1,223 research outputs found

    Production of carbon nanotubes by PECVD and their applications to supercapacitors

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    Màster en Nanociència i NanotecnologiaPlasma enhanced chemical vapor deposition (PECVD) is a versatile technique to obtain vertically dense-aligned carbon nanotubes (CNTs) at lower temperatures than chemical vapor deposition (CVD). In this work, we used magnetron sputtering to deposit iron layer as a catalyst on silicon wafers. After that, radio frequency (rf) assisted PECVD reactor was used to grow CNTs. They were treated with water plasma and finally covered by MnO2 as dielectric layer in order to use CNTs as electrode for supercapacitors. Optimization of annealing time, reaction time and temperature, water plasma time and MnO2 deposition time were performed to find appropriate conditions to improve the characteristics of supercapacitors. SEM (Scanning Electron Microscopy), TEM (Transmission Electron Microscopy), AFM (Atomic Force Microscopy) and Raman spectroscopy were used to characterize obtained electrodes

    Dynamics and Limiting Mechanisms of Self-Aligned Carbon Nanotube Growth.

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    Carbon nanotubes (CNTs) are long, cylindrical molecules, which boast exceptional tensile strength and large thermal and electrical conductivities. Vertically aligned CNT “forests” have promising potential uses, including dry adhesives, electrical interconnects, light emitters, thermal interface materials, gas and liquid filters, composite reinforcements, and photonic crystals. Manufacturing indefinitely long CNTs may realize dreams of CNT-based cables and wires having stiffness, strength, and transport properties exceeding today’s best metal alloys and advanced fibers. However, the functional properties of CNT forests have so far fallen short of those of individual CNTs due to low packing fraction, polydisperse diameters, and relatively short lengths. Toward the eventual goal of bridging this structure-property relationship, my dissertation presents a novel set of in situ and ex situ characterization tools for CNT forest growth by chemical vapor deposition (CVD), as well as the use of these tools to investigate the limiting mechanisms thereof. In situ X-ray scattering reveals the dynamics of catalyst thin film dewetting into nanoparticle growth sites, the initial self-organization of the CNT forest, and the abrupt self-termination of growth. Quantification of catalyst and CNT sizes show that they are inevitably polydisperse, regardless of synthesis conditions. To overcome this, a novel method is introduced for templated dewetting of the catalyst film toward the formation of ordered, monodisperse particles using nanoporous anodic alumina. Further, a map of thermal conditions is explored by independently tuning the temperatures of the catalyst and gaseous precursors, thereby establishing a set of rules for engineering crucial characteristics of forest growth, including CNT diameter, structural quality, vertical alignment, as well as rate and lifetime of the reaction. Finally, aligned CNT ensembles are used as templates to direct the self-assembly of fullerene C60, creating hybrid films with high photoconductive gain, thereby demonstrating an immediate application of this exciting material. These studies represent many new insights into the so-called “birth, life, and death” of CNT growth, and they have important implications for future work in synthesis of advanced carbon materials, including CNTs, fullerenes, and graphene. Meanwhile, these results have immediate applicability to efficient CNT manufacturing, improved characterization, and new hybrid materials for energy conversion.Ph.D.Mechanical EngineeringUniversity of Michigan, Horace H. Rackham School of Graduate Studieshttp://deepblue.lib.umich.edu/bitstream/2027.42/91427/1/emeshot_1.pd

    Biomimetic route to hybrid nano-Composite scaffold for tissue engineering

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    Hydroxyapatite-poly(vinyl) alcohol-protein composites have been prepared by a biomimetic route at ambient conditions, aged for a fortnight at 30±2°C and given a shape in the form of blocks by thermal cycling. The structural characterizations reveal a good control over the morphology mainly the size and shape of the particles. Initial mechanical studies are very encouraging. Three biocompatibility tests, i.e., hemocompatibility, cell adhesion, and toxicity have been done from Shree Chitra Tirunal, Trivandrum and the results qualify their standards. Samples are being sent for more biocompatibility tests. Optimization of the blocks in terms of hydroxyapatite and polymer composition w.r.t the applications and its affect on the mechanical strength have been initiated. Rapid prototyping and a β-tricalcium – hydroxyapatite combination in composites are in the offing

    Design of carbon nanotube-based sensors for the detection of catalytic activity

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    Thèse réalisée en cotutelle avec l'Université catholique de Louvain, BelgiqueLes nanotubes de carbone possèdent des propriétés uniques qui en font des matériaux prometteurs dans de nombreux domaines. En particulier, leur structure quasi-unidimensionnelle et leur rapport surface/volume élevé font de ces matériaux des candidats de choix pour leur utilisation comme senseurs. A ce jour, les études concernant l'utilisation des nanotubes de carbone pour la conception de senseurs se concentrent principalement sur la détection de gaz, de molécules biologiques ou chimiques. Dans le cadre de cette thèse, nous nous intéressons à l'utilisation des nanotubes de carbone comme senseurs pour détecter en temps réel une transformation chimique, au travers d'une réaction catalytique. Pour ce faire, des catalyseurs supportés sur nanotubes de carbone sont préparés grâce à des méthodes de fonctionnalisation appropriées de ces matériaux. En pratique, nous développons dans ce travail deux approches distinctes pour la préparation de catalyseurs supportés sur nanotubes de carbone. D'une part, nous mettons au point une méthode de fonctionnalisation monovalente des nanotubes de carbone, permettant de déposer des nanoparticules métalliques à la surface des nanotubes en vue de la préparation de catalyseurs hétérogènes supportés. A cette fin, les nanotubes sont dans un premier temps fonctionnalisés par des sels de diazonium. Cette première étape permet d'établir un point d'accroche sur les nanotubes permettant une post-fonctionnalisation ultérieure, en vue de l'ancrage de clusters métalliques. Une étape d'activation thermique permet ensuite de former des nanoparticules métalliques, au départ de ces précurseurs moléculaires. D'autre part, un catalyseur homogène supporté est préparé via l'ancrage de complexes à base de Pd(0) sur des nanotubes de carbone fonctionnalisés de manière à présenter des liaisons triples. Pour ce faire, les nanotubes de carbone sont fonctionnalisés de façon divalente, par la réaction de Bingel-Hirsch. Cette approche divalente assure l'ancrage covalent des sites actifs, tout en préservant la conductivité électrique des nanotubes de carbone. Quelle que soit l'approche envisagée, la préparation de ces catalyseurs est attentivement suivie par des méthodes classiques de caractérisation telles que la spectroscopie Raman, la spectroscopie des photoélectrons X et l'analyse thermogravimétrique. En outre, une caractérisation électrique est également effectuée à chaque étape de la préparation des catalyseurs, afin d'étudier l'influence des différentes étapes de fonctionnalisation sur les propriétés électriques du nanotube. Ces matériaux sont ensuite testés en catalyse, pour la transformation hydrolytique du diméthylphénylsilane en diméthylphénylsilanol ou pour la réaction de couplage croisée de Suzuki-Miyaura, respectivement pour les catalyseurs hétérogènes et homogènes supportés. L'activité de ces catalyseurs, ainsi que leur recyclabilité, est étudiée grâce à un suivi réactionnel par chromatographie gazeuse. Enfin, nous démontrons dans cette thèse la possibilité d'utiliser les nanotubes de carbone comme senseurs pour détecter in situ l'activité catalytique. A cette fin, des mesures électriques en temps réel sont enregistrées au cours de la réaction de catalyse. L'activité catalytique se traduit par des changements de la conductivité des nanotubes au cours du temps.Due to their outstanding properties, carbon nanotubes are being considered as promising materials in various fields. Namely, their quasi-one-dimensionality and their high surface/volume ratio make them ideal candidates for sensing applications. To date, studies dealing with the use of carbon nanotubes in sensing mainly focus on gas, biological and chemical molecules detection. In this thesis, we aim to use carbon nanotubes as sensors for the real-time detection of a chemical transformation through a catalytic reaction. In order to do this, carbon nanotube supported catalysts are prepared thanks to appropriate functionalization methods. In practice, we develop in this work two distinct approaches for the preparation of carbon nanotube supported catalysts. On one hand, we develop a monovalent functionalization pathway for the deposition of metallic nanoparticles on carbon nanotube surface. For this purpose, carbon nanotubes are first functionalized by diazonium salts. This first step allows to bind a tethering point for a subsequent post-functionalization. Metallic clusters are then coordinated on these functionalized moieties. A thermal activation step ensures the formation of metallic nanoparticles from these nanoparticle molecular precursors. On the second hand, a homogeneous supported catalyst is prepared by anchoring Pd(0) complexes on carbon nanotube surface. In order to do this, carbon nanotubes are divalently functionalized by Bingel-Hirsch reaction to present dangling triple bonds at their surfaces. This divalent approach ensures a covalent anchoring of the active sites on the nanotube surface, while preserving their electrical conductivity. Whichever the considered approach, the catalyst preparation is carefully analyzed by common characterization techniques, such as Raman spectroscopy, X-ray photoelectron spectroscopy and thermogravimetric analysis. Moreover, the materials are also electrically characterized at each step of the catalyst preparation process. This electrical characterization allows to study the influence of the different steps of the functionalization strategy on the nanotube electrical properties. These materials are then tested in catalysis, for the hydrolytic transformation of dimethylphenylsilane in dimethylphenylsilanol or for the Suzuki-Miyaura cross-coupling reaction, respectively for heterogeneous and homogeneous supported catalysts. The activity and recyclability of these catalysts is monitored by gas chromatography. Finally, we demonstrate in this thesis the possibility of using carbon nanotubes as sensors for the in situ detection of catalytic activity. For this purpose, real-time electrical measurements are recorded during the catalytic reaction. The catalytic activity is revealed by fluctuations of the nanotube conductivity over time

    Effect of Annealing on Metal-Oxide Nanocluster

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    Recently, the development of optoelectronic devices based on metal-oxide nanocluster has attracted intensive research interest. Nanoclusters are suitable for these because of their large surface-to-volume ratio and the presence of abundant oxygen vacancies or trap states. Metal–oxides such as ZnO, In2O3, and TiO2 synthesized using different technique produces high surface area films consisting of clusters and provides complete control over the film morphology. In this chapter, some of the metal oxides nanocluster film has investigated, and the effect of annealing on the structural, optical and electrical properties of the grown films when subjected to different annealing temperatures will be studied. Theoretically, these properties are presumed to improve after the heat treatment as the crystallinity, and the grain size of the film has increased due to the diminishing of oxygen vacancies. Thus, the greater surface-to-volume ratio, the better stoichiometry and higher level of crystallinity compared to bulk materials make nanocluster-based devices very promising for the mentioned application

    Optical, Mechanical, and Electrical Properties of Polymer Composites Doped by Multiwalled Carbon Nanotubes

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    Three-dimensional networks can be hydrophilic and/or hygroscopic. Optical, mechanical, and electrical properties of these materials encompass many fields of technology. Composites of carbon nanotubes (CNTs) in polymeric materials have attracted considerable attention in the research and industrial communities due to their unique optical, mechanical, and electrical properties. CNT polymer nanocomposites possess high stiffness, high strength, and good electrical conductivity at relatively low concentrations of CNT filler. Here, in this chapter, we survey the optical, mechanical, and electrical mechanisms for various polymeric systems. Composite gels and films were prepared with various molar percentages of multiwalled carbon nanotubes (MWCNTs). The optical, mechanical, and electrical behaviors of various composite gels doped by MWCNT are also discussed in the each sections of the chapter. The optical behaviors of the composites were performed by the UV-Vis spectroscopy and fluorescence spectroscopy in the first part of the chapter. On the other hand, compressive testing technique and rheological measurements were employed to determine the variations of mechanical properties of the composites in the second part of the chapter. Lastly, we review the electrical properties of the composites improved significantly by addition of MWCNTs researches

    DEVELOPMENT OF ADSORBENTS FOR THE CAPTURE AND STORAGE OF HYDROGEN AND CARBON DIOXIDE BY MAGNETRON SPUTTERING

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    Concerns about climate change have rejuvenated global efforts in reducing carbon dioxide (CO2) emissions. Tactics include capture and sequestration of CO2 from point sources and the promotion of hydrogen (H2) as a “transport fuel”. Current H2 vehicles use high pressure H2 tanks which lack the convenience of their fossil fuel counterparts and present potential safety hazards. Development of adsorbent materials that reduce the energetic costs of H2 and CO2 capture, facilitating reversible storage under safer conditions, are hoped to increase the viability of these technologies for industrial application. This thesis is the first to utilise magnetron sputtering, a technique allowing fine control over nano-material synthesis, for the design of novel solid adsorbents and deposition of novel dopants for H2 storage and CO2 capture. Work includes an in-depth study of the influence of nitrogen as a sputter gas on the growth of carbonaceous films, and is the first to explore these films performance as H2 and CO2 adsorbents. Several conflicting nitrogen effects were identified, their influence on the films growth dependent upon the nitrogen fraction of the sputter gas. Performance of the deposited films as adsorbents was also dependent on the growth conditions. The H2 storage capacity at 77 K and 20 bar of an optimised adsorbent, synthesised by magnetron sputtering, was 4.7 wt.%, comparable in performance to alternatives from the literature. Further work provides the first evidence that cerium, deposited by magnetron sputtering, can function as an adsorbent catalyst and identified that sputtering is a worthwhile, yet slow process for adsorbent doping as it facilitates intimate binding between the adsorbent and the dopant. The novel synthesis of graphene by magnetron sputtering was also attempted. Whilst tests failed, results collected could provide guidance for more successful attempts in the future

    Catalyst‐mediated enhancement of carbon nanotube textiles by laser irradiation: Nanoparticle sweating and bundle alignment

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    The photonic post-processing of suspended carbon nanotube (CNT) ribbons made by floating catalyst chemical vapor deposition (FC-CVD) results in selective sorting of the carbon nanotubes present. Defective, thermally non-conductive or unconnected CNTs are burned away, in some cases leaving behind a highly crystalline (as indicated by the Raman G:D ratio), highly conductive network. However, the improvement in crystallinity does not always occur but is dependent on sample composition. Here, we report on fundamental features, which are observed for all samples. Pulse irradiation (not only by laser but also white light camera flashes, as well as thermal processes such as Joule heating) lead to (1) the sweating-out of catalyst nanoparticles resulting in molten catalyst beads of up to several hundreds of nanometres in diameter on the textile surface and (2) a significant improvement in CNT bundle alignment. The behavior of the catalyst beads is material dependent. Here, we show the underlying mechanisms of the photonic post-treatment by modelling the macro- and microstructural changes of the CNT network and show that it is mainly the amount of residual catalyst which determines how much energy these materials can withstand before their complete decomposition
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