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Wang, Qingyang. "Fabrication et propriétés physiques de conducteurs multifilamentaires MgB2 dopés au carbone." Phd thesis, Université de Grenoble, 2012. http://tel.archives-ouvertes.fr/tel-00950672.
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Des conducteurs mono- et multi-filamentaires de MgB2 dans une gaine de Nb/Cu ont été élaborés par la technique PIT (powder in tube) avec des dopages de carbone et de TiC. Les résultats montrent qu'il y a une couche de diffusion non supraconductrice à l'interface entre le Nb et MgB2 pour les échantillons traités à haute température, couche qui empêche la pénétration du courant dans le conducteur. Les traitements thermiques doivent être inférieurs à 750°C. Les effets des dopages au carbone amorphe et au TiC ont été étudiés par XRD,MEB et aimantation. La substitution du bore par du carbone diminue légèrement la Tc mais augmente la piégeage des vortex, conduisant à un optimum du courant critique. Des multi-filaments de 6, 12 et 36 filaments sans dopage ont été élaborés par la technique PIT. Les propriétés mécaniques de ces conducteurs ont été renforcées en utilisant un filament central en Nb. L'assemblage MgB2/Nb/Cu est très adapté pour obtenir de grandes longueurs de conducteurs par la méthode PIT.
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Kleinsorge, Britta Yvonne. "Doping of amorphous carbon." Thesis, University of Cambridge, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.621744.
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RIBEIRO, MARIO LUIS PIRES GONCALVES. "CARBON DOPING IN INAIAS EPITAXIAL LAYERS." PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO, 2002. http://www.maxwell.vrac.puc-rio.br/Busca_etds.php?strSecao=resultado&nrSeq=2651@1.
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COORDENAÇÃO DE APERFEIÇOAMENTO DO PESSOAL DE ENSINO SUPERIORERICSSON DO BRASIL
É reconhecido o potencial de usar carbono como um dopante tipo p em InAlAs devido a obtenção de elevados níveis de dopagem [1,2]. Entretanto, níveis elevados de dopagem só são alcançados em baixas temperaturas de crescimento (Tg inferiores a 600°C). Nessas temperaturas, as camadas crescidas apresentam qualidade ótica inferior quando comparadas com camadas crescidas em temperaturas mais altas, o que é prejudicial para dispositivos de optoeletrônica. Neste trabalho, é apresentada uma investigação sistemática das propriedades de transporte e óticas em camadas de InAlAs dopadas com carbono para diferentes temperaturas de crescimento. É observado que quanto mais baixa for a Tg maior será a incorporação de carbono e maior a atividade elétrica. Este resultado indica que o carbono é incorporado de diversas maneiras, bem como um aceitador raso. O carbono também pode ser incorporado como um doador raso, pois é um dopante anfotérico. Entretanto, este fato, não é suficiente para explicar os resultados de transporte. A diferença entre a concentração Hall e a concentração CV indica a incorporação de doadores profundos. Provavelmente, o carbono participa na formação desses doadores profundos, uma vez que a concentração de doador profundo varia linearmente com a densidade atômica de carbono, determinada pela técnica SIMS. Por outro lado, centros não radiativos são mais facilmente incorporados em baixas Tg e a eficiência da fotoluminescência é reduzida. Essa degradação da fotoluminescência é independente da concentração de carbono, consequentemente, pode-se concluir que essa redução na eficiência da fotoluminescência não está associada à presença de doadores profundos. Com a finalidade de obter um incremento na atividade elétrica do carbono e melhoria na qualidade ótica das camadas, as amostras foram submetidas a tratamentos térmicos. Os tratamentos térmicos aumentaram a concentração de buracos mas não influenciaram na densidade de doadores profundos ou na qualidade ótica das camadas. Para a utilização de InAlAs dopado com carbono em dispositivos, deve-se obter simultaneamente uma boa qualidade ótica e elevada atividade elétrica das camadas.Então, deve-se identificar o doador profundo, que está associado ao carbono, com o objetivo de reduzí-lo ou eliminá-lo e consequentemente, obter um incremento na atividade elétrica das camadas. Desta forma as camadas podem ser crescidas a temperaturas mais altas adequadas para uma emissão de fotoluminescência eficiente. Cálculos teóricos são apresentados de modo a ajudar essa identificação. Outra possibilidade é usar diferentes fontes de arsina em que as moléculas se dissociem em temperaturas mais baixas.
The potential of using carbon as a p-type dopant for InAlAs has already been recognized due to the achievable high hole concentration [1,2]. However, high doping levels are reached only for low growth teperatures (Tg below 600°C). These temperatures produce layers with poor optical quality as compared to those grown at higher temperatures, which can be detrimental for optoeletronic device. In this work we present crystal, transport and optical properties of such layers grown at different temperatures. We find that the lower Tg, the more efficient the carbon incorporation and its electrical activity are. This result indicates that carbon is incorporated in forms different from a shallow acceptor, as well. Carbon can also be incorporated as a shallow donor since it is an amphoteric dopant. However, this alone does not explain the transport results. The difference between the net free charge density determined from capacitance measurements indicates that a deep donor is also incorporated. Carbon most likely participates in the deep donor formation since the inferred deep donor concentration varies linearly with the carbon atomic density measured by SIMS. On the other hand, non- radiative deep levels are more efficiently incorporated as Tg is reduced degrading the photoluminescence characteristics. Such degration is independent of the carbon doping. Therefore, one concludes that the decrease in the photoluminescence efficiency cannot be related to the presence of the deep donor mentioned in the previous paragraph. To further probe the carbon electrical activity and its effect on the optical properties of the layers, the samples have been subjected to a heat-treatment. Annealing the samples increases the hole concentration, but neither affects the deep donor density nor improves the layers optical quality. In order to use carbon doped InAlAs in devices which simultaneously require good optical quality and high electrical activity of the layers, one should identify the deep donor involving carbon in order to try to reduce its concentration or even eliminate it, consequently improving the electrical activity of the layers. In such a way the layers can be grown at higher temperatures, adequate for an efficient photoluminescence emission. Theoretical calculations are being carried out to help with such identification. Another possibility is to use other arsine sources which crack at lower temperatures.
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Alluqmani, Saleh Marzoq B. "Growth and doping of carbon nanotubes and graphene." Thesis, Durham University, 2015. http://etheses.dur.ac.uk/10949/.
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Single walled carbon nanotubes (SWCNTs) have been doped with nitrogen (N) by two ion-mediated approaches: directly through irradiation with N+ ions and by a novel indirect technique, creating defects through Ar+ ion irradiation which then react with nitrogen upon annealing in a N2 atmosphere. X-ray photoelectron spectroscopy (XPS) was then employed to determine the chemical environment of the nitrogen within the resulting SWCNT material. Depending upon the exact preparation conditions, nitrogen in graphitic (substitutional) pyridinic and pyrrolic configurations could be identified. Nitrogen doping through the novel method was found to introduce the largest concentration of chemisorbed nitrogen within the SWCNT films, dominated by thermodynamically unstable pyrrolic species at low process temperatures (500ºC). The maximum concentration of nitrogen in graphitic sites was achieved by direct ion bombardment, although both XPS and Raman spectroscopy indicated that this approach to doping led to the greatest damage. The ability to vary both bsolute and relative composition of chemisorbed nitrogen species is expected to be valuable for a range of fundamental studies, particularly of the catalytic behaviour of these materials. The growth of graphene on copper under atmospheric pressure using a soft solid source (nonadecane) is reported. It is found that the growth rate is best described by a model which involves the continuous supply of reactive species during the entire growth period. This observation is explained in terms of the formation of decomposition produces which reside on an otherwise clean surface after nonadecane desorption and provide a series of ‘mini carbon sources’ for graphene growth. XPS analysis indicates that, as expected, increased growth temperature leads to greater graphitisation at the surface (and hence graphene ‘quality’) which is not accompanied by any substantial change in island size and coverage. It is found that although graphene islands can be produced it is not possible to form continuous films, demonstrating the limitations of this technique. Although limited in some ways, the use of soft solid precursors for graphene growth allows the ready introduction of potential dopant materials. XPS, Raman and SEM data provide strong evidence that a PDMS precursor can be employed in atmospheric pressure solid-phase CVD to produce graphene heavily doped with silicon, which has not been previously achieved. Since silicon-doped graphene is predicted to possess a band gap related to the Si concentration, this may provide a route to produce a graphene-based material of use in digital electronics.
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Sanwick, Alexis. "Heteroatom-Doped Chemical Vapor Deposition Carbon Ultramicroelectrodes." Digital Commons @ East Tennessee State University, 2020. https://dc.etsu.edu/honors/592.
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Metal nanoparticles have been a primary focus in areas of catalysis and electrocatalysis applications as a result of their large surface area-to-volume ratios. While there is an increased interest in understanding the properties and behaviors of metal nanoparticles, they can become expensive over time. Recent research has incorporated the idea of using heteroatom-doped materials as a cheaper catalytic alternative to metal nanoparticles. In this study nitrogen-doping and phosphorous-doping techniques were applied to chemical vapor-deposited carbon ultramicroelectrodes in order to study the electrocatalytic properties toward the oxygen reduction reaction and the enhanced affinity for the deposition of gold nanoparticles onto the electrodes.
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Liang, Meng Suan. "Carbon doping in GaAs, AlGaAs, InGaAs and distributed Bragg reflectors." Thesis, University of Liverpool, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.399255.
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Sojoudi, Hossein. "The synthesis, doping, and characterization of graphene films." Diss., Georgia Institute of Technology, 2012. http://hdl.handle.net/1853/50125.
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Graphene, a two-dimensional counterpart of three-dimensional graphite, has attracted significant interest, due to its distinctive electrical and mechanical properties, for developing electronic, optoelectronic, and sensor technologies. In general, doping of graphene is important, as it gives rise to p-type and n-type materials, and it adjusts the work function of the graphene. This adjustment is necessary in order to control charge injection and collection in devices such as solar cells and light emitting devices. Current methods for graphene doping involve high temperature process or interactions with chemicals that are not stable. Moreover, the process of transferring graphene from its growth substrate and its exposure to the environment results in a host of chemical groups that can become attached to the film and alter its electronic properties by accepting or donating electrons/holes. Intentional and controllable doping of the graphene, however, requires a deeper understanding of the impact of these groups. The proposed research will attempt to clarify the unintentional doping mechanism in graphene through adsorption or desorption of gas/vapor molecules found in standard environments. A low temperature, controllable and defect-free method for doping graphene layers will also be studied through modifying the interface of graphene and its support substrate with self-assembled monolayers (SAMs) which changes the work function and charge carriers in the graphene layer. Furthermore, current methods of chemical vapor deposition synthesis of graphene requires the film to be transferred onto a second substrate when the metal layer used for growth is not compatible with device fabrication or operation. To address this issue, the proposed work will investigate a new method for wafer scale, transfer-free synthesis of graphene on dielectric substrates using new carbon sources. This technique allows patterned synthesis on the target substrate and is compatible with standard device fabrication technologies; hence, it opens a new pathway for low cost, large area synthesis of graphene films.
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Pinto, Hugo Manuel. "Defects and dopants in carbon related materials." Thesis, University of Exeter, 2012. http://hdl.handle.net/10036/3601.
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This thesis presents theoretical studies of the optical and electronic properties of defects in diamond and of the mechanisms of doping graphene. The birefringence of the four petalled defect commonly observed in CVD diamond is explained by four linear arrays of dislocations along ⟨110⟩ directions with ⟨110⟩ Burgers vectors. Such an arrangement of dislocations reproduces the extension and the features of the birefringence patterns observed experimentally. Density functional theory via the AIMPRO code was used to study the electronic and optical properties of different nitrogen-related point defects in diamond. It was found that the zero-phonon luminescence line of the NV− defects can split in the presence of a surface or other NV− defects. Since VNH and VN2 are expected to have similar optical properties, the optical transi- tions for VN2 were used to correct the transitions for VNH calculated by local density approximation. The absorption band at 2.38 eV (520 nm) observed in CVD diamond is then attributed to an internal transition of VNH. The weak zero-phonon line and broad vibronic sidebands for VN− and VN−2 and its absence for VNH− is explained by the large structural change when the defect is excited. Finally, different mechanisms for doping graphene were considered. The calculations predict the electropositive metals, such as Ti and Cr, act as donors, while molecules with strong electron affinity, such as F4-TCNQ, act as acceptors in graphene. An unexpected mechanism of doping graphene was shown by Au which dopes bilayer graphene but not single layer. In the presence of water, electrochemical reactions on the graphene can also lead to p or n-type doping.
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Ashourirad, Babak. "HETEROATOM-DOPED NANOPOROUS CARBONS: SYNTHESIS, CHARACTERIZATION AND APPLICATION TO GAS STORAGE AND SEPARATION." VCU Scholars Compass, 2015. http://scholarscompass.vcu.edu/etd/4062.
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Activated carbons as emerging classes of porous materials have gained tremendous attention because of their versatile applications such as gas storage/separations sorbents, oxygen reduction reaction (ORR) catalysts and supercapacitor electrodes. This diversity originates from fascinating features such as low-cost, lightweight, thermal, chemical and physical stability as well as adjustable textural properties. More interestingly, sole heteroatom or combinations of various elements can be doped into their framework to modify the surface chemistry. Among all dopants, nitrogen as the most frequently used element, induces basicity and charge delocalization into the carbon network and enhances selective adsorption of CO2. Transformation of a task-specific and single source precursor to heteroatom-doped carbon through a one-step activation process is considered a novel and efficient strategy.
With these considerations in mind, we developed multiple series of heteroatom doped porous carbons by using nitrogen containing carbon precursors. Benzimidazole-linked polymers (BILP-5), benzimidazole monomer (BI) and azo-linked polymers (ALP-6) were successfully transformed into heteroatom-doped carbons through chemical activation by potassium hydroxide. Alternative activation by zinc chloride and direct heating was also applied to ALP-6. The controlled activation/carbonization process afforded diverse textural properties, adjustable heteroatom doping levels and remarkable gas sorption properties. Nitrogen isotherms at 77 K revealed that micropores dominate the porous structure of carbons. The highest Brunauer-Emett-Teller (BET) surface area (4171 m2 g-1) and pore volume (2.3 cm3 g-1) were obtained for carbon synthesized by KOH activation of BI at 700 °C. In light of the synergistic effect of basic heteroatoms and fine micropores, all carbons exhibit remarkable gas capture and selectivity. Particularly, BI and BIPL-5 derived carbons feature unprecedented CO2 uptakes of 6.2 mmol g-1 (1 bar) and 2.1 mmol g-1 (0.15 bar) at 298 K, respectively. The ALP-6 derived carbons retained considerable amount of nitrogen dopants (up to 14.4 wt%) after heat treatment owing to the presence of more stable nitrogen-nitrogen bonds compared to nitrogen-carbon bonds in BILP-5 and BI precursors. Subsequently, the highest selectivity of 62 for CO2/N2 and 11 for CO2/CH4 were obtained at 298 K for a carbon prepared by KOH activation of ALP-6 at 500 °C.
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Anwar, Abdul Waheed. "Investigation of doping and photoexcitation in carbon nanotubes using Raman spectroscopy." Toulouse 3, 2011. http://thesesups.ups-tlse.fr/1156/.
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La spectroscopie Raman est une technique de caractérisation non destructive appropriée pour l'étude des nanotubes des carbone. Des différences dans le décalage spectral des bandes Raman D et G, correspondant aux effets anharmoniques, sont observées lors d'un chauffage des nanotubes de carbone par irradiation photonique intense ou en faisant varier la température d'un thermostat. Les modifications spectrales du mode D sont attribués à des modifications du processus de double résonance Raman en raison de la variation de la structure de bande électronique provoquée par la creation des excitons. L'enquête de l'influence du dopage et de photoexcitation sur la bande G et la D de nanotubes de carbone montrent que la spectroscopie Raman peut être utilisé comme un outil de diagnostic. Les bandes spectrales élargir et décale vers le haut fréquence pour l'azote dopé nanotubes de carbone multi parois. Le décalage vers le haut fréquence pour l'acide sulfurique dopé double parois nanotubes de carbone est attribuée à transfert de charge et la déformation dans le réseau. Nous avons combiné le dopage de l'acide sulfurique et haute pression spectroscopie Raman pour étudier les propriétés de DWCNT. Le DWCNT dopé avec différentes concentrations d'acide sulfurique sous haute pression, suggère un effet de l'ordre des molécules autour de nanotubes à concentrations d'acide supérieur. Spectres Raman de double parois nanotube de carbone individual sur la silice en évidence un éclatement de la bande G grâce aux contributions du tube interne et externe lorsque utilisez une énergie d'excitation en résonance avec le tube métallique interne et tube semionducteurs externe. Les largeurs des bandes sont comparables à ce qui a été observé pour le nanotube de carbone monoparoi individul ou le graphène. Augmentation de la puissance du laser décale la bande G du tube extérieur vers les énergies plus élevées et modifie sa forme en ligneRaman spectroscopy is a non-invasive characterization technique suitable for the study of carbon nanotubes. Differences in the spectral shift of the Raman D and G bands are observed when heating carbon nanotubes through intense photon irradiation and by varying the temperature in a thermostat. These spectral changes in D mode are attributed to the variation of the electronic band structure by excitons creation. The investigation of the influence of doping and photoexcitation on the Raman G and D band of carbon nanotubes show that Raman spectroscopy can be used as a diagnostic tool. The spectral bands broaden and up shifts for nitrogen doped multi walled carbon nanotubes (MWCNT). The up shift for sulphuric acid doped double wall carbon nanotubes (DWCNT) synthesized from catalytic chemical vapor deposition method (CCVD) is attributed to charge transfer and strain in the lattice. We have combined sulphuric acid doping and high pressure Raman spectroscopy to investigate the properties of DWCNT. The DWCNT doped with different concentrations of sulphuric acid are explored under high pressure suggesting an effect of the molecular ordering around carbon nanotubes at higher acid concentrations. Raman spectra of individual double wall carbon nanotubes on silica show a splitting of the G band due to contributions of the inner and outer tube when using a excitation energy in resonance with the inner metallic tube and outer semiconducting tube. The spectral line widths are comparable to what has been observed for individual single wall carbon nanotubes (SWCNT) or graphene. Increased laser power shifts the G band of the outer tube to higher energies and modifies its line shape
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Hopkin, Amy L. "Methane conversion over supported nickel catalysts : influence of gold doping, support material and preparation method." Thesis, Keele University, 2002. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.288499.
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Ye, Jianting. "Fabrication analysis and lithium doping in 4 Å carbon nanotubes in the channels of AlPO4̳-5 crystal /." View Abstract or Full-Text, 2002. http://library.ust.hk/cgi/db/thesis.pl?PHYS%202002%20YE.
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Thesis (M. Phil.)--Hong Kong University of Science and Technology, 2002.On t.p. "4̳" is subscript. Includes bibliographical references (leaves 84-86). Also available in electronic version. Access restricted to campus users.
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Wang, Rongrong. "Dopage de nanostructures de carbone pour l'émission de champ." Thesis, Toulouse 3, 2016. http://www.theses.fr/2016TOU30358/document.
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Ce travail de thèse a porté sur l'étude des nanostructures (fondamentalement des nanotubes (NTs)) à base de carbone pour leurs applications sur l'émission de champ, en particulière, sur leur potentielle utilisation dans les canons d'émission de champ froide (C-FEG, d'après son acronyme anglais). Nous nous sommes intéressés à l'incorporation des atomes dopants (l'azote et/ou le bore) dans la structure de ces nanomatériaux pour pouvoir moduler les propriétés électroniques (d'émission de champ). Pour doper ces nanostructures, nous avons développé la voie carbo-thermique. Elle est base sur la réduction thermique de l'acide borique en employant du carbone, en tant qu'agent réducteur, et en présence de l'azote. Nous avons donc exposé des NTs multi-parois de carbone, en présence d'un mélange de poudres de nitrure de bore et de l'acide borique, à des températures entre 1350-1500 °C, sous différentes atmosphères (hydrogène/argon et/ou de l'azote). Nous avons également proposé et exploré une nouvelle voie de dopage via la réaction d'un précurseur d'azote (le nitrure de fer) avec les nanotubes de carbone, sous azote et à des températures entre 1000-1200 °C. Nous avons combiné des études par microscopie électronique en transmission (imagerie d'haute résolution (HRTEM) et spectroscopie des pertes d'énergie (EELS, d'après son acronyme anglais) en mode balayage (STEM)) dans des microscopes corrigés d'aberrations avec des mesures de spectroscopie photo-électronique par rayons X (XPS). L'ensemble de ces analyses nous a permis d'étudier la structure de ces nano-objets ainsi que d'identifier et de connaître précisément leur composition élémentaire, même locale, au niveau sous-nanométrique (à l'échelle de ~2 angströms). Nous avons montré qu'il est possible de doper ces nanotubes de carbone en incorporant du nitrure de bore dans leur structure originale. Deux systèmes différents ont été observés : 1) la substitution des feuillets/parois internes de carbone des nanotubes par du nitrure de bore, en faisant des nanotubes hybrides carbone/nitrure de bore/carbone, à ne pas exclure de phases mixtes BxCyNz dans ces parois ; 2) la présence de nano-domaines de nitrure de bore, de quelques nanomètres (entre 2-10 nm) dans la structure des nanotubes de carbone. Nous avons aussi développé un banc d'émission de champ pour étudier ces propriétés des différentes nanostructures. Le banc équipé avec un canon d'un microscope électronique en transmission (MET) permet d'évaluer les performances émettrices de ces nanostructures dans des conditionnes réelles de fonctionnement (dans un vide de 10-7 Pa) et en permettant des flashes de dégazage. Nous avons également étudié l'influence des flashes dans un microscope électronique à balayage (MEB). D'après ces résultats, nous avons conclu que le point d'équilibre des flashes est de 4 A. Deux situations différentes ont été observées : 1) un flash insuffisant entraine des instabilités du courant d'émission dû à la présence d'impuretés ; 2) un flash excessif provoque la réduction des performances d'émission dû à l'arrondissement de la pointe émettriceThis research work concerns the study of carbon-based nanostructures (mainly nanotubes (NTs)) and their field emission properties, for their potential use in cold field emission guns (C-FEG). We focus on the incorporation of dopant atoms (nitrogen and/or boron) in the structure of these nanomaterials in order to modulate the electronic (field emission) properties. The doping of these nanostructures has been achieved using the carbothermal method. This technique consists in the thermal reduction of boron oxide using carbon as reducing agent and in presence of nitrogen. Thus, a mixture of multi-walled carbon NTs, boron nitride and boric acid powders have been heated at temperatures between 1350-1500 °C, under different atmospheres (hydrogen/argon and/or nitrogen). In addition, we have also proposed and explored a new way for achieving the doping of such nanostructures via the reaction of a precursor of nitrogen (iron nitride) with the carbon nanotubes, under nitrogen and at temperatures ranging 1000-1200 °C. We present a detailed characterization study combining transmission electron microscopy (high-resolution imaging (HRTEM) and electron energy-loss spectroscopy (EELS) in scanning mode (STEM), all these techniques developed using aberration-corrected microscopes) investigations, with X-ray photoelectron spectroscopy (XPS) measurements. These studies allow us to study the structural modification after thermal treatments as well as the incorporation of hetero elements of these nanostructures, at local (sub-nanometer level ~ 2 Å) and macro scales. We have demonstrated the doping of these nanostructures via the incorporation of boron nitride in the pristine structure of the carbon nanotubes. Two different systems were observed: 1) the substitution of the inner walls of carbon nanotubes by boron nitride, producing hybrid nanotubes (carbon/boron nitride/carbon), it is worth to mention that BxCyNz mixed phases in these walls cannot be excluded; 2) the presence of boron nitride nano-domains of few nanometers (2-10 nm) incorporated in the structure of the carbon nanotubes. We also developed a field emission bench to study the properties of individual nanostructures. This bench, which is equipped with the gun of a transmission electron microscope (TEM), allows to evaluate the emission performances of these nanostructures under real work conditions (vacuum of 10-7 Pa), including the flashing. In addition, we have also studied the influence of these flashes via scanning electron microscopy (SEM). From these studies, we have concluded that the equilibrium point of the flashes is 4 A. Two different situations have been observed: 1) a deficient flash leads to instable emission currents due to the presence of impurities; 2) an excessive flash leads to a reduction of the emission performances due to the modification of the tip's morphology
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Mawudoku, Daniel, George Affadu_Danful, Caitlin Millsaps, and Gregory Bishop. "Immobilization of Electrocatalytically Active Gold Nanoparticles on Nitrogen-Doped Carbon Fiber Electrodes." Digital Commons @ East Tennessee State University, 2019. https://dc.etsu.edu/asrf/2019/schedule/106.
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Immobilization of Electrocatalytically Active Gold Nanoparticles on Nitrogen-Doped Carbon Fiber Electrodes
ABSTRACT
Recently, immobilization of single metal nanoparticles on nanometer-sized electrodes has been demonstrated as a means to electrochemically probe the relationship between nanoparticle structure and function. Such studies of individual, isolated nanoparticles enable investigation of electrochemical behavior and electrocatalytic properties in the absence of complicating factors like interparticle distance and nanoparticle loading that are typically associated with collections of particles distributed on electrode supports. However, interpretation of electrochemical data obtained from single nanoparticle immobilization experiments can also be difficult since the underlying nanoelectrode platform can sometimes contribute to the measured current or the immobilization strategy may have adverse effects on electron transfer. Here we report immobilization of gold nanoparticles on relatively catalytically inert carbon fiber ultramicro- and nanoelectrodes through a modification method based on recently reported soft nitriding process found to be effective in attaching ligand-free ultrasmall noble metal catalysts to activated carbons. X-ray photoelectron spectroscopy results reveal that the nitriding of carbon fibers provides 3.5 times increase in surface nitrogen content, introducing mostly pyridinic and amine nitrogen groups. The nitrogen-containing surface sites proved to be beneficial to the deposition of gold nanoparticles (AuNPs), as sodium borohydride reduction of tetrachloroaurate resulted in attachment of AuNPs on nitrided carbon fiber ultramicroelectrodes (N-CF-UMEs) in as little as 10 seconds while immobilization of AuNPs on unmodified CF-UMEs required at least 12 hours. A recently reported electrochemical method was employed to characterize immobilized AuNPs, and AuNP size was found to be directly related to deposition time. AuNPs immobilized on N-CF-UMEs also exhibited electrocatalytic activity towards methanol oxidation. Reduction of electrode size will enable this strategy to be employed to investigate electrochemical behavior of individual gold nanoparticles, while the ligand-free nature of the immobilized particles also provides the opportunity to investigate effects of surface capping agents on electrocatalytic properties.
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Chindanon, Kritsa. "Nitrogen doping in low temperature halo-carbon homoepitaxial growth of 4H-silicon carbide." Master's thesis, Mississippi State : Mississippi State University, 2008. http://library.msstate.edu/etd/show.asp?etd=etd-07102008-045510.
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Villalpando, Paéz Federico. "Effects of doping single and double walled carbon nanotubes with nitrogen and boron." Thesis, Massachusetts Institute of Technology, 2006. http://hdl.handle.net/1721.1/36215.
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Thesis (S.M.)--Massachusetts Institute of Technology, Dept. of Materials Science and Engineering, 2006.Includes bibliographical references (p. 135-143).
Controlling the diameter and chirality of carbon nanotubes to fine tune their electronic band gap will no longer be enough to satisfy the growing list of characteristics that future carbon nanotube applications are starting to require. Controlling their band gap, wall reactivity and mechanical properties is imperative to make them functional. The solution to these challenges is likely to lie in smart defect engineering. Defects of every kind can induce significant changes on the intrinsic properties of carbon nanotubes. In this context, this thesis analyzes the effects of doping single and double walled carbon nanotubes with nitrogen and boron. We describe the synthesis of N-doped single-walled carbon nanotubes (N-SWNTs), that agglomerate in bundles and form long strands (<10cm), via the thermal decomposition of ferrocene/ethanol/benzylamine (FEB) solutions in an Ar atmosphere at 950°C. Using Raman spectroscopy, we noted that as the N content is increased in the starting FEB solution, the growth of large diameter tubes is inhibited. We observed that the relative electrical conductivity of the strands increases with increasing nitrogen concentration. Thermogravimetric analysis (TGA) showed novel features for highly doped tubes, that are related to chemical reactions on N sites.
(cont.) We also carried out resonance Raman studies of the coalescence process of double walled carbon nanotubes in conjunction with high resolution transmission electron microscope (HRTEM) experiments on the same samples, heat treated to a variety of temperatures and either undoped or Boron doped. As the heat treatment temperatures are increased (to 1300°C) a Raman mode related to carbon-carbon chains (w = 1855cm-1) is observed before DWNT coalescence occurs. These chains are expected to be 3-5 atoms long and they are established covalently between adjacent DWNTs. The sp carbon chains trigger nanotube coalescence via a zipper mechanism and the chains disappear once the tubes merge. Other features of the Raman spectra were analyzed as a function of heat treatment with special emphasis on the metallic or semiconducting nature of the layers constituting the DWNTs. DWNTs whose outer wall is metallic tend to interact more with the dopant and their outer tubes are the predominant contributors to the line shape of the G and G' bands.
(cont.) The metallic or semiconducting nature of the layers of the DWNTs does not affect their coalescence temperature. All the experiments and analysis presented in this thesis are the result of a collaborative effort between Professor Dresselhaus' group at MIT and its international collaborators, including Professor Endo's group at Shinshu University, Nagano, Japan, Professors Pimenta's and Jorio's group at the Federal University of Minas Gerais, Belo Horizonte, Brazil, and Professors M. and H. Terrones' group at IPICYT, San Luis Potosi, Mexico.
by Federico Villalpando Paéz.
S.M.
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Kuo, Ming-Tsun. "Field emission and annealing studies of n-type doped hydrogenated amorphous carbon films." Thesis, University of Bristol, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.340300.
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Webb, Kimberly Faye. "Synthesis, blending, and doping of electrically conducting poly(3-undecylbithiophene) in supercritical carbon dioxide." Diss., Georgia Institute of Technology, 2000. http://hdl.handle.net/1853/10129.
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Wohlgemuth, Stephanie-Angelika. "Functional nanostructured hydrothermal carbons for sustainable technologies : heteroatom doping and superheated vapor." Phd thesis, Universität Potsdam, 2012. http://opus.kobv.de/ubp/volltexte/2012/6012/.
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The underlying motivation for the work carried out for this thesis was the growing need for more sustainable technologies. The aim was to synthesize a “palette” of functional nanomaterials using the established technique of hydrothermal carbonization (HTC). The incredible diversity of HTC was demonstrated together with small but steady advances in how HTC can be manipulated to tailor material properties for specific applications. Two main strategies were used to modify the materials obtained by HTC of glucose, a model precursor representing biomass.
The first approach was the introduction of heteroatoms, or “doping” of the carbon framework. Sulfur was for the first time introduced as a dopant in hydrothermal carbon. The synthesis of sulfur and sulfur/nitrogen doped microspheres was presented whereby it was shown that the binding state of sulfur could be influenced by varying the type of sulfur source. Pyrolysis may additionally be used to tune the heteroatom binding states which move to more stable motifs with increasing pyrolysis temperature. Importantly, the presence of aromatic binding states in the as synthesized hydrothermal carbon allows for higher heteroatom retention levels after pyrolysis and hence more efficient use of dopant sources. In this regard, HTC may be considered as an “intermediate” step in the formation of conductive heteroatom doped carbon. To assess the novel hydrothermal carbons in terms of their potential for electrochemical applications, materials with defined nano-architectures and high surface areas were synthesized via templated, as well as template-free routes. Sulfur and/or nitrogen doped carbon hollow spheres (CHS) were synthesized using a polystyrene hard templating approach and doped carbon aerogels (CA) were synthesized using either the albumin directed or borax-mediated hydrothermal carbonization of glucose. Electrochemical testing showed that S/N dual doped CHS and aerogels derived via the albumin approach exhibited superior catalytic performance compared to solely nitrogen or sulfur doped counterparts in the oxygen reduction reaction (ORR) relevant to fuel cells. Using the borax mediated aerogel formation, nitrogen content and surface area could be tuned and a carbon aerogel was engineered to maximize electrochemical performance. The obtained sample exhibited drastically improved current densities compared to a platinum catalyst (but lower onset potential), as well as excellent long term stability.
In the second approach HTC was carried out at elevated temperatures (550 °C) and pressure (50 bar), corresponding to the superheated vapor regime (htHTC). It was demonstrated that the carbon materials obtained via htHTC are distinct from those obtained via ltHTC and subsequent pyrolysis at 550 °C. No difference in htHTC-derived material properties could be observed between pentoses and hexoses. The material obtained from a polysaccharide exhibited a slightly lower degree of carbonization but was otherwise similar to the monosaccharide derived samples. It was shown that in addition to thermally induced carbonization at 550 °C, the SHV environment exhibits a catalytic effect on the carbonization process. The resulting materials are chemically inert (i.e. they contain a negligible amount of reactive functional groups) and possess low surface area and electronic conductivity which distinguishes them from carbon obtained from pyrolysis. Compared to the materials presented in the previous chapters on chemical modifications of hydrothermal carbon, this makes them ill-suited candidates for electronic applications like lithium ion batteries or electrocatalysts. However, htHTC derived materials could be interesting for applications that require chemical inertness but do not require specific electronic properties. The final section of this thesis therefore revisited the latex hard templating approach to synthesize carbon hollow spheres using htHTC. However, by using htHTC it was possible to carry out template removal in situ because the second heating step at 550 °C was above the polystyrene latex decomposition temperature. Preliminary tests showed that the CHS could be dispersed in an aqueous polystyrene latex without monomer penetrating into the hollow sphere voids. This leaves the stagnant air inside the CHS intact which in turn is promising for their application in heat and sound insulating coatings.
Overall the work carried out in this thesis represents a noteworthy development in demonstrating the great potential of sustainable carbon materials.Das Ziel der vorgelegten Arbeit war es, mit Hilfe der Hydrothermalen Carbonisierung (HTC) eine Palette an verschiedenen Materialien herzustellen, deren physikalische und chemische Eigenschaften auf spezifische Anwendungen zugeschnitten werden können. Die Motivation hierfür stellt die Notwendigkeit, Alternativen zu Materialien zu finden, die auf fossilen Brennstoffen basieren. Dabei stellen vor allem nachhaltige Energien eine der größten Herausforderungen der Zukunft dar. HTC ist ein mildes, nachhaltiges Syntheseverfahren welches prinzipiell die Nutzung von biologischen Rohstoffen (z. B. landwirtschaftlichen Abfallprodukten) für die Herstellung von wertvollen, Kohlenstoff-basierten Materialien erlaubt. Es wurden zwei verschiedene Ansätze verwendet, um hydrothermalen Kohlenstoff zu modifizieren. Zum einen wurde HTC unter „normalen“ Bedingungen ausgeführt, d. h. bei 180 °C und einem Druck von etwa 10 bar. Der Zucker Glukose diente in allen Fällen als Kohlenstoff Vorläufer. Durch Zugabe von stickstoff und /oder schwefelhaltigen Additiven konnte dotierte Hydrothermalkohle hergestellt werden. Dotierte Kohlenstoffe sind bereits für ihre positiven Eigenschaften, wie verbesserte Leitfähigkeit oder erhöhte Stabilität, bekannt. Zusätzlich zu Stickstoff dotierter Hydrothermalkohle, die bereits von anderen Gruppen hergestellt werden konnte, wurde in dieser Arbeit zum ersten Mal Schwefel in Hydrothermalkohle eingebaut. Außerdem wurden verschiedene Ansätze verwendet, um Oberfläche und definierte Morphologie der dotierten Materialien zu erzeugen, welche wichtig für elektrochemische Anwendungen sind. Schwefel- und/oder stickstoffdotierte Kohlenstoff Nanohohlkugeln sowie Kohlenstoff Aerogele konnten hergestellt werden. Mit Hilfe von einem zusätzlichen Pyrolyseschritt (d. h. Erhitzen unter Schutzgas) konnte die Leitfähigkeit der Materialien hergestellt werden, die daraufhin als Nichtmetall-Katalysatoren für Wasserstoff-Brennstoffzellen getestet wurden. Im zweiten Ansatz wurde HTC unter extremen Bedingungen ausgeführt, d. h. bei 550 °C und einem Druck von ca. 50 bar, welches im Wasser Phasendiagram dem Bereich des Heißdampfes entspricht. Es konnte gezeigt werden, dass die so erhaltene Hydrothermalkohle ungewöhnliche Eigenschaften besitzt. So hat die Hochtemperatur-Hydrothermalkohle zwar einen hohen Kohlenstoffgehalt (mehr als 90 Massenprozent), enthält aber auch viele Wasserstoffatome und ist dadurch schlecht leitfähig. Da damit elektrochemische Anwendungen so gut wie ausgeschlossen sind, wurde die Hochtemperatur-Hydrothermalkohle für Anwendungen vorgesehen, welche chemische Stabilität aber keine Leitfähigkeit voraussetzen. So wurden beispielsweise Hochtemperatur-Kohlenstoff-Nanohohlkugeln synthetisiert, die großes Potential als schall- und wärmeisolierende Additive für Beschichtungen darstellen. Insgesamt konnten erfolgreich verschiedenste Materialien mit Hilfe von HTC hergestellt werden. Es ist zu erwarten, dass sie in Zukunft zu nachhaltigen Technologien und damit zu einem weiteren Schritt weg von fossilen Brennstoffen beitragen werden.
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Kanakaraj, Sathya Narayan. "Processing Carbon Nanotube Fibers for Wearable Electrochemical Devices." University of Cincinnati / OhioLINK, 2019. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1573224577754985.
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Wornyo, Eric. "Nitrogen-Doped Carbon Fiber Ultramicroelectrodes as Electrochemical Sensors for Detection of Hydrogen Peroxide." Digital Commons @ East Tennessee State University, 2021. https://dc.etsu.edu/etd/3960.
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Carbon fiber ultramicroelectrodes (CF-UMEs) are commonly used as electrochemical probes and sensors due to their small size, fast response, and high signal-to-noise ratio. Surface modification strategies are often employed on CF-UMEs to improve their selectivity and sensitivity for desired applications. However, many modification methods are cumbersome and require expensive equipment. In this study, a simple approach known as soft nitriding is used to prepare nitrogen-doped CF-UMEs (N-CF-UMEs). Nitrogen groups introduced via soft nitriding act as electrocatalytic sites for the breakage of O-O bonds during the reduction of peroxides like H2O2, a common target of biosensing strategies. Voltammetric studies confirm that, compared to CF-UMEs, N-CF-UMEs possess enhanced electrocatalytic activity towards H2O2 reduction as evidenced by an increase in current and positive shift in onset potential for the reaction. N-CF-UMEs also proved capable for amperometric detection of H2O2, exhibiting good linear response from 0.1 to 5.6 mM at -0.4 V vs. Ag/AgCl.
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Louisia, Stéphane. "Synthèse de catalyseurs bimétalliques supportés sur nanotubes de carbone dopés pour pile à combustible PEM." Phd thesis, Toulouse, INPT, 2017. http://oatao.univ-toulouse.fr/17815/7/louisia.pdf.
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Les recherches menées dans le domaine des piles à combustibles à membrane échangeuse de protons (PEMFCs) depuis le début des années 1980 ont permis de considérablement améliorer leurs performances. Deux principaux verrous persistent néanmoins au niveau des catalyseurs : le coût et la stabilité. En effet, pour obtenir de bonnes performances, il faut que la couche active cathodique soit relativement chargée en métaux nobles, comme le platine, ce qui a un coût important. En plus d’être couteux, les catalyseurs utilisés commercialement sont sujets à différents phénomènes de dégradation, notamment l’oxydation du support carboné. Les travaux décrits dans cette thèse visent à produire des catalyseurs bimétalliques supportés sur des nanotubes de carbones dopés, afin de préparer des structures actives pour la Réaction de Réduction de l’Oxygène (ORR) et résistantes dans les conditions de fonctionnement des PEMFCs. La première étape a été la synthèse de nanotubes de carbone dopés à l’azote (N-CNT) ou au soufre (S-CNT). Différents traitements et fonctionnalisations ont été testés pour faciliter le dépôt et la dispersion de nanoparticules métalliques à la surface des nanotubes, faciliter l’intégration du catalyseur dans la couche active et ralentir le phénomène d’oxydation du carbone. Des nanoparticules bimétalliques PtCo et PtNi ont été préparées en utilisant une méthode de synthèse originale utilisant un liquide ionique comme stabilisant. Tous les catalyseurs ainsi synthétisés ont présenté des surfaces électro-actives (ECSA) élevées et de bonnes activités pour l’ORR. Les plus pertinents ont été étudiés en mono-cellules de 25 cm². Ils présentent de meilleurs résultats aux tests de dégradation accélérés du support carboné, comparés à une référence commercial PtCo supporté sur noir de carbone. Une diminution du chargement en platine de la couche active cathodique de 0,4 mgPt/cm² à 0,2 mgPt/cm² a permis d’améliorer les performances de la mono-cellule en diminuant notamment les limitations dûes au transport de matière dans la couche active.
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Xhyliu, Fjorela. "Surface Functionalization and Optical Spectroscopy of Single-wall Carbon Nanotubes." Cleveland State University / OhioLINK, 2020. http://rave.ohiolink.edu/etdc/view?acc_num=csu1599143727075125.
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Mishra, Siddharth. "Plasma Enhanced Synthesis of Novel N Doped Vertically Aligned Carbon Nanofibers-3D Graphene hybrid structure." University of Cincinnati / OhioLINK, 2019. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1552380299631335.
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Ciarkowski, Timothy A. "Low Impurity Content GaN Prepared via OMVPE for Use in Power Electronic Devices: Connection Between Growth Rate, Ammonia Flow, and Impurity Incorporation." Diss., Virginia Tech, 2019. http://hdl.handle.net/10919/94551.
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GaN has the potential to revolutionize the high power electronics industry, enabling high voltage applications and better power conversion efficiency due to its intrinsic material properties and newly available high purity bulk substrates. However, unintentional impurity incorporation needs to be reduced. This reduction can be accomplished by reducing the source of contamination and exploration of extreme growth conditions which reduce the incorporation of these contaminants. Newly available bulk substrates with low threading dislocations allow for better study of material properties, as opposed to material whose properties are dominated by structural and chemical defects. In addition, very thick films can be grown without cracking due to exact lattice and thermal expansion coefficient match. Through chemical and electrical measurements, this work aims to find growth conditions which reduces contamination without a severe impact on growth rate, which is an important factor from an industry standpoint. The proposed thicknesses of these devices are on the order of one hundred microns and requires tight control of the intentional dopants.Doctor of Philosophy
GaN is a compound semiconductor which has the potential to revolutionize the high power electronics industry, enabling new applications and energy savings due to its inherent material properties. However, material quality and purity requires improvement. This improvement can be accomplished by reducing contamination and growing under extreme conditions. Newly available bulk substrates with low defects allow for better study of material properties. In addition, very thick films can be grown without cracking on these substrates due to exact lattice and thermal expansion coefficient match. Through chemical and electrical measurements, this work aims to find optimal growth conditions for high purity GaN without a severe impact on growth rate, which is an important factor from an industry standpoint. The proposed thicknesses of these devices are on the order of one hundred microns and requires tight control of impurities.
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Ogbu, Chidiebere. "Peroxide Sensing Using Nitrogen-Doped and Platinum Nanoparticle-modified Screen-Printed Carbon Electrodes." Digital Commons @ East Tennessee State University, 2019. https://dc.etsu.edu/etd/3622.
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Nitrogen-doped carbon materials have garnered much interest due to their abilities to behave as electrocatalysts for reactions important in energy production (oxygen reduction) and biosensing (hydrogen peroxide reduction). Here, we demonstrate fabrication methods and determine electrocatalytic properties of nitrogen-doped screen-printed carbon (N-SPCE) electrodes. Nitrogen doping of graphite was achieved through a simple soft-nitriding technique which was then used in lab-formulated screen-printing inks to prepare N-SPCEs. N-SPCEs displayed good electrocatalytic activity, reproducibility and long term stability towards the electrochemical reduction of hydrogen peroxide. N-SPCEs exhibited a wide linear range (20 µM to 5.3 mM), reasonable limit of detection of 2.5 µM, with an applied potential of -0.4 V (vs. Ag/AgCl). We also demonstrate that nitrided-graphite can similarly be used as a platform for the deposition of electrocatalytic platinum nanoparticles, resulting in Pt-N-SPCEs with a lower limit of detection (0.4 µM) and better sensitivity (0.52 µA cm-2 µM-1) towards H2O2 reduction.
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Davies, Sean. "In-situ optical monitoring of growth processes during the carbon doping and nitridation of GaAs in CBE." Thesis, University of Liverpool, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.399266.
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HINOJOSA, PAOLA ALEXANDRA AYALA. "IMPLICATIONS OF THE C/N FEEDSTOCK ON CONTROLLING THE NITROGEN DOPING AND BONDING ENVIRONMENT IN CARBON NANOTUBES." PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO, 2007. http://www.maxwell.vrac.puc-rio.br/Busca_etds.php?strSecao=resultado&nrSeq=10399@1.
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CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICOOs tópicos mais importantes a ser tratados nesta tese de doutorado são os vários problemas envolvidos na síntese de nanotubos contendo nitrogênio. Isto é principalmente motivado pelas possíveis aplicações que podem ser dadas a este tipo de estruturas. A motivação central está relacionada ao fato da possibilidade de fazer dopagens tipo -p e -n em nanotubos de carbono, incorporando átomos como boro ou nitrogênio. Isto está muito longe de ser uma trivialidade devido a que devemos levar em conta que se os nanotubos de carbono forem pensados como bases estruturais para nanocompósitos e dispositivos nanoeletronicos, é necessário controlar cuidadosamente a reatividade das paredes, sua dureza mecânica e o gap eletrônico por meio de um controle da quantidade de átomos inseridos nas paredes ou entre elas. Portanto, do ponto de vista de diferentes aplicações, é importante ter a possibilidade de dopar controladamente os nanotubos. Neste trabalho apresentam-se o quadro descritivo da dependência dos parâmetros de síntese, assim como uma investigação detalhada da formação de outras estruturas co-produto do processo de formação de nanotubos. Como uma idéia pioneira proposta neste trabalho, é enfatizado o uso de fontes puras de C/N em processos de síntese baseados em deposição química na fase de vapor. Desta maneira foi possivel determinar os efeitos da atmosfera de reação e o pretratamento do catalizador como agentes favoráveis ou desfavoráveis para a síntese efetiva de nanotubos de carbono.
The main topic of this thesis is the study of various issues related to the synthesis of nitrogen containing nanotubes. This is mainly inspired in the possible applications such structures can have. The practical background lies in the fact that defined n- and p-doping of carbon nanotubes can be achieved by substituting carbon atoms from the tube walls by heteroatoms such as boron or nitrogen (N). This is far from been a triviality because we must keep in mind that if carbon nanotubes are to be used as future building blocks in nanocomposites and nanoelectronic devices, it is imperative to fine tune their wall reactivity, mechanical strength and electronic band gap by controlling the amount of foreign atoms inserted into the tube lattices. Therefore, from an applications standpoint, it is important to be able to carefully control the insertion of different dopants into nanotubes. In this work, a complete picture of the dependence on the combined synthesis parameters is established and a fundamental insight into the formation of N doped nanotubes and other structures (co- products) is provided. As a pioneering idea of this whole work, the use of pure C/N feedstocks in chemical vapor deposition methods is emphasized. With this, it was possible to determine the effects of the reaction atmosphere and the catalyst pretreatment as either favoring or disfavoring agents towards the synthesis of N-doped nanotubes.
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Haugen, Neale O. "Spectroscopic Studies of Doping and Charge Transfer in Single Walled Carbon Nanotubes and Lead Sulfide Quantum Dots." University of Toledo / OhioLINK, 2015. http://rave.ohiolink.edu/etdc/view?acc_num=toledo1438768843.
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Al, abboodi Mohammed Halool. "ELECTRONIC AND VIBRATIONAL PROPERTIES OF SINGLE WALL CARBON NANOTUBES AND BORON NITRIDE NANOTUBES IN THE PRESENCE OF VARIOUS IMPURITIES." OpenSIUC, 2015. https://opensiuc.lib.siu.edu/theses/1672.
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The major objective of this thesis is to systematically investigate the effect of hexagonal BN (h-BN) islands on electronic and vibrational properties of single wall carbon Nanotubes. All our investigation are based on first principle Density Functional Theory (DFT) calculations. Our study is motivated by interesting metal-semiconductor transition recently found in periodically patterned graphene with h-BN islands. After reproducing the electronic band structure for pristine single wall zigzag carbon nanotubes (which shows metallic or semiconducting properties depending on their chirality), we investigated their electronic band structure in the presence of h-BN islands. The band structure depends not only on the defect concentration, but also on the pattern of the defect atoms. Our results also suggest that, if we start with a metallic /semiconducting mixture of ZSWCNTs, upon h-BN addition, the sample converts to fully semiconducting. This is a promising result for applications of CNTs in molecular electronics. Fundamental understanding of vibrational properties of nano electronics component is equally important in their applications especially in thermal management and thermoelectric applications. Defect engineering is one of the potential approach for tuning nanoelectronic devices for optimal thermal management and thermoelectric devices. In this work, I present a systematic investigation on how the group velocity and frequency of different phonon modes depend on various h-BN defect concentrations and defect patterns in ZSWCNTs. The study was extended to investigate the effect of hexagonal-C defects on the electronic and vibrational properties of zigzag single wall Boron Nitride nanotubes (ZSWBNNTs).
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Silva, Lucas Barboza Sarno da. "Otimização das propriedades de transporte em supercondutores de MgB2 com a adição de compostos de estrutura cristalina tipo AlB2 e fontes distintas de carbono." Universidade de São Paulo, 2013. http://www.teses.usp.br/teses/disponiveis/97/97135/tde-08102013-085005/.
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Em Janeiro de 2001, um supercondutor totalmente novo foi apresentado por Nagamatsu, o diboreto de magnésio (MgB2), com uma temperatura crítica, Tc, surpreendentemente alta de 39 K. Atualmente, o MgB2 é considerado o condutor de alto campo do futuro. É claramente aceito que os valores excepcionais de altos campos magnético crítico superior, Hc2, (Hc2 + (0) ? 40 T para Tc ? 35 - 40 K) mostram que o MgB2 é capaz de substituir o Nb3Sn (Hc2 (0) ? 30 T para Tc ? 18 K) como a escolha para aplicações de altos campos magnéticos. Neste trabalho foram preparadas pastilhas supercondutoras de MgB2 utilizando adições de diboretos metálicos de ZrB2, TaB2, VB2 e AlB2 e adições simultâneas de diboretos metálicos e fontes diversas de carbono, como carbeto de silício, grafite e nanotubos de carbono. O objetivo da adição desses novos elementos foi criar mecanismos para melhorar a capacidade de transporte do material, tanto pela dopagem substitucional como pela geração de defeitos na matriz supercondutora, atuando como eficientes centros de aprisionamento das linhas de fluxo magnético. Para isso foram utilizados dois diferentes métodos de preparação de amostras, insitu e ex-situ. O método de preparação in-situ seguiu padrões convencionais, como mistura em moinho de bola e tratamento térmico em fluxo de argônio. Para a preparação das amostras utilizando-se o método ex-situ foram utilizadas técnicas mais sofisticadas, como moagem de alta energia e tratamento térmico em altas pressões (Hot Isostatic Press, HIP). Em geral, as adições dos diboretos metálicos melhoraram a capacidade de transporte do material em baixos campos, as fontes de carbono aumentaram os valores de densidade de corrente crítica em altos campos magnéticos, enquanto que as combinações das duas adições melhoram a capacidade de transporte, para algumas amostras, em toda a faixa de campo magnético medida.In January 2001, a new superconductor was presented by Nagamatsu, the magnesium diboride (MgB2), with a critical temperature, Tc, extremely high of 39 K. MgB2 is considered the high field conductor of the future. The exceptional high values of upper critical magnetic field, Hc2, (Hc2 + (0) ? 40 T for Tc ? 35 - 40 K) show that the MgB2 is able to replace the Nb3Sn (Hc2 (0) ? 30 T for Tc ? 18 K) as the choice for applications in high magnetic fields. In this work, superconducting pellets of MgB2 were prepared with addition of other metal diborides of ZrB2, TaB2, VB2, and AlB2, and simultaneous additions of metal diborides and different carbon sources, such as silicon carbide, graphite and carbon nanotubes. The objective of these additions of new elements was to create mechanisms to improve the transport capacity of the material, by substitutional doping and by generation of defects in the superconducting matrix, acting as effective pinning centers of magnetic flux lines. Two different methods for sample preparation were used, the in-situ and the ex-situ method. The in-situ preparation method followed conventional standards, such as powder mixing in a ball mill and heat treatment in argon flow. The ex-situ preparation method used more sophisticated techniques, such as high energy ball milling and heat treatment under high pressures (Hot Isostatic Press, HIP). In general, the additions of metal diborides improved the transport capacity of the material at low fields, the carbon sources increased the critical current density at high magnetic fields, whereas the combination of these two additions improved the transport capacity, for some samples, in all range of applied magnetic field.
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Solmi, Matilde Valeria. "Sintesi e caratterizzazione di carboni per applicazioni in catalisi." Master's thesis, Alma Mater Studiorum - Università di Bologna, 2015. http://amslaurea.unibo.it/9014/.
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I materiali a base di carbone vengono utilizzati in catalisi come supporti per fasi attive, ma anche direttamente come catalizzatori essi stessi, grazie soprattutto alla versatilità delle loro proprietà di massa e superficiali. L’attività catalitica dei carboni è influenzata soprattutto dalla natura, dalla concentrazione e dall’accessibilità dei siti attivi tra cui i più comuni sono: gruppi funzionali superficiali, difetti, ed eteroatomi inseriti nella struttura. Per ridurre i problemi diffusionali legati alla microporosità dei carboni attivi sono in corso numerosi studi sulla sintesi di carboni mesoporosi, i quali possono fornire benefici unici come alta area superficiale ed elevato volume dei pori, uniti a buone proprietà chimiche e stabilità meccanica. Nel corso di questa tesi, sono state svolte diverse attività finalizzate principalmente alla preparazione e alla caratterizzazione di carboni mesoporosi da utilizzare in ambito catalitico. La sintesi di carboni porosi è stata eseguita con la metodologia soft-templating, un metodo basato sulla replica di un agente templante polimerico che si organizza in micelle attorno alle quali avviene la reticolazione di un precursore polimerico termoindurente. Precursore e templante vengono pirolizzati ad elevate temperature per rimuovere in un primo momento l’agente templante e successivamente carbonizzare il precursore.
Sono state scelte due metodologie di sintesi riportate in letteratura con lo scopo di sintetizzare due tipologie di carboni. La sintesi Mayes è stata utilizzata per sintetizzare carboni mesoporosi classici, mentre la sintesi Hao è stata utilizzata per ottenere carboni porosi contenenti azoto. Le due sintesi sono state ottimizzate variando diversi parametri, tra cui il tempo di reticolazione (curing) e la temperatura di pirolisi.
Sui diversi carboni ottenuti sono stati effettuati alcuni trattamenti superficiali di ossidazione al fine di modificarne la funzionalità. In particolare si sono utilizzati agenti ossidanti come HNO3, H2O2 e N2O.
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Oishi, Silvia Sizuka [UNESP]. "Síntese, dopagem e caracterização das resinas furfurílica e fenol-furfurílica visando a otimização do processamento de carbono vítreo." Universidade Estadual Paulista (UNESP), 2009. http://hdl.handle.net/11449/94398.
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Em função da crescente importância do material carbono vítreo em áreas estratégicas, devido às suas características intrínsecas, tais como menor massa específica e bons valores de condutividades térmica e elétrica, tem se observado vários estudos na busca de novos precursores poliméricos, assim como no ajuste mais sistemático de seu processamento. Nesse sentido, este trabalho tem como objetivo o estabelecimento de rotas de síntese de resinas furfurílica e fenol-furfurílica e suas dopagens com partículas de cobre, visando o processamento de eletrodos de carbono vítreo reticulado (CVR). Neste contexto foram sintetizadas diferentes formulações de resinas furfurílica e fenol-furfurílica a partir da variação dos monômeros – álcool furfurílico, fenol e formaldeído, respectivamente. A confirmação do sucesso das sínteses foi realizada por análises de espectroscopia de infravermelho com transformada de Fourier, cromatografia gasosa, análises térmicas por calorimetria exploratória diferencial e medidas dos teores de carbono fixo, que mostram resultados entre 27 e 45% em carbono. Em seguida, estas amostras foram dopadas com um colóide contendo as partículas de cobre. As resinas, com e sem dopagem, foram catalisadas, impregnadas em espumas de poliuretano (PU) e carbonizadas, obtendo-se assim, o CVR. Análises por microscopias óptica e eletrônica de varredura mostram a homogeneidade na impregnação das espumas de PU e a textura uniforme das amostras de CVR. Os resultados de resistência à compressão apresentam os melhores valores para o CVR resultante da carbonização com a resina furfurílica ácida (0,55 MPa).
Due to the growing importance of glassy carbon material in strategic areas, due to its intrinsic characteristics, such as lower density and good thermal and electrical conductivities values, has been observed several studies looking for new polymeric precursors and tighter processing parameters. In this way, this study aims on the establishment of synthesis routes of furfuryl and phenol-furfuryl alcohol resins and their doping with cupper particles, in order to produce reticulated glassy carbon (RGC) electrodes. Inside of this context were synthesized different formulations of furfuryl and phenol-furfuryl alcohol resins by the monomers variation – furfuryl alcohol, phenol and formaldehyde, respectively. The success confirmation of the synthesis has been done by using FT-IR spectroscopy, gas chromatography, thermal analyses by differential scanning calorimetry (DSC) and carbon yield content measurements that present results between 27 and 45% of carbon. After this, the specimens were doped with a colloid contend the copper particles. The doped and non doped resins were catalyzed, impregnated in polyuretane (PU) foams and carbonized, in order to obtain the reticulated glassy carbon. Optical and Scanning Electron Microscopy analysis show the homogeneity of PU foams impregnation and uniform texture of RGC specimens. Compression results present the best values for RGC resulting from the carbonization with furfuryl alcohol acid resin (0,55 MPa).
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Shcherbakova, Olga V. "Development of MgB₂-xCx superconductors and understanding their electromagnetic behaviour." Institute for Superconducting and Electronic Materials - Faculty of Engineering, 2008. http://ro.uow.edu.au/theses/11.
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Discovered in 2001, magnesium diboride (MgB2) is the latest superconductor suitable for large scale applications (magnetic resonance imaging systems (MRI), fault current limiters (FCL), high-field magnets). Compared to other metallic superconductors like NbTi (Tc = 9 K) and Nb3Sn (Tc = 18 K), it has the advantage of a higher critical temperature (Tc = 39 K), which enables its application at the temperature of 20 K and, hence, significantly reduces the cost of the cooling system. This, together with the abundance of the magnesium and boron raw materials, as well as the relatively simple fabrication of MgB2 wires and tapes, has motivated the active investigation and study of this superconductor by many research groups all over the world. As a result, a significant breakthrough for application of MgB2 conductors at high fields has been made with introduction of carbon into the crystal lattice of MgB2 via chemical doping. The main focus of this work was on the study of the microstructural and superconducting properties of MgB2-xCx superconductors and establishing correlations between them. To obtain MgB2-x Cx compounds with different characteristics, various C-based doping materials and processing parameters were employed. The systematic study of the microstructural and superconducting properties of MgB2-x Cx samples conducted in this work allowed us: (i) to predict suitable dopants for MgB2; (ii) to improve chemical doping by carbon; (iii) to identify the relevant negative microstructural factors and estimate their effects on limitation of the current-carrying ability in MgB2-xCx samples. The results described in this work can be used as a guide for the achievement of the characteristics required for practical applications of MgB2 superconductors. Investigation of the properties of MgB2-xCx superconductors as a function of the processing parameters showed that the doping level, sintering temperature, and cooling time control the density of pinning centers in MgB2-xCx, and affect the connectivity of grains and transparency of grain boundaries to current flow. Analysis of the pinning mechanism in the samples studied has led to establishing that the dominant pinning is on grain boundaries in the pure MgB2 samples, and on grain boundaries and crystal lattice defects in the MgB2-xCx samples. To demonstrate the effect of the pinning environment on the current-carrying ability in MgB2-xCx superconductors, a comparative study of the microstructural and superconducting properties for pure, nano SiC-, and C-doped MgB2 wires was carried out. In both SiC- and C-doped samples carbon substitution into the MgB2 crystal lattice results in the enhancement of the upper critical field, Bc2. However, it was revealed that the presence of SiC dopant allowed carbon substitution and MgB2 formation to take place simultaneously at low temperatures. Therefore, the microstructure of this SiC-doped sample assures maximal density of pinning centers (large number of grain boundaries, i.e. small grain sizes, and crystal lattice defects) and enhances pinning. These factors (higher Bc2 value and stronger pinning) are responsible for the superior enhancement in critical current density at relatively high fields in the SiC-doped sample. In contrast, for C-doping, higher processing temperatures are required for generation of a dense network of crystal lattice defects. In this case, the microstructure consists of larger grains, and the pinning on smaller number of grain boundaries becomes weaker, reducing the total pinning force and critical current density. An important outcome of this study was the establishment of the dual reaction model (simultaneous formation of MgB2 compound and C substitution into the lattice), which enables us to predict desirable dopants for enhancing the properties of MgB2. These should be C-based compounds which decompose, producing highly reactive C at temperatures below the temperature of MgB2 formation. Ideally, dopants should be homogeneously distributed within host the Mg and B powders and not contaminate grain boundaries in formed MgB2. The liquid mixing approach, a new advanced and at the same time simplified approach to chemical doping of MgB2 superconductor with carbon, was found to partially fulfill these requirements. Carbohydrates (sugar and malic acid) and polycarbosilane (a polymer analog to nano SiC-doping) were employed as doping materials. Liquid mixing has been shown to coat each individual nano sized boron powder particle with a nano-layer of amorphous carbon. Fresh unpassivated carbon extracted from carbohydrates or polycarbosilane easily incorporates itself into the MgB2 crystal lattice. This enhanced incorporation promoted by the maximal reaction surface assured by coating generates microstructure with a dense network of pinning sites and results in significant improvement of the superconducting properties in MgB2-xCx material. The results observed suggest that sugar as a dopant exhibits a stronger potential for practical application of MgB2 superconductor in the high field region than nano carbon doping. Similarly, stronger enhancement of superconducting properties was observed in polycarbosilane-doped MgB2 compared to nano SiC doping. The latter was ascribed to the formation of a microstructure with Mg2Si impurity phases mainly distributed within superconducting MgB2 grains. In this case, transparency of grain boundaries was likely improved, which resulted in the observed enhancement of critical current density over the entire field range. Systematic analysis of the microstructures and superconducting properties of sugar-, malic acid-, and polycarbosilane-doped MgB2 samples demonstrated that the critical current density was also significantly affected by the microstructural properties in the low field region. The results observed led to the development of a model, which allowed us to estimate the level of critical current density (Jc) limitation due to the microstructural features of pure and C-doped MgB2 samples. This model is based on the identification of individual contributions by various defects to critical current density limitation. These defects in the MgB2 microstructure include porosity and non-superconducting phase inclusions (so-called “geometrical” defects), as well as the connectivity and transparency of grain boundaries. The results observed showed that a higher level of “geometrical” defects results in stronger limitation of critical current flow through the sample and lower measured Jc values. The elimination of the “geometrical” defects would result in critical current densities that are a factor of 1.5 - 2 higher than currently measured values. The role of grain boundaries connectivity was found to be even more dramatic. For samples with fully connected grains, the estimated critical current densities were about one order of magnitude higher than the measured values. Moreover, the results of analysis showed that the low field Jc values are mainly determined by the connectivity and transparency of grain boundaries, while in field Jc(Ba) performance is affected by these defects in the microstructure to a lesser extent, and its behaviour is mainly determined by the pinning environment in the samples. It also was observed that while a denser pinning network favors in field Jc(Ba) behaviour, this results in reduction of grain boundary transparency and more pronounced critical current density limitation in the low field region.
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Bhagurkar, Ashutosh. "Processing of MgB2 bulk superconductor by infiltration and growth." Thesis, Brunel University, 2017. http://bura.brunel.ac.uk/handle/2438/14777.
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Superconductivity in magnesium diboride (MgB2) was discovered in 2001. The relatively high Tc (39 K), high critical current density, long coherence length (∼6 nm), low raw material cost, lower density and relative ease of fabrication make this material an exciting choice for practical applications. Furthermore, lower anisotropy and strongly linked current flow in untextured polycrystalline samples, unlike its HTS counterparts, has enabled the development of different processing routes to fabricate MgB2 in the form of wires, tapes, thin films and bulks. Conventionally, MgB2 is synthesized by in situ sintering, where elemental Mg and B powders are reacted to produce MgB2. Although the superconducting phase can be obtained with relative ease, the resulting sample is generally only around 50% dense, due to formation of large pores inside sintered bulks arising from the volatility of magnesium and 25% volume contraction in MgB2 phase formation. Although the use of high pressure is effective to promote sintering and subsequent densification, the need to use large pressure vessels represents a significant practical limitation for the development of a practical process and of the achievable dimensions in the final MgB2 sample. As a result, the fabrication of high density, bulk MgB2 remains a challenging processing problem. This study explores the “Infiltration and Growth” (IG) technique, an established processing route for fabrication of dense ceramics/ceramic matrix composites, as a potential solution. Boron powders of varying characteristics were infiltrated with Mg(l) to obtain bulk MgB2 samples. The samples were analysed using techniques such as XRD, SEM and hardness to analyse various phases formed during the process. These samples typically contained MgB2 with minor quantities of Mg. Physical properties of superconducting MgB2, such as Tc, Jc and Hc2, were established. Furthermore, the effective current carrying cross-section was estimated from resistivity measurements using Rowel’s analysis. Continuous Mg channels were major defects in IG processed samples and their presence was found to limit long range current flow. These channels are eliminated by incorporating Mg/AlB2/MgB2 powders in the precursor to facilitate in-flux of Mg, leading to a more uniform infiltration process, thereby enabling fabrication of near-net shaped MgB2 bulk superconductors. Such samples showed an almost identical value of trapped magnetic flux at the top and bottom surfaces, suggesting a high degree of uniformity in MgB2. A careful microstructural analysis of a series of samples indicated that MgB2 phase formation in IG process occurred in three distinct stages: (1) Intermediate boride formation (2) Bulk liquid Mg infiltration and (3) MgB2 layer formation. Due to volume expansion involved in stage 1, cracks formed in the β-Boron particles and propagated radially inwards during stage 3. The growing MgB2 particles sintered simultaneously with the formation of grain boundaries during the process. Much enhanced performance of MgB2 was achieved by virtue of C-doping. Increased Jc was attributed to generation of lattice strains and loss of crystallinity in MgB2 as a result of C-doping. Finally, trapped field measurements were performed on homogeneous C-doped MgB2 bulks. The trapped field obtained (4.13 T) in five stacked of bulks is the highest obtained in MgB2 bulks synthesized under ambient pressure conditions.
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Skipa, Tetyana. "Modification of the electronic properties of carbon nanotubes by bundling, temperature, B- and N-doping a resonance Raman study /." Karlsruhe : Forschungszentrum Karlsruhe, 2006. http://d-nb.info/983613184/34.
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Hsieh, Yu-Yun. "Nanostructured Carbon-Based Composites for Energy Storage and Thermoelectric Applications." University of Cincinnati / OhioLINK, 2019. http://rave.ohiolink.edu/etdc/view?acc_num=ucin157322525150617.
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Tran, Hoang Anh. "One-Dimensional Nanostructure and Sensing Applications: Tin Dioxide Nanowires and Carbon Nanotubes." PDXScholar, 2016. http://pdxscholar.library.pdx.edu/open_access_etds/2689.
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The key challenge for a nanomaterial based sensor is how to synthesize in bulk quantity and fabricate an actual device with insightful understanding of operational mechanisms during performance. I report here effective, controllable methods that exploit the concepts of the "green approach" to synthesize two different one-dimensional nanostructures, including tin oxide nanowires and carbon nanotubes. The syntheses are followed by product characterization and sensing device fabrications as well as sensor performance understanding at the molecular level. Sensor-analyte response and recovery kinetics are also presented.
The first part of the thesis describes bulk-scale synthesis and characterization of tin oxide nanowires by the molten salt synthetic method and the nanowire doping with antimony (n-types) and lithium. The work builds on the success of using n-doped SnO2 nanoparticles to selectively detect chlorine gas at room temperature. Replacing n-doped nanoparticles with n-doped nanowires reduces the number of inter-particle electron hops between sensing electrodes. The nanowire based sensors show unprecedented 5 ppb detectability of corrosive Cl2 gas concentration in air. At the higher range, 10 ppm of Cl2 gas leads to a 250 fold increase in the device resistance. During sensor recovery, FT-IR studies show that dichlorine monoxide (Cl2O) and chlorine dioxide (ClO2) are the desorbing species. Long term stability of devices is affected by lattice oxygen vacancies replaced by chlorine atoms.
Bulk-scale synthesis of multiwall carbon nanotube (MWCNTs) was achieved by a novel inexpensive synthetic method. The green chemistry method uses the non-toxic and easy to handle solid carbon source naphthalene. The synthesis is carried out by simply heating naphthalene and organometallic precursors as catalysts in a sealed glass tube. Synthesis at 610º C leads to MWCNTs of 50 nm diameter and lengths exceeding well over microns. MWCNT doping is attempted with nitrogen (n-type) and boron (p-type) precursors. Palladium nanoparticles decorated on as-synthesized MWCNTs are employed for specific detection of explosive hydrogen gas with concentrations far below the explosive concentration limits. During performance, the sensor exhibits abnormal response behaviors at hydrogen gas concentrations higher than 1%. A model of charge carrier inversion, brought about by reduction of MWCNT by hydrogen molecules dissociated by Pd nanoparticles is proposed.
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Bourke, Jared. "Preparation and Properties of Natural, Demineralized, Pure, and Doped Carbons from Biomass; Model of the Chemical Structure of Carbonized Charcoal." The University of Waikato, 2007. http://hdl.handle.net/10289/2330.
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Pioneering work performed by Rosalind Franklin over half a century ago provided the first structural models of two distinct carbon types: those that become graphitic during carbonization at high temperatures, and those that do not. Moreover it is known that certain properties of carbonaceous materials including combustion, surface area, electrical resistivity, and catalytic properties are influenced by mineral impurities. The nature of this division in biocarbon structure and the known effects of minerals on carbon properties have led to this work; three principal topics were addressed; (1) the investigation of the solid state structure of biocarbons derived from various biomass feedstocks, (2) the removal of inorganic minerals from biomass, and (3) the investigation of biocarbon electronic structure subsequent to doping with select inorganic minerals. Charcoals and carbonized charcoals (i.e. biocarbons) were prepared from a wide variety of biomass substrates, including pure sugars containing 5- and 6-membered rings with furanose and pyranose configurations, lignin, agricultural residues (corncob and nut shells) and a hard wood. These biocarbons were subject to proximate and elemental analysis, gas sorption analysis, and analysis by ICP-MS, SEM, XRD, ESR, 13C CPMAS NMR, and MALDI-TOF MS. All the carbonized charcoals contained oxygen heteroatoms, had high surface areas, and were excellent conductors of electricity. Doping the biocarbon with boron or phosphorus resulted in a slight improvement in its electrical conductivity. The XRD analysis indicated that the carbonized charcoals possess an aromaticity of about 71% that results from graphite crystallites with an average size of about 20 . The NMR analysis confirmed the highly aromatic content of the carbonized charcoals. The ESR signals indicated two major types of carbon-centered organic radicals. A number of techniques employed highlighted differences between carbonized charcoals and synthetic graphite but none more so than MALDI-TOF spectrometry. The biocarbons contained readily desorbed discrete ions with m/z values of 701, 685, 465, 453, 429, and 317. All of the above findings were used to develop a model for the structure of carbonized charcoal that is consistent with the biocarbon's oxygen content, microporosity and surface area, electrical conductivity, radical content, and its MALDI-TOF spectra. The removal of inorganic mineral constituents from various biomass feedstocks was achieved via simple washing/soaking techniques using two different aqueous media; deionized water and citric acid. The most effective and consistent demineralization treatment for removing minerals from biomass involved a hot 0.1 molL-1 citric acid percolation treatment, ca. 67% of inorganic mineral matter was removed. Mineral matter at the levels present in typical biomass derived charcoals and carbons had no significant influence upon the surface area or the electrical resistivity in carbonaceous materials after high heat treatment (950 C).
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Guazzagaloppa, Jérémy. "Matériaux super-isolants thermiques à propriétés thermoélectriques intégrées." Thesis, Montpellier, 2019. http://www.theses.fr/2019MONTS086.
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Dans le cadre du développement de nouvelles sources d’énergie durables, la récupération d'énergie est essentielle. La plupart des processus industriels entraînent une perte colossale de chaleur, la thermoélectricité a donc pleinement son rôle à jouer dans ce développement grâce à l'effet Seebeck qui consiste à convertir un gradient de température en énergie électrique. Un bon matériau thermoélectrique nécessite une conductivité électrique σ élevée, un grand coefficient Seebeck α ainsi qu'une conductivité thermique λ faible. Cependant, malgré de récentes avancées dans le domaine, l’utilisation en masse des matériaux thermoélectriques usuels devient difficile du fait de leur toxicité, leur faible abondance et leur coût. Le développement de nouveaux matériaux en respect des contraintes environnementales devient alors nécessaire. Ainsi, avec l’émergence d’une nouvelle famille de matériaux, à savoir les matériaux organiques thermoélectriques, à base de polymères conducteurs et de gels (aérogels/xérogels), de nouvelles perspectives sont envisageables. A l’instar de ces nouvelles avancées, le but de ce travail est de fonctionnaliser des matériaux super-isolants thermiques possédant une très faible conductivité thermique en leur conférant des propriétés thermoélectriques. Cela a d’abord été réalisé par des simulations numériques basées sur la théorie de la fonctionnelle de la densité (DFT), ainsi que sur la dynamique moléculaire classique (DM), via différents modules appartenant au logiciel Materials Studio. Cela a permis de représenter numériquement et valider la structure de notre matériau, le xérogel de Résorcinol/Formaldéhyde. Une étude de dopage avec 5 % en particules de fer a ensuite été réalisée en DM afin d’étudier la dispersion des charges au sein du réseau RF et représenter le numériquement le matériau dopé en vue d’une future étude de ses propriétés thermoélectriques.Dans un second temps, l’objectif a été de définir le protocole de synthèse optimal en fonction des différents paramètres de synthèse et des différentes charges conductrices utilisées. L’étude de l’influence d’un traitement thermique par pyrolyse a alors permis l’amélioration de la conductivité électrique du matériau pur présentant un facteur de mérite ZT=2.7×〖10〗^(-16), (ZT=α^2 σT/λ permet de quantifier le rendement de la conversion thermoélectrique). Des dopages ont par la suite été effectués durant l’étape de gélification suivant différents taux de charge en vue d’atteindre un seuil de percolation. Un facteur de mérite ZT=2.4×〖10〗^(-3) a alors été obtenu avec un taux de dopage de 60 % en oxyde de graphène (GO). Cependant, ce type de dopant engendre un coût de synthèse trop important, nous nous sommes alors orientés vers d’autres types de charges, à savoir des fibres conductrices. Ceci a permis d’obtenir un ZT= 8.0×〖10〗^(-4) avec un taux de dopage de 10 % en fibres de polyacrylonitrile oxydée (PANOX). L’assemblage du module ainsi que la réalisation d’un banc d’essais ont par la suite permis de caractériser la performance thermoélectrique de nos différents matériaux. Une densité de puissance de l’ordre de 2 mW.m-2 a alors été obtenue avec le xérogel RF fibré PANOX d’une épaisseur de 1 cm et d’une surface de 50 cm² pour une différence de température de 30°C. Ce matériau a alors permis d’identifier une application dans le cadre de l’isolation thermique d’une batterie de véhicule hybride en vue de détecter une défaillance associée à la perte du vide. Finalement une étude se basant sur des modèles théoriques a démontré l’intérêt de poursuivre les recherches dans le but d’améliorer les propriétés thermoélectriques. Nous avons alors envisagé l’assemblage de modules composés de 1000 jonctions (p-p) puis (n-p) avec des matériaux cibles afin d’atteindre des niveaux de densité de puissance de plusieurs W.m-2 et des tensions de sortie de plusieurs V permettant de produire suffisamment d’énergie pour l’alimentation d’auxiliaires tels que des capteurs par exempleIn the search of new sustainable energies, the issue of energy harvesting is essential. Heat loss is involved in most of the industrial processes, thus thermoelectricity has its full role to play in this search through the Seebeck effect which consists in converting a temperature gradient into an electrical current. A good thermoelectric material requires a high electrical conductivity σ and Seebeck coefficient α and a low thermal conductivity λ. However, despite recent advances in the field, the use of conventional thermoelectric materials on a large scale becomes difficult due to their toxicity, low abundance and high cost. The development of new materials that respect environmental considerations has thus become necessary. Hence, with the emergence of a new family of materials, namely organic thermoelectric materials, based on conductive polymers and gels (aerogels/xerogels), new perspectives are now possible. In the frame of these new advances, the aim of this work is to functionalize thermal super-insulating materials with a very low thermal conductivity by adding thermoelectric properties. This was first done by numerical simulations based on density functional theory (DFT) and classical molecular dynamics (MD), via different modules included in the Materials Studio software. This allowed us to numerically represent and validate the structure of our thermal insulating material, the Resorcinol/Formaldehyde (RF) xerogel. A doping process with 5 % in iron particles was then performed using MD calculations in order to evaluate the dispersion of the charges within the RF network and to represent numerically the doped material for a future study of its thermoelectric properties via a Boltzmann formalism.In a second step, the objective was to identify the optimal synthesis protocol as a function of the different synthesis parameters and the different conductive dopants. The study of the influence of a thermal treatment by pyrolysis then allowed the improvement of the electrical conductivity of the pure material having a very low figure of merit ZT=2.7×〖10〗^(-16), (ZT=α^2 σT/λ is a measure of the efficiency of the thermoelectric conversion). A study of doping was then carried out during the gelling process according to different loading rates in order to reach a percolation threshold. A figure of merit ZT=2.4×〖10〗^(-3) was then obtained with a doping level of 60 % in graphene oxide (GO). However, this type of dopant generates a very high synthesis cost, which explain why we investigated other types of charges, namely electrically conductive fibers. In that case, we obtained a ZT= 8.0×〖10〗^(-4) with a doping level of 10 % in oxidized polyacrylonitrile fibers (PANOX). The assembly of the module and the realization of a test bench have made it possible to characterize the thermoelectric performance of our different materials. A power density of the order of 2 mW.m-2 was then obtained with the PANOX fiber-reinforced RF xerogel with a thickness of 1 cm and an surface area of 50 cm² for a temperature difference of 30°C. Thanks to this materials, we have identified an application as part of the thermal insulation of a hybrid vehicle battery in order to detect a failure associated with a vacuum loss. Finally, a study based on theoretical models has shown the interest of continuing research activities in order to improve the thermoelectric properties. We then considered the assembly of modules composed of 1000 junctions (pp) then (np) with target materials in order to reach higher power density levels of several W.m-2 and output voltages of several V to produce enough energy for the supply of auxiliaries such as sensors for example
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Yeghoyan, Taguhi. "Dépôt de silicium polycristallin contenant du carbone pour des applications radiofréquence." Thesis, Lyon, 2019. http://www.theses.fr/2019LYSE1059.
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Pour les futures applications en télécommunications 5G, des substrats à base de silicium présentant une faible perte de signal et une excellente linéarité sont nécessaires. Parmi les solutions envisagées, la technologie RF-SOI est la plus avancée. Son empilement contient une couche de Haute Résistivité (HR), riche en pièges pour les porteurs de charges, composée de silicium polycristallin (poly-Si) de haute pureté déposée sur l’oxyde natif d'un substrat HR (HR-Si). Ce système présente certaines limitations provenant essentiellement de l'interface HR-Si/SiO2 et de sa stabilité thermique, mais également de la résistivité insuffisante de la couche riche en pièges. L'objectif principal de cette thèse était d'explorer des approches innovantes pour résoudre ces difficultés tout en restant compatible avec la technologie silicium. Afin d’atteindre ces objectifs, du carbone a été ajouté dans le système au cours des différentes étapes d'élaboration: i) remplacement de la couche interfaciale de SiO2 par une couche mince de 3C-SiC et ii) ajout de carbone pendant le dépôt de poly-Si.En utilisant la technique de dépôt chimique en phase vapeur à pression atmosphérique, des couches HR de poly-Si à l'état de l'art ont été déposée sur oxyde natif avec une épaisseur pouvant aller jusqu'à quelques dizaines de µm. Les résultats ont montré que la résistivité de la couche de poly-Si n'était pas directement dépendante de la taille moyenne des grains. Le remplacement de l'oxyde interfacial par une couche mince de mono- ou de poly-SiC, ainsi que l'adaptation des conditions de croissance ont permis d'atteindre des propriétés équivalentes à l'état de l'art des couches HR de poly-Si. Cet empilement a l'avantage d'être plus stable thermiquement en évitant la dissolution de la couche interfaciale. Cependant, ces améliorations sont accompagnées d’une chute de la résistivité à l’interface attribuée à la conductivité importante du matériau SiC. Par ailleurs, les propriétés de la couche HR et sa stabilité thermique peuvent être améliorées en dopant le poly-Si avec du Carbone, si une concentration adéquate de cette impureté est utilisée. L'insertion périodique de couches minces de SiC dans le poly-Si conduit à la stabilité thermique la plus élevée et à une augmentation de la résistivité moyenne de la couche. Néanmoins, des diminutions périodiques de la résistivité sont observées à chaque insertion de SiCFor future 5G telecommunication applications, Si-based substrates with low signal loss and excellent linearity are required. Among the envisaged solutions, RF-SOI is the most advanced. Its stack contains a High Resistivity (HR) Trap-Rich (TR) layer composed of high purity polycrystalline silicon (poly-Si) deposited on thin SiO2 native oxide of a HR-Si substrate (HR-Si). Some limitations of such system come from the HR-Si/SiO2 interface and its thermal stability, while increasing the resistivity of the TR-layer is also suited. The main objective of this thesis was to explore innovative approaches for solving these difficulties while staying Si-compatible. Towards this end, carbon was added in the system at different elaboration stages by i) replacing the SiO2 interfacial layer by 3C-SiC and by ii) C-engineering of the poly-Si layer during deposition.Using Atmospheric Pressure Chemical Vapor Deposition technique, state-of-the-art poly-Si TR-layers were grown on native oxide with thickness up to few tens of µm. It was found that the resistivity of the poly-Si was not directly dependent on the average grain size. Replacing the interfacial oxide by a thin mono- or poly-SiC layer and adapting the growth process allowed reaching equivalent properties of the poly-Si with the benefit of superior thermal stability by avoiding the interfacial layer dissolution. But it is accompanied by the presence of a resistivity drop at the interface due to the conductivity of the SiC material. By doping the poly-Si with C, both the TR-layer properties and thermal stability can be improved when adequate concentration of this impurity is used. Periodic insertion of thin SiC layers inside the poly-Si led to the highest thermal stability and an increase of the layer mean resistivity while periodic resistivity reductions were observed at each SiC insertion
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Pereira, Viviane Santos. "Preparação de suportes de carbono dopados com nitrogênio (N), enxofre (S) e fósforo (P) para aplicação na oxidação eletroquímica do metanol." Universidade de São Paulo, 2016. http://www.teses.usp.br/teses/disponiveis/85/85134/tde-23092016-101551/.
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Neste trabalho o carbono comercial Vulcan XC72 foi modificado com heteroátomos de N, S e P por meio do tratamento térmico a 800 °C com ureia, ácido sulfúrico e ácido fosfórico, respectivamente. Os carbonos modificados foram utilizados na preparação de eletrocatalisadores Pt/C e PtRu/C e aplicados na oxidação eletroquímica do metanol. Os materiais obtidos foram caracterizados por espectroscopia dispersiva de raios X, difração de raios X, espectroscopia Raman, microscopia eletrônica de transmissão e voltametria cíclica. A oxidação eletroquímica do metanol foi estudada por voltametria cíclica e cronoamperometria. Os espectros Raman mostraram que as razões de intensidades das bandas D e G dos suportes de carbono modificados com heteroátomos foram maiores que a observada para o carbono Vulcan XC72 sugerindo a incorporação na estrutura do carbono. As análises por difração de raios X mostraram para todos os eletrocatalisadores Pt/C a estrutura cúbica de face centrada (cfc) e as micrografias eletrônicas de transmissão que todos materiais apresentaram tamanhos de partícula na faixa 4-5 nm. Para os eletrocatalisadores PtRu/C preparados com os suportes de carbono modificados com N e S, os difratogramas de raios-X apresentaram apenas a fase Pt (cfc) não havendo deslocamento dos picos desta fase. Nestes materiais os picos referentes a fases de Ru não foram identificados sugerindo que o Ru apresenta-se como uma fase amorfa. Por outro lado, para o material modificado com P, observou-se um deslocamento dos picos da fase Pt(cfc) para ângulos maiores, sugerindo a formação de liga Pt-Ru e também foi observado a presença da fase Ru hexagonal compacta. Os eletrocatalisadores Pt/C e PtRu/C preparados com os suportes contendo heteroátomos apresentaram uma melhora significativa na atividade eletrocatalítica quando comparados aos materiais preparados com o suporte não modificado. A melhora na atividade pode estar relacionada a modificações na interação metal-suporte, bem como, as diferentes espécies Pt e Ru presentes no caso do eletrocatalisador PtRu/C preparado utilizando o suporte modificado com P.In this work, commercial Vulcan XC72 carbon was modified with heteroatoms like N, S and P by thermal treatment at 800 ° C in the presence of urea, sulfuric acid and phosphoric acid, respectively. The modified carbons were used in the preparation of Pt/C and PtRu/C electrocatalysts and tested for methanol electro-oxidation. The materials were characterized by dispersive X-ray spectroscopy, X-ray diffraction, Raman spectroscopy, transmission electron microscopy and cyclic voltammetry. The methanol electro-oxidation was studied by cyclic voltammetry and chronoamperometry. The Raman spectra showed that the intensity ratios of D- and G- bands of the carbon supports modified with heteroatoms were higher than that observed for Vulcan XC72 carbon suggesting the incorporation in the structure. X-ray diffraction analysis showed that Pt/C electrocatalysts have face-centered cubic structure (fcc) and transmission electron micrographs presented particle sizes in the range 4-5 nm. For PtRu/C electrocatalysts made with carbon supports modified with N and S, the X-ray diffraction patterns showed only the presence of Pt(fcc) phase with no shift of the Pt peaks. Peaks of Ru crystalline phases were not identified suggesting that in these materials Ru appears as an amorphous phase. On the other hand, for PtRu/C electrocatalyst prepared with carbon support modified with P, there was a shift of Pt(fcc) peaks to higher angles suggesting Pt-Ru alloy formation and the presence of Ru hexagonal close-packed phase was also observed. Pt/C and PtRu/C electrocatalysts prepared with carbon support modified with heteroatoms showed a significant improvement of electrocatalytic activity when compared to the unmodified material. The improvement in electrocatalytic activity can be related to changes in the metal-support interaction, as well as to the different Pt and Ru species for PtRu/C electrocatalyst prepared with carbon support modified with P.
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Skipa, Tetyana [Verfasser]. "Modification of the electronic properties of carbon nanotubes by bundling, temperature, B- and N-doping : a resonance Raman study / Tetyana Skipa." Karlsruhe : Forschungszentrum Karlsruhe, 2006. http://d-nb.info/983613184/34.
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Wohlgemuth, Stephanie-Angelika [Verfasser], and Markus [Akademischer Betreuer] Antonietti. "Functional nanostructured hydrothermal carbons for sustainable technologies : heteroatom doping and superheated vapor / Stephanie-Angelika Wohlgemuth. Betreuer: Markus Antonietti." Potsdam : Universitätsbibliothek der Universität Potsdam, 2012. http://d-nb.info/1024202682/34.
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Gonçalves, Rebeca Dourado. "Estudo de Impurezas de Carbono em Nanoestruturas de BN." Universidade Federal da Paraíba, 2008. http://tede.biblioteca.ufpb.br:8080/handle/tede/5734.
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Previous issue date: 2008-08-21Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES
In this work, we performed an analysis of the structural and electronic stability of nanostructures of Boron Nitride (BN), such as layers, tubes and cones, when doped with Carbon, through first-principles calculations as implemented in code SIESTA. We found that substitutional doping of Carbon for either a single Boron or a single Nitrogen atom produces significant changes in the conductive properties of each material. Such replacement process transforms the formerly insulating material, in a n-type conductor, donnor of electrons, for Boron replaced by Carbon, and the p-type, acceptor of electrons, for the Nitrogen substitution. Furthermore, we also performed calculations with spin-polarization and found occurrence of spontaneous magnetization of 1μB for all doped structures, except for tube (6,0), which presented a magnetic moment of 0;2μB. This magnetization is attributed to the unpaired electron located in the pz orbital of carbon. It was also noted that the doped layers become more energetically stable as the number of atoms increases. To the tubes, increased stability occurs with the increase in diameter combined with the consequent increase in the number of atoms. At the cones, stability energy is reduced with the increase in the angle of disclination. These effects are the result of a combination of percentage concentration of the defect and the greater or lesser degree of hybridization.
Neste trabalho, fizemos uma análise da estabilidade estrutural e eletrônica de nanoestruturas de Nitreto de Boro (BN), tais como planos, tubos e cones, quando dopadas com carbono, através do uso de cálculos de primeiros princípios como implementado no código SIESTA. Encontramos que a dopagem substitucional de carbono por boro ou nitrogênio provoca mudanças significativas nas propriedades condutoras de cada material. Tais substituições transformam o material que antes era isolante, em condutor do tipo n, doador de elétrons, para o boro substituído pelo carbono, e do tipo p, receptor de elétrons, para a substituição do nitrogênio. Além disso, realizamos cálculos com polarização de spin e verificamos a ocorrência de um momento magnético de 1μB para todas as estruturas dopadas, com exceção do tubo (6;0) que apresentou um momento magnético de 0;2μB. Essa magnetização é atribuída ao elétron desemparelhado localizado no orbital pz do carbono. Foi verificado também que os planos dopados se tornam mais estáveis energeticamente à medida que o número de átomos aumenta. Para os tubos, o aumento da estabilidade ocorre com o aumento do diâmetro combinado com o consequente aumento do número de átomos. Já nos cones, a estabilidade energética é diminuída com o aumento do ângulo de disclinação. Esses efeitos são fruto de uma combinação entre porcentagem de concentração do defeito e do maior ou menor grau de hibridização.
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Oishi, Silvia Sizuka 1981. "Síntese, dopagem e caracterização das resinas furfurílica e fenol-furfurílica visando a otimização do processamento de carbono vítreo /." Guaratinguetá : [s.n.], 2009. http://hdl.handle.net/11449/94398.
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Resumo: Em função da crescente importância do material carbono vítreo em áreas estratégicas, devido às suas características intrínsecas, tais como menor massa específica e bons valores de condutividades térmica e elétrica, tem se observado vários estudos na busca de novos precursores poliméricos, assim como no ajuste mais sistemático de seu processamento. Nesse sentido, este trabalho tem como objetivo o estabelecimento de rotas de síntese de resinas furfurílica e fenol-furfurílica e suas dopagens com partículas de cobre, visando o processamento de eletrodos de carbono vítreo reticulado (CVR). Neste contexto foram sintetizadas diferentes formulações de resinas furfurílica e fenol-furfurílica a partir da variação dos monômeros - álcool furfurílico, fenol e formaldeído, respectivamente. A confirmação do sucesso das sínteses foi realizada por análises de espectroscopia de infravermelho com transformada de Fourier, cromatografia gasosa, análises térmicas por calorimetria exploratória diferencial e medidas dos teores de carbono fixo, que mostram resultados entre 27 e 45% em carbono. Em seguida, estas amostras foram dopadas com um colóide contendo as partículas de cobre. As resinas, com e sem dopagem, foram catalisadas, impregnadas em espumas de poliuretano (PU) e carbonizadas, obtendo-se assim, o CVR. Análises por microscopias óptica e eletrônica de varredura mostram a homogeneidade na impregnação das espumas de PU e a textura uniforme das amostras de CVR. Os resultados de resistência à compressão apresentam os melhores valores para o CVR resultante da carbonização com a resina furfurílica ácida (0,55 MPa).Abstract: Due to the growing importance of glassy carbon material in strategic areas, due to its intrinsic characteristics, such as lower density and good thermal and electrical conductivities values, has been observed several studies looking for new polymeric precursors and tighter processing parameters. In this way, this study aims on the establishment of synthesis routes of furfuryl and phenol-furfuryl alcohol resins and their doping with cupper particles, in order to produce reticulated glassy carbon (RGC) electrodes. Inside of this context were synthesized different formulations of furfuryl and phenol-furfuryl alcohol resins by the monomers variation - furfuryl alcohol, phenol and formaldehyde, respectively. The success confirmation of the synthesis has been done by using FT-IR spectroscopy, gas chromatography, thermal analyses by differential scanning calorimetry (DSC) and carbon yield content measurements that present results between 27 and 45% of carbon. After this, the specimens were doped with a colloid contend the copper particles. The doped and non doped resins were catalyzed, impregnated in polyuretane (PU) foams and carbonized, in order to obtain the reticulated glassy carbon. Optical and Scanning Electron Microscopy analysis show the homogeneity of PU foams impregnation and uniform texture of RGC specimens. Compression results present the best values for RGC resulting from the carbonization with furfuryl alcohol acid resin (0,55 MPa).
Orientador: Edson Cochieri Botelho
Coorientadora: Mirabel Cerqueira Rezende
Banca: Choyu Otani
Banca: Pedro Carlos de Oliveira
Mestre
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Saraiva, Gilberto Dantas. "Espectroscopia Raman ressonante em nanotubos de carbono funcionalizados." reponame:Repositório Institucional da UFC, 2008. http://www.repositorio.ufc.br/handle/riufc/11917.
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SARAIVA, Gilberto Dantas. Espectroscopia Raman ressonante em nanotubos de carbono funcionalizados. 2008. 145 f. Tese (Doutorado em Física) - Programa de Pós-Graduação em Física, Departamento de Física, Centro de Ciências, Universidade Federal do Ceará, Fortaleza, 2008.Submitted by Edvander Pires (edvanderpires@gmail.com) on 2015-05-04T19:13:31Z No. of bitstreams: 1 2008_tese_gdsaraiva.pdf: 6765379 bytes, checksum: ded06cc237d77dabfc5886e3ed738be4 (MD5)
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In this Thesis we report a study of the synthesis and functionalization of carbon nanotubes. Regarding the synthesis, we produced carbon nanotubes samples using the chemical vapor deposition method. Both single-wall and multi-wall carbon nanotubes were produced. The basic difference between these two growth results was the catalyst employed. We also have changed the exposure time of catalyst particle to the hydrogen gas to find out the optimal parameters for growing the nanotubes. The obtained samples were characterized by resonance Raman spectroscopy and thermal analysis. The obtained samples show higher thermal stability compared with some commercially available samples. Regarding functionalization of the tubes we studied three different systems. Firstly, we investigated the effect of Si+ and C+ ions bombardment on the structural and electronic properties of highly pure double wall carbon nanotubes (DWNTs). The implantation was performed at room temperature with high fluencies of ions varying from 1 to 100 x( 10 13 ions/cm2) and the Raman spectroscopy was the main technique employed for studying the ion implantation-induced changes in the nanotubes. The effects of the Si+ implantation is stronger than that of C+ and this is attributed to the larger ionic radius of Si. The D to G band intensity ratio was used for probing the ion concentration for which the system looses its sp2 character leading to a highly disordered system with a high concentration of sp3 bonds. We observed that as the ion implantation dosage increases, the D-band intensity increases and the radial breathing modes (RBM) of the semiconducting (outer) and metallic (outer) tube disappear first, before from the inner tubes. At higher ion-implantation dosage, the carbon nanotubes are completely deformed and the Raman spectrum is typical of highly disordered graphite. Secondly, we investigated the effects of H2SO4 doping on DWNTs and SWNTs where the diameter of SWNTs are in the same range as the inner tube of the DWNTs. The comparison of these two systems allow to further improve the knowledge of doping effects on the constituents of DWNTs as well as to establish differences between the exohedral doping of SWNTs and DWNTs bundles. Upon doping with H2SO4 the Breit-Wigner-Fano lineshape of metallic tubes in the SWNTs samples decreases and the G band frequencies increase thus indicating that an electronic charge transfer is occurring from the nanotubes to the dopant molecule. The effect on the DWNTs is opposite to that of SWNTs thus evidencing that the inner and outer shell interaction seems to affect the inner tube electronic transitions more than those of the outer tubes. Thirdly, we report a detailed characterization of a novel carbon nanotube-based system that is a coaxial nanocable made of carbon as core and selenium as shell. Carbon nanotube bundles are wrapped up within a trigonal selenium shell. We have demonstrated that the Butyl-lithium compound plays an important role in promoting the interaction between the carbon nanotubes and the selenium shells and thus enables the preparation of these nanocable structures. The Raman spectra of the SWNTs in the residue and the Se-CNT nanocables suggests that this selenium-carbon interaction is stronger for semiconducting nanotubes than for metallic nanotubes. The chemistry of Selenium would allow the synthesis of carbon nanotubes decorated with other functional Se-based structures, such as CdSe, ZnSe, among others.
Esta tese consiste no estudo do processo de síntese e funcionalização de nanotubos de carbono. A síntese dos nanotubos de carbono foi realizada usando a técnica de deposição química a partir da fase vapor (CVD). Foram sintetizados Nanotubos de parede simples (SWNTs) e múltipas (MWNTs) . A diferença básica das metodologias usadas para preparar as amostras foi o uso de diferentes catalisadores expostos ao gás hidrogênio por diferentes intervalos de tempo. As amostras obtidas foram caracterizadas por espectroscopia Raman ressonante e análise térmica. Os resultados de análise térmica mostraram que as amostras sintetizadas apresentam uma excelente estabilidade térmica, quando comparada com algumas amostras disponíveis no mercado. Foram estudados três diferentes sistemas em relação ao processo de funcionalização de nanotubos de carbono. No primeiro sistema, investigamos o efeito da irradiação de íons de silício (Si+) e carbono (C+) nas propriedades eletrônicas e estruturais dos nanotubos de parede dupla (DWNTs). A implantação foi realizada à temperatura ambiente com concentrações de íons que variam de 1 a 100 x (1013 íons/cm2); e a espectroscopia Raman ressonante foi a principal técnica utilizada para estudar os efeitos da implantação. Os efeitos da implantação dos íons de Si+ na estrutura dos nanotubos são mais fortes do que os íons de C+ o que é atríbuido ao maior raio iônico do Si+. A razão das intensidades das bandas D e G foi usada para investigar a concentração de íons para a qual o sistema perde a característica sp2, deixando o sistema muito desordenado e com grande concentrações de ligações sp3. Observamos que o aumento da dosagem de íons aumenta a intensidade da banda D e os modos radiais de respiração dos nanotubos semicondutores (tubo externo) e metálicos (tubo externos) desaparecem primeiramente do que os tubos internos. Para altas dosagens de implantação de íons de silício ou carbono observamos que os nanotubos são completamente deformados e os espectros Raman apresentam aspectos de grafite altamente desordenados. No segundo sistema estudado, investigamos os efeitos da dopagem da molécula de H2SO4 nos SWNTs e DWNTs com distribuição de diâmetros dos SWNTs similar aos tubos internos dos DWNTs. A comparação destes dois sistemas permitiu ter um maior conhecimento dos efeitos da molécula H2SO4 nos sistemas DWNTs como também estabelecer diferenças entre a dopagem por intercalação nos feixes de SWNTs e DWNTs. A dopagem com H2SO4 torna o perfil Breit-Wigner-Fano (BWF) dos nanotubos metálicos nos sistemas SWNTs menos acentuado e a freqüência da banda G aumenta indicando que uma transferência de carga ocorre dos nanotubos para as moléculas de H2SO4. O efeito nos DWNTs é o oposto ao que foi evidenciado para os SWNTs, mostrando que a interação entre os tubos internos e externos no sistema DWNTs parece afetar mais fortemente as transições eletrônicas dos tubos internos do que as transições dos tubos externos. No terceiro sistema estudado, caracterizamos de maneira detalhada um novo sistema híbrido baseado em nanotubos de carbono que consiste de um cabo coaxial com carbono no interior e uma casca de selênio como tubo exterior. Demonstramos que o composto Butil-Lítio promove a interação entre os nanotubos de carbono e a casca de selênio levando a formação destes nanocabos. O espectro Raman dos SWNTs da amostra resíduo e selênio-nanotubos sugere que os nanocabos de selênio carbono interagem mais fortemente com os nanotubos semicondutores do que com os nanotubos metálicos. Estimamos que a química do selênio permitirá sintetizar nanocabos de selênio-carbono decorados com outros compostos funcionais tais como CdSe, ZnSe entre outros.
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Liu, Ye. "Tailored carbon based nanostructures as components of flexible thermoelectric and other devices." Doctoral thesis, SLUB Dresden, 2018. https://tud.qucosa.de/id/qucosa%3A33190.
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Carbon based nanostructures, such as fullerenes, carbon nanotubes and graphene showed a high potential for a vast of electronic and energy applications. However, properties of such materials in pristine forms can be insufficient to satisfy diverse specific demands, and tailoring their intrinsic properties is of increasing importance. In this work, different types of single-walled carbon nanotubes (SWCNTs) with controlled semiconducting fractions are p-/n-type doped by chemical doping in an attempt to tailor physical properties of the SWCNTs for the use in flexible thermoelectric (TE) devices and thermoplastic polymer-based conducting composites. Several p-/n-type doping schemes and an electronic type separation strategy have been developed to fulfill the task. A complete solution for efficient and scalable production of doped SWCNTs for the fabrication of flexible thermoelectric components is developed in this work.
For p-type doping, a combined experimental and theoretical work demonstrates that boron atomic doping is an efficient way to simultaneously improve Seebeck coefficient (S) and electrical conductivity (σ) of SWCNT films, showing an increased thermoelectric power factor (S2σ) up to 255 μW/mK2 by a factor of 2.5 comparing to the pristine SWCNTs. For n-type doping, treatment of SWCNTs with potassium oxide and crown ether solution lead to a negative Seebeck coefficient of -30 μV/K and a promising S2σ up to 50 μW/mK2.
A gel chromatography method has been developed to separate large-diameter (1.2-1.8nm) SWCNTs by electronic properties and to increase the purity of the sorted semiconducting carbon nanotubes (sc-SWCNTs) up to 95%.
Effects of p-/n-type doping induced by different plasma treatments on the thermoelectric properties have been investigated for thin films made of sorted sc-SWCNTs. The high-purity sc-SWCNTs show significantly improved S of 125 μV/K. As the effects of p-type doping, air plasma treatments with proper duration (40s) lead to the increase of S, σ and thus S2σ up to 190 μW/mK2. The n-type doping for the SWCNT films have been performed via ammonia plasma treatment, and a negative S value of -80 μV/K has been achieved in air at 110oC, which is one of the best values ever reported for n-type carbon nanotube films.
A flexible thermoelectric module was fabricated by printing ink made of the prepared boron doped SWCNTs and an organic solvent as an example for producing efficient all-carbon thermoelectric generators. At a temperature difference ΔT=60 K, the output voltage reaches 20 mV and the power output of 400 nW is obtained, although no “n”-legs are used in this module.
At last, a work has been done on the development of melt mixed composites as TE materials, in which polypropylene is used as the matrix and boron-doped SWCNTs are used as conducting fillers. A percolation threshold lower than 0.25wt. % and a maximum conductivity up to 125 S/m at 5wt. % of SWCNT load have been achieved. The maximum conductivity is more than two times higher than that of the composites made with pristine SWCNTs as fillers.
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Krüner, Benjamin [Verfasser], and Volker [Akademischer Betreuer] Presser. "Polymer-derived carbides and carbons with and without nitrogen-doping for electrochemical energy applications / Benjamin Krüner ; Betreuer: Volker Presser." Saarbrücken : Saarländische Universitäts- und Landesbibliothek, 2018. http://d-nb.info/1173703136/34.
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Krüner, Benjamin Verfasser], and Volker [Akademischer Betreuer] [Presser. "Polymer-derived carbides and carbons with and without nitrogen-doping for electrochemical energy applications / Benjamin Krüner ; Betreuer: Volker Presser." Saarbrücken : Saarländische Universitäts- und Landesbibliothek, 2018. http://nbn-resolving.de/urn:nbn:de:bsz:291-scidok-ds-275535.
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