When bonds between copper and printed circuit board laminates are subjected to impulsive forces, the need arises to characterize fracture energies corresponding to related, high-speed failure events. Work (or energy) is required to create new surface area—with associated dissipation events—during fracture, and this energy (for a given material system) is dependent on the speed of crack propagation, the locus of failure, and the temperature of the bond when it is broken. Since the 90° peel test has been widely employed in quasi-static fracture testing of film adhesion for printed circuit board applications, this test was first used as a basis to which other test results could be compared. A test fixture was designed and built for quasi-static peel testing that accommodated peeling at different angles and temperatures. A similar test was then desirable for the direct comparison of dynamic fracture events to those quasi-static results. The “loop peel test” was thus developed to mimic the common 90° peel test and to quantify the time- and temperature-dependent fracture energies of peel specimens during low-velocity impact. This test has been successfully used to determine the apparent critical strain energy release rate of copper/epoxy bonds for low-velocity impact conditions (1-10 m/s), for a case of near-interfacial failure. The falling wedge test has also been adapted to estimate the apparent critical strain energy release rate at similar fracture conditions. Four types of printed circuit boards have been analyzed with the above impact test methods as well as with their corresponding quasi-static tests, and the fracture energies measured with the impact tests have been compared to those obtained using quasi-static tests. Fracture energies of the material systems considered were dependent on time (speed of fracture), temperature, and the amount of moisture migration, as determined via humidity conditioning parameters. / Master of Science

La détermination de la tenue mécanique de points soudés est un enjeu industriel important, eten particulier dans le cas d’aciers à Très Haute Résistance. Actuellement, l’essai de tractionen croix est l’essai mécanique le plus répandu caractérisant la tenue des points soudés.Toutefois, l’étude de l’influence des différentes zones constituant le point soudé sur la tenueest difficile en se basant sur cet essai.Un essai d’enfoncement de coin a été développé afin de caractériser les ruptures interfacialesdes points soudés. Une section transverse d’un point soudé est observée tandis qu’un coin estinséré entre les deux tôles soudés. Une caméra CCD enregistre l'observation de lapropagation de la fissure.Le pliage limité des tôles durant la fissuration rend efficace la classification des différentspoints soudés par l'énergie totale dissipée par unité de surface rompue. De plus, la mesure insitu de l’angle d’ouverture de fissure caractérise la fissuration stable de la zone fondue. Dessimulations par éléments finis de l’essai sont conduites afin d’estimer un lien entre cesmesures et la rupture du matériau, modélisée par des zones cohésives.La rupture interfaciale de points soudés d’aciers DP et TRIP a été étudiée. Les mesuresexpérimentales permettent d’estimer les paramètres de modèles cohésifs représentatifs de larupture de la zone fondue, constituant des données fiables susceptibles d’être utilisées danstoute simulation numérique du comportement du point soudé. / Characterization of spot weld strength is a key industrial issue, particularly in the case of Advanced High Strength Steels. Today, the most widely used mechanical test evaluating this strength is the Cross Tensile Test. However, investigating the role of the different zones of one spot weld based on this test is difficult.A wedge test has been developed in order to characterize interfacial failures of spot welds. A cross section of one spot weld is observed while a wedge is inserted in between the two welded sheets. A CCD camera records the observation of the propagating crack. The limited sheet bending occurring during crack propagation allows the spot weld classification based on the total energy dissipated per unit fractured area to be efficient.Furthermore, the stable crack propagation is characterized by the in situ measurement of the crack opening angle. Finite element simulations of the test are carried out to estimate a relation between these measurements and the material resistance, approached by a cohesive zone model.Interfacial failures of spot welds of DP and TRIP steels have been investigated. The experimental measurements allow to estimate parameters of a cohesive zone model representative of the molten material failure, providing reliable and appropriate data for simulations of the mechanical behavior of the complete spot weld.

Fracture mechanics is an effective approach for characterizing material resistance to interfacial failure and for making interface reliability predictions. Because interfacial bond integrity is a major concern for performance and reliability, the need to evaluate the fracture and delamination resistance of an interface under different environmental conditions is very important. This study investigates the effects of temperature, solution chemistry and environmental preconditioning, in several solutions on the durability of silicon/epoxy and glass/epoxy systems. A series of experiments was conducted using wedge test specimens to investigate the adhesion performance of the systems subjected to a range of environmental conditions. Both silicon and glass systems were relatively insensitive to temperature over a range of 22-60°C, but strongly accelerated by temperatures above 60°C, depending on the environmental chemistry and nature of the adhesive system used. Silicon/commercial epoxy specimens were subjected to preconditioning in deionized (DI) water and more aggressive solution mixtures prior to wedge insertion to study the effect of prior environmental exposure time on the system. The wedge test data from preconditioned specimens were compared with standard wedge test results and the system was insensitive to preconditioning in DI water but was affected significantly by preconditioning in aggressive environments. Plots describing - G (crack velocity versus applied strain energy release rate) characteristics for a particular set of environmental conditions are presented and a comparison is made for different environmental conditions to quantify the subcritical debonding behavior of systems studied. A kinetic model to characterize subcritical debonding of adhesives for microelectronic applications is also proposed based on molecular interactions between epoxy and a silane coupling agent at the interface and linear elastic fracture mechanics, which could help predict long-term deterioration of interfacial adhesion. / Master of Science

The objective of this study was to evaluate and gain a better understanding of the short-term impact performance and the long-term durability of electrically conductive adhesives for electronic interconnection applications. Three model conductive adhesives, designated as ECA1, ECA2 and ECA3, supplied by Emerson & Cuming, were investigated, in conjunction with printed circuit board (PCB) substrates with metallizations of Au/Ni/Cu and Cu, manufactured by Triad Circuit Inc. Effects of environmental aging on the durability of conductive adhesives and their joints were evaluated. All the samples for both mechanical tests and thermal tests were aged at 85%, 100%RH for periods of up to 50 days. Studies of bulk conductive adhesives suggested that both plasticization, which is reversible and further crosslinking and thermal degradation, which are irreversible, might have occurred upon exposure of ECAs to the hot/wet environment. The durability of electrically conductive adhesive joints was then investigated utilizing the double cantilever beam (DCB) test. It was observed that the conductive adhesive joint was significantly weakened following hydrothermal aging, and there was a transition from cohesive failure to interfacial failure as aging continued. A comparative study of the durability of different conductive adhesive and substrate metallization combinations suggested that the resistance of the adhesive joints to moisture attack is related to the adhesive properties, as well as the substrate metallizations. It was noted that the gold/adhesive interface had better resistance to moisture attack than the copper/adhesive interface. A reasonable explanation of this phenomenon was given based upon the concept of surface free energy and interfacial free energy. XPS analysis was performed on the fractured surfaces of DCB samples. For adhesive joints with copper metallization, copper oxide was detected on the failed surfaces upon exposure of the conductive adhesive joints following aging. XPS analysis on the fractured surfaces of adhesive joints with Au metallization suggested that diffusion of Cu to the Au surface might have happened on the Au/Ni/Cu plated PCB substrates during aging. The impact performance of conductive adhesives was quantitatively determined using a falling wedge test. This unique impact resistance testing method could serve as a useful tool to screen conductive adhesives at the materials level for bonding purpose. Moreover, this test could also provide some useful information for conductive adhesive development. This study revealed that the viscoelastic energy, which is a result of the internal friction created by chain motions within the adhesive material, played an important role in the impact fracture behavior of the conductive adhesives. This study also demonstrated that the loss factor, evaluated at the impact environment conditions, is a good indicator of a conductive adhesive's ability to withstand impact loading. / Ph. D.

The lap shear strength of chromic acid anodized, primed, Ti-6Al-4V alloy bonded with a high performance FM-5 polyimide adhesive has been investigated as a function of thermal treatment for selected times at various temperatures in air. The research findings indicate that the lap shear strength decreases with the increase in duration of the thermal treatment at constant temperature and with the increase in temperature at constant time. The bond fails increasingly in the oxide coating with increasing treatment temperature and time of treatment. Surface analysis results for debonded specimens suggest that the process leading to failure is the formation of fluorine-containing materials within the oxide, which weakens the adherend-adhesive bond. The formation of the fluorine components is facilitated by treatment at elevated temperatures. This study suggests that the presence of fluoride ions in the anodic oxide coating, prior to bonding, is detrimental to the bond strength of adhesively bonded Ti-alloy when exposed to high temperatures. The wedge test configuration was used to investigate the influence of temperature on the bond durability of adhesively bonded chromic acid anodized Ti-6Al-4V alloy in air. Based on the average crack length vs. exposure time data, the bond durability varied in the order -25°C > 24°C > 177°C. In each case, the bonded joint failed cohesively within the adhesive, irrespective of the temperature of exposure. XPS analysis and scanning electron photomicrographs of failure surfaces revealed that the failure occurred at the scrim cloth/adhesive interface. The influence of thermal treatment history on the bond durability of adhesively bonded chromic acid anodized Ti-6Al-4V alloy immersed in boiling water was also investigated. The average crack length vs. immersion time indicated no significant differences for specimens that were thermally treated and then bonded compared to the non-thermally treated specimens. In addition, the failure mode was cohesive within the adhesive for specimens prepared using various thermal treatment conditions. The crack growths for samples treated for 0.5 hour and 1.0 hour and for non-thermally treated specimens for any given exposure time were equivalent. In addition, cohesive failure (failure within adhesive) was observed for each specimen under each treatment condition. The specimens that were bonded and then thermally treated for 3 hours, failed in the oxide coating immediately upon insertion of the wedge. Surface analysis results for debonded specimens suggest that the process leading to failure is the formation of fluorine-containing materials within the oxide. The measured average activation energy for the formation of aluminum fluoride species is 149 kJ/mol. The high activation energy suggests that the rate of aluminum fluoride formation is substantial only at high temperatures. In summary, the presence of fluorides in the anodic oxide coatings prior to bonding is detrimental to the overall strength and durability of adhesively bonded chromic acid anodized Ti-6Al-4V joints which have been exposed to high temperatures (350°C-399°C). / Ph. D.

The objective of this study was to evaluate and develop an understanding of durability of an adhesive bonded system, for application in a future high speed civil transport (HSCT) aircraft structure. The system under study was comprised of Ti-6Al-4V metal adherends and a thermosetting polyimide adhesive, designated as FM-5, supplied by Cytec Engineered Materials, Inc. An approach based on fracture mechanics was employed to assess Ti-6Al-4V/FM-5 bond durability. Initially, wedge tests were utilized to find a durable surface pretreatment for the titanium adherends. Based on an extensive screening study, chromic acid anodization (CAA) was chosen as the standard pretreament for this research project. Double cantilever beam specimens (DCB) were then made and aged at 150° C, 177° C, and 204° C in three different environments; ambient atmospheric air (14.7 psia), and reduced air pressures of 2 psi air (13.8 KPa) and 0.2 psi air (1.38 KPa). Joints were aged for up to 18 months (including several intermediate aging times) in the above environments. The strain energy release rate (G) of the adhesive joints was monitored as a function of exposure time in the different environments. A 40% drop in fracture toughness was noted over the 18 month period, with the greatest degradation observed in samples aged at 204° C in ambient atmospheric air pressure. The loss in adhesive bond performance with time was attibutable to a combination of physical and chemical aging phenomena in the FM-5 resin, and possible degradation of the metal-adhesive interface(s). Several mechanical and material tests, performed on the bonded joints and neat FM-5 resin specimens, confirmed the above statement. It was also noted that physical aging could be "erased" by thermal rejuvenation, partially restoring the toughness of the FM-5 adhesive material. The FM-5 adhesive material displayed good chemical resistance towards organic solvents and other aircraft fluids such as jet fuel and hydraulic fluid. The results from the FM-5 adhesive and its bonded joints were compared and contrasted with VT Ultem and REGULUS polyimide adhesives. The FM-5 adhesive showed the best performance among the three adhesive systems. The effect of mode-mixity on the fracture toughness of the Ti-6Al-4V/FM-5 adhesive bonded system was also evaluated. DCB tests in conjunction with end-notched flexure (ENF) and mixed-mode flexure (MMF) tests, were used to fracture the bonded joints under pure mode I, pure mode II, and a combination of mode I and II loadings. The results showed that the mode I fracture toughness was twice as large as the mode II toughness. This was a rather surprising find, in sharp contrast to what several researchers have observed in the past. Our current understanding is that the crack path selection during the failure process plays a significant role in explaining this anomalous behavior. Finally, failure envelopes were generated for the titanium/FM-5 bonded system, both prior to and following thermal aging. These envelopes could serve as useful tools for engineers designing with Ti-6Al-4V/FM-5 bonds. / Ph. D.

Water-assisted crack growth at an epoxy/glass interface was measured as a function of applied strain energy release rate, G, and temperature using a wedge test geometry. The specimens consist of two glass plates bonded with a thin layer of proprietary epoxy adhesive. The crack fronts along the epoxy/glass interfaces were measured using an optical stereomicroscope. The relationship between G and the debonding rate, v, can be measured using this method, and the threshold value of strain energy release rate, Gth, can be determined from the measured data. Two types of testing procedures were conducted in this study: ex situ, i.e., pre-conditioned wedge tests and in situ ones, in which wedges were applied before the specimens were submerged into water. A preliminary model was developed based on the thermal activation barrier concept, and allows the prediction of Gth for the temperatures beyond the testing region. Changes in interfacial strain energy release rate caused by thermal residual stresses in a triple-layered specimen were analyzed in Chapter Three. The method is based on linear elastic fracture mechanics and simple beam theory. The curvature of a bimaterial strip was chosen to characterize the residual stress in the specimen, and the strain energy release rate, caused by both tensile and compressive residual stresses in the adhesive, was derived for an asymmetric double cantilever beam (ADCB) geometry. The contribution of the thermal residual and mechanical stress to the global energy release rate was analyzed. The thermally induced energy release rate, GT, is found to be independent of crack length, but is a function of residual stress level and geometric and material parameters of the specimen. The adhesion of films and coatings to rigid substrates is often measured using blister geometries, which are loaded either by an applied pressure or a central shaft. The measurement will be affected if there are residual stresses that make a contribution to the energy release rate. This effect is investigated using analytical solutions based on the principle of virtual displacements. A geometrically nonlinear finite element analysis is conducted for comparison. Furthermore, the relationships among strain energy release rate, load, deflection, and fracture radius are discussed in detail in Chapter Four. Both analytical solutions and numerical results reveal that uniform tensile residual stresses reduce a specimen's deflection if it experiences plate behavior under small loads. However, this effect diminishes when membrane behavior is dominant. The mechanics of a single-lap joint with different boundary conditions subjected to tensile loading are investigated. Closed-form solutions are obtained for a specimen configuration considering different clamping methods. Based on the approach pioneered by Goland and Reissner, the solutions reported in this paper provide a simple but useful way to understand the effects of boundary conditions on this test geometry. The solutions in this study suggest that different grip configurations mainly affect the response of the specimens if the grip position is close to the joint edge or the loads are small. Generally, the influence caused by different gripping methods is only limited to the boundary region, and the behavior of the joint part subjected to tensile loading is almost the same as that for a simply-supported case. / Ph. D.