The present thesis focuses on characterisation of microstructure and the resulting mechanical and tribological properties of CVD and PVD coatings used in metal cutting applications. These thin and hard coatings are designed to improve the tribological performance of cutting tools which in metal cutting operations may result in improved cutting performance, lower energy consumption, lower production costs and lower impact on the environment.  In order to increase the understanding of the tribological behaviour of the coating systems a number of friction and wear tests have been performed and evaluated by post-test microscopy and surface analysis. Much of the work has focused on coating cohesive and adhesive strength, surface fatigue resistance, abrasive wear resistance and friction and wear behaviour under sliding contact and metal cutting conditions. The results show that the CVD deposition of accurate crystallographic phases, e.g. α-Al2O3 rather than κ-Al2O3, textures and multilayer structures can increase the wear resistance of Al2O3. However, the characteristics of the interfaces, e.g. topography as well as interfacial porosity, have a strong impact on coating adhesion and consequently on the resulting properties.  Through the deposition of well designed bonding and template layer structures the above problems may be eliminated. Also, the presence of macro-particles in PVD coatings may have a significant impact on the interfacial adhesive strength, increasing the tendency to coating spalling and lowering the surface fatigue resistance, as well as increasing the friction in sliding contacts. Finally, the CVD-Al2O3 coating topography influences the contact conditions in sliding as well as in metal cutting. In summary, the work illuminates the importance of understanding the relationships between deposition process parameters, composition and microstructure, resulting properties and tribological performance of CVD and PVD coatings and how this knowledge can be used to develop the coating materials of tomorrow.

In this thesis a new design concept of tribologically active coatings aimed for low friction applications, have been explored. Materials modeled by ab initio DFT calculations were realized through deposition of carbide and nanocomposite coatings by DC-magnetron sputtering. The design concept employs destabilization of a carbide material by alloying with a weak carbide-forming element, which refines the structure into a nanocomposite. The destabilization creates a driving force for superficial ejection of carbon in a tribological contact, forming a lubricious graphitic carbon layer. The otherwise hard material limits the real contact area and the transformed layer accounts for low shear resistance. Hence, the ideal situation for low friction is provided by formation of an easily sheared thin surface layer on a hard material. TiAlC was chosen as a model system for the theoretical modeling as well as for the depositions. The elemental composition, microstructure and mechanical properties of the coatings were characterized to relate the inherent properties to the experimentally achieved tribological response. As predicted by theory, TiAlC coatings were shown to provide self-lubrication on the atomic scale by giving low friction through a tribologically induced surface restructuring. It was shown possible to reduce the friction coefficient from 0.35 for TiC to 0.05 by addition of Al. Alloying with Al also proved to be a potent method in tailoring residual stresses from high and often detrimental levels to acceptable levels, with no significant reduction in either hardness or Young’s modulus. The effect of adding Al into TiC on the oxidation resistance was also explored. The critical temperature for onset of oxidation proved to increase with the Al-content from about 350°C for TiC to about 450°C for TiAlC with about 7 at% Al. A further increase in Al content did not change the onset temperature further but reduced the oxidation rate.

Crystalline silicon (Si) wafers used as substrates in the semiconductor and photovoltaic (PV) industries are traditionally manufactured using a multi-wire slurry sawing (MWSS) technique. Due to its high productivity potential, the fixed abrasive diamond wire sawing (DWS) technique is of considerable interest to Si wafer producers. Although both sawing techniques are currently used in the industry, a fundamental understanding of the underlying process is still lacking, particularly for diamond wire sawing. Consequently, optimization of the wire sawing process is carried out largely based on experience and trial and error. This thesis aims to develop a systematic fundamental understanding of diamond wire sawing of Si materials used for PV applications. First of all, a comparative analysis of the characteristics of silicon wafers cut by slurry and fixed abrasive diamond wire sawing is presented. The analysis results indicate that fixed abrasive diamond wire sawing may be a viable alternative to slurry wire sawing. Modeling and experimental studies of single grit diamond scribing of Si are proposed to shed light on the basic cutting mechanisms. Although Si is brittle at room temperature, it is possible to properly control the cutting conditions to obtain a completely ductile mode of material removal. The effects of material anisotropy, abrasive grit shape, friction condition and external hydrostatic pressure on the ductile-to-brittle mode transition in cutting of single crystal Si (sc-Si) are systematically investigated. Multicrystalline Si (mc-Si) based solar cells take up the majority of the global PV market. Hard inclusions (Silicon carbide and Silicon nitride) in multicrystalline Si (mc-Si) ingots may cause wire breakage and negatively impact the process, surface/subsurface morphology and mechanical properties of the resulting wafer. Their effects are experimentally studied through the single grit diamond scribing on the mc-Si sample with high density of inclusions. Finally, it is identified that there is a correlation between the high dislocation density and the increase of fracture toughness in mc-Si. The increase in fracture toughness leads to greater capability of ductile mode of cutting and higher specific scribing energy in the brittle fracture regime. Results of these fundamental investigations are expected to generate useful knowledge for optimizing the diamond wire sawing process in order to achieve high productivity and minimum surface/subsurface damage.

The influence of the tribology during resistance spot welding (RSW) of aluminum alloy 5182 with spherical-tip electrode has been investigated at both the electrode-worksheet (E/W) and faying surface (FS) interfaces. In RSW, electrode life is limited by poor current transport to the FS interface caused by extensive pitting of the electrode tip surface. The primary focus of the present research was to extend electrode life by using the knowledge gained from studying the contact mechanics at both of these interfaces. Series of experiments were conducted and finite element analysis was employed to investigate the contact mechanics at the interfaces. Based on these findings, a practical way to extend the electrode life was developed. In a series of initial experiments, it was found that attempts to alter the worksheet surface roughness caused damage to the surface oxide layer which resulted in decrease of electrical contact resistance at the E/W interface. The oxide layer on the worksheet surface contained aluminum and magnesium oxide regions and abrasion of the worksheet surface reduced the oxide layer thickness and made it more uniform in composition because when the magnesium oxide regions were abraded, a thin layer of aluminum oxide re-formed immediately while it take specific conditions to re-form magnesium oxide. These factors decreased the electrical contact resistance of the E/W interface compared with the as-received surface, thus reducing heat generation and the associated pitting of the electrode surface during RSW. Further experimental investigations and finite element analysis showed that the contact mechanics that occurred during the loaded “squeezing” phase of the welding sequence, but before current was applied to cause RSW, had a significant effect on the electrode pitting behaviour and nugget formation. At the E/W interface, squeezing caused high shear stress and slip at the periphery of the contact region. This slip disrupted the oxide layer and reduced the electrical resistance. At the beginning of the current phase of the weld sequence, the reduced electrical resistance caused current to concentrate near the periphery but constriction resistance still produced enough heat generation to cause alloying, pickup and eventually pitting of electrode in a ring around the contact centre. At the FS interface, experiments and finite element analysis showed that sheet separation and thus bending occurred during the squeezing phase and this had a profound influence on nugget formation. Experimental observations showed that the bending caused enlarged and aligned cracks in the surface oxide layers which promoted good metal-to-metal contact near the periphery of the FS. As at the E/W interface, high current densities occurred at the beginning of the current phase and the constriction resistance caused significant heat generation in this zone due to an increasing constriction resistance. Consequently, the melting at the FS started near the periphery and moved in towards the central zone of the contact region melted to produce a “doughnut-shaped” nugget with a filled-in but thin central region. Low electrical contact resistance at the E/W interface led to longer electrode tip life because less pitting occurred. In addition, higher current densities could then develop at the FS to affect RSW and achieve good nugget formation despite the rather uneven peripheral heat generation. In attempts to reduce the electrical resistance at the E/W interface, several boundary lubricants were placed on the worksheet surface a short time before starting RSW and they altered the tribology. Both increased and decreased electrode degradation rate were found in electrode life tests. One lubricant was found to be particularly effective in lowering the electrode pitting rate. It extended the electrode life to almost double that occurring with as-received (unlubricated) surfaces. Detailed analysis revealed that the effective boundary lubricant had a beneficial chemical influence on the surface of the AA5182 worksheet. The lubricant chemically attacked the oxide layer thus reducing its thickness and reducing electrical contact resistance of the E/W interface at the critical peripheral region. The result was a lower electrode pitting rate and an extended electrode life. The improved understanding of the current flow during the critical initial period and its dependence on the contact mechanics of the E/W and FS interfaces was considered important in developing ways of improving weld strength and increasing electrode life. The finding of a boundary lubricant that acted to reduce oxide layer thickness was considered an important starting point for industrial development of RSW with longer electrode life. It could be employed without interrupting the RSW process and its efficacy was well-supported by the present contact mechanics studies in which the key role of the oxide layer was demonstrated.

The influence of the tribology during resistance spot welding (RSW) of aluminum alloy 5182 with spherical-tip electrode has been investigated at both the electrode-worksheet (E/W) and faying surface (FS) interfaces. In RSW, electrode life is limited by poor current transport to the FS interface caused by extensive pitting of the electrode tip surface. The primary focus of the present research was to extend electrode life by using the knowledge gained from studying the contact mechanics at both of these interfaces. Series of experiments were conducted and finite element analysis was employed to investigate the contact mechanics at the interfaces. Based on these findings, a practical way to extend the electrode life was developed. In a series of initial experiments, it was found that attempts to alter the worksheet surface roughness caused damage to the surface oxide layer which resulted in decrease of electrical contact resistance at the E/W interface. The oxide layer on the worksheet surface contained aluminum and magnesium oxide regions and abrasion of the worksheet surface reduced the oxide layer thickness and made it more uniform in composition because when the magnesium oxide regions were abraded, a thin layer of aluminum oxide re-formed immediately while it take specific conditions to re-form magnesium oxide. These factors decreased the electrical contact resistance of the E/W interface compared with the as-received surface, thus reducing heat generation and the associated pitting of the electrode surface during RSW. Further experimental investigations and finite element analysis showed that the contact mechanics that occurred during the loaded “squeezing” phase of the welding sequence, but before current was applied to cause RSW, had a significant effect on the electrode pitting behaviour and nugget formation. At the E/W interface, squeezing caused high shear stress and slip at the periphery of the contact region. This slip disrupted the oxide layer and reduced the electrical resistance. At the beginning of the current phase of the weld sequence, the reduced electrical resistance caused current to concentrate near the periphery but constriction resistance still produced enough heat generation to cause alloying, pickup and eventually pitting of electrode in a ring around the contact centre. At the FS interface, experiments and finite element analysis showed that sheet separation and thus bending occurred during the squeezing phase and this had a profound influence on nugget formation. Experimental observations showed that the bending caused enlarged and aligned cracks in the surface oxide layers which promoted good metal-to-metal contact near the periphery of the FS. As at the E/W interface, high current densities occurred at the beginning of the current phase and the constriction resistance caused significant heat generation in this zone due to an increasing constriction resistance. Consequently, the melting at the FS started near the periphery and moved in towards the central zone of the contact region melted to produce a “doughnut-shaped” nugget with a filled-in but thin central region. Low electrical contact resistance at the E/W interface led to longer electrode tip life because less pitting occurred. In addition, higher current densities could then develop at the FS to affect RSW and achieve good nugget formation despite the rather uneven peripheral heat generation. In attempts to reduce the electrical resistance at the E/W interface, several boundary lubricants were placed on the worksheet surface a short time before starting RSW and they altered the tribology. Both increased and decreased electrode degradation rate were found in electrode life tests. One lubricant was found to be particularly effective in lowering the electrode pitting rate. It extended the electrode life to almost double that occurring with as-received (unlubricated) surfaces. Detailed analysis revealed that the effective boundary lubricant had a beneficial chemical influence on the surface of the AA5182 worksheet. The lubricant chemically attacked the oxide layer thus reducing its thickness and reducing electrical contact resistance of the E/W interface at the critical peripheral region. The result was a lower electrode pitting rate and an extended electrode life. The improved understanding of the current flow during the critical initial period and its dependence on the contact mechanics of the E/W and FS interfaces was considered important in developing ways of improving weld strength and increasing electrode life. The finding of a boundary lubricant that acted to reduce oxide layer thickness was considered an important starting point for industrial development of RSW with longer electrode life. It could be employed without interrupting the RSW process and its efficacy was well-supported by the present contact mechanics studies in which the key role of the oxide layer was demonstrated.

This research studies individual and combined effects of hydrogen gas exposure and low temperature on the tribological characteristics of Ti-6Al-4V. Experimental approaches include test system modification and tribological analysis. An existing ballon- disk tribometer was modified to allow liquid nitrogen to be constantly injected into an insulated test chamber to enable testing at low temperature. Twelve 3.8 cm diameter Ti-6Al-4V disks were manufactured and polished, then half were exposed to pure hydrogen gas at elevated temperature and pressure and the remaining disks were untreated. The testing was split in to four groups of three disks based on testing temperature and previous hydrogen exposure. A silicon nitride ball was used for all tests. Each group was tested at two normal loads, 10N and 20N, at the same linear speed. Group 1 was unexposed and tested at room temperature, Group 2 was unexposed and tested at low temperature, Group 3 was exposed and tested at room temperature and Group 4 was exposed and tested at low temperature. Average friction coefficients and the specific wear rate were calculated from the test data. Also high-resolution digital microscope imaging was used to observe and characterize the wear mechanisms of the four groups of samples. Results show that hydrogen exposure facilitated adhesive wear of the surface and that low temperature induced a slip-stick wear mechanism under higher loads, but not at lower loads and regardless of exposure to hydrogen gas. This research opens avenues for future investigation in effects of hydrogen and low temperature embrittlement on the tribological performance of materials. With the increasing interests in hydrogen energy, the present work established a foundation for future study.

Perception and sense of touch are extremely important factors in design, but until recently, the exploration of skin tribology related to tactility has been relatively untouched. In this emergence, skin-on-polymer interactions are becoming more widely investigated due to the prevalence of polymers in everyday life, and the ability to define these interactions in terms of tactility would be hugely beneficial to the engineering and design process. Previous work has investigated polymer textiles concerning tactility, examining environmental and material properties that affect skin on fabric coefficient of friction. In this study, similar friction procedure was used to compare coefficients of friction of a fingerpad across varying polymer fabrics. Forces were applied in both longitudinal and lateral directions, and it was discovered that force directionality greatly affects coefficient of friction. Specific causes have yet to be determined, but it is suspected that material weave and microscopic surface properties play a major role in this directional behavior. To complement these studies and relate them to tactility, trained human evaluators rated the samples against four tactile attributes: abrasiveness, slipperiness, sensible texture, and fuzziness. These ballots were then analyzed with Quantitative Data Analysis and shown to be repeatable among the participants, and each of the attributes were shown to be statistically independent of coefficient of friction. It should be noted, however, that fuzziness showed the greatest correlation coefficient of R^2=0.27. Material selection plays an integral role in frictional behavior, and researchers have been studying contact theory on both microscopic and macroscopic levels to determine how surface topography affects skin-polymer tribology. To negate material effects discussed in the Greenwood-Williamson contact model, frictional tests were performed on identical polypropylene plaques with textured grooves of varying dimensions. Both geometry and directionality proved to be major frictional contributors; as groove size increased, finger friction in the longitudinal direction decreased, but friction increased laterally. In addition to testing a fingerpad, friction was measured with a silicone wand to simulate a finger with different material properties. The silicone exhibited the opposite trend as skin; as groove width decreased, frictional forces increased longitudinally and decreased laterally. While topography affects frictional behavior, counterface stiffness, and intrinsic material properties may cause the trend shift between skin and silicone.

This thesis includes two parts. The first part reviews the history and fundamentals of surface science and tribology. The second part presents the major research outcomes and contributions. This research explores the aspects of friction, wear, and surface modification for tribological augmentation of surfaces. An effort has been made to study these aspects through gaining insights by fundamental studies leading to specific practical applications in railroads. The basic idea was to surface engineer metals for enhanced surface properties. A micro- and nano- scale experimental approach has been used to achieve these objectives. Novel principles of nano technology are incorporated into the experiments. Friction has the potential to generate sufficient energy to cause surface reactions through high flash temperatures at the interface of two materials moving in relative motion. This allows surface modifications which can be tailored to be tribologically beneficial through a controlled process. The present work developed a novel methodology to generate a functional tribofilm that has combined properties of high hardness and high wear resistance. A novel methodology was implemented to distinguish sliding/rolling contact modes during experiments. Using this method, a super hard high-performance functional tribofilm with “regenerative” properties was formed. The main instrument used in this research for laboratory experiments is a tribometer, using which friction, wear and phase transformation characteristics of railroad tribo-pairs have been experimentally studied. A variety of material characterization techniques have been used to study these characteristics at both micro and nano scale. Various characterization tools used include profilometer, scanning electron microscope, transmission electron microscope, atomic force microscope, X-ray diffractometer, nanoindenter, and X-ray photon spectroscope. The regenerative tribofilms promise exciting applications in areas like gas turbines, automotive industry, compressors, and heavy industrial equipment. The outcome of this technology will be an economical and more productive utilization of resources, and a higher end performance.

Copper polishing performance depends significantly on the properties of pads, slurries, conditioning, pressure, sliding velocity, slurry flow rate and temperature. A slight variance in each of these parameters will cause significant change in polising results. Various investigations are performed during this study to understand the effect of consumables and other main operating parameters on copper polishing in terms of removal rate, lubrication mechanism, and temperature transients. A modified two-step Langmuir-Hinshelwood removal rate model and a flash heating thermal model are developed to describe the removal mechanism.Results indicate that grain size plays an important role during copper polishing. Smaller grain size may enhance the chemical rate by providing a higher density of favorable reaction sites. However, denser grain boundaries due to smaller grain size may reduce the mechanical rate by increasing the probability of disruption of three body sliding contact. It is found that removal rate increases as slurry flow increases from 60 to 80 cc/min because higher slurry flow rate can provide more reactants to the system. Then removal rate decreases as slurry flow rate is further increased to 140 cc/min, which is due to synergic effects of the wafer temperature, slurry flow and slurry residence time under the wafer. The observed removal rate drop is thought to be due to the change of the wafer temperature at high sliding velocity.Experimental results from eight slurry formulations with various abrasize size and content show that in the case of 13-nm abrasives, the dominant tribological mechanism is that of partial lubrication, while in the case of 35-nm abrasives, the dominant tribological mechanism is that of boundary lubrication. COF values of the slurry with surfactant are generally lower that those of the slurry without surfactant.Logarithmic spiral positive pad, whose spiral groove is at a slight angle to the pad rotation direction, shows the highest average COF. The radial pad results in the smallest average COF. For all types of the grooved pads investigated, CMP is mechanically limited at low pV, and chemically limited at high pV. Non-Prestonian behavior is thought to be due to variations of COF and substrate temperatures.Dual Emission UV Light Enhanced Fluorescence results indicate that during polishing the wafer is tilted towards the center of the pad and that the extent of wafer tilt is a strong function of diamond disc pressure. Increasing the oscillation frequency of the diamond disc or the rotation rate decreases slurry film thickness. Slurry film thickness increases with the slurry flow rate. Also slurry film thickness strongly depends on diamond disc design.

This dissertation presents a series of studies relating to kinetics and kinematics of inter-layer dielectric and metal chemical mechanical planarization processes. These are also evaluated with the purposes of minimizing environmental and cost of ownership impact.The first study is performed to obtain the real-time substrate temperature during the polishing process and is specifically intended to understand the temperature distribution across the polishing wafer during the chemical mechanical planarization process. Later, this technique is implemented to study the effect of slurry injection position for optimum slurry usage. It is known that the performance of chemical mechanical planarization depends significantly on the polishing pad and the kinematics involved in the process. Variations in pad material and pad grooving type as well as pressure and sliding velocity can affect polishing performance. One study in this dissertation investigates thermoset and thermoplastic pad materials with different grooving methods and patterns. The study is conducted on multiple pressure and sliding velocity variations to understand the characteristic of each pad. The analysis method elaborated in this study can be applied generically.A subsequent study focuses in a slurry characterization technique. Slurry, a critical component in chemical mechanical planarization, is typically a water-based dispersion of fine abrasive particles with various additives to control material removal rate and microscratches. Simultaneous turbidity and low angle light scattering methods under well-defined mixing conditions are shown to quantify the stability of abrasive particle from aggregations. Further contribution of this dissertation involves studies related to the spectral analysis of raw shear force and down force data obtained during chemical mechanical planarization. These studies implemented Fast Fourier Transforms to convert force data from time to frequency domain. A study is performed to detect the presence of larger, defect-causing particles during polishing. In a further application on diamond disc conditioning work is performed to achieve optimum break-in time and an optimum conditioning duty cycle. Studies on spectral analysis are also extended to planarization of shallow trench isolation pattern wafers to monitor the polishing progress in real-time.