolation threshold (~0.4 wt %) at low temperatures down to 1.4 K. Metallic-like transport behavior is observed in composite sample of 0.4 wt %, which is quite unusual. In general, the usual activated transport is observed for systems near the percolation threshold. The unusual weak temperature dependence of conductivity in MWNT-PS sample at percolation threshold is further verified from the negligible frequency dependence of conductivity, in the temperature range from 300 to 5 K.
Chapter 6 accounts on the experimental results of magnetization studies of MWNTs and MWNT-PS composites. The observation of maxima in coercivity and squareness ratio at 1 wt % of Fe-MWNT in a polymer matrix show the dominance of dipolar interactions among the encapsulated Fe-nanorods within MWNTs. The hysteresis loop of 0.1 wt % sample shows anomalous narrowing at low temperatures, which is due to significant contribution from shape anisotropy of Fe-nanorods.
Chapter 7 presents brief summary and future perspectives of the research work reported in the thesis.
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