D.Phil. (Chemistry) / Please refer to full text to view abstract

The aim of this study was to prepare composite materials based on titanium dioxide (TiO2) and silicon dioxide (SiO2), and to evaluate their photo-catalytic and antimicrobial properties. Carbon and nitrogen doped TiO2nano-particles were prepared via a sol gel synthesis, which is a simple hydrolysis and condensation technique. In situ doping was carried out using glucose and urea as carbon and nitrogen sources respectively. Doping increased the spectral response of titanium dioxide photo-catalyst, allowing it to utilise the visible region which is much wider than the UV region (about 40 % of the solar spectrum), thus making it a more efficient photo-catalyst. The carbon and nitrogen doped TiO2-SiO2nano-particles were immobilized on glass support material to allow for easy separation of the spent photo-catalyst after the photo-degradation process. Tetraethyl orthosilicate (TEOS) was employed as both a binder and precursor for silicon dioxide. A mixture of TiO2 and TEOS in a 1:1 ratio was allowed to polymerize on a glass support which had been treated with hydrofluoric acid to introduce OH groups. The prepared photo-catalytic material was characterized by FT-IR, XRD, DRS, TEM, EDX, and BET analyses. Carbon was found to be more effective as a dopant than nitrogen. It brought about a band gap reduction of 0.30 eV and a BET surface area of 95.4 m2g-1 on the photo-catalyst as compared to a gap reduction of 0.2 eV and surface area of 52.2 m2g-1 for nitrogen doped TiO2. On the other hand, introduction of SiO2 allowed utilization of visible light by the TiO2-SiO2 nano-composite leading to an improved rate of photo-degradation of both methyl orange and phenol red. However, the immobilization of TiO2 on support material made it less effective towards inactivation of E. coli ATCC 25922 bacterial cells when compared to powdered TiO2 which was able to inactivate about 98 % of the bacterial cells within an hour of treatment.

Submitted in fulfilment of the requirements for the degree of Master of Engineering: Mechanical Engineering, Department of Mechanical Engineering, Faculty of Engineering and the Built Environment, Durban University of Technology, Durban, South Africa. 2017. / In this study, the fatigue life of fiber reinforced composite (FRC) materials system was investigated. A nano-filler was used to increase the service life of the composite structures under cyclical loading since such structures require improved structural integrity and longer service life. Behaviour of glass fiber reinforced composite (GFRC) enhanced with various weight percentages (1 to 5 wt. %) of Cloisite 30B montmorillonite (MMT) clay was studied under static and fatigue loading. Epoxy clay nanocomposite (ECN) and hybrid nanoclay/GFRC laminates were characterised using differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). The mechanical properties of neat GFRC and hybrid nanoclay/GFRC laminates were evaluated. Fatigue study of the composite laminates was conducted and presented using the following parameter; matrix crack initiation and propagation, interfacial debonding, delamination and S–N relationship. Residual strength of the materials was evaluated using DMA to determine the reliability of the hybrid nanoclay/GFRC laminates. The results showed that ECN and hybrid nanoclay/GFRC laminates exhibited substantial improvement in most tests when compared to composite without nanoclay. The toughening mechanism of the nanoclay in the GFRC up to 3 wt. % gave 17%, 24% and 56% improvement in tensile, flexural and impact properties respectively. In the fatigue performance, less crack propagations was found in the hybrid nanoclay/GFRC laminates. Fatigue life of hybrid nanoclay/GFRC laminate was increased by 625% at the nanoclay addition up to 3 wt. % when compared to neat GFRC laminate. The residual strength of the composite materials revealed that hybrid nanoclay/GFRC showed less storage modulus reduction after fatigue. Likewise, a positive shift toward the right was found in the tan delta glass transition temperature (Tg) of 3 wt. % nanoclay/GFRC laminate after fatigue. It was concluded that the application of nanoclay in the GFRC improved the performance of the material. The hybrid nanoclay/GFRC material can therefore be recommended mechanically and thermally for longer usage in structural application. / M

M.Sc. (Chemistry) / Please refer to full text to view abstract.

M.Sc. (Chemistry) / The fabrication of multiwalled carbon nanotube/polyvinyl chloride (PVC) composites and a study of their thermal, fire retardancy and mechanical properties are reported. Triphenylphosphine linked - multiwalled carbon nanotube (TPP-MWCNT) and pristine MWCNT were used. The MWCNT were embedded in the polymer matrix through melt blending and solvent casting. The phosphorylation of the MWCNT and their dispersion in the PVC matrix was characterized by scanning electron microscopy and Raman spectroscopy. Thermal analysis of the nanocomposites by thermal gravimetric analysis (TGA) in both solvent casting and melt bending processes, showed different results when compared with the neat PVC. The modulus of the MWCNTs / PVC nanocomposites synthesized via melt blending increased, whilst there was a reduction in their tensile strength, indicating a decrease in polymer toughness. The tensile modulus and strength of MWCNTs / PVC nanocomposite synthesized via Solvent casting decreased whilst there was an increase in Tpp-MWCNT/PVC nanocomposite when compared with its counterpart MWCNTs / PVC nanocomposite, indicating an increase in stiffness and strength. The limited oxygen index (LOI) fire retardant tests of all the neat PVC and its nanocomposites showed no value difference.

>Magister Scientiae - MSc / Magnetic luminescent nanoparticles of an iron oxide (Fe₃O₄) superparamagnetic core and an indium phosphide/zinc selenide (InP/ZnSe) quantum dot shell are reported. The magnetic nanoparticles (MNP’s) and quantum dots (QD’s) were each synthesized separately before conjugation. The MNP’s were functionalized with a thiol-group allowing the QD shell to bind to the surface of the MNP by the formation of a thiol-metal bond. The nanocomposite was capped with 3-mercaptopropionic acid, 1-propanethiol, 2-methyl-1-propanethiol and their properties investigated using the characterization techniques: high- resolution transmission electron microscopy (HR-TEM), energy-dispersive spectroscopy (EDS), UV-vis, scanning electron microscopy (SEM), superconducting quantum interference device (SQUID), and photoluminescence. These techniques yielded significant information on particle size, morphology, dispersion, and chemical composition including luminescence and florescence.

No description available.

Orientador: João Sinézio de Carvalho Campos / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Química / Made available in DSpace on 2018-08-27T19:06:13Z (GMT). No. of bitstreams: 1 Conceicao_RafaelNovaesda_M.pdf: 10111957 bytes, checksum: 9168b5514bd29d6ead99888af5052aab (MD5) Previous issue date: 2015 / Resumo: É bem conhecida a necessidade de energia elétrica para o bem estar e desenvolvimento tecnológico da população em nosso planeta. Ao lado dos avanços científicos de novas tecnologias para geração, existem interesses na melhoria do transporte da energia. Dentre estes se encontram materiais para isolação elétrica de barras estatóricas, quer sejam para melhorar a isolação ou mesmo para reduzir custos. Assim, o presente trabalho visa apresentar resultados da aplicação de uma nova resina epóxi bisfenólica (DGEBF) (RN) à base de nanopartículas de sílica e comparar suas propriedades com a resina epóxi bisfenólica (DGEBA) (RE), atualmente utilizada para a isolação de hidrogeradores. Neste sentido, fabricaram-se protótipos de barras estatóricas, destinadas a hidrogeradores, sendo as resinas impregnadas em sistema VPI (Vácuo-Pressão-Impregnação) e avaliaram-se as propriedades físico-químicas pelas técnicas de viscosimetria, TGA, DSC, MEV e EDS. As propriedades elétricas foram avaliadas pelas técnicas de fator de dissipação (tan delta), descargas parciais, envelhecimento acelerado (VET) e tensão de ruptura. Dentre os resultados das propriedades físico-químicas pode-se comprovar um aumento inicial de três vezes o valor de viscosidade para resina RN em comparação com RE. Entretanto, não houve detrimento das características dielétricas em função da viscosidade, o que foi comprovado através dos resultados de tan delta e VET. Obteve-se um valor de Tg de 116°C e 145°C para RN e RE, respectivamente, o que limitaria a aplicação da resina em geradores por estar abaixo da temperatura de operação. Dentre os resultados dos testes elétricos para as resinas observou-se que: (i) o fator de dissipação e de envelhecimento são praticamente os mesmos para ambas as resinas; (ii) o valor de tip-up resultaram em 0,014 % para RE e 0,020 % para a resina RN, sendo que a norma EN 50209 exige que seja inferior a 0,25% e (iii) a estimativa do tempo de vida útil obtida foi de cerca de 40 anos para os dois tipos de resina, o que é aplicável para maioria dos enrolamentos em operação. Neste sentido sugere-se que a resina RN pode ser uma boa alternativa a resina RE, com um desempenho elétrico equivalente, desde que ajustadas suas condições de processamento e temperatura de aplicação / Abstract: It is well know the demand of electrical energy for the wellbeing and technological development of the population in our planet. Among the scientific development of new technologies for generation, are interests to optimize the energy transport. Among them are materials for electrical insulation of stator bars, whether for improving the insulation or even to reduce the costs. Therefore, the present work aim to present the results of the employment of a new bisphenolic epoxy resin (DGEBF) (RN) containing silica nanoparticles and compare its properties with the bisphenolic epoxy resin (DGEBA) (RE) currently used for the insulation of hydrogenerators. In this context, it was manufactured prototype stator bars, designed for hydrogenerators, being the resins impregnated through VPI (Vacuum-Pressure-Impregnation) system and their physicochemical properties evaluated with the technics of viscosimetry, TGA, DSC, MEV and EDS. The electrical properties were evaluated with the tests of dissipation factor (tan delta), partial discharges, voltage endurance test (VET) and breakdown. Among the results of the physicochemical properties it was possible to verify an initial increase of three times the value of viscosity for RN resin compared to RE. However there was no detriment of the dielectric characteristics depending on the viscosity, what was proven with the results of dissipation factor and VET. It was obtained a value of Tg of 116°C and 145°C for RN and RE respectively, what could limit its employment for hydrogenerators as being below the operational temperature. Among the results of electrical tests for the resins it was observed that: (i) the dissipation factor and VET are practically the same for both resins; (ii) the tip-up value resulted in 0,014% for RE and 0,020% for RN, being required lower than 0,25% according to the norm EN 50209 and (iii) the estimating lifecycle was approximately 40 years for both types of resin, what is applicable for most windings under operation. In this context it is suggested that the RN resin can be a good alternative for RE resin with an equivalent performance once the process conditions and employment temperature are adjusted / Mestrado / Ciencia e Tecnologia de Materiais / Mestre em Engenharia Química

The use of polymer nanocomposites (PNCs) for their unique properties has been around for over a century, used in anything from airplanes to raincoats. In the past 30 years, the fabrication of advanced composite materials has expanded this field into a vast array of applications, tailoring the optical, mechanical, and electrical properties of the material for any specific use. As with any composite, the goal is to take advantage of the desirable properties in each individual component and form an overall superior material. In this body of work, we focus on mixing inorganic nanoparticles (NPs), which are strong and dense, with various polymers, typically used for being tough, light, and easy to work with. The reason for using nano-sized fillers is to maximize the inorganic surface area with which the polymer can interact with, allowing for a minimum amount of filler to be used with maximum benefit, though this is not always practically the case. The interaction between the NP and polymer is only optimized if the NP structure can be controlled. Each of the chapters in this thesis work toward finding new, and practical, methods for understanding and controlling NP dispersions in polymers. In each of the chapters, we focus primarily on the use of silica NPs, ranging from 10-100 nm in diameter, studying methods for controlling their dispersion in polymers like polystyrene (PS), polyethylene (PE), polyisoprene (PI), poly(2-vinyl pyridine) (P2VP), poly(ethylene oxide) (PEO), poly(methyl acrylate) (PMA), and others. First, we take a closer look at how to control and quantify “well-dispersed” NPs in a polymer matrix, taking advantage of various techniques to stabilize the NPs in solution before casting them into the polymer. Once we understand how to reliably disperse the NPs, we can begin to find ways to reorganize them into structures that could provide further improvements in the mechanical properties of the composites, again focusing on methods that would be practically relevant in any polymer system. These techniques take advantage of thermodynamic and kinetic drivers to reorder the NPs in amorphous and semi-crystalline polymers. Forming bound layers of a polymer on a favorably interacting NP surface can stabilize the NPs in a variety of polymer systems, providing initially well-dispersed systems for further study. Alternatively, the grafting of chains onto the NP surface leads to various self-assemblies of the NPs in different matrices, depending on the interaction of the grafted and matrix chains. Starting with well-dispersed NPs in a semi-crystalline polymer allows us to take advantage of the crystallization process to kinetically force NPs into hierarchical structures throughout the composite. This concept alone encompasses a bulk of this thesis – a technique that simply requires the isothermal crystallization of the polymer at different temperatures to achieve vastly different NP structures. Understanding the interaction of the NPs and the crystal is studying using extensive calorimetry and microscopy experiments, specifically determining how to define the confinement of the system due to the presence of NPs and their effect on growth and nucleation. The resulting alignment of NPs into the interlamellar region of the crystal is then analyzed in detail using a correlation function, commonly applied to neat semi-crystalline structures, but applied here for the first time to a PNC. This analysis provides new insights into the alignment process and ways for quantifying the degree of NP alignment. The alignment technique is then applied to several other systems for the specific focus of improving the mechanical properties of unique and industrially relevant PNCs, specifically using polymer grafted NPs. Finally, we briefly discuss the effect of annealing time and temperature on NP dispersion, dynamics, and resulting in unprecedented changes in the macroscopic properties of the material, uncovering new insights in the aging of PNCs. Each of these techniques provides details around controlling the organization and structure of NPs in polymers for the purpose of improving their mechanical properties, all while simply changing the way in which the material is processed.

Polymer nanocomposites are a going part of Materials Science and Engineering. These new composite materials exhibit dimensional and thermal stability of inorganic materials and toughness and dielectric properties of polymers. Development of nanocomposites become an important approach to create high-performance composite materials. In this study silica, fly ash, silica nanotubes and carbon black particles have been added to modify polyurethane foam and thermoplastic polyurethanes. It has been found that the addition of silica can diminish the size of foam bubbles, resulting in an increased stiffness of the material, increase of the compressive strength, and greater resistance to deformation. However, the uniformity of bubbles is reduced, resulting in increased friction of the material. Fly ash added to the foam can make bubbles smaller and improve uniformity of cells. Therefore, the material stiffness and compressive strength, resistance to deformation, and has little impact on the dynamic friction of the material. Adding nanotubes make bubble size unequal, and the arrangement of the bubble uneven, resulting in decreased strength of the material, while the friction increases. After the addition of carbon black to the polyurethane foam, due to the special surface structure of the carbon black, the foam generates more bubbles during the foaming process changing the foam structure. Therefore, the material becomes soft, we obtain a flexible polyurethane foam. The results of mechanical properties determination of the thermoplastic polyurethane that adding particles may increase the stiffness and wear resistance of the thermoplastic polyurethane, while the tensile properties of the material are reduced. This phenomenon may be due to agglomeration of particles during the mixing process. Possibly the particles cannot be uniformly dispersed in the thermoplastic polyurethane.