This PhD thesis presents an experimental investigation into the tensile properties, strengthening mechanics and failure mechanisms of three-dimensional (3D) woven composites with through-the-thickness (z-binder) reinforcement. 3D composites are being developed for the aerospace industry for structural applications in next-generation aircraft, such as wing panels, joints and stiffened components. The use of 3D woven composites in primary aircraft structures cannot occur until there has been a detailed assessment of their mechanical performance, including under tensile loading conditions. The aim of this PhD project is to provide new insights into the in-plane tensile properties, fatigue life, tensile delamination resistance and failure mechanisms of 3D woven composites with different amounts of z-binder reinforcement. Previous research has revealed that excessive amounts of z-binder reinforcement dramatically improves the tensile delamination toughness, but at the expense of the in-plane structural properties. For this reason, this PhD project aims to evaluate the tensile performance of 3D woven composites with relatively small z-binder contents (less than ~1%). The research aims to provide a better understanding of the manufacture, microstructure and tensile properties of 3D woven composites to assist the process of certification and application of these materials to aircraft structures as well as high performance marine and civil structures.

The tensile behavior of the monolithic amorphous ZrCu and crystalline Cu thin films and the ZrCu/Cu multilayered thin films, coated on polyimide (PI) substrates in different layer thicknesses has been investigated. The scanning electron microscope (SEM) morphology of the as-deposited thin film is composed of sphere domains. Between the domains, stress concentration is induced. The cracks perpendicular to the loading direction would propagate along the domains. The constituent component examined by energy dispersive X-ray spectrometer (EDS) shows that the average composition (in atomic percent) amorphous thin film is Zr46.78Cu53.22, closed to the designed Zr50Cu50 goal. The X-ray diffraction (XRD) results show that the multilayered specimens are composed of both amorphous ZrCu and nanocrystalline Cu crystal structure. As the monolayer thickness become lower, the normalized peak height and grain sizes of Cu become lower. To obtain the mechanical properties of the coated films, deducting the contribution of substrates is used in this study. The tensile Young¡¦s moduli of monolithic amorphous ZrCu and nanocrystalline Cu thin films are close to the results extracted from micro-compression. Based on the current tensile results for the moduli of multilayered thin films, the obtained mechanical data are demonstrated to be reliable and are consistent with the theoretical values predicted by Rule of Mixture. As the thickness decreases from 100 nm down to 10 nm, the tensile Young¡¦s moduli do not vary much. On the other hand, the maximum tensile stress shows strong variation, being highest for the layer thickness of 25 nm. The deformed surface morphologies characterized by scanning electron microscopy also exhibit a similar trend. The optimum tensile properties of the monolithic and multilayered thin film combinations are examined and discussed in this thesis.

The influence of manganese (Mn) addition on the tensile properties of recovery-annealed aluminum alloy sheet was studied. After 200 ~ 220¢X C annealing, these alloys exhibit hardening as compared to the as-rolled state. Besides the amount of Mn in solution, the presence of Fe and Si in these alloys was also a vital factor responsible for the hardening. These recovery annealed aluminum alloy sheets show increased tensile elongation with increasing annealing temperature, which is mainly due to the contribution of post-uniform elongation (PUE). The plastic deformation during PUE is associated with development of fine slip bands distributed in the gauge length of the specimen. It was noted that after recovery anneal, the alloy with 0.74 wt% Mn exhibit better combination of strength and ductility as compared to alloys with lower Mn content. In general, these alloys in partially annealed condition show poor tensile ductility at RT, which is mainly attributed to the low work hardening rate associated with the UFG structure. These partially annealed aluminum alloys exhibit highly anisotropic tensile properties, specially a rather poor ductility along the direction of 45o or 90o from the rolling direction at RT. The poor ductility in 45o or 90o direction could be related to flow localization associated with intense shear banding. Discontinuous yielding plays a pivotal role to trigger the flow localization which is affected by the strain path change. However, for alloys tested at 77 K in 45¢X or 90¢X direction, the deformation proceeds by the propagation of Lüders band initially and followed by strain hardening. In general, the tensile elongation can be enhanced greatly irrespective of the stress direction, because a higher work hardening rate can be maintained due to reduced dynamic recovery rate. The yield stress is orientation dependent, which is in the order of 90¢X > 0¢X > 45¢X. The anisotropic tensile behavior has its origin in the rolling texture. The Schmid factor analysis indicates that specimens tested in 45o direction would have lower yield strength as compared to those tested in 0o or 90o direction. Both experimental measurements and simulation indicate that after 30% tensile straining, the copper texture in the partially annealed aluminum alloy is enhanced 0¢X test, and the brass texture is enhanced in 90¢X test, while the texture distribution does not change significantly in 45¢X test. It is suggested that the texture evolution during tensile straining has significant effect on the anisotropy of work hardening rate.

Oligomers of hard and soft segments of unsaturated polyesters (UP) were synthesized. They were blended in different ratios and cured with various amounts of styrene. Based on the criteria of tensile strength and strain, hard segment/soft segment (60/40 wt %) UPs containing 35 wt % and 45 wt % of extra amount of styrene were chosen for further studies. Inorganic-organic hybrid materials were prepared by incorporating tetraethoxysilane and poly(dimethylsiloxane) into the UP resins via the sol-gel process by changing the ratios of HCl/TEOS, H2O/TEOS, TEOS/PDMS and the reaction time. The specimens of these hybrid materials after curing were characterized using the tensile tester, rheometer, scanning electron microscope (SEM), 29Si-NMR and thermogravimeter. In the condition of HCl/TEOS molar ratio 0.07, H2O/TEOS molar ratio 4, TEOS/PDMS weight ratio 90/10 and the reaction time 3 hours, the results of 29Si-NMR, SEM and silicone mapping indicate that these silica gels with 3D network were well dispersed in the UP resins. These specimens had tensile strength of 512¡Ó16 kgf/cm2 and elongation of 11¡Ó4 % which are above the criteria of inhibitors. From the erosion testing, flame retardants was added unsaturated polyester and inorganic-organic hybrid materials that can help to resist heat flame, remain of a fire on the surface had the char forming.

The incompatibility of cement and shale and the subsequent failure of primary cementing jobs is a very significant concern in the oil & gas industry. On wells ranging from hydraulically fractured shale land wells to deepwater wells, this incompatibility leads to an increased risk in failing to isolate zones, which could possibly present a well control hazard and can lead to sustained casing pressure. The cement-shale interface presents a weak link that often becomes compromised by the loads incurred either during drilling, completion/stimulation or production phases. To formulate cements for effective zonal isolation, it is crucial to evaluate the bond strength of the cement-shale interface. Although several studies have focused on the interactions between cement and sandstone, very few studies have addressed the bonding behavior of cement with shale. The conventional push-out test protocol used to measure cement-to-sandstone shear bond strength has proven to be difficult to apply on shale due to its laminated or brittle nature that complicates sample preparation and can lead to shale or cement matrix failure instead of failure at the interface. In this paper, we present a novel, simple and versatile laboratory test procedure to measure the shear bond strength between cement and shale. The new procedure was used to develop cement formulations to improve the cement-to-shale bond. Two different design approaches were investigated. One involves introducing Gilsonite into cement to maintain shale integrity. The second design involves using surfactant to improve cement interfacial sealing property. Our results indicate that bond strength of cement with shale can be enhanced significantly incorporating surfactant in cement slurries. / text

This thesis reports the systematic approaches to overcome the key drawbacks of the pure PHBV, namely low crystallisation rate, tensile strength, ductility, melt viscosity, thermal stability and high materials cost. The physical, mechanical, thermal, and rheological properties of the pure PHBV were studied systematically first to lay a solid foundation for formulation development. The influence of blending with other biopolymers, inclusion of filler, and chain extender additives in terms of mechanical properties, rheology, thermal decomposition and crystallization kinetics were then followed. Creating lightweight structures by foaming is considered to be one of the effective ways to reduce material consumption, hence the reduction of density and morphology of PHBV-based foams using extrusion foaming technique were studied comprehensively in terms of extrusion conditions (temperature profiles, screw speed and material feeding rate) and the blowing agent content. The material cost reduction was achieved by adding low-cost filler (e.g. CaCO3) and reduction of density by foaming. The thermal instability was enhanced by incorporation of chain extender (e.g. Joncryl) and blending with a high thermal stability biopolymer (e.g. PBAT). The polymer blend also improved the ductility. Adding nucleation agent enhanced the crystallization rate to reduce stickiness of extruded sheet. The final formulation (PHBV/PBAT/CaCO3 composite) was successfully extruded into high quality sheet and thermoformed to produce prototype trays in an industrial scale trial. The effect of the extrusion conditions (temperature profiles, screw speed and material feeding rate) and the blowing agent content are correlated to the density reduction of the foams. 61 and 47 % density reduction were achieved for the commercial PHBV and the PHBV/PBAT/CaCO3 composite respectively and there exists further scope for more expansion if multiple variable optimisation of the conditions are carried out.

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Thesis(M.S.)--Auburn University, 2007. / Abstract. Vita. Includes bibliographic references.