Doctor of Philosophy (PhD) / This thesis aims to establish a sound scientific methodology for the effective and efficient polishing of thermally stable PCD composites (consisting of diamond and SiC) for cutting tools applications. The surface roughness of industrial PCD cutting tools, 0.06 μm Ra is currently achieved by mechanical polishing which is time consuming and costly because it takes about three hours to polish a 12.7 mm diameter PCD surface. An alternative technique, dynamic friction polishing (DFP) which utilizes the thermo-chemical reactions between the PCD surfaces and a catalytic metal disk rotating at high peripheral speed has been comprehensively investigated for highly efficient abrasive-free polishing of PCD composites. A special polishing machine was designed and manufactured in-house to carry out the DFP of PCD composites efficiently and in a controllable manner according to the requirements of DFP. The PCD polishing process and material removal mechanism were comprehensively investigated by using a combination of the various characterization techniques: optical microscopy, SEM and EDX, AFM, XRD, Raman spectroscopy, TEM, STEM and EELS, etc. A theoretical model was developed to predict temperature rise at the interface of the polishing disk and PCD asperities. On-line temperature measurements were carried out to determine subsurface temperatures for a range of polishing conditions. A method was also developed to extrapolate these measured temperatures to the PCD surface, which were compared with the theoretical results. The material removal mechanism was further explored by theoretical study of the interface reactions under these polishing conditions, with particular emphasis on temperature, contact with catalytic metals and polishing environment. Based on the experimental results and theoretical analyses, the material removal mechanism of dynamic friction polishing can be described as follows: conversion of diamond into non-diamond carbon takes place due to the frictional heating and the interaction of diamond with catalyst metal disk; then a part of the transformed material is detached from the PCD surface as it is weakly bonded; another part of the non-diamond carbon oxidizes and escapes as CO or CO2 gas and the rest diffuses into the metal disk. Meanwhile, another component of PCD, SiC also chemically reacted and transformed to amorphous silicon oxide/carbide, which is then mechanically or chemically removed. Finally an attempt was made to optimise the polishing process by investigating the effect of polishing parameters on material removal rate, surface characteristics and cracking /fracture of PCD to achieve the surface roughness requirement. It was found that combining dynamic friction polishing and mechanical abrasive polishing, a very high polishing rate and good quality surface could be obtained. The final surface roughness could be reduced to 50 nm Ra for two types of PCD specimens considered from pre-polishing value of 0.7 or 1.5 μm Ra. The polishing time required was 18 minutes, a ten fold reduction compared with the mechanical abrasive polishing currently used in industry.

This study examines the lapping machining process used during the manufacturing of polycrystalline diamond compacts (PDCs). More specifically, it is aimed at improving the productivity of the process by developing a better understanding of the parameters that affect the material removal rate (MRR) and MRR uniformity of lapped PDC samples. Experiments that focused on several controllable lapping parameters were performed to determine to what extent they affected the process. It was determined that the MRR can be modeled with the Preston equation under certain ranges of pressure and speed. It was also found that using a hard and rigid sample holder produces higher MRRs than soft and flexible sample holders. The results have also shown that MRRs in excess of 300 micrometers per hour can be achieved while using 10 grams of diamond abrasive per PDC per hour of lapping. The productivity of the lapping process can also be improved by placing the maximum allowed PDC samples in a concentric circle on the edge of the sample holder. The MRR uniformity between samples lapped on the same sample holder was found to be dependent on the sample holder material. This thesis is composed of six chapters. The first chapter introduces the need for PDC's as extreme cutting tools, the manufacturing process of PDC's, and the lapping process. The second chapter discusses the motivation behind this research and the primary objectives that were established. The third chapter details the materials and the experimental procedure, and the fourth chapter presents the results. The fifth chapter discusses the results, and the sixth chapter presents conclusions and information on possible future work.

Doctor of Philosophy (PhD) / This thesis aims to establish a sound scientific methodology for the effective and efficient polishing of thermally stable PCD composites (consisting of diamond and SiC) for cutting tools applications. The surface roughness of industrial PCD cutting tools, 0.06 μm Ra is currently achieved by mechanical polishing which is time consuming and costly because it takes about three hours to polish a 12.7 mm diameter PCD surface. An alternative technique, dynamic friction polishing (DFP) which utilizes the thermo-chemical reactions between the PCD surfaces and a catalytic metal disk rotating at high peripheral speed has been comprehensively investigated for highly efficient abrasive-free polishing of PCD composites. A special polishing machine was designed and manufactured in-house to carry out the DFP of PCD composites efficiently and in a controllable manner according to the requirements of DFP. The PCD polishing process and material removal mechanism were comprehensively investigated by using a combination of the various characterization techniques: optical microscopy, SEM and EDX, AFM, XRD, Raman spectroscopy, TEM, STEM and EELS, etc. A theoretical model was developed to predict temperature rise at the interface of the polishing disk and PCD asperities. On-line temperature measurements were carried out to determine subsurface temperatures for a range of polishing conditions. A method was also developed to extrapolate these measured temperatures to the PCD surface, which were compared with the theoretical results. The material removal mechanism was further explored by theoretical study of the interface reactions under these polishing conditions, with particular emphasis on temperature, contact with catalytic metals and polishing environment. Based on the experimental results and theoretical analyses, the material removal mechanism of dynamic friction polishing can be described as follows: conversion of diamond into non-diamond carbon takes place due to the frictional heating and the interaction of diamond with catalyst metal disk; then a part of the transformed material is detached from the PCD surface as it is weakly bonded; another part of the non-diamond carbon oxidizes and escapes as CO or CO2 gas and the rest diffuses into the metal disk. Meanwhile, another component of PCD, SiC also chemically reacted and transformed to amorphous silicon oxide/carbide, which is then mechanically or chemically removed. Finally an attempt was made to optimise the polishing process by investigating the effect of polishing parameters on material removal rate, surface characteristics and cracking /fracture of PCD to achieve the surface roughness requirement. It was found that combining dynamic friction polishing and mechanical abrasive polishing, a very high polishing rate and good quality surface could be obtained. The final surface roughness could be reduced to 50 nm Ra for two types of PCD specimens considered from pre-polishing value of 0.7 or 1.5 μm Ra. The polishing time required was 18 minutes, a ten fold reduction compared with the mechanical abrasive polishing currently used in industry.

Polycrystalline diamond (PCD) is used as a cutting tool in many industries because of its superior wear resistance compared to single crystal diamond. Engineers who design new PCD materials must have an understanding of the tradeoffs between material properties in order to tailor a product for different applications. Two competing material properties that are often encountered in PCD are transverse rupture strength and thermal-resistance. Thermal-resistance is directly related to the cobalt content of PCD, and is the ability of the material to withstand thermally induced degradation. In this thesis, we characterize the tradeoff boundary between transverse rupture strength and cobalt content of PCD. We also characterize the tradeoff boundary between cost and cobalt content, and show how both of these tradeoff boundaries can be used to manage product development, which adds value for managers in both engineering and business. In order to characterize these tradeoffs, empirical models are developed for each material property in terms of the design variables of sintering pressure and diamond grain size, where the pressure ranges from 55 kbar to 77 kbar and the grain size ranges from 12 μm to 70 μm in diameter. Then the models are used as optimization objectives in the normal constraint method to generate the tradeoff boundary. Finally, the tradeoff boundary is validated through additional experiments. The tradeoff boundary shows that the relationship between transverse rupture strength and cobalt content is not linear. It also shows that the optimal PCD designs can occur over a wide range of pressures and grain sizes, but pressures above 66 kbar and grain sizes between 20 and 30 μm appear to offer the best compromise between these material properties. These results are compared to the wear rates of PCD compacts in rock cutting tests. The rock cutting test results confirm that the designs with the best compromise between transverse rupture strength and cobalt content also have the highest wear resistance. In general, the designs that offer the best compromise between the properties are also the most expensive to manufacture.

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L’objectif de cette étude était la caractérisation chimique de cristaux et films de diamant élaborés par dépôt chimique en phase vapeur assisté par plasma micro-ondes sur silicium. Il s’agit d’une approche pluritechnique fondée essentiellement sur les techniques spectroscopiques. La spectroscopie Raman, la spectroscopie XPS, la diffraction des rayons X et la microscopie électronique à balayage ont fournis des informations essentielles et complémentaires sur les propriétés physico-chimiques et structurales des dépôts de diamant en fonction de différents paramètres de synthèse. A titre d’illustration, une nouvelle transition électronique a été observée pour les films présentant des surfaces hydrogénées. Cette transition présente un gap de surface voisin de 2,7 eV mise en évidence par un effet Raman de résonance. Des contraintes internes anisotropes sont observées pour les films présentant un axe de fibre <110> et pour des cristaux multimaclés isolés présentant une germination secondaire. / The aim of this work was to investigate chemical characterization of diamond crystals and films elaborated by microwave plasma assisted chemical vapour deposition on silicon. This study was focused on a pluri-technique approach founded on the spectroscopic techniques. Raman spectroscopy, XPS spectroscopy, X-ray diffraction and scanning electron microscopy have provided essential and additional information about physico-chemical and structural properties of diamond deposits according to a various synthesis parameters. As examples, a new electronic transition was observed for hydrogen-terminated diamond surface films. This transition presents a surface gap at 2,7 eV provided by a resonant Raman. Anisotropic internal stresses were observed for films presenting a fiber axis <110> and for isolated twinned crystals presenting a secondary nucleation.

La possibilité de fabriquer des dispositifs optiques pour la détection d’interactions chimiques,sans marquage et en temps réel, présente un intérêt croissant. Notamment, les cristaux photoniques(CPh) présentent un fort potentiel pour une telle application. Contrairement au silicium, majoritairementexploité pour la réalisation de telles structures, le diamant possède l’avantage d’avoir unesurface carbonée biocompatible permettant une fonctionnalisation covalente et stable de biomoléculesspécifiques. Dans ce contexte, cette thèse vise à étudier la potentialité qu’offre ce matériau pour la réalisationde CPh 2D destinés à des applications de biodétection. Pour cela, une plateforme photoniquemonolithique compacte, intégrable sur silicium et optimisée pour un fonctionnement aux longueursd’onde proches de 1.55 μm a été développée. Une géométrie de cavité à fente a été retenue afin demaximiser la sensibilité des structures photoniques à leur environnement extérieur. Des méthodesnumériques ont permis de préciser les paramètres géométriques des CPh. Des procédés de microstructurationde films minces de diamant polycristallin sur substrat silicium 2 pouces ont été développéset optimisés, pour aboutir à la réalisation de CPh caractérisés par des facteurs de qualité pouvantatteindre 6500. Deux procédés technologiques spécifiques aux films de diamant polycristallin ont notammentété développés : un procédé de lissage et un procédé de transfert de films de diamant surisolant. La sensibilité optique des CPh en diamant à une modification chimique de surface a ensuiteété étudiée et a tout d’abord montré une forte dépendance de leurs performances optiques à de simplesvariations des terminaisons chimiques du matériau. Par la suite, une preuve de concept de détectionsurfacique de protéines en milieu liquide par les CPh en diamant a été réalisée en utilisant le systèmede bioreconnaissance biotine/streptavidine, donnant une limite de détection estimée pour le systèmeà 10 μg/mL. Enfin, des travaux préliminaires de détection dans le visible ont été engagés via la réalisationde cavités à CPh fonctionnant à 600 nm, présentant déjà des facteurs de qualité dépassant les1500. / The ability to fabricate optical devices enabling the real time detection of chemical interactions,avoiding the use of markers, has motivated a growing interest. In particular, photonic crystals (PhC)based structures are promising candidates for such applications. Unlike silicon, that has currentlybeen used for most of these demonstrations, diamond offers a high stability and a versatile carbonsurface that can be functionalized to covalently bond specific organic or bio-molecules on its surface.In this context, this thesis aims at studying the interests of diamond for the realization of novel 2DPhC dedicated to biodetection applications. A fully monolithic compact photonic platform, integratedon silicon and optimized to work at wavelength of 1.55 μm was developed. A geometry consistingin a slotted cavity was chosen in order to maximize the sensitivity of such photonic structures totheir environment. Numerical methods allowed to determine the geometrical parameters of the PhC.Diamond microstructuration processes of polycrystalline diamond films deposited on two-inch siliconwafers were developed and optimized for the realization of PhC cavities with quality factors up to6500. Two technological processes specifically dedicated to polycrystalline diamond were developed : asmoothing process and a diamond layer on insulator integration by wafer bonding technology process.The optical sensitivity of diamond PhCs to simple surface modifications was studied and showed that,depending on the chemical surface termination, these diamond PhCs exhibit a strong modification oftheir spectral features. A proof of concept for surface detection in a water environment was realizedusing the biotin/streptavidin biorecognition system. The detection limit of the system was estimatedto be 10 μg/mL. Finally, first steps to detection in the visible range were made with the realization ofPhC working at 600 nm and exhibiting Q factors exceeding 1500.

Germanium is a brittle semi-metal, used for lenses and windows in Thermal Imaging Systems since it transmits infrared energy in the 2 &micro / m - 12 &micro / m wavelength range at peak. In this thesis study, polycrystalline diamond is used as cutting tool material to machine germanium. Diamond is the hardest, most abrasion-resistant material and polycrystalline diamond is produced by compacting small diamond particles under high pressure and temperature conditions, which results more homogeneous, improved strength and a durable material. However, slightly reduced hardness is obtained when compared with natural diamond. Different from finish cutting, rough cutting, performed before finishing, is used to remove most of the work-piece material. During rough cutting, surface roughness is still an important concern, since it affects the finishing operations. Roughness of the surface of product is affected by a number of factors such as cutting speed, depth of cut, feed rate as cutting parameters, and also rake angle as tool geometry parameter. In the thesis, the optimum cutting and tool geometry parameters are investigated by experimental studies for rough cutting of germanium with polycrystalline diamond tools. Single Point Diamond Turning Machine is used for rough cutting, and the roughness values of the optical surfaces are measured by White Light Interferometer. Experiments are designed by making use of &ldquo / Full Factorial&rdquo / and &ldquo / Box-Behnken&rdquo / design methods at different levels considering cutting parameters as cutting speed, depth of cut, feed rate and tool geometry parameter as rake angle.

Diploma thesis is focused on the superhard cutting materials (polycrystalline diamond, polycrystalline boron nitride) and presents their physico-mechanical properties, production, efficient use, new trends. It assesses the range of cutting tool materials and individual front world producers in terms of optimum cutting conditions for turning operations and type of material to be machined. Further, these cutting materials are compared between different manufacturers to bring out thein differences in cutting conditions.