Thesis (M.S.)--University of Alabama at Birmingham, 2010. / Title from PDF t.p. (viewed July 19, 2010). Includes bibliographical references (p. 67-70).

Phosphorus containing monomers, bis(3-aminophenyl)methyl phosphine oxide (m-DAMPO) and bis(3-aminophenyl)phenyl phosphine oxide (m-DAPPO), were synthesized and incorporated into a thermoplastic poly(arylene ether imide) based upon 2,2'-bis[4-(3,4-dicarboxyphenoxy)phenyl]propane dianhydride and 1,3-phenylene diamine, in order to study their influence on flame resistance and other properties. DAMPO or DAPPO were quantitatively incorporated in concentrations of 25, 50, 75 and 100 mole percent, using the "one pot" ester-acid method. The number average molecular weights of the prepared materials were controlled to 20,000g/mol by off-setting the stoichiomety and endcapping with phthalic anhydride. This strategy enabled one to distinguish the effects of the phosphine oxide incoporation from the influence of molecular weight. The resulting copolymers demonstrated a significant increase in char yield as a function of the phosphine oxide content, thus suggesting improved fire resistance. Glass transition temperatures similar to the control were determined by DSC analysis. Analysis of the mechanical behavior of the DAMPO system at room temperature showed that tensile strength and elongation at failure values were comparable to the control system, while the DAPPO containing copolymers were surprisingly brittle. The influence of the reactive endgroup on the synthesis, cure behavior and network properties of thermosetting polyetherimides was investigated. Reactive phenylacetylene, acetylene and maleimide terminated poly(ether imide) oligomers were prepared and characterized. Optimal reaction conditions were established to produce fully endcapped oligomers with imidized structures and controlled molecular weight. The phenylacetylene endcapped system was synthesized by a conventional ester-acid method. The acetylene endcapped system was prepared via modified ester-acid method and the maleimide endcapped system was fabricated utilizing an amic-acid route. It was determined that phenylethynyl endcapped polymers could be thermally cured at high temperatures (350-380°C) providing good processibility. The networks exhibited thermal stability, chemical resistance and good adhesion strength, ideal as "primary" bonding adhesives. Acetylene and maleimide endcapped systems were prepared for application as "secondary" bonding materials, meaning that they are cured at a lower temperature than that of the Tg of the primary structure. Lap shear test results indicated good adhesion to titanium when cured at 250°C -280°C. The cured materials showed high glass transition temperatures and good thermal and thermo-oxidative stability as determined by DSC, TGA and DMA. Good chemical resistance was demonstrated via solvent extraction measurements. The influence of molecular weight between crosslinks (Mc) on thermal and mechanical behavior was also investigated. Lower molecular weight oligomers exhibited lower Tg and cure temperatures, whereas the cured networks resulting from lower molecular weight oligomers afforded higher Tg and higher gel fractions, but reduced toughness. / Ph. D.

A non-isothermal autohesion model was developed by combining a transient finite element heat transfer model with the isothermal autohesion model. Heat transfer analyses and the interfacial strength development analyses were conducted using the non-isothermal autohesion model on a polysulfone (Udel P1700) compact tension specimen, a 64-ply graphic (Thomel T300)/P1700 unidirectional composite, and a 192-ply graphite (Hercules AS4)/P1700 unidirectional composite. A 64-ply T300/P1700 unidirectional composite was processed in a matched metal mold. Temperature data were taken and compared with the calculated values. Good agreement was observed between the calculated and the measured temperature values. A healing test which aimed at studying the interplay bond development in AS4/P1700 unidirectional composites was performed. The double cantilevered beam (DCD) Mode l fracture toughness test was selected. The DCB specimens were fractured and healed in a special fixture with different combinations of temperature pressure, and time. The healed DCB specimens were refractured and the critical strain energy release rates (G_IC) were measured. The pressure was found to be a key factor in the healing process. Temperature and time dependencies of the interply bond development were also observed. The non-isothermal autohesion model predicted a higher strength achieved in a shorter time. This was due to the extra time which was needed for the fracture interface to achieve intimate contact, and the assumption of the initial intimate contact achievement of the non-isothermal autohesion model. / Master of Science

Les travaux de recherche présentés portent sur l'utilisation des produits de la liquéfaction des écorces d'épicéa dans le phénol pour la préservation du bois. Les produits de la liquéfaction permettent la synthèse d'une résine thermodurcissable de type phénolique. Les résines formulées sont imprégnées dans le bois suivi d'un durcissement in situ. Un prétraitement est mis au point dans le but d'enrichir la fraction phénolique des écorces. Ce prétraitement consiste à hydrolyser les polysaccharides principalement la cellulose et les hémicelluloses dans une solution acide. Ce prétraitement permet d'obtenir un taux de lignine dans les écorces de 60 %, et un taux de cellulose de 28 %. Un procédé de liquéfaction dans un système composé de phénol, d'eau et d'éthanol est optimisé dans le but d'obtenir des taux de liquéfaction supérieur à 85 %, et un taux d'écorces liquéfiées par rapport à la masse de phénol supérieur à 50 %. Les produits de la liquéfaction présentent l'avantage de polymériser sans ajout de formaldéhyde. La durabilité conférée au bois par les résines est bonne, surtout pour les résines phénol/formaldéhyde. Les résines sont peu lessivables. L'imprégnation du bois par les résines provoque un gonflement du bois ce qui améliore la stabilité dimensionnelle de ce dernier / This work focuses on the use of liquefaction products of spruce bark in phenol for the wood preservation. The liquefaction products allow the synthesis of phenolic thermosetting resins. The formulated resins were impregnated into the wood followed by in situ polymerization. A pretreatment was developed in order to increase the phenolic compounds in the spruce bark. This step is an acid hydrolysis of polysaccharides. This pretreatment allowed obtaining a Klason lignin content of 60 %, and a cellulose content of 28 %. A liquefaction process was developed in a mixture of solvent composed of phenol, ethanol, and water. The optimized experimental conditions allowed obtaining a liquefaction yield superior to 85 %, with liqui?ed bark/phenol ratio superior to 50 %. The lique?ed products had the advantage to polymerize without formaldehyde. The resins enhanced the wood durability especially for the phenol/formaldehyde resins. The leaching was low. The wood impregnation allowed a wood swelling, thereby the impregnated wood had a better dimensional stability

Low profile additives (LPA) are thermoplastics that are incorporated to unsaturated polyester (UP) resins in order to improve the surface finish of UP/fibreglass composites, widely used in automotive applications. The effect of using LPA on the thermo-mechanical properties of resin transfer moulded UP/fibreglass composites is investigated. The flexural and shear properties are measured by three-point bending tests. The trend of these mechanical properties is identified for 0% to 40% LPA content. All the mechanical properties like flexural strength, flexural modulus and short beam strength reduce upon addition of LPA. The specimens fail by tension in the flexural test and show a mixed shear/tension failure mode in case of short beam tests. From scanning electron microscopy, morphological change of the fractured surface is observed with an LPA-rich phase. Glass transition temperature (Tg) measured by thermal mechanical analysis (TMA) and dynamic mechanical analysis (DMA) show reproducible data and compare well with each other. Tg is improved by LPA addition due to the development of a more compatible system compared to neat resin. Differential scanning calorimetry (DSC) is also performed to detect Tg, which gives unreliable results.

The interpretation and modelling of the dielectric response of thermosetting materials during cure was the main focus of this study. The equivalence of complex permittivity and complex impedance in terms of information content was outlined in a series of case studies covering the separate effects of dipolar movements and charge migration as well as the combined effect of the two polarisation mechanisms. Equivalent electrical circuits were used in order to model the evolution of the complex impedance during cure. A numerical method that can model consecutive spectra throughout the cure was developed. The method is based on Genetic Algorithms and requires only input from the modelling of the initial spectra. Complex impedance spectra were collected during the cure of a commercial epoxy resin formulation under isothermal and dynamic heating conditions. The spectra were analysed and modelled. The modelling was successful over the whole frequency range of the measurements (1 Hz – 1 MHz). The analysis of the estimated model parameters showed that charge migration dominates the dielectric response in a wide frequency range. In addition, the modelling algorithm also distinguished between the effects of electrode polarisation and dipolar movements in the signal. A new equivalent circuit was used in order to map the frequency regions where the each one of the three phenomena that together comprise the dielectric signal can be monitored most effectively. A chemical cure kinetics model was developed for the studied system. A correlation between the maximum point of the imaginary impedance spectrum and the reaction conversion was established. A mathematical model, based on a simple linear dependence of the dielectric signal on conversion and temperature, was built. The model predictions agreed well with the experimental data. The aim of simplifying the interpretation of the dielectric signals led to the development of a new experimental technique. Temperature Modulated Dielectric Analysis employs temperature modulations superimposed on an underlying thermal profile in order to separate the influence on the signal of the temperature alone from that of the cure reaction. The early study carried out here shows that such measurements are feasible and reveals important issues for its further development.

My thesis presents the process of electromagnet production, including how the process is organised. My goal is to improve these techniques by refining them. To obtain the required data, the company's records were extracted and measurements were taken directly from the manufacturing process. Through examination of the data, any processes which created financial or temporal deficits were identified. Conclusions were then offered to solve these problem areas. These mainly involve alterations to the machinery settings, the delivery of materials and the management of production.

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