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When bonded joints are subjected to harsh environmental conditions, the interphase, the three-dimensional region surrounding the adhesive/substrate interface, becomes critically important. Frequently, failure occurs in this region after adhesively bonded systems are subjected to elevated temperature oxidative aging. In a previous study, this was found to be the case with a polyimide adhesive bonded to chromic acid anodized (CAA) Ti-6Al-4V. The objective of the current research has been twofold: 1) to investigate the effect of thermal aging on the interphase region of polyimide/titanium adhesive joints, and 2) to evaluate the method used in the current study for durability characterization of other adhesive/substrate systems. The method used in this research has been to characterize the effect of elevated temperature aging on the following systems: 1) Notched coating adhesion (NCA) specimens and 2) bulk samples of dispersed substrate particles in an adhesive matrix. The NCA test has the advantages of an accelerated aging geometry and a mode mix that leads to failure through the interphase, the region of interest. The bulk samples have the advantage of an increased interphase volume and allow for the application of bulk analysis techniques to the interphase, a region that is traditionally limited to surface analysis techniques. The adhesive systems studied consisted of one of two polyimide adhesives, LaRC© PETI-5 or Cytec Fiberite© FM-5, bonded to CAA Ti-6Al-4V. The model filled system consisted of a PETI-5 matrix with amorphous titanium dioxide filler. Through the use of the NCA test, it was determined that bonded specimens made with FM-5 lose approximately 50% of their original fracture energy when aged in air at 177°C for 30 days. This aging temperature is well below the glass transition temperature of the adhesive, 250°C. At the same time, the failure location moves from the anodized oxide layer to the adhesive that is directly adjacent to the substrate surface, the interphase region. Through surface analysis of this region, it is determined that the adhesive penetrates the pores of the CAA surface to a depth of 70 to 100 nm, promoting adhesion at the interface. With aging, the adhesive in the interphase region appears to be weakening, although analysis of the bulk adhesive after aging shows little change. This indicates that adhesive degradation is enhanced in the interphase compared to the bulk. Analysis of the model filled system gave similar information. Specimens containing titanium dioxide filler had glass transition temperatures that were approximately 20°C lower than the neat polyimide samples. In addition, the filled samples contained a significant portion of low molecular weight extractable material that was not present in the neat specimens. The tan delta spectra from dynamic mechanical thermal analysis of the filled specimens exhibited a shoulder on the high-temperature side of the glass transition peak. This shoulder is attributed to the glass transition of the interphase, a distinct phase of the polyimide which is constrained by adsorption onto the filler particle surfaces. As a function of aging time at 177° or 204°C, the shoulder decreases substantially in magnitude, which may relate to loss of adhesive strength between the polyimide and the filler particles. From this research, it has been illustrated that information relating to the durability of adhesively bonded systems is gained using an interfacially debonding adhesive test and a model system of substrate particles dispersed in an adhesive matrix / Ph. D.

This thesis describes advancements in the modelling, optimisation, process control and mechanical performance of novel high deposition rate gas metal arc welding processes for large scale additive manufacturing applications. One of the main objectives of this study was to develop fundamental understanding of the mechanisms involved during processing with particular focus on single layer welds made of carbon steel using both pulsed-current gas metal arc welding and cold metal transfer processes. The effects of interactions between critical welding process variables and weld bead and plate fusion characteristics are studied for single and multi-layers. It was shown that several bead and plate fusion characteristics are strongly affected by the contact tip to work distance, TRIM, wire feed speed, wire feed speed to travel speed ratio, and wire diameter in pulsed-current gas metal arc welding. The arc-length control, dynamic correction and the contact tip to work distance are shown to strongly influence the weld bead geometry in the cold metal transfer process. This fundamental knowledge was essential to ensure the successful development of predictive interaction models capable of determining the weld bead geometry from the welding process parameters. The models were developed using the least-squares analysis and multiple linear regression method. The gas tungsten constricted arc welding process was utilised for the first time for out-of-chamber fabrication of a large scale and high-quality Ti-6Al-4V component. The main focus was, however, in the use of the cold metal transfer process for improving out-of-chamber deposition of Ti-6Al-4V at much higher deposition rates. The effect of the cold metal transfer process on the grain refinement features in the fusion zone of single layer welds under different torch gas shielding conditions was investigated. It was shown that significant grain refinement occurs with increasing helium content. The morphological features and static mechanical performance of the resulting multi-layered Ti-6Al-4V walls were also examined and compared with those in gas tungsten constricted arc welding. The results show that a considerable improvement in static tensile properties is obtained in both testing directions with cold metal transfer over gas tungsten constricted arc welding. It was suggested that this improvement in the mechanical behaviour could be due to the formation of more fine-grained structures,which are therefore more isotropic. The average ultimate tensile strength and yield strength of the as-deposited Ti-6Al-4V material processed via cold metal transfer meet the minima specification values recommended for most Ti-6Al-4V products. Neutron diffraction technique was used to establish the effect of repeated thermo-mechanical cycling on the generation, evolution and distribution of residual stresses during wire and arc additive manufacturing. The results show a significant redistribution of longitudinal residual stresses along both the substrate and multi-bead with repeated deposition. However, a nearly complete relaxation occurs along the built, once the base plate constraint is removed.

Alloys of titanium are highly preferred materials for their excellent strength to weight ratio but the tribological issues while using them has been posing challenging issues for the tribological analyst, which are still areas of active research. Ti-6Al-4V (Ti64) is the most popular alloy of titanium and our understanding of the fundamental mechanisms of wear and friction of this alloy is still not complete. Previous investigations related to the tribology of these alloys have suggested a synergistic effect of plastic deformation and tribo-oxidation. The present investigation described in this thesis explores the existence of one more mode, namely the formation of a Mechanically Mixed Layer (MML). The thesis examines the effect of these modes one by one and analyses the synergistic effect of these mechanisms, and also the effect of heat generation during sliding. The tribological condition existing have been varied by doing wear experiments using Ti64 pins sliding against alumina and SS316L (controls MML), diameter of pin (expected to control debris entrapment and thus MML formation), tribo-system (horizontal disc Vs vertical disc, which is also expected to control debris entrapment and thus MML formation), environment (ambient and vacuum, expected to control tribo-oxidation) and sliding speed (expected to control interface temperature and thus plastic deformation mechanism and tribo-oxidations). The division of the main chapters has been so made to present the findings spread over Chapters 5-8, with each chapter dealing with specific tribological test conditions. In each chapter, results from the tribological experimentations in the form of wear and friction are presented, together with the characterization methods which throw light into the tribological mechanisms. These characterization methods include Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDAX), X-Ray Diffraction (XRD) and Electron probe micro-analyzer (EPMA). Wherever possible, the debris collected from the experiments have been subjected to morphological and detailed chemical analysis, and a feature which has not been explored much in detail by tribological investigators, but having a promising potential. Experimental results from tribological testing when Ti64 pins slides against two different materials (Alumina and SS316L) in pin-on-disc tribometers under two different environmental conditions (ambient /vacuum) are analyzed. Each set of experiments looks at two different effects - (1) the effect of sliding speed on the tribological behavior while using a pin of a fixed diameter (all other parameters remaining the same) and (2) the effect of using pins of different diameters for a given set of parameters. Three different pin-sizes were employed (2.1 mm. 4.6 mm and 6.6 mm), the normal loads on these pins were changed according to the pin-size used so that all experiments were done at the same contact pressure (2.8 MPa). By performing the experiments against the ceramic disc (alumina) under vacuum conditions, the effect of this plastic deformation is studied in isolation because the possibility of the Tribo Chemical Reaction (TCR) due to oxidation is inhibited and no MML was found to be formed due to poor compatibility of mixing between the metallic pin and the ceramic disc. For the low speeds/strain rates experiments, the effect of plastic deformation as influenced by the adiabatic shear banding is seen to influence wear which progressively changes to temperature induced plastic deformation and wear. The situation is found to be different when we change the environmental conditions from vacuum to ambient for the same tribo-combination. The tests shows a reduction in wear rate with speed, and this is due to the oxide formations due to TCR as confirmed from the SEM/EDAX characterization. In contrast to previous experiments under vacuum, these permit the effect of TCR also to influence the tribological behavior. The scenario changes when the alumina disc is replaced by a metallic one (SS316L) and tests carried out in vacuum, as the MML was found to be formed with this tribo-pair. Because of the mutual affinity of the materials in the tribo-pair, the wear damage is severe in this case and the flash temperatures crossing the phase transition temperature (~880oC) for Ti64 at high speeds. The growth of the β phase with increase in the sliding (temperature) conditions is captured from the XRD spectra of the wear debris. Synergistic effect of all these mechanisms (plastic deformation, MML, and TCR) is permitted by conducting experiments with Ti64 pin against stainless steel and in ambient conditions. A comparison of the tribological response by presenting results when experiments are run over a range of speeds while using different sized pins under ambient conditions (and compared with similar results in vacuum) while using SS316L disc serve to demarcate the differences in the wear modes which are active/inactive depending on the tribological conditions. In addition a study incorporating the effect of frictional heating and its influence on the tribological phenomena is analyzed. Main conclusions from the thesis are: The wear resistance of Ti64 alloy when sliding against SS316L is found to be influenced by Strain Rate Response (SRR), Tribo Oxidation (TO), Mechanically Mixed Layer (MML) and the prevailing heat flux conditions at the contact. The wear rates were found to decrease marginally with sliding speeds (strain rates) up to a certain speed, which is ascribed to reduction in adiabatic shear band intensity with increase in strain rate. Adiabatic Shear Band (ASB), which allows easy crack propagation, intensity reduces as temperature of deformation of Ti64 is increased. From the results it can be confirmed that the propensity for formation of MML depends on compatibility of the disc and the pin material. The contribution due to of entrapment and retention of debris in the contact zone also would influence formation of the MML. The effect of frictional heating plays an influential role as it can affect the factors (TO, ASB, MML) governing the tribological response. The sensitivity to temperature, which is a marked feature of this alloy in undergoing softening, as confirmed by previous researchers, is reflected in the experimental results. Since the main factor that triggers the micro-structural instability is the energy dissipation that accompanies deformation more fundamental research which can improve the thermal transport properties of this alloy, would be the future scope of work of this thesis. Also, the unique composition of the MML which offers high wear resistance under specific operating conditions opens up the possibility of new such alloy formulations, production routes and techniques which should improve the tribological response of this alloy.

This thesis focuses on testing and improving Ti-6Al-4V ELI biomaterials, which are currently one of the most used titanium alloys in biomedicine (predominantly in orthopaedics and dentistry), in cooperation with research institutions and private companies developing and producing such materials. The metallic samples were previously modified by plasma electrolytic oxidation (PEO) with use of electrolytes of a different composition to induce development of a homogeneous TiO2 layer on its surface. In vitro interactions of human osteoblast-like cell line Saos-2 with the surface of Ti-6Al-4V ELI alloy samples are investigated. Initial cell attachment, spreading, morphology, cell population density, viability, calcium deposition and expression of selected osteogenic markers, e.g. collagen type I, alkaline phosphatase and osteocalcin, were evaluated on cultured cells. The cells behavior were then correlated with physicochemical properties of the material surface, such as its topography, roughness, wettability, surface layer chemical composition etc. The results are also compared with those obtained in cells cultured on control samples of untreated alloys as well as microscopic glass coverslips and bottom of standard polystyrene cell culture wells. The aim of this thesis is to select the most promising...

Plasma pretreatments are environmentally benign and energy efficient processes for modifying the surface chemistry of materials. In an effort to improve the strength of the titanium alloy/FM-5 polyimide adhesive joint for aerospace applications, oxygen plasma pretreatments and novel thin plasma polymerized (PP) films were investigated as adhesion promoters. Plasma treatments were carried out using custom-built, low pressure, radio frequency, inductively coupled plasma reactors. Ti-6Al-4V coupons were plasma treated and used to prepare miniature single lap shear (SLS) joints. The effects of plasma pretreatments on surface chemistry were studied using x-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), Fourier transform infrared analysis (FTIR), and contact angle measurements. Relationships between composition, mechanical properties, and adhesion of PP films on Ti-6Al-4V and silicon wafers were investigated. The nanomechanical properties (modulus, hardness and adhesion) were studied using atomic force microscopy (AFM) nanoindentation and nanoscratch testing. A design of experiments (DOE) three factorial model was used to optimize the parameters for oxygen plasma treatments. Oxygen plasma pretreatments enhanced joint strength by cleaning the titanium surface and creating an extended oxide layer. Nanoindentation of oxygen plasma treated substrates showed no change in the surface mechanical properties due to the oxygen plasma treatment. This suggested that the improved SLS strength of the oxygen plasma pretreated substrates was due to the cleaning of the substrate and the removal of carbonaceous contaminants, rather than any changes in the morphology of the oxide layer. PP acetylene films were predominantly carbon, with oxygen as the other main constituent (incorporated mostly as C-O and C=O). For all SLS specimens tested, the adhesion between PP acetylene and FM-5 adhesive was adequate. However, the strength of SLS joints was limited by the adhesion of the PP acetylene to the Ti-6Al-4V substrate. The effects of a large number of plasma parameters, such as substrate pretreatment, carrier gas, input power, flow rate and film thickness were investigated. All samples failed at the PP film/Ti-6Al-4V interface or within the PP acetylene film, and thicker PP films yielded lower SLS strengths. PP films deposited at lower power exhibited higher hardness and reduced modulus than films deposited at higher power. Overall, thinner films exhibited higher hardness and reduced Young's modulus than thicker films. PP films of higher hardness yielded higher critical loads at debond (thickness normalized) during the nanoscratch test. Thin films were developed via the vapor plasma polymerization of titanium(IV) isobutoxide (TiiB). XPS results suggested that titanium was incorporated into the film as TiO2 clusters dispersed in an organic matrix. No evidence for Ti-C was obtained from the XPS spectra. PP films of TiiB were much more compliant than PP acetylene films. This behavior was attributed to decreased fragmentation and lower crosslinking that occurred during PP TiiB film deposition. These PP films did not exhibit sol-gel-like qualities, and because of the way titanium was incorporated into the films, a more appropriate name for these films might be "titanium dioxide-doped plasma polymerized films." / Ph. D.

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The goal of the present dissertation is to develop and apply novel and systematic data-driven optimization approaches that can efficiently optimize Additive Manufacturing (AM) systems with respect to targeted properties of final parts. The proposed approaches are capable of achieving sets of process parameters that result in the satisfactory level of part quality in an accelerated manner. First, an Accelerated Process Optimization (APO) methodology is developed to optimize an individual scalar property of parts. The APO leverages data from similar—but non-identical—prior studies to accelerate sequential experimentation for optimizing the AM system in the current study. Using Bayesian updating, the APO characterizes and updates the difference between prior and current experimental studies. The APO accounts for the differences in experimental conditions and utilizes prior data to facilitate the optimization procedure in the current study. The efficiency and robustness of the APO is tested against an extensive simulation studies and a real-world case study for optimizing relative density of stainless steel parts fabricated by a Selective Laser Melting (SLM) system. Then, we extend the idea behind the APO in order to handle multi-objective process optimization problems in which some of the characteristics of the AMabricated parts are uncorrelated. The proposed Multi-objective Process Optimization (m-APO) breaks down the master multi-objective optimization problem into a series of convex combinations of single-objective sub-problems. The m-APO maps and scales experimental data from previous sub-problems to guide remaining sub-problems that improve the solutions while reducing the number of experiments required. The robustness and efficiency of the m-APO is verified by conducting a series of challenging simulation studies and a real-world case study to minimize geometric inaccuracy of parts fabricated by a Fused Filament Fabrication () system. At the end, we apply the proposed m-APO to maximize the mechanical properties of AMabricated parts that show conflicting behavior in the optimal window, namely relative density and elongation-toailure. Numerical studies show that the m-APO can achieve the best trade-off among conflicting mechanical properties while significantly reducing the number of experimental runs compared with existing methods.

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