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Farghaly, Ahmed A. "Fabrication of Multifunctional Nanostructured Porous Materials". VCU Scholars Compass, 2016. http://scholarscompass.vcu.edu/etd/4189.
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Nanostructured porous materials generally, and nanoporous noble metals specifically, have received considerable attention due to their superior chemical and physical properties over nanoparticles and bulk counterparts. This dissertation work aims to develop well-established strategies for the preparation of multifunctional nanostructured porous materials based on the combination of inorganic-chemistry, organic-chemistry and electrochemistry. The preparation strategies involved one or more of the following processes: sol-gel synthesis, co-electrodeposition, metal ions reduction, electropolymerization and dealloying or chemical etching. The study did not stop at the preparation limits but extended to investigate the reaction mechanism behind the formation of these multifunctional nanoporous structures in order to determine the different factors controlling the nanoporous structures formation. First, gold-silica nanocomposites were prepared and used as a building blocks for the fabrication of high surface area gold coral electrodes. Well-controlled surface area enhancement, film thickness and morphology were achieved. An enhancement in the electrode’s surface area up to 57 times relative to the geometric area was achieved. A critical sol-gel monomer concentration was also noted at which the deposited silica around the gold coral was able to stabilize the gold corals and below which the deposited coral structures are not stable. Second, free-standing and transferable strata-like 3D porous polypyrrole nanostructures were obtained from chemical etching of the electrodeposited polypyrrole-silica nanocomposite films. A new reaction mechanism was developed and a new structural directing factor has been discovered for the first time. Finally, silver-rich platinum alloys were prepared and dealloyed in acidic medium to produce 3D bicontinuous nanoporous platinum nanorods and films with a nanoporous gold-like structure. The 3D-BC-NP-Pt displayed high surface area, typical electrochemical sensing properties in an aqueous medium, and exceptional electrochemical sensing capability in a complex biofouling environment containing fibrinogen. The 3D-BC-NP-Pt displayed high catalytic activity toward the methanol electro-oxidation that is 30 times higher that of planar platinum and high volumetric capacitance of 400 F/cm3. These findings will pave the way toward the development of high performance and reliable electrodes for catalysis, sensing, high power outputs fuel cells, battery-like supercapacitors and miniaturized device applications.
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Scanlon, Shane. "Nanostructured porous materials based on designed self-assembling biopolymers". Thesis, University of Leeds, 2006. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.434581.
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Berrigan, John Daniel. "Biomimetic and synthetic syntheses of nanostructured electrode materials". Diss., Georgia Institute of Technology, 2012. http://hdl.handle.net/1853/53143.
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The scalable syntheses of functional, porous nanostructures with tunable three-dimensional morphologies is a significant challenge with potential applications in chemical, electrical, electrochemical, optical, photochemical, and biochemical devices. As a result, several bio-enabled and synthetic approaches are explored in this work (with an emphasis on peptide-enabled deposition) for the generation of aligned nanotubes of nanostructured titania for application as electrodes in dye-sensitized solar cells and biofuel cells. As part of this work, peptide-enabled deposition was used to deposit conformal titania coatings onto porous anodic alumina templates under ambient conditions and near-neutral pH to generate aligned, porous-wall titania nanotube arrays that can be integrated into dye-sensitized solar cells where the arrays displayed improved functional dye loading compared to sol-gel-derived nanotubes. A detailed comparison between synthetic and bioorganic polyamines with respect to titania film properties deposition rate provided valuable information for future titania coating experimental design given specific applications. The development of template-based approaches to single-wall titania nanotube arrays led to the development of a new synthetic method to create aligned, multi-walled titania nanotube arrays. Lastly, peptide-enabled deposition methods were extended beyond inorganic mineral and used for enzyme immobilization by cross-linking the peptide with the multicopper oxidase laccase. Peptide-laccase hybrid enzyme coatings improved both the amount of enzyme adsorbed onto carbon nanotube “buckypaper” and allowed the enzyme to retain more activity upon immobilization onto the surface.
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Zhang, Jin. "Electrodeposition of novel nanostructured and porous materials for advanced applications: synthesis, structural characterization and physical/chemical performance". Doctoral thesis, Universitat Autònoma de Barcelona, 2016. http://hdl.handle.net/10803/393985.
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Aquesta tesi doctoral comprèn la síntesi electroquímica de materials metàl·lics avançats en dues configuracions diferents, capes poroses i nanofils segmentats. Les capes poroses s’han preparat per electrodeposició fent ús de les bombolles d’hidrogen que es generen durant el procés com a plantilles (sistemes de Ni i Cu-Ni macroporós) i també per electrodeposició en presència del polímer P123 que actua com a plantilla autoorganitzada (Ni nanoporós). Les capes de Cu-Ni presenten una porositat jeràrquica (estan formades per microporus esfèrics i les partes de porus són nanodendrítiques), caràcter superhidrofòbic i propietats ferromagnètiques a temperatura ambient (gràcies a la separació de fases que s’aconsegueix durant el procés de deposició). A més, aquestes capes són electroquímicament actives vers la reacció d’evolució d’hidrogen en medi alcalí, bo i presentant millor resposta que les capes de Cu i Ni poroses preparades en condicions similars.
D’altra banda, s’han fabricat nanofils segmentats de CoPt/Cu/Ni i CoPt/Ni amb un control acurat de la llargada dels segments en membranes de policarbonat (PC). Gràcies al fet que els segments de CoPt i Ni presenten propietats ferromagnètiques distintes (l’un és magnèticament dur i l’altre magnèticament tou), es pot aconseguir un alineament antiparal·lel de la magnetització de saturació dels segments si llurs llargades es dissenyen de forma apropiada. Això faria possible minimitzar-ne la seva aglomeració un cop els nanofils fossin alliberats de la membrana de PC. Les troballes experimentals han estat validades mitjançant càlculs analítics.
S’han utilitat les capes macroporoses de Cu-Ni i Ni com a matrius per a la fabricació de noves làmines de nanocompòsit, en particular ZnO@CuNi, Al2O3@Ni i Co2FeO4@Ni, mitjançat processos de sol-gel i deposició de capa atòmica (en anglès, ALD). L’ALD permet la formació d’un recobriment conformal de gruix nanomètric en l’esquelet metàl·lic porós. Els nanocompòsits resultants combinen les propietats de la matriu metàl·lica i les del recobriment (fotoluminescència i propietats fotocatalítiques en el cas del ZnO, canvis en la mullabilitat en el cas de Al2O3 i Co2FeO4).
Finalment, s’han avaluat les propietats nanomecàniques de films de Ni nanoporós i s’ha vist que existeix una dependència tant del mòdul de Young com del límit d’elasticitat amb la força màxima aplicada durant els assaigs de nanoindentació, atès que aquetes capes presenten una gradació de la porositat en funció del gruix.This Thesis dissertation covers the electrochemical synthesis of advanced metallic materials in two different configurations, namely porous films and segmented nanowires (NWs). Porous films are prepared by hydrogen bubble-assisted electrodeposition (macroporous Ni and Cu-Ni systems) and self-organized template (block-copolymer P123) assisted electrodeposition (nanoporous Ni). The Cu-Ni films exhibit a hierarchical porosity (they consist of micron-sized roughly spherical pores and nanodendritic walls), superhydrophobic character and ferromagnetic properties at room temperature (due to the occurrence of phase separation during deposition). Furthermore, they are electrocatalytically active toward hydrogen evolution reaction in alkaline media, outperforming pure Cu and Ni porous films prepared under similar conditions. Meanwhile, segmented CoPt/Cu/Ni and CoPt/Ni NWs with controlled segment lengths are prepared by electrodeposition in polycarbonate (PC) membranes. Due to the dissimilar ferromagnetic properties of CoPt and Ni segments (hard- and soft-ferromagnetic character, respectively), it is possible to achieve an antiparallel alignment of the magnetization of the segments if their lengths are properly tuned. This would make it possible to minimize aggregation of the NWs once released from the PC template. These findings have been validated by analytical calculations. The macroporous Cu-Ni and Ni films are used as scaffolds for the fabrication of novel nanocomposite layers, namely ZnO@CuNi, Al2O3@Ni and Co2FeO4@Ni, by applying sol-gel coating and atomic layer deposition techniques. The latter allows a nanometer-thick conformal coating of the metallic host. The resulting nanocomposites combine the properties coming from the metallic matrix and those arising from the coating (photoluminescence and photocatalytic properties in the case of ZnO, changes in the wettability for Al2O3 and Co2FeO4). Finally, the nanomechanical properties of nanoporous Ni films are evaluated and a thickness-dependence of both the Young’s modulus and the yield strength with the maximum applied force during nanoidentation is disclosed, due to the graded porosity of these films.
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Su, Zixue. "Porous anodic metal oxides". Thesis, University of St Andrews, 2010. http://hdl.handle.net/10023/1019.
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An equifield strength model has been established to elucidate the formation mechanism for the highly ordered alumina pore arrays and titanium oxide nanotubular arrays prepared via a common electrochemical methodology, anodisation. The fundamentals of the equifield strength model was the equilibrium between the electric field driven oxidation rate of the metal and electric field enhanced dissolution rate of oxide. During the anodic oxidation of metal, pore initiation was believed to generate based on dissolution rate difference caused by inhomogeneity near the metal/oxide interface. The ionic nanoconvection driven by the electric force exerted on the space charge layer in the vicinity of electrolyte/oxide interface is established to be the main driving force of the pore ordering at the early stage of the anodisation. While the equifield strength requirement governs the following formation of the single pore and the self-ordering of random distributed pore arrays during the anodisation process. Hexagonal patterned Al2O3 nanopore arrays and TiO2 nanotubular arrays have been achieved by anodisation of corresponding metal substrates in proper electrolytes. The two characteristic microstructural features of anodic aluminium oxide (AAO) and anodic titanium oxide (ATO) were investigated using scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). The observations of the hemispherical electrolyte/oxide and oxide/metal interfaces, uniform thickness of the oxide layer, as well as self-adjustment of the pore size and pore ordering can be well explained by the equifield strength model. Field enhanced dissociation of water is extremely important in determination of the porosity of anodic metal oxide. The porosity of AAO and ATO films was found to be governed by the relative dissociation rate of water which is dependent on anodisation conditions, such as electrolyte, applied voltage, current density and electric field strength. Using an empirical method, the relations between the porosity of the AAO (ATO) films and the anodisation parameters, such as electric field strength, current density and applied voltage, have been established. Besides, the extent that an external electric field can facilitate the heterolytic dissociation of water molecule has been estimated using quantum-chemical model computations combined with the experimental aspect. With these achievements, the fabrication of anodic metal oxide films can be understood and controlled more precisely. Additionally, the impacts of other factors such as the electrolyte type and the temperature effect on the morphology of the anodic products were also investigated. Some important experimental evidences on the pore diameters variation with applied voltage in the anodisation of aluminium and the titanium were obtained for future investigation of the anodic metal oxide formation processes.
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King, L. J. "Aligned nanorods of A1PO4-5 within the pores of anodic alumina : a thesis submitted to the Victoria University of Wellington in fulfilment of the requirements for the degree of Master of Science with Honours in Chemistry /". ResearchArchive@Victoria e-thesis, 2010. http://hdl.handle.net/10063/1289.
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Gu, Xingxing. "Environmentally-benign, Porous and Conductive Carbon Materials for Lithium-Sulphur Batteries". Thesis, Griffith University, 2017. http://hdl.handle.net/10072/366860.
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Materials engineering and nano-manipulation play a key role in the development of advanced Lithium-Sulphur (Li–S) batteries in terms of energy and power density (both gravimetric and volumetric), cycling stability, rate capability, safety and the cost of production. In this thesis, two strategies are used to address the demands, i.e. fabrication of low cost, environmentally benign and conductive carbon-sulphur (C−S)
nanostructured cathodes, and the use of interlayers as a novel battery configuration in Li–S battery systems.
In the first strategy, inexpensive, scalable, environmentally-friendly and commercial bamboo biochar was activated via a KOH/annealing process to create an abundant microporous structure. This was then used to encapsulate sulphur to prepare a microporous bamboo carbon–sulphur (BC-S) nanocomposite as the cathode for Li–S batteries. The bamboo carbon micropores can encapsulate sulphur and polysulphides
to reduce the shuttle phenomenon during cycling while simultaneously maintaining electrical contact between the sulphur and the conductive carbon framework during the charge/discharge process. The treated BC-S (T_BC-S) nanocomposite with 50 wt% sulphur content delivers a high initial capacity of 1295 mA·h·g−1 at a low discharge rate of 160 mA·g−1 and high capacity retention of 550 mA·h·g−1 after 150 cycles at a high discharge rate of 800 mA·g−1 with excellent coulombic efficiency (≥ 95%).Thesis (PhD Doctorate)
Doctor of Philosophy (PhD)
Griffith School of Environment
Science, Environment, Engineering and Technology
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Hou, Chia-Hung. "Electrical double layer formation in nanoporous carbon materials". Diss., Atlanta, Ga. : Georgia Institute of Technology, 2008. http://hdl.handle.net/1853/22698.
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Thesis (Ph. D.)--Civil and Environmental Engineering, Georgia Institute of Technology, 2008.Committee Chair: Sotira Yiacoumi; Committee Co-Chair: Costas Tsouris; Committee Member: Ching-Hua Huang; Committee Member: Sankar Nair; Committee Member: Spyros G. Pavlostathis.
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Bimbo, Nuno Maria Marques dos Santos. "Modelling and analysis of hydrogen storage in nanostructured solids for sustainable energy systems". Thesis, University of Bath, 2013. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.577745.
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As societies depart from current economic models which are built around affordable and easily accessible fossil fuels to energy systems increasingly based on the use of renewable energies, the need grows for a wide-scale clean and sustainable energy vector. Hydrogen fulfils most of the needed equirements, but implementation and large scale penetration, especially for mobile applications, is precluded by technical issues. Among these, arguably the most complex is how to safely, economically and efficiently store hydrogen. Storage in a porous material offers some attractive features, which include fast kinetics, reversibility and moderate energy penalties. A new methodology to analyse hydrogen adsorption isotherms in microporous materials is presented in this thesis. The methodology is applied to hydrogen adsorption in different classes of high-surface area materials but could in principle be used for any supercritical fluid adsorbed onto a microporous material. To illustrate the application of the methodology, high-pressure hydrogen adsorption isotherms of four different materials were analysed, metal-organic frameworks MIL-101 and NOTT-101 and carbons AX-21 and TE7. The analysis extracts important information on the adsorptive capacities of the materials and compares them with conventional storage methods, which include compression, liquefaction and cryogenic compression. The methodology also aids in the calculation of the thermodynamics of adsorption, providing a more accurate calculation method than currently reported techniques, demonstrated with the calculation of the differential isosteric enthalpies for metal-organic framework NOTT-101. NMR and INS are used in a novel way at the same operating conditions of sorption experiments to validate the findings of the analysis. Both methods provide a qualitative validation for the analysis. Remarkably, the INS reveals that the adsorbed hydrogen in TE7 is in a solid-like state. GCMC simulations were also used to compare with the application and findings of the methodology, using silicalite-1 as a test material.
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Masika, Eric. "Fabrication of nanostructured inorganic and carbon porous materials for catalysis and gas storage applications". Thesis, University of Nottingham, 2013. http://eprints.nottingham.ac.uk/14590/.
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This thesis details the preparation and subsequent characterisation of novel nanostructured porous materials with tuneable porosity. The main focus is the development of inorganic and carbonaceous porous materials for catalysis, templating and gas storage applications. Three distinct methods of synthesis are investigated, namely: (i) hydrothermal synthesis of zeotype aluminosilicates, (ii) nanocasting techniques for templated carbons and (iii) sol-gel processes, with/without metal salt 'porogen', to carbon aerogels. Post-synthesis modification methods for carbonaceous materials include supercritical carbon dioxide mediated incorporation of palladium nanoparticles into zeolite templated carbons and chemical activation for carbon aerogels resulting in enhanced textural properties. Chapter 1: Provides the foundation and background to the main themes of nanostructured porous materials investigated in this work. Information about fundamental properties and applications is emphasised. Chapter 2: Gives a brief background of techniques used for characterisation of the porous materials generated in this research programme. Gas sorption techniques used to probe hydrogen storage and carbon dioxide uptake are also presented. Chapter 3: Describes stepwise experimental techniques followed in the preparation of various porous materials. The chapter also describes the instrumentation used in these techniques. Chapter 4 - 7: Each chapter reports a separate but sequential area of research in which appropriate additional theory and background is provided with associated literature review. This is followed by a results and discussion section, with a concluding summary for each chapter. Chapter 4: Details the synthesis of ordered mesoporous aluminosilicates, which exhibit some zeolitisation, prepared from a recipe conventionally used for the synthesis of microporous zeolite SEA. The porosity of the aluminosilicates is modified by simple washing and/or refluxing (in water) of either on the as-synthesised mesophase or the calcined material. The aluminosilicates have excellent hydrothermal stability and strong acidity and thus combine the best properties from mesoporous materials and zeolites. Chapter 5: Describes the preparation of zeolite templated carbons (ZTC) generated as replicas of zeolite Y via a hard template nanocasting process. In order to enhance hydrogen storage, the ZTCs are impregnated with Palladium nanoparticles using supercritical carbon dioxide solvent, scC02, as environmentally benign reaction media. The Pd-doped ZTCs exhibit enhanced hydrogen storage due to optimised (with respect to metal content and particle size) incorporation of Pd. Chapter 6: A two-step process for the generation of zeolite template carbons (ZTCs) was investigated. In this case the nanocasting technique involves liquid impregnation of zeolite 13X with furfuryl alcohol followed by chemical vapour deposition (CVD) of ethylene at variable CVD temperatures. The two-step process was a successful attempt to optimise the replication of the zeolite structure in the carbons. The ZTCs had very high surface area and excellent mechanical stability, and achieved the highest hydrogen storage capacity (7.3 wt% at 77 K and 20 bar) ever reported for any carbon material. Chapter 7: Organic Sol-gel chemistry is explored in the formation of carbon aerogels via conventional methods involving the use of resorcinolformaldehyde resins and melamine-formaldehyde with or without metal salt as a porogen and subcritical drying. Chemical activation is used to modify the porosity of aerogels for potential applications in carbon dioxide uptake. Chapter 8: A brief overall conclusion to this research work is presented together with recommendations for future research.
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Huang, Xuezhen. "Fabrication and optical properties of (I) erbium-doped nanowires containing germanium and/or zinc oxide and (II) porous germanium nanowires". [Fort Worth, Tex.] : Texas Christian University, 2010. http://etd.tcu.edu/etdfiles/available/etd-04282010-134727/unrestricted/Huang.pdf.
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Zhang, Wei. "Controllable growth of porous structures from co-continuous polymer blend". Diss., Georgia Institute of Technology, 2011. http://hdl.handle.net/1853/39608.
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Due to their large internal surface area, microporous materials have been widely used in applications where high surface activity is desired. Example applications are extracellular scaffolds for tissue engineering, porous substrates for catalytic reaction, and permeable media for membrane filtration, etc. To realize these potential applications, various techniques such as TIPS (thermal induced phase separation), particle leaching, and SFF (solid freeform fabrication) were proposed and investigated. Despite of being able to generate microporous for specific applications, these available fabrication techniques have limitations on controlling the inner porous structure and the outer geometry in a cost-effective manner. To address these technical challenges, a systematic study focusing on the generation of microporous structures using co-continuous polymer blend was conducted. Under this topic, five subtopics were explored: 1) generation of gradient porous structures; 2) geometrical confining effect in compression molding of co-continuous polymer blend; 3) microporous composite with high nanoparticle loading; 4) micropatterning of porous structure; 5) simulation strategy for kinetics of co-continuous polymer blend phase coarsening process.
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Zhai, Guiming, i 翟桂明. "Nanoparticle transport in porous medium and nanosized zero-valent iron(nZVI) for environmental remediation". Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2010. http://hub.hku.hk/bib/B44907199.
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Cheng, Chuan, i 程川. "Electro-chemo-mechanics of anodic porous alumina nano-honeycombs: self-ordered growth and actuation". Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2013. http://hub.hku.hk/bib/B50899582.
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Self-ordered anodic porous alumina with a nano-honeycomb structure has recently been extensively used as templates for the synthesis of various nanomaterials for diverse applications. However, due to the insufficient knowledge on the combined electro-chemo-mechanical processes, the formation mechanism of self-ordering has been under debate for decades without clear conclusions. Also, fast fabrication of highly self-ordered and mechanically stable anodic porous alumina is still a challenge. Furthermore, the actuation behavior of anodic porous alumina upon external mechanical and electrical triggering in an electrochemical cell has not been exploited.
In this work, firstly, we investigated the self-ordering mechanism by establishing a kinetics model involving the Laplacian electric potential distribution and a continuity equation for current density within the oxide body. Current densities governed by the Cabrera-Mott equation are formed by ion migration within the oxide as well as across the interfaces. The pore channel growth, due to electric-field-assisted reactions, is governed by Faraday’s law. Real-time evolution of pre-patterned pore channel growth was simulated in two-dimensional cases by finite element method. The simulations revealed a parameter domain within which pre-patterned pore channels will continue to grow in a stable manner during the subsequent anodization if the pre-patterns are commensurate with the self-ordered configurations, or these are driven into stable if the pre-patterns do not initially match the self-ordered configurations. This was verified in experimentally observed pore channel growth under the guidance of pre-patterns made by focused-ion-beam milling. Furthermore, the simulations revealed that ionization reaction on (001) oriented Al grain is relatively easier than that on (101) grain, which results in stable and unstable pore channel growth on (001) and (101) Al grains, respectively, both of which were observed from the simulations and experiments.
Secondly, a scheme on quantitative evaluation of self-ordering qualities in anodic porous alumina has been developed, based on which we systematically searched the optimum self-ordering conditions, by varying the key anodization factors, including substrate grain orientation, electrolyte concentration, temperature, voltage, and time. A high acid concentration and high temperature anodization method was found. Compared with conventional methods, the present method can realize fast formation of highly self-ordered, and mechanically stable anodic porous alumina under a continuous range of anodization voltage with tunable interpore distances.
Thirdly, reversible bending was found in anodic porous alumina-Al composites upon cyclic electric actuation, as directly observed by an optical microscope and detected by in situ nanoindentation. The bending is thought to be the result of charge-induced surface stresses in the nanoporous alumina. The results suggest a new type of composite materials for applications as micro-scale actuators to transform electrical energy into mechanical energy. Furthermore, the composite exhibits significant softening during in situ nanoindentation when the estimated maximum stress underneath the indenter is exerted on the metal/oxide interface. Softening was further verified by in situ microindentation. Electron microscopy examination indicated that the softening is due to a combination of high compression stress and electric field acting near the interface, which enhance ionization reaction and cause the interface to move faster into the substrate.published_or_final_version
Mechanical Engineering
Doctoral
Doctor of Philosophy
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May, Masnou Anna. "Insights into nanomaterials: from surfactant systems to meso/macroporous materials and nanoparticles". Doctoral thesis, Universitat de Barcelona, 2014. http://hdl.handle.net/10803/285940.
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Nanomaterials have structured components with at least one dimension of less than 100 nm. Their novel properties stem from their nanoscale dimensions and increased relative surface area, and they have a wide range of applications in several key fields, including medicine.
In this thesis we focus on meso- and meso/macroporous silica materials and nanoparticle. We examine how the properties of nanomaterials are influenced by the experimental conditions used in their synthesis. We then explore the possibility of tailoring such properties by varying the parameters in the process of manufacture.
To this end we prepared a range of materials, including mesoporous silica, meso/macroporous silica, silica porous spheres and silica nanoparticles and studied their properties. We also examined the micellar solutions and emulsions that are used in the synthesis of these materials, their micellar and droplet size, the phase behavior of the surfactant systems involved in the synthesis, the stability and rheological behavior of the emulsions and the scale up parameters for their preparation at different scales. The synthesis and characterization techniques include rheology, optical microscopy, nitrogen adsorption-desorption, X-ray scattering (SAXS and XRD), transmission and scattering electron microscopy (TEM and SEM), dynamic light scattering (DLS), zeta potential and thromboelastography, among others.
In the first study we examined water-in-oil emulsions with a liquid crystal phase as continuous phase. These systems are stable and highly elastic. Their microstructure is discussed by fitting the data with several rheological models. These systems are also compared with water-in-oil emulsions with a micellar phase in the continuous phase, and as a function of surfactant concentration and volume fraction of dispersed phase.
In the second study, the process variables that have a significant effect on the properties of the emulsions are identified, including stirring rate, dispersed phase addition flow rate, surfactant concentration and scale up. Droplet size and rheological properties are considered as response variables. Stirring rate is the parameter that most influences the emulsion properties, followed by surfactant concentration. Vessel size is also important. To study the scale up, emulsions were prepared at three scales with geometric similarity and we identified the parameters that must be kept constant to obtain the same emulsion in the three scales, i.e. emulsions with the same droplet size, viscosity, yield stress, viscoelastic parameters and stability. The scale invariants take into account the stirring rate (N) and the scale (D, impeller diameter).
The third study focuses on the preparation of meso and meso/macroporous materials. Bimodal mesoporous materials with an ordered hexagonal structure and two interconnected networks are prepared from a mixture of two surfactants, one hydrogenated and the other fluorinated, through the cooperative templating mechanism, using tetramethyl orthosilicate as silica source. The synthesis of ordered mesoporous materials from a novel surfactant consisting of a modified block copolymer with amino-groups on the ends (Jeffamine) is also studied. In this case, the best ordering of the mesopores is obtained at low temperature. In both studies, the surfactant phase behavior, and the structural properties of both surfactants and materials are determined, and the experimental conditions (pH, temperature, agitation) are optimized. Macroporous materials are then prepared from the oil-in-water emulsions stabilized with modified Jeffamine and using decane as organic phase, through the emulsion templating mechanism. Finally, mesoporous silica spheres are prepared from highly concentrated water-in-oil emulsions.
The last study focuses on the synthesis and applications of silica nanoparticles. The process variables that have a direct effect on the size are identified, like the silica source concentration and the pH. The growth mechanism of these particles is studied through turbidimetry and explained in terms of nuclei formation and aggregation of the hydrolyzed species. The clotting properties of the particles are analyzed, in order to use these particles as a scaffold for further functionalization and application in the control of internal hemorrhages. First, the particles are functionalized to reduce the clotting activity, in order to avoid the formation of unwanted clots. Amino-functionalization and PEGylation are analyzed in this case. Second, functionalization with polyphosphate chains is studied in order to enhance the clotting activity, not only in normal conditions, but also under coagulopathy and hypothermia.Els nanomaterials són materials amb propietats morfològiques entre 1 i 100 nm en almenys una direcció. En aquesta tesi s'estudien els materials meso- i meso/macroporosos de sílice, que tenen porus en aquestes dimensions, i nanopartícules, la grandària de les quals es troba també en aquest rang. En una primera fase s'estudien els sistemes tensioactius, com les solucions micel·lars i les emulsions, que s'usen per a la síntesi d’aquests materials. El primer estudi consta de l’anàlisi de les emulsions formades amb cristall líquid a la fase contínua. La microestructura d'aquests sistemes s'estudia amb diversos models reològics. També es comparen amb sistemes amb fase micel·lar en la fase contínua i a diferents concentracions de tensioactiu i fase dispersa. En un segon estudi es determinen les variables de procés que tenen un efecte significatiu sobre les propietats de les emulsions. Com a variables de resposta s'usen la mida de gota i les propietats reològiques. També s'estudia l'escalat en la preparació de les emulsions altament concentrades i es determinen els invariants d’escala. El tercer estudi se centra en la preparació de materials meso i meso/macroporosos. Es sintetitza un material amb mesoporus bimodals i estructura hexagonal ordenada a partir d'una barreja de dos tensioactius, i la síntesi de materials mesoporosos ordenats a partir d'uns tensioactius amb grups amino. També es preparen materials amb macroporus a partir d'emulsions formades amb aquest tensioactiu i, en última instància, es preparen esferes mesoporoses de sílice a partir d'emulsions aigua-en-oli altament concentrades. L'últim estudi se centra en la síntesi de nanopartícules de sílice, en les variables de procés que tenen un efecte directe sobre la mida obtinguda, i en l'aplicació d'aquestes nanopartícules en la coagulació de la sang per controlar hemorràgies internes. S'estudien les propietats de coagulació i es funcionalitzen amb agents que acceleren o disminueixen aquesta activitat. Les tècniques de síntesi i caracterització inclouen reologia, microscòpia òptica, adsorció-desorció de nitrogen, dispersió de raigs X, microscòpia electrònica de transmissió i de rastreig (TEM i SEM) i potencial zeta, entre altres.
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DEMONTIS, VALERIA. "Porous Silicon applications in biotechnology". Doctoral thesis, Università degli Studi di Cagliari, 2007. http://hdl.handle.net/11584/266040.
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Biotechnology is a field in great expansion and the continuous boost for obtaining smaller and more efficient devices stimulates the increase of interest from the research community. Nanostructured materials, and among them porous silicon (PS), appear to be good candidates for coupling with biological molecules because of their peculiar characteristics. In the case of porous silicon, the most noticeable are the very large specific area, which allows the loading of large amounts of biological material in a very small volume, and the possibility to easily tailor the pore size and morphology as function of the kind of molecules to be introduced.
Besides, the proven biocompatibility and non toxicity of PS allow the development of electronic devices to be directly implanted into living organisms without risk of rejection.
In this thesis we mainly focus our attention on the fabrication and characterization of a porous silicon-based potentiometric biosensor for triglycerides analysis, made of a lipase immobilized on a mesoporous Si matrix. Prototypes, realized on 1 x 1 cm n+-type silicon wafers, show a very high enzymatic activity. Moreover the properties of these biosensors have been shown to be stable in a several months time interval, clearly showing their advantages with respect to traditional triglycerides detection systems. The Michaelis Menten curve is obtained to demonstrate the absence of diffusion problems. Potentiometric measurements are also shown.
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Parkinson, Mark. "Structural and optical properties in porous nanostructured semiconductors". Thesis, De Montfort University, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.391476.
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Szeifert, Johann. "Mesoporous Titania Materials - Tuning and Optimizing Nanostructures and Porous Morphologies". Diss., lmu, 2011. http://nbn-resolving.de/urn:nbn:de:bvb:19-132055.
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Azevedo, Raquel Cristina de Souza. "Síntese e caracterização de um sistema multifuncional SBA-16/Nanopartículas magnéticas/gel polimérico para bioaplicações". CNEN - Centro de Desenvolvimento da Tecnologia Nuclear, Belo Horizonte, 2014. http://www.bdtd.cdtn.br//tde_busca/arquivo.php?codArquivo=316.
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Coordenação de Aperfeiçoamento de Pessoal de Nível SuperiorA combinação do material mesoporoso SBA-16 com o gel polimérico poli(N-isopropilacrilamida) contendo nanopartículas magnéticas pode conduzir à formação de um material híbrido interessante para aplicação em magnetohipertemia e liberação controlada de fármacos. Neste trabalho, foi explorada a estratégia de síntese de um sistema multifuncional, constituído por SBA-16/Fe3O4/P(N-iPAAm) com o objetivo de avaliar sua potencialidade de geração de calor a partir da magnetita e sua contribuição nos estudos de liberação controlada de fármacos. A caracterização dos materiais foi feita por Microscopia Eletrônica de Varredura (MEV), Microscopia Eletrônica de Transmissão (MET), Adsorção de Nitrogênio, Espalhamento de Raios X a Baixos Ângulos (SAXS), Análise Termogravimétrica (TG), Análise Elementar (CHN), Espectroscopia na Região do Infravermelho com Transformada de Fourier (FTIR), Difração de Raios X (DRX), Espectroscopia Mössbauer, Medidas Magnéticas e Espectroscopia de Fotoelétrons Excitados por Raios X (XPS). Através da análise dos resultados obtidos foi possível confirmar a formação do híbrido, e elucidar as propriedades físico-químicas, estruturais e magnéticas das amostras. Medidas das propriedades de geração de calor mostraram que o híbrido apresentou uma variação de temperatura (T) de 11 e 35C nas concentrações de 10 e de 20 mg/mL, respectivamente, no campo magnético alternado de 126 Oe; e apresentou uma variação de temperatura (T) de 32 e 39C nas concentrações de 10 e de 20 mg/mL, respectivamente, no campo magnético alternado de 168 Oe. Este resultado demonstrou que este sistema multifuncional apresenta potencial como agente de hipertermia para o tratamento do câncer. Por fim, foi feito o estudo da influência dessas nanopartículas magnéticas com a presença do gel na cinética de liberação do fármaco Doxorrubicina (DOX) sob condições in vitro. A liberação foi estudada na ausência e na presença de um campo magnético alternado de 126 Oe, que se constatou a influência do campo magnético no aumento da taxa de liberação da DOX. Este resultado demonstrou que a propriedade da magnetita de gerar calor aliada às propriedades do P(N-iPAAm) de transição de fases (contração) contribuiu para uma melhor taxa de liberação da DOX.
The combination of SBA-16 mesoporous materials with gel polymer poly (N-isopropylacrylamide) containing magnetic nanoparticles can lead to the formation of an interesting hybrid material for use in hybrid magnetic hyperthermia and controlled drug release. In this study, we explored the strategy of synthesis of a multifunctional system consisting of SBA-16/Fe3O4/P(N-iPAAm) in order to assess its potential for heat generation from magnetite and its contribution in the controlled drug release. The materials were characterized by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Nitrogen Adsorption, Small Angle X Ray Scattering (SAXS), Thermogravimetric Analysis (TG), Elemental Analysis (CHN), Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), 57Fe Mössbauer spectroscopy, magnetic measures and X-Ray Photoeletron Spectroscopy (XPS). Through the analysis of the results it was possible to confirm the formation of the hybrid system, and elucidate the physicochemical, structural and magnetic properties of the samples. Measurements of the properties of heat generation showed that the hybrid presents a temperature variation (T) of 11 and 35C in concentrations of 10 and 20 mg/mL, respectively, in the alternating magnetic field of 126 Oe, and presents a temperature variation (T) 32 and 39C at concentrations of 10 and 20 mg/mL, respectively, in alternating magnetic field of 168 Oe. This result indicates that the multifunctional system shows great potential as a hyperthermia agent for cancer treatment. Finally, the study of the influence of these magnetic particles in the kinetics of release of the doxorubicin (DOX) was made in the presence of gel under in vitro conditions. The release was studied in the absence and in the presence of an alternating magnetic field of 126 Oe; it was found that the presence of magnetic field increased the release rate of DOX. This result demonstrated that the property of heat generate from magnetite combined with phase transition (contraction) properties of P(N-iPAAm) contributed to a better control of release of DOX from hybrid system.
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Dickinson, Calum. "Metal oxide porous single crystals and other nanomaterials : an HRTEM study". Thesis, University of St Andrews, 2007. http://hdl.handle.net/10023/217.
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Three-dimensional porous single crystals (PSCs) are a recent development in the growing world of mesoporous material. The mesoporosity allows for the material to retain their nanoproperties whilst being bulk in size. The current work concentrates on chromium oxide and cobalt oxide PSCs formed in the templates SBA-15 and KIT-6. HRTEM is the main technique used in this investigation, looking at the morphology and single crystallinity of these materials. A growth mechanism for the PSC material is proposed based on HRTEM observations. XRD studies revealed that the confinement effect, caused by the mesopores, reduces the temperature for both cobalt and chromium oxide crystallisation, as well as a different intermediate route from the metal nitrates. The properties of chromium oxide PSC are also investigated magnetically and catalytically. Some metal oxides in different templates are also presented, despite no PSC forming. HRTEM work on other nanomaterials, based on collaboration, is also presented.
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Li, Yuan. "Synthesis and mechanical characterization of transversely isotropic nanoporous platinum". Thesis, Georgia Institute of Technology, 2011. http://hdl.handle.net/1853/42927.
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Nanoporous (NP) metal foams combine desirable characteristics of metals with unique nanoarchitectural features to yield weight normalized properties far superior than either dense metals or bulk metal foams. Due to their high surface to volume ratios these structures show great promise as components of fuel cells, as sensors and have been suggested for use in biological applications, for example as antimicrobial scaffolds or as platforms on which to explore biological material behavior. While most NP metal foams are isotropic, structures with anisotropic features spanning different length scales can further extend applications. This work examines the parameters controlling the synthesis of transversely isotropic NP Platinum foam by dealloying an amorphous Pt-Si alloy. The structure that is examined in this work is hierarchical with Voronoi polyhedra that form on the free surface and under each polyhedral hyper-structure, nanocrystalline NP Pt foam forms with radial struts of length ~60 nm and grain size of 5 nm. The size of the polyhedra can be tailored by changing the dealloying potential. In turn, the mechanical properties of these structures as assessed by nanoindentation can range from 1 to 3GPa depending on the geometric arrangement of the struts. Finally, the initiation location of these structures and the relationship between electrochemical parameters and dealloying front evolution is examined.
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Wells, Brendan Christopher 1979. "Commercial applications of nanostructures created with ordered porous alumina". Thesis, Massachusetts Institute of Technology, 2004. http://hdl.handle.net/1721.1/28875.
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Thesis (M. Eng.)--Massachusetts Institute of Technology, Dept. of Materials Science and Engineering, 2004.Includes bibliographical references (leaves 82-86).
In the drive from microfabrication to nanofabrication, porous alumina templates may play a key role in technological evolution. Under the right processing conditions, ordered pores can grow in anodic aluminum oxide, which is a high strength, thermally and electrically insulating material. There are many potential applications for porous alumina templates, ranging from the simple fabrication of nanostructure arrays to the more complex processing of components for end-user products such as nano-integrated circuits and gas sensors. Porous alumina templates can also be processed to have long-range pore ordering on an entire twelve-inch silicon wafer, which may be of unique benefit to processes requiring such pore precision, such as parallel electron beam lithography. The high aspect ratios which can be attained through porous alumina template technology may also offer unique advantages in applications such as field-emission-based devices. As a durable high strength material, porous alumina templates are not limited by extreme process conditions, further extending the reach of their application. The vast array of applications allows the technology to be financially attractive inside business models ranging from sustaining to disruptive innovation. Porous alumina template technology has the necessary multitude and diversity of attributes to play a crucial role in the future of nanotechnology.
by Brendan Christopher Wells.
M.Eng.
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Andrews, Gordon Todd. "Elastic and structural properties of supported porous silicon layers". Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1999. http://www.collectionscanada.ca/obj/s4/f2/dsk1/tape9/PQDD_0004/NQ42470.pdf.
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Ghanem, Mohamed Ali M. A. "Electrochemical synthesis of nanostructured porous materials using liquid crystal and colloidal templates and their magnetic and optical properties". Thesis, University of Southampton, 2002. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.392824.
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Hudiono, Yeny C. "Thermal transport properties of nanoporous zeolite thin films". Diss., Atlanta, Ga. : Georgia Institute of Technology, 2008. http://hdl.handle.net/1853/24748.
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Thesis (Ph.D.)--Chemical Engineering, Georgia Institute of Technology, 2009.Committee Chair: Prof. Sankar Nair; Committee Co-Chair: Prof. Samuel Graham; Committee Member: Prof. Amyn S. Teja; Committee Member: Prof. Mo Li; Committee Member: Prof. Peter Ludovice.
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Pinto, Sanz Javier. "Fabrication and characterization of nanocellular polymeric materials from nanostructured polymers". Thesis, Bordeaux, 2014. http://www.theses.fr/2014BORD0380/document.
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Cette thèse porte sur la production et l’étude de mousses de polymères micro ou nanoporeux à partir de mélanges nanostructurés à base de PMMA (poly(méthyl méthacrylate)) par dissolution et moussage avec CO2. D’autre part, plusieurs techniques expérimentales ont été améliorées ou adaptées afin de fournir de précieuses informations sur les systèmes étudiés. La nanostructuration de mélanges solides denses à base de PMMA est induite par l’addition d’un copolymère à blocs (MAM, poly(méthyl méthacrylate)-co-poly(butylacrylate)-co-poly(méthyl méthacrylate)). Les structures cellulaires des mousses produites à partir de ces mélanges ont été caractérisées et expliquées ; on a démontré que la nanostructuration agit comme un modèle (un gabarit) pour la structure cellulaire, permettant l’obtention d’un large éventail de structures cellulaires et en particulier des mousses nanocellulaires. De plus il est démontré que les paramètres du procédé, tels que la pression et la température, permettent la différenciation entre les deux voies de moussage utilisées ;ceux-ci ont une influence significative sur les caractéristiques finales des mousses de PMMA seul, mais peu sur celles des mélanges PMMA/MAM. Les mousses dans ces mélanges présentent un mécanisme de nucléation hétérogène contrôlée par la nanostructuration, ce qui permet de limiter l’influence des paramètres de traitement thermique dans la nucléation de la cellule. En outre, certains mélanges de PMMA/MAM présentent également une remarquable stabilité de leur morphologie au cours de la croissance cellulaire, ce qui évite l’effondrement cellulaire et la coalescence.Enfin, on a étudié l’influence de la transition entre les structures micro-cellulaires et les structures nano-cellulaires sur les propriétés : une nette diminution de la conductivité thermique en raison de l’effet de Knudsen que nous avons mis en évidence, une augmentation notable de la température de transition vitreuse en raison de l’isolement des chaînes de polymères dans les parois (les murs) de la cellule ; mais n’avons pas noté d’influence importante de cette transition sur le module de YoungThis dissertation focuses on the production and study of nanocellular foams from PMMA based(poly(methyl methacrylate) materials by CO2 gas dissolution foaming.Due to the novelty of this research field several experimental techniques have been improved or adapted in order to provide valuable information from the systems understudy. Nanostructuration of PMMA-based blends induced by the addition of a block copolymer (MAM, poly(methyl methacrylate)-b-poly(butyl acrylate)-b-poly(methyl methacrylate)) and the cellular structure of the foams produced from these blends have been characterized and related; obtaining that the nanostructuration acts as a pattern for the cellular structure, allowing obtaining a wide range of cellular structures and in particular nanocellular foams. It is demonstrated that processing parameters, such as pressure and temperature, allow differentiating between two foaming routes ; and present a significant influence on the foaming process and final characteristics of neat PMMA foams, but not on PMMA/MAM blends. PMMA/MAM blends present a heterogeneous nucleation mechanism controlled by the nanostructuration that avoid the influence of the processing parameters in the cell nucleation. In addition, some PMMA/MAM blends also present a high stability during the cell growth, avoiding the cellular collapse and coalescence. Finally, it has been studied the influence on the foams properties of the transition between the microcellular and the nanocellular ranges; obtaining that there is a clear influence on the thermal conductivity, which decreases in nanocellular foams due to the Knudsen effect,and the glass transition temperature, which increases in nanocellular foams due to the confinement of the polymer chains in the cell walls, but not on the Young’s modulus
Esta tesis se centra en la producción y estudio de de espumas poliméricas nanocelulares producidas a partir de materiales basados en PMMA (poli(metil metacrilato)), mediante la técnica de espumado por disolución de gas usando CO2. Debido a la novedad de este campo de investigación ha sido necesario mejorar o adaptar varias técnicas experimentales para obtener la información necesaria de los sistemas bajo estudio. Se han caracterizado y relacionado la nanoestructuración de mezclas basadas en PMMA, inducida por la adición de un copolímero de bloque (MAM, poli(metil metacrilato)-copoli(butil acrilato)-co-poli(metil metacrilato)), y la estructura celular de las espumas producidas a partir de esas mezclas; obteniéndose que la nanoestructuración actúa como patrón para la estructura celular, permitiendo obtener una amplia variedad de estructuras celulares y en particular de estructuras nanocelulares.Se ha demostrado que los parámetros de procesado, como la presión y temperatura,permiten diferenciar entre dos rutas de espumado y presentan una influencia significativa en las características finales de las espumas de PMMA puro, pero no en las mezclas de PMMA/MAM. Estas mezclas presentan un mecanismo de nucleación heterogénea controlado por la nanoestructuración, que evita que los parámetros de procesado influyanen el proceso de nucleación de las celdas. Además, algunas mezclas de PMMA/MAM también presentan una alta estabilidad durante el crecimiento de las celdas, evitando el colapso de la estructura celular y la coalescencia.Finalmente, se ha estudiado la influencia en las propiedades de las espumas de la transición entre el rango microcelular y el rango nanocelular; obteniéndose que hay una clara influencia sobre la conductividad térmica, que decrece en las espumas nanocelulares debido al efecto Knudsen, y sobre la temperatura de transición vítrea, que se incrementa debido al confinamiento de las cadenas poliméricas en las paredes de las celdas, pero no sobre el módulo de Young
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Massoud, Mouhannad. "Experimental characterization of heat transfer in nanostructured silicon-based materials". Thesis, Lyon, 2016. http://www.theses.fr/2016LYSEI063/document.
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Ce mémoire de thèse aborde la caractérisation expérimentale du transfert thermique à l’échelle nanométrique dans des matériaux compatibles avec les procédés de la micro-électronique. Pour cela deux techniques de caractérisation sont appliquées chacune à deux différents systèmes, le silicium mésoporeux irradié et les membranes de silicium suspendues. La première technique de caractérisation est la thermométrie micro-Raman. La puissance du laser chauffe l'échantillon exposé. La détermination de la conductivité thermique nécessite la modélisation de la source de chaleur par la méthode des éléments finis. Dans les cas considérés la modélisation de la source de chaleur repose sur différents paramètres qui doivent être soigneusement déterminés. La seconde technique de caractérisation est la microscopie à sonde locale (d’acronyme anglais SThM), basée sur le principe de la microscopie à force atomique (d’acronyme anglais AFM). Utilisée en mode actif, la sonde AFM est remplacée par une sonde résistive de type Wollaston qui est chauffée par effet Joule. Utilisée en mode AFM contact, cette technique permet une excitation thermique locale du matériau étudié. La détermination de la conductivité thermique nécessite l'analyse de la réponse thermique de la sonde au moyen d'échantillons d'étalonnage et également via la modélisation dans le cas des géométries complexes. L'effet de la position de la pointe sur le transfert de chaleur entre la pointe et l'échantillon est étudié. Une nouvelle méthode de découplage entre le transfert de chaleur entre la pointe et l'échantillon, respectivement à travers l'air et au contact, est proposée pour la détermination de la conductivité thermique des géométries complexes. Les résultats obtenus avec les deux techniques pour les échantillons de silicium mésoporeux irradiés à l’aide d’ions lourds dans le régime électronique sont en bon accord. Ils montrent la dégradation de la conductivité thermique du silicium mésoporeux suite à une augmentation dans la phase d’amorphe lorsque la dose d’irradiation croît. Les résultats obtenus sur les membranes de silicium suspendues montrent une réduction de la conductivité thermique de plus de 50 % par rapport au silicium massif. Lorsque la membrane est perforée périodiquement afin de réaliser une structure phononique de période inférieure à 100 nm, cette réduction est approximativement d’un ordre de grandeur. Un chapitre introduisant un matériau prometteur à base de silicium pour observer des effets de cohérence phononique conclut le manuscritThis PhD thesis deals with the experimental characterization of heat transfer at the nanoscale in materials compatible with microelectronic processes. Two characterization techniques are applied to two different systems, irradiated mesoporous silicon and suspended silicon membranes. The first characterization technique is micro-Raman thermometry. The laser power heats up the exposed sample. The determination of the thermal conductivity requires the modeling of the heat source using finite element simulations. The modeling of the heat source relies on different parameters that should be carefully determined. The second characterization technique is Scanning Thermal Microscopy (SThM), an Atomic Force Microscopy (AFM)-based technique. Operated in its active mode, the AFM probe is replaced by a resistive Wollaston probe that is heated by Joule heating. Used in AFM contact mode, this technique allows a local thermal excitation of the studied material. The determination of the thermal conductivity requires the analysis of the thermal response of the probe using calibration samples and modeling when dealing with complicated geometries. The effect of the tip position on heat transfer between the tip and the sample is studied. A new method decoupling the heat transfer between the tip and the sample, at the contact and through air, is proposed for determining the thermal conductivity of complicated geometries. The results obtained from the two techniques on irradiated mesoporous silicon samples using heavy ions in the electronic regime are in good agreement. They show a degradation of the thermal conductivity of mesoporous silicon due to the increase in the amorphous phase while increasing the ion fluence. The results obtained on suspended silicon membrane strips show a decrease in the thermal conductivity of more than 50 % in comparison to bulk silicon. When perforated into a phononic structure of sub-100 nm period, the membrane thermal conductivity is about one order of magnitude lower than the bulk. A chapter introducing a promising silicon-based material for the evidence of phonon coherence concludes the manuscript
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Szeifert, Johann Martin [Verfasser], i Thomas [Akademischer Betreuer] Bein. "Mesoporous Titania Materials : Tuning and Optimizing Nanostructures and Porous Morphologies / Johann Szeifert. Betreuer: Thomas Bein". München : Universitätsbibliothek der Ludwig-Maximilians-Universität, 2011. http://d-nb.info/1015083846/34.
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Araújo, Sandra Maria Santos de Oliveira 1954. "Obtenção e caracterização de corpos densos e porosos de campósitos de alumina e zircônia para utilização como biomaterial". [s.n.], 2012. http://repositorio.unicamp.br/jspui/handle/REPOSIP/263580.
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Orientador: Cecília Amélia de Carvalho ZavagliaTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica
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Resumo: Nesta tese foram investigadas as propriedades físicas, mecânicas e microestruturais de compósitos cerâmicos densos e porosos de Al2O3-ZrO2 cujas matérias primas foram previamente moídas em moinho vibratório com a finalidade de se obter nanocompósitos com melhores propriedades que as cerâmicas de alumina e de zircônia puras, e compósitos microestruturados. A finalidade desses estudos foi desenvolver um processamento de matérias primas para aplicações biomédicas futuras, como por exemplo: cabeça de fêmur e acetábulo cerâmicos, para implantes coxofemorais, pilares cerâmicos, para implantes dentais e braquetes cerâmicos, usados em ortodontia. As matérias primas, Al2O3 e ZrO2-3%Y2O3 foram caracterizadas quanto à composição e suas estruturas cristalinas. Foram cominuídas em moinho vibratório desenvolvido na Escola de Engenharia de São Carlos-USP, por 2, 4, 6 e 10 horas. Os pós resultantes da moagem por seis horas foram misturados e homogeneizados em três proporções, 15, 30 e 45 % de zircônia em alumina por 22 horas. O corpo denso foi conformados convencionalmente, por prensagem uniaxial (50MPa), prensagem isostática (200MPa) e sinterização em 1450°C por 2 horas. Por seu conjunto de características mecânicas a composição com 30% de zircônia e 70% de alumina foi usada para produção do corpo poroso, características estas superiores tanto às do compósito nanoestruturado como às do corpo monolítico e compatíveis à aplicação estrutural. O corpo poroso foi obtido pelo método da esponja, sinterizado em 1600°C e apresentou resistência à compressão de 6,71 MPa, valor que está contido na faixa de resistência do osso esponjoso para uma porosidade acima de 60%, poros interconectados e de tamanho compatíveis aos exigidos pela engenharia tecidual. O teste de citotoxicidade confirmou a biocompatibilidade do compósito poroso. A biocompatibilidade associada ao valor da resistência mecânica à compressão e ao tamanho dos poros permite afirmar a potencialidade do compósito obtido nas condições do trabalho como material a ser testado para crescimento de células
Abstract: In this thesis it was investigated the mechanical properties of a Al2O3-ZrO2 ceramic composite which raw materials were previously ground on a vibratory mill in order to obtain a micro structured nanocomposite with better properties than pure alumina and zirconium. The purpose of this paper was to develop raw materials for future biomedical applications, as: femoral head and ceramic acetabulum, for hip implants, ceramic abutments, for dental implants and ceramics brackets, used in orthodontics. The raw materials, Al2O3 e ZrO2-3%Y2O3 were characterized as to composition and crystal structures. They were comminuted in a vibratory mill designed by Escola de Engenharia-USP/ São Carlos, for 2, 4, 6 e 10 hours. The 6-hours milling post-derived were mixed and homogenized in three ratios, 15, 30 e 45 % of zirconium in alumina for 22 hours. The dense body was conventionally shaped, by single axial pressing (50MPa), isostatic pressing (200MPa) and sintering in 1450°C for 2 hours. Due the set of mechanical characteristic, compositions 30%-zirconium and 70%-alumina was used to produce the porous body production and supported for structural applications. The porous specimen was obtained by the sponge method sintered at 1600ºC showed a compressive strength of 6,71 MPa, a value which is in the resistance in the range of cancellous bone resistance, for a porosity above 60%, interconnected pores and size compatible with those required by tissue engineering. Citotoxicity test confirmed the composite biocompatibility. Biocompatibility associated with mechanical strength and pores size allows to affirm the potential of the composite obtained in those conditions as a material to be tested for cell growth
Doutorado
Materiais e Processos de Fabricação
Doutora em Engenharia Mecânica
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Letant, Sonia. "Transfert d'excitation dans les nanocomposites à base de silicium poreux". Université Joseph Fourier (Grenoble), 1998. http://www.theses.fr/1998GRE10117.
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Ce travail a ete consacre a l'etude du transfert d'excitation dans les nanocomposites a base de silicium poreux. Le but etait d'etudier le couplage des porteurs photogeneres dans les nanocristaux de silicium avec leur environnement, liquide, solide ou gazeux. Nous presentons ici l'investigation par des methodes de luminescence continue et resolue dans le temps, de trois structures composites : * le silicium poreux dans sa solution acide de formation : un processus de photodissolution des couches poreuses sous lumiere est mis en evidence et caracterise ; dans ce cas, les porteurs fuient physiquement les cristallites pour participer a la reaction photochimique permettant le passage des atomes de silicium dans la solution. * le silicium poreux impregne de colorants laser : il est demontre que les couches poreuses peuvent etre utilisees comme matrice d'accueil passive (excitation directe des molecules) ou active (transfert d'excitation de la matrice vers les molecules via un couplage dipolaire). * le silicium poreux couvert de liaisons si-h : une conversion de l'energie optique en energie vibrationnelle via un couplage dipolaire entre les porteurs et les vibrations de surface a lieu. Le role important de la surface specifique est alors mis en evidence malgre l'origine quantique de l'emission. Il ressort de cette etude que le silicium poreux, malgre sa faible efficacite quantique, est une bonne matrice d'accueil, grace a sa porosite ouverte et a sa grande surface specifique, et qu'il possede les proprietes d'un donneur d'excitation.
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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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Wanibuchi, Mizue. "Three-dimensional Structural Effects of Porous Materials on the Direct-electron-transfer-type Bioelectrocatalysis of Bilirubin Oxidase". Doctoral thesis, Kyoto University, 2021. http://hdl.handle.net/2433/263704.
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Ünal, Bayram. "Optical, electrical and structural properties of nanostructured silicon and silicon-germanium alloys". Thesis, De Montfort University, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.391480.
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Bao, Zhihao. "Conversion of 3-D nanostructured biosilica templates into non-oxide replicas". Diss., Georgia Institute of Technology, 2008. http://hdl.handle.net/1853/33983.
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Diatoms possess characteristics such as abundance, diversity, and high reproductivity, which make their nano-structured frustules (diatom frustules) attractive for a wide range of applications. To overcome the limitation of their silica based frustule composition, diatom frustules have been converted into a variety of materials including silicon, silicon carbide, silver, gold, palladium and carbon in the present study. The compositions and the extent of shape preservation of the replicas are examined and evaluated with different characterization methods such as X-ray diffraction, SEM, TEM and FTIR analyses. These replicas still retained the complex 3D structures and nano-scaled features of the starting diatom frustules. Some properties and possible applications of converted materials are explored and the kinetics and thermodynamics related to the successful replications (conversions) are also studied and discussed.
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Treideris, Marius. "Formation and investigation of hybryd nanostructures". Doctoral thesis, Lithuanian Academic Libraries Network (LABT), 2011. http://vddb.laba.lt/obj/LT-eLABa-0001:E.02~2011~D_20111102_110700-00011.
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Over the past decade, the intensive development of nanotechnology was made to increase significantly the number of methods to form the structures of a size between 1 and 100 nm. It should be emphasized that nanostructured materials are interesting both because of perspectives in practical applications and new physical phenomena. In this work the electrochemical technique for the control of morphology of porous silicon matrix developed. Hybrid por-Si structures with metals were made. The method for infiltration of biomolecules into the porous silicon structures was developed and the interaction between silicon and bio-molecules was investigated. GaP nanostructures were formed by electrochemical etching and the possibilities of their application for gas sensors were estimated. Nanoporous and Fe-doped silica films on Si were made and the developed structures were characterized by their structural, optical or magnetic properties.Pastarąjį dešimtmetį, intensyviai vystantis nanotechnologijoms, ženkliai išaugo technologinių metodų, įgalinančių suformuoti darinius, kuriuose elementų dydžiai būtų tarp 1 ir 100 nm, paieška. Šiai specifinei nanostruktūrinių medžiagų grupei skiriamas ypatingas dėmesys dėl naujų fizikinių reiškinių ir ypač - praktinių taikymų, kuriuos atveria šie dariniai. Šiame darbe aptariamos elektrocheminės technologijos, skirtos kontroliuojamos morfologijos porėtojo silicio formavimui. Suformuoti hibridiniai por-Si dariniai su metalais. Sukurta biomolekulių įterpimo į porėtuosius silicio darinius technologija bei tirta biomolekulių sąveika su kietakūniais padėklais. Nagrinėjami GaP nanodarinių formavimo elektrocheminio ėsdinimo būdu dėsningumai bei jų taikymo galimybės dujų sensoriuose. Įsisavinta nanoporėtųjų dielektrinių terpių ir hibridinių nanodarinių formavimo technologija bei tirtos jų savybės.
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Zhang, Yuelan. "Synthesis and Characterization of Nanostructured Electrodes for Solid State Ionic Devices". Diss., Georgia Institute of Technology, 2006. http://hdl.handle.net/1853/14000.
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The demands for advanced power sources with high energy efficiency, minimum environmental impact, and low cost have been the impetus for the development of a new generation of batteries and fuel cells. One of the key challenges in this effort is to develop and fabricate effective electrodes with desirable composition, microstructure and performance. This work focused on the design, fabrication, and characterization of nanostructured electrodes in an effort to minimize electrode polarization losses.
Solid-state diffusion often limits the utilization and rate capability of electrode materials in a lithium-ion battery, especially at high charge/discharge rates. When the fluxes of Li+ insertion or extraction exceed the diffusion-limited rate of Li+ transport within the bulk phase of an electrode, concentration polarization occurs. Further, large volume changes associated with Li+ insertion or extraction could induce stresses in bulk electrodes, potentially leading to mechanical failure. Interconnected porous materials with high surface-to-volume ratio were designed to suppress the stress and promote mass transport. In this work, electrodes with these unique architectures for lithium ion batteries have been fabricated to improve the cycleability, rate capability and capacity retention.
Cathodic interfacial polarization represents the predominant voltage loss in a low-temperature SOFC. For the first time, regular, homogeneous and bimodal porous MIEC electrodes were successfully fabricated using breath figure templating, which is self-assembly of the water droplets in polymer solution. The homogeneous macropores promoted rapid mass transport by decreasing the tortuosity. And mesoporous microstructure provided more surface areas for gas adsorption and more TPBs for the electrochemical reactions. Moreover, composite electrodes were developed with a modified sol-gel process for honeycomb SOFCs. The sol gel derived cathodes with fine grain size and large specific surface area, showed much lower interfacial polarization resistances than those prepared by other existing processing methods.
Nanopetals of cerium hydroxycarbonate have been synthesized via a controlled hydrothermal process in a mixed water-ethanol medium. The formation of the cerium compound depends strongly on the composition of the precursors, and is attributed to the favored ethanol oxidation by Ce(IV) ions over Ce(IV) hydrolysis process. Raman studies showed that microflower CeO2 preferentially stabilizes O2 as a peroxide species on its surface for CO oxidation.
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Silva, Karina Rodrigues da. "Caracterização da alumina anódica porosa modificada por plasma". Universidade Federal de São Carlos, 2015. https://repositorio.ufscar.br/handle/ufscar/8331.
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In this study, the wettability of porous anodic alumina (PAA) surfaces modified by plasma was investigated. The porous anodic alumina films were grown on aluminum substrate using a two step anodization procedure in oxalic acid solution under potentiostatic regime. The surfaces of PAA films were modified by plasma treatment or plasma deposition techniques. Prior to surface modification, the impurities were removed by a plasma cleaning procedure. Oxygen was used in plasma treatment in order to produce hydrophilic surfaces. On the other hand, the plasma deposition (in HMDSO or HMDSO + argon mixture) was performed to produce hydrophobic surfaces or less hydrophilic surface. Electropolished aluminum without PAA film were used as reference. The influence of substrate morphology on wettability was analyzed. The morphological characterization was performed by scanning electron microscopy (SEM). The microstructural analysis was carried out using Fourier Transformed Infrared Spectroscopy (FTIR). A goniometer was used to measure the contact angle and evaluate the wettability of electroplished aluminum and PAA films. The results showed that the wettability of the samples was affect by chemical interactions of functional groups on the surface deposited after plasma treatment. The effect of the porous surface morphology on wettability was not significant compared to the plasma treated films with new chemical interactions effects.
Neste trabalho foram investigadas as propriedades de molhabilidade das superfícies nanoestruturadas da alumina anódica porosa (AAP) modificadas por plasma. Os filmes de AAP foram produzidos sobre substrato de alumínio pelo método de anodização potenciostática em duas etapas em solução de ácido oxálico. Após a fabricação, as amostras foram submetidas a um tratamento a plasma (com oxigênio) ou a deposição a plasma (em HMDSO ou em uma mistura de HMDSO e argônio). Antes das modificações das superfícies, removeram-se as impurezas das amostras através de técnicas de limpeza a plasma. No tratamento a plasma, o gás oxigênio foi utilizado para a obtenção de superfícies hidrofílicas. Por outro lado, para tornar a superfície hidrofóbica ou menos hidrofílica, foram feitas duas séries de deposição a plasma, uma contendo uma mistura de argônio e HMDSO e outra série somente com HMDSO. O tratamento ou deposição a plasma também foram feitas em amostras de alumínio eletropolido, sem a camada de AAP, a fim de verificar a influência morfológica do substrato na molhabilidade. A caracterização morfológica dos filmes de AAP foi feita por microscopia eletrônica de varredura (MEV), onde foi verificada a formação dos poros na superfície. A caracterização microestrutural foi feita por espectroscopia de absorção no infravermelho por transformada de Fourier (FTIR) com o objetivo de verificar as alterações químicas na superfície. A molhabilidade foi analisada utilizando um goniômetro, equipamento que realiza medição direta do ângulo de contato. Os resultados mostram que a molhabilidade da superfície é afetada por interações químicas dos grupos funcionais na superfície dos filmes. Por outro lado, o efeito da morfologia sobre a molhabilidade da superfície não é significativo nas condições estudadas.
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Ebert, T., A. Wollbrink, A. Seifert, R. John i S. Spange. "Multiple polymerization – formation of hybrid materials consisting of two or more polymers from one monomer". Universitätsbibliothek Chemnitz, 2017. http://nbn-resolving.de/urn:nbn:de:bsz:ch1-qucosa-220106.
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Hybrid materials consisting of three different components were synthesized by the polymerization of one heterotrifunctional monomer in just one reaction step using, at the most, one catalyst. The polymerization of 2-furfuyloxy-2-methyl-4H-1,3,2-benzodioxasiline leading to a hybrid material consisting of phenolic resin, poly(furfuryl alcohol), and polymethylsilsesquioxane is, to the best of our knowledge, the first polymerization of this kind. The influence of different catalysts on the polymerization behavior and thus on the structure of the hybrid material was investigated. In accordance with the term “twin polymerization”, which is used for the polymerization of one monomer yielding two separate polymers, this type of polymerization could be called “triple polymerization”. The term “multiple polymerization” is introduced as a general term for the underlying concept of the synthesis of multiple polymers starting from one monomer in one process stepDieser Beitrag ist aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich
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Duong, Tuan Nghia. "Développement de la polarisation dynamique nucléaire à haut champ magnétique pour la caractérisation des matériaux nanostructurés". Thesis, Université Grenoble Alpes (ComUE), 2015. http://www.theses.fr/2015GREAV019/document.
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La spectroscopie de RMN des solides est une méthode de choix pour la caractérisation de la structure et de la dynamique à l'échelle atomique des matériaux ordonnés et désordonnés. Cependant, l'utilisation de cette technique est limitée par son manque de sensibilité qui empêche l'observation de la surface des matériaux, souvent responsable de leurs propriétés chimiques. Il a été récemment montré que la Polarisation Nucléaire Dynamique (en anglais, Dynamic Nuclear Polarization, DNP) dans les conditions de rotation à l'angle magique (en anglais Magic-Angle Spinning, MAS) permet de surmonter cette limitation. Cette technique permet d'augmenter la sensibilité de la RMN de plusieurs ordres de grandeur. Elle consiste à transférer la polarisation élevée des électrons non-appariés vers les noyaux grâce une irradiation micro-onde. L'objectif de cette thèse consiste à appliquer la MAS-DNP pour sonder la structure de matériaux nanostructurés inorganiques et hybrides. Ces nouvelles informations faciliteront l'amélioration raisonnée de leurs propriétés. Deux classes de matériaux ont été étudiées : des nanoparticules (NP) de silice fonctionnalisées avec des chaînes siloxane et deux formes d'alumine. Les NP de silice fonctionnalisées permettent d'accroître la durée de vie des piles à combustible. Grâce au gain en sensibilité offert par la DNP, il a été possible de sonder les connectivités et les proximités 29Si-29Si dans ces matériaux et ainsi d'élucider le mode de condensation des chaînes siloxane à la surface des NP de silice. La seconde classe de matériaux étudiés comprend deux formes d'alumine : l'alumine- et l'alumine mésoporeuse. La première est largement utilisée dans l'industrie comme catalyseur, support de catalyseur et adsorbant, tandis que la seconde est un matériau prometteur du fait de sa porosité contrôlée et de son accessibilité élevée. Néanmoins, la structure de ces alumines est toujours largement débattue car elles ne forment pas des monocristaux. Grâce à une meilleure compréhension des performances de la MAS-DNP, conduisant notamment à une optimisation de la préparation des échantillons, il a été possible de compenser la très faible efficacité des expériences 27Al sélectives de la surface. La structure de la surface d'alumine a été sondée par des expériences RMN avancées à deux dimensions et une nouvelle expérience a été proposée pour l'observation sélective du cœur de l'alumine. Afin d'obtenir davantage d'informations sur les proximités 27Al-27Al, nous avons cherché à mieux comprendre les séquences de recouplage dipolaire homonucléaire pour des noyaux 27Al. Pour ce faire, la dynamique de spin au cours de ces séquences a été analysée par la théorie de l'hamiltonien moyen et des simulations numériques. En résumé, au cours de cette thèse, nous avons montré comment la MAS-DNP ouvre de nouvelles perspectives pour l'étude des matériaux nanostructurésSolid-state NMR spectroscopy is a powerful analytical technique to characterize the atomic-level structure and dynamics of both ordered and disordered materials. However, its main limitation is the lack of sensitivity, particularly preventing studies on the surface of materials, an important region determining their chemical properties. It has been recently shown that Magic Angle Spinning Dynamic Nuclear Polarization (MAS-DNP) could overcome this difficulty. This technique can provide an enhancement of NMR sensitivity of many orders of magnitude. It is based on the partial microwave-driven transfer of the large intrinsic polarization of electron spins to nuclear spins, making impractical NMR experiments feasible. The aim of this work is to use this MAS-DNP technique to help gain new insights into the structure of inorganic and hybrid nanostructured materials. Such knowledge will facilitate the rational improvement of their properties. Two classes of materials are investigated. The first ones are siloxane-functionalized silica nanoparticles (NPs), which can be used to extend the working durability of fuel cells. Owing to the sensitivity enhancement achieved by MAS-DNP, the condensation network structure of siloxanes bound to the surface of silica NPs could be elucidated using 29Si-29Si homonuclear correlation NMR experiments. The second class of investigated systems encompasses two forms of aluminas, -alumina and mesoporous alumina. The former is widely used in industry as a catalyst, catalyst support, and adsorbent, whereas the latter is a promising material owing to its highly controlled porosity and its high surface accessibility. Nevertheless, their structures are still under heavy investigation since they do not form single crystals. Due to an improved comprehension of MAS-DNP performance, including optimized sample preparation, the obstacle of extremely low efficiency for surface-selective 27Al NMR experiments is circumvented. Sophisticated two-dimensional NMR experiments are employed to provide selective insights into structures on the surface and a new experiment is proposed to study only the bulk of these materials. For achieving further information on the spatial proximities between different 27Al sites, a thorough understanding of homonuclear dipolar recoupling pulse sequences for half-integer quadrupolar nuclei is required. In order to do this, Average Hamiltonian theory and numerical simulations are used to analyze the spin dynamics resulting from these pulse sequences, giving insights into their relative performances. Overall, it is shown that the use of MAS-DNP can be crucial for the characterization of state-of-the-art materials, highlighting the future importance of this technique
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Kitschke, Philipp. "Experimental and theoretical studies on germanium-containing precursors for twin polymerization". Doctoral thesis, Universitätsbibliothek Chemnitz, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:ch1-qucosa-205443.
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Im Fokus dieser Arbeit standen zwei Ziele. Zum einem war es Forschungsgegenstand, dass Konzept der Zwillingspolymerisation auf germaniumhaltige, molekulare Vorstufen wie zum Beispiel Germylene, spirozyklische Germaniumverbindungen und molekulare Germanate zu erweitern und somit organisch-anorganische Komposite beziehungsweise Hybridmaterialien darzustellen. Dazu wurden neuartige Germaniumalkoxide auf der Basis von Benzylalkoholaten, Salicylalkoholaten sowie Benzylthiolaten synthetisiert, charakterisiert und auf ihre Fähigkeit Komposite beziehungsweise Hybridmaterialien über den Prozess der Zwillingspolymerisation zu erhalten studiert.
Ein zweites Ziel dieser Arbeit war es, Beziehungen zwischen der Struktur und der Reaktivität dieser molekularen Vorstufen sowie deren Einfluss auf die Eigenschaften der erhaltenen Polymerisationsprodukte zu identifizieren und systematisch zu untersuchen. Hierfür wurden zum einen verschiedene Substituenten, welche unterschiedliche elektronische sowie sterische Eigenschaften aufweisen, an den aromatischen Einheiten der molekularen Vorstufen eingeführt. Die Effekte der Substituenten auf den Prozess der Zwillingspolymerisation und auf die Eigenschaften der Komposite beziehungsweise Hybridmaterialien wurden für die Verbindungsklasse der Germanium(II)salicylalkoholate, der molekularen Germanate sowie der spiro-zyklischen Siliziumsalicylalkoholate untersucht. Spirozyklische Siliziumsalicylalkoholate, wie zum Beispiel 4H,4’H-2,2‘-Spirobi[benzo[d][1,3,2]dioxasilin], wurden im Rahmen dieser Arbeit mit einbezogen, da sie aufgrund ihres nahezu idealen Zwillingspolymerisationsprozesses geeignete Modelverbindungen für Reaktivitätsstudien darstellen. Zudem wurde der Einfluss der Substituenten auf die Charakteristika der aus den Kompositen beziehungsweise Hybridmaterialien erhaltenen Folgeprodukte (poröse Kohlenstoffmaterialien und oxydische Materialien) studiert. Des Weiteren wurde eine Serie von spirozyklischen Germaniumthiolaten, welche isostrukturell zu 4H,4’H-2,2‘-Spirobi[benzo[d][1,3,2]dioxasilin] sind, synthetisiert, um systematisch den Einfluss der Chalkogenide, Sauerstoff und Schwefel, in benzylständiger sowie phenylständiger Position auf deren Reaktionsvermögen im Polymerisationsprozess zu untersuchen.
Die experimentellen Ergebnisse zu den Struktur-Reaktivitätsbeziehungsstudien wurden, soweit es jeweils durchführbar war, mittels quantenchemische Rechnungen validiert und die daraus gezogenen Schlüsse in die Diskussion zur Interpretation der experimentellen Ergebnisse mit einbezogen.
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Finnemore, Alexander. "On biomimetic nanostructured materials". Thesis, University of Cambridge, 2012. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.610543.
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Smith, Steven P. "Lanthanide-containing Nanostructured Materials". Diss., The University of Arizona, 2011. http://hdl.handle.net/10150/145459.
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The research described in this Dissertation is concerned generally with the exploration of the potential use of lanthanide elements in nanostructured materials for the purpose of modification of the magnetic and optical properties. This is explored through a focus on the development of lanthanide-containing iron oxide nanosystems. Our objectives of producing lanthanide containing nanostructured materials with potentially useful optical and magnetic applications has been achieved through the development of lanthanide-doped Fe3O4 and -Fe2O3 nanoparticles, as well as a unique core-shell magnetic-upconverting nanoparticle system.Necessary background information on nanomaterials, rationale for the study of lanthanide-containing iron oxide nanosystems and context for discussion of the results obtained in each project is provided in the Introduction Chapter. The syntheses of Fe3O4 nanoparticles doped with Eu(III) and Sm(III) are discussed, along with structural characterization and magnetic property investigation of products In Chapter 2. The following Chapter expands the study of lanthanide doping to -Fe2O3, a closely related yet distinct magnetic nanoparticle system. A completely different synthesis is attempted, and comparisons between the two systems are made.The development of novel synthetic methodologies used to create such products has yielded high-quality lanthanide-containing materials and are evidenced by TEM images displaying nearly monodisperse particles in each of our efforts. The modifications to the magnetic properties resulting from lanthanide doping include theobservation of ferromagnetism in the Fe3O4 system and increased magnetic saturation of -Fe2O3 nanoparticles, and are characterized by VSM and the visual observation of magnetic alignment of products. Our efforts towards developing a novel methodology capable of producing high quality Fe3O4 nanoparticles, and subsequent characterization of products, were published in the Journal of the American Chemical Society.Optically active, magnetic, core-shell nanoparticles are investigated in Chapter 4 for the potential uses in diagnosis and treatment of cancer. This multifunctional system uses Fe3O4 as a magnetic core, shelled by upconverting lanthanide-containing nanomaterials, and is rendered biocompatible through encapsulation of the core-shell structure by a silica shell. Added functionality is achieved through amine functionalization of the silica surface, with the goal of coupling the inorganic nanoparticle with drug targeting groups. TEM results indicate successful formation of the core-shell nanoparticles, and expected magnetic and optical properties are shown by visual observation and luminescence spectroscopy, respectively.
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Guillemin, Yann. "Électrogénération sol-gel de films minces siliceux mésostructurés : méthylation, variations structurales, contrôle morphologique et microlithographie". Thesis, Université de Lorraine, 2012. http://www.theses.fr/2012LORR0249/document.
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Grâce à un mécanisme coopératif d'auto-assemblage électro-assisté ("Electro-Assisted Self-Assembly" : EASA), l'électrogénération de couches minces sol-gel à partir d'un sol constitué d'alcoxysilanes et d'un tensioactif cationique (bromure de cétyltriméthylammonium : CTAB) permet l'accès à des films mésostructurés présentant des mésopores orientés perpendiculairement au support. Des films mésostructurés à base de silice méthylée présentant une porosité organisée et "verticalement" orientée ont été électrogénérés en réalisant la co-condensation en une étape d'un alcoxysilane et d'un organo-alcoxysilane en présence de CTAB. Une étude des transferts de matière au sein de ces couches minces démontre que leur perméabilité peut être modulée par la teneur en groupements -CH3. Le procédé EASA a ensuite été étendu à l'utilisation de sols principalement aqueux. Ceci permet l'accès à de nouvelles structures, au contrôle de l'orientation du réseau poreux et à la possibilité de moduler la morphologie du matériau déposé en faisant varier les contre-anions associés aux édifices micellaires. Différentes stratégies de synthèse visant à augmenter la porosité de films électrogénérés ont été évaluées (utilisation d'agents gonflants et d'un copolymère triblocs). Des résultats probants concernant l'électrogénération de couches minces à porosité hiérarchisée (interconnexion de mésopores et de macropores) sont aussi présentés. Enfin, la dernière partie s'attache à étendre le concept EASA à l'échelle locale (micrométrique) par l'utilisation d'un microscope électrochimique à balayage en tant que moyen de synthèse, ceci ouvrant la voie à l'électromicrolithographie sol-gelThanks to an Electro-Assisted Self-Assembly (EASA) cooperative process, the sol-gel electrogeneration of silica thin films from sols containing alkoxysilanes and cationic surfactant molecules (cetyltrimethylammonium: CTAB) allows to obtain mesostructured films exhibiting mesopore channels orthogonal to the substrate. Organized methylated silica thin films with "vertically"-aligned mesopores were electrogenerated by performing a one-step co-condensation between alkoxysilanes and organo-alkoxysilanes in the presence of CTAB. Monitoring mass transport issues inside these thin layers demonstrates that their permeability can be modulated by the -CH3 moieties ratio. The EASA process was then extended to the use of mainly aqueous sols. This permits the electrogeneration of new structures, the control of the porous network orientation and a modulation of the deposited material morphology by changing the CTA+ counter-anion. Various synthesis strategies aiming at increasing the porosity of electrogenerated films were evaluated (use of swelling agents and a triblock copolymer). Some convincing results dealing with the electrogeneration of silica films exhibiting a hierarchical porosity (combination of mesopores with macropores) are also presented. Finally, the last part of this work demonstrates how the EASA process can be applied at the local scale (micrometric) by using a scanning electrochemical microscope as a synthesis tool, thus opening the way to the sol-gel electromicrolithography
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Озчелік, Батухан. "Сенсор вологості на основі пористих матеріалів". Bachelor's thesis, КПІ ім. Ігоря Сікорського, 2019. https://ela.kpi.ua/handle/123456789/28888.
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Дана дипломна робота містить 99 сторінок загального обсягу, з яких 90 сторінок основного тексту. В структурі роботі міститься 4 таблиці, 24 рисунки, 5 схем, 52 бібліографічні найменування за переліком посилань.
Мета дослідження - ознайомиться з характеристиками і властивостями пористих матеріалів і проаналізувати будову сенсора вологості на основі пористих матеріалів.
Проведено комплексні дослідження пористих матеріалів як основи для виготовлення сенсорів вологості. Розроблено оптимальну технологічну схему і параметри процесу структурування даного приладу.This thesis contains 99 pages of the total volume, of which 90 pages of the main text. The structure of the work contains 4 tables, 24 figures, 5 schemes, 52 bibliographic titles in the list of references. The purpose of the study - acquainted with the characteristics and properties of porous materials and analyze the structure of moisture sensor based on porous materials. Complex researches of porous materials as bases for manufacturing sensors of humidity are carried out. The optimal technological scheme and parameters of the structuring process of this device are developed.
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Ebert, Thomas. "Mehrlingspolymerisation in Substanz und an Oberflächen zur Synthese nanostrukturierter und poröser Materialien". Doctoral thesis, Universitätsbibliothek Chemnitz, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:ch1-qucosa-215817.
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Die vorliegende Arbeit befasst sich mit der Synthese und Charakterisierung von unterschiedlichen nanostrukturierten Hybridmaterialien ausgehend von nur einem Monomer. Dabei wird ein neuartiges Monomer vorgestellt, welches in einem Prozessschritt ein Hybridmaterial bestehend aus drei Polymeren bilden kann. Dies erweitert das Konzept der Zwillingspolymerisation, bei der zwei Polymere aus einem Monomer erhalten werden. Aus diesem Grund wurde der Überbegriff „Mehrlingspolymerisation“ für die Synthese von zwei oder mehr Polymeren aus nur einem Monomer eingeführt. Ein weiterer Schwerpunkt lag auf der gezielten Beschichtung verschiedener Partikeloberflächen mit nanostrukturierten Hybridmaterialien mittels Zwillingspolymerisation. Dabei wird der Einfluss der Oberfläche auf die Polymerisation verschiedener Zwillingsmonomere untersucht. Durch Nachbehandlung sind daraus poröse Kompositmaterialien zugänglich. Je nach Beständigkeit der Substrate sind diese in den Nachbehandlungsschritten stabil oder werden entfernt und dienen nur als Template zur Strukturierung der porösen Materialien. Es wurden unterschiedliche poröse Kohlenstoffe und Kohlenstoffkompositmaterialien hergestellt und charakterisiert. Ausgewählte Materialien wurden mit Schwefel verschmolzen und in Lithium-Schwefel-Zellen untersucht (Kooperation Dr. S. Choudhury, Leibniz-Institut für neue Materialien Saarbrücken).
Die Charakterisierung der Proben erfolgte unter anderem mithilfe der Festkörper-NMR-Spektroskopie, Elektronenmikroskopie, dynamischen Differenzkalorimetrie, Röntgenpulver-diffraktometrie, Infrarotspektroskopie, Raman-Spektroskopie, Thermogravimetrie und Stickstoffsorption.
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Kariuki, Nancy N. "Nanostructured materials for electroanalytical applications". Diss., Online access via UMI:, 2005.
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Assfour, Bassem. "Hydrogen Storage In Nanostructured Materials". Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2011. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-65858.
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Hydrogen is an appealing energy carrier for clean energy use. However, storage of hydrogen is still the main bottleneck for the realization of an energy economy based on hydrogen. Many materials with outstanding properties have been synthesized with the aim to store enough amount of hydrogen under ambient conditions.
Such efforts need guidance from material science, which includes predictive theoretical tools.
Carbon nanotubes were considered as promising candidates for hydrogen storage applications, but later on it was found to be unable to store enough amounts of hydrogen under ambient conditions. New arrangements of carbon nanotubes were constructed and hydrogen sorption properties were investigated using state-of-the-art simulation methods. The simulations indicate outstanding total hydrogen uptake (up to 19.0 wt.% at 77 K and 5.52wt.% at 300 K), which makes these materials excellent candidates for storage applications. This reopens the carbon route to superior materials for a hydrogen-based economy.
Zeolite imidazolate frameworks are subclass of MOFs with an exceptional chemical and thermal stability. The hydrogen adsorption in ZIFs was investigated as a function of network geometry and organic linker exchange. Ab initio calculations performed at the MP2 level to obtain correct interaction energies between hydrogen molecules and the ZIF framework. Subsequently, GCMC simulations are carried out to obtain the hydrogen uptake of ZIFs at different thermodynamic conditions. The best of these materials (ZIF-8) is found to be able to store up to 5 wt.% at 77 K and high pressure.
We expected possible improvement of hydrogen capacity of ZIFs by substituting the metal atom (Zn 2+) in the structure by lighter elements such as B or Li. Therefore, we investigated the energy landscape of LiB(IM)4 polymorphs in detail and analyzed their hydrogen storage capacities. The structure with the fau topology was shown to be one of the best materials for hydrogen storage. Its total hydrogen uptake at 77 K and 100 bar amounts to 7.8 wt.% comparable to the total uptake reported of MOF-177 (10 wt.%), which is a benchmark material for high pressure and low temperature H2 adsorption.
Covalent organic frameworks are new class of nanoporous materials constructed solely from light elements (C, H, B, and O). The number of adsorption sites as well as the strength of adsorption are essential prerequisites for hydrogen storage in porous materials because they determine the storage capacity and the operational conditions. Currently, to the best of our knowledge, no experimental data are available on the position of preferential H2 adsorption sites in COFs. Molecular dynamics simulations were applied to determine the position of preferential hydrogen sites in COFs. Our results demonstrate that H2 molecule adsorbed at low temperature in seven different adsorption sites in COFs. The calculated adsorption energies are about 3 kJ/mol, comparable to that found for MOF systems. The gravimetric uptake for COF-108 reached 4.17 wt.% at room temperature and 100 bar, which makes this class of materials promising for hydrogen storage applications.
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Kubo, Shiori. "Nanostructured carbohydrate-derived carbonaceous materials". Phd thesis, Universität Potsdam, 2011. http://opus.kobv.de/ubp/volltexte/2011/5315/.
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Nanoporous carbon materials are widely used in industry as adsorbents or catalyst supports, whilst becoming increasingly critical to the developing fields of energy storage / generation or separation technologies. In this thesis, the combined use of carbohydrate hydrothermal carbonisation (HTC) and templating strategies is demonstrated as an efficient route to nanostructured carbonaceous materials. HTC is an aqueous-phase, low-temperature (e.g. 130 – 200 °C) carbonisation, which proceeds via dehydration / poly-condensation of carbon precursors (e.g. carbohydrates and their derivatives), allowing facile access to highly functional carbonaceous materials. Whilst possessing utile, modifiable surface functional groups (e.g. -OH and -C=O-containing moieties), materials synthesised via HTC typically present limited accessible surface area or pore volume. Therefore, this thesis focuses on the development of fabrication routes to HTC materials which present enhanced textural properties and well-defined porosity.
In the first discussed synthesis, a combined hard templating / HTC route was investigated using a range of sacrificial inorganic templates (e.g. mesoporous silica beads and macroporous alumina membranes (AAO)). Via pore impregnation of mesoporous silica beads with a biomass-derived carbon source (e.g. 2-furaldehyde) and subsequent HTC at 180 oC, an inorganic / carbonaceous hybrid material was produced. Removal of the template component by acid etching revealed the replication of the silica into mesoporous carbonaceous spheres (particle size ~ 5 μm), representing the inverse morphological structure of the original inorganic body. Surface analysis (e.g. FTIR) indicated a material decorated with hydrophilic (oxygenated) functional groups. Further thermal treatment at increasingly elevated temperatures (e.g. at 350, 550, 750 oC) under inert atmosphere allowed manipulation of functionalities from polar hydrophilic to increasingly non-polar / hydrophobic structural motifs (e.g. extension of the aromatic / pseudo-graphitic nature), thus demonstrating a process capable of simultaneous control of nanostructure and surface / bulk chemistry.
As an extension of this approach, carbonaceous tubular nanostructures with controlled surface functionality were synthesised by the nanocasting of uniform, linear macropores of an AAO template (~ 200 nm). In this example, material porosity could be controlled, showing increasingly microporous tube wall features as post carbonisation temperature increased. Additionally, by taking advantage of modifiable surface groups, the introduction of useful polymeric moieties (i.e. grafting of thermoresponsive poly(N-isopropylacrylamide)) was also demonstrated, potentially enabling application of these interesting tubular structures in the fields of biotechnology (e.g. enzyme immobilization) and medicine (e.g. as drug micro-containers).
Complimentary to these hard templating routes, a combined HTC / soft templating route for the direct synthesis of ordered porous carbonaceous materials was also developed. After selection of structural directing agents and optimisation of synthesis composition, the F127 triblock copolymer (i.e. ethylene oxide (EO)106 propylene oxide (PO)70 ethylene oxide (EO)106) / D-Fructose system was extensively studied. D-Fructose was found to be a useful carbon precursor as the HTC process could be performed at 130 oC, thus allowing access to stable micellular phase. Thermolytic template removal from the synthesised ordered copolymer / carbon composite yielded functional cuboctahedron single crystalline-like particles (~ 5 μm) with well ordered pore structure of a near perfect cubic Im3m symmetry. N2 sorption analysis revealed a predominantly microporous carbonaceous material (i.e. Type I isotherm, SBET = 257 m2g-1, 79 % microporosity) possessing a pore size of ca. 0.9 nm. The addition of a simple pore swelling additive (e.g. trimethylbenzene (TMB)) to this system was found to direct pore size into the mesopore size domain (i.e. Type IV isotherm, SBET = 116 m2g-1, 60 % mesoporosity) generating pore size of ca. 4 nm. It is proposed that in both cases as HTC proceeds to generate a polyfuran-like network, the organised block copolymer micellular phase is essentially “templated”, either via hydrogen bonding between hydrophilic poly(EO) moiety and the carbohydrate or via hydrophobic interaction between hydrophobic poly(PO) moiety and forming polyfuran-like network, whilst the additive TMB presumably interact with poly(PO) moieties, thus swelling the hydrophobic region expanding the micelle template size further into the mesopore range.Nanoporöse kohlenstoffbasierte Materialien sind in der Industrie als Adsorbentien und Katalysatorträger weit verbreitet und gewinnen im aufstrebenden Bereich der Energiespeicherung/erzeugung und für Trennverfahren an wachsender Bedeutung. In der vorliegenden Arbeit wird gezeigt, dass die Kombination aus hydrothermaler Karbonisierung von Zuckern (HTC) mit Templatierungsstrategien einen effizienten Weg zu nanostrukturierten kohlenstoffbasierten Materialien darstellt. HTC ist ein in Wasser und bei niedrigen Temperaturen (130 - 200 °C) durchgeführter Karbonisierungsprozess, bei dem Zucker und deren Derivate einen einfachen Zugang zu hochfunktionalisierten Materialien erlauben. Obwohl diese sauerstoffhaltige Funktionalitäten auf der Oberfläche besitzen, an welche andere chemische Gruppen gebunden werden könnten, was die Verwendung für Trennverfahren und in der verzögerten Wirkstofffreisetzung ermöglichen sollte, ist die mittels HTC hergestellte Kohle für solche Anwendungen nicht porös genug. Das Ziel dieser Arbeit ist es daher, Methoden zu entwickeln, um wohldefinierte Poren in solchen Materialien zu erzeugen. Hierbei führte unter anderem der Einsatz von anorganischen formgebenden mesoporösen Silikapartikeln und makroporösen Aluminiumoxid-Membranen zum Erfolg. Durch Zugabe einer Kohlenstoffquelle (z. B. 2-Furfural), HTC und anschließender Entfernung des Templats konnten poröse kohlenstoffbasierte Partikel und röhrenförmige Nanostrukturen hergestellt werden. Gleichzeitig konnte durch eine zusätzliche Nachbehandlung bei hoher Temperatur (350-750 °C) auch noch die Oberflächenfunktionalität hin zu aromatischen Systemen verschoben werden. Analog zur Formgebung durch anorganische Template konnte mit sog. Soft-Templaten, z. B. PEO-PPO-PEO Blockcopolymeren, eine funktionelle poröse Struktur induziert werden. Hierbei machte man sich die Ausbildung geordneter Mizellen mit der Kohlenstoffquelle D-Fructose zu Nutze. Das erhaltene Material wies hochgeordnete Mikroporen mit einem Durchmesser von ca. 0,9 nm auf. Dieser konnte desweiteren durch Zugabe von Quell-Additiven (z. B. Trimethylbenzol) auf 4 nm in den mesoporösen Bereich vergrößert werden. Zusammenfassend lässt sich sagen, dass beide untersuchten Synthesewege nanostrukturierte kohlenstoffbasierte Materialien mit vielfältiger Oberflächenchemie liefern, und das mittels einer bei relativ niedriger Temperatur in Wasser ablaufenden Reaktion und einer billigen, nachhaltigen Kohlenstoffquelle. Die so hergestellten Produkte eröffnen vielseitige Anwendungsmöglichkeiten, z. B. zur Molekültrennung in der Flüssigchromatographie, in der Energiespeicherung als Anodenmaterial in Li-Ionen Akkus oder Superkondensatoren, oder als Trägermaterial für die gezielte Pharmakotherapie.
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Clavel, Guylhaine. "Magnetic impurities in nanostructured materials". Doctoral thesis, Universidade de Aveiro, 2009. http://hdl.handle.net/10773/3210.
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Doutoramento em QuímicaOs resultados apresentados aqui foram alcançados no âmbito do programa de doutoramento intitulado “Impurezas Magnéticas em Materiais Nanoestruturados”. O objectivo do estudo foi a síntese e caracterização de óxido contendo impurezas magnéticas. Durante este trabalho, sínteses de sol-gel não-aquoso têm sido desenvolvidos para a síntese de óxidos dopados com metais de transição (ZnO e ZrO2). A dopagem uniforme é particularmente importante no estudo de semicondutores magnéticos diluídos (DMSs) e o ponto principal deste estudo foi verificar o estado de oxidação e a estrutura local do dopante e para excluir a existência de uma fase secundária como a origem do ferromagnetismo. Para alargar o âmbito da investigação e explorar plenamente o conceito de "impurezas magnéticas em materiais nanoestruturados" estudamos as propriedades de nanopartículas magnéticas dispersas em uma matriz de óxido. As nanopartículas (ferrita de cobalto) foram depositadas como um filme e cobertas com um óxido metálico semicondutor ou dielétrico (ZnO, TiO2). Estes hetero-sistemas podem ser considerados como a dispersão de impurezas magnéticas em um óxido. As caracterizações exigidas por estes nanomateriais têm sido conduzidas na Universidade de Aveiro e Universidade de Montpellier, devido ao equipamento complementar.
The results presented here have been achieved under the PhD program entitled “Magnetic Impurities in Nanostructured Materials”. This study had as purpose the synthesis and characterization of oxidic semiconductor containing magnetic impurities. During this work we have developed non-aqueous sol-gel routes, leading to well controlled oxide nanomaterials, to the synthesis of transition-metal doped oxides (ZnO and ZrO2). Homogeneous doping is particularly important in the comprehensive study of diluted magnetic semiconductors (DMSs), and the main point of this study was to ascertain the oxidation state and local structure of the dopant, as well as to exclude the existence of secondary phase as the origin of ferromagnetism. To enlarge the field of research and fully explore the concept of “magnetic impurities in nanostructured materials” we have studied the magnetic properties of nanoparticles embedded in an oxide matrix. The nanoparticles (cobalt ferrite) were deposited as a film and coated by a semiconducting or dielectric metal oxide (ZnO, TiO2). These hetero-systems can be regarded as dispersion of magnetic impurities in oxides. The characterizations needed by these nanomaterials were performed at the University of Aveiro and University of Montpellier because of complementary available equipments.
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Li, Guangru. "Nanostructured materials for optoelectronic devices". Thesis, University of Cambridge, 2016. https://www.repository.cam.ac.uk/handle/1810/263671.
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This thesis is about new ways to experimentally realise materials with desired nano-structures for solution-processable optoelectronic devices such as solar cells and light-emitting diodes (LEDs), and examine structure-performance relationships in these devices. Short exciton diffusion length limits the efficiency of most exciton-based solar cells. By introducing nano-structured architectures to solar cells, excitons can be separated more effectively, leading to an enhancement of the cell’s power conversion efficiency. We use diblock copolymer lithography combined with solvent-vapour-assisted imprinting to fabricate nano-structures with 20-80 nm feature sizes. We demonstrate nanostructured solar cell incorporating the high-performance polymer PBDTTT-CT. Furthermore, we demonstrated the patterning of singlet fission materials, including a TIPS-pentacene solar cell based on ZnO nanopillars. Recently perovskites have emerged as a promising semiconductor for optoelectronic applications. We demonstrate a perovskite light-emitting diode that employs perovskite nanoparticles embedded in a dielectric polymer matrix as the emissive layer. The emissive layer is spin-coated from perovskite precursor/polymer blend solution. The resultant polymer-perovskite composites effectively block shunt pathways within the LED, thus leading to an external quantum efficiency of 1.2%, one order of magnitude higher than previous reports. We demonstrate formations of stably emissive perovskite nanoparticles in an alumina nanoparticle matrix. These nanoparticles have much higher photoluminescence quantum efficiency (25%) than bulk perovskite and the emission is found to be stable over several months. Finally, we demonstrate a new vapour-phase crosslinking method to construct full-colour perovskite nanocrystal LEDs. With detailed structural and compositional analysis we are able to pinpoint the aluminium-based crosslinker that resides between the nanocrystals, which enables remarkably high EQE of 5.7% in CsPbI3 LEDs.