Inconel 718 has widespread use in critical industries like aerospace, marine, and power generation. However, its challenging machinability, characterized by tool chipping/failure, and poor surface quality, remains a significant concern. Despite numerous efforts to enhance tool performance in machining hard-to-machine materials, the issue of sudden tool failure and chipping persists. This study presents an innovative in-situ tool treatment method, complemented by an optimized recoating strategy, aimed at tackling these challenges. The approach involves the application of a lubricating soft metallic Al-Si alloy coating to the tool’s faces, which can be recoated when needed. During subsequent Inconel machining, the Al-Si layer deposited on the tool melts due to high temperatures. The molten material fills microcracks on the tool surface, preventing their propagation. Moreover, the tool can slide on the beneficial tribo-films Al-Si layer which reduces friction, sticking, seizure, and built-up edge formation, resulting in decreased tool wear and chipping. The newly developed pre-machined recoating method has yielded promising outcomes, reducing cutting force and significantly improving tool lifespan compared to the PVD benchmark and uncoated tools. Additionally, this novel method enhances surface quality and minimizes undesirable microstructural alterations induced by machining. / Thesis / Master of Applied Science (MASc) / Chipping and excessive tool wear pose significant challenges in machining high-strength alloys like Inconel 718, limiting their applicability across various industries. According to research, conventional strategies used to deal with the machining challenges posed by Inconel 718 have not produced the best results. The goal of this research is to overcome the machining issues associated with such a difficult-to-cut material innovatively by depositing soft metallic coatings as a solid lubricant to enhance the machining performance. In this study, a cost-effective novel in-situ deposition technique with recoating capability as an alternative to conventional coatings is presented to achieve this goal. This innovative approach aims to improve tool performance during Inconel 718 machining significantly. This study also provides a thorough insight into the application of solid lubricants in machining, discussing their mechanisms, effectiveness, constraints, and potential to boost productivity and environmental sustainability. Furthermore, comprehensive investigations have been conducted to gain deeper insights into the prevalent wear mechanisms and surface treatments that can lead to improved machining performance for Inconel 718.

Mechanical components operating at elevated temperatures can be identified in the aerospace industry as well as in metal forming. Hot stamping is a metal forming technique utilized for manufacturing high strength lightweight components for the automotive industry. Three types of Ni-based hardfacings doped with solid lubricants were manufactured using laser cladding. An additional hardfacing was also manufactured using the Ni-based alloy only as a reference. Solid lubricants added were Ag+WS2, WS2 and Cu+MoS2. These hardfacings were manufactured and tribologically evaluated for potential application in hot stamping tooling. Direct diode laser was used for the cladding process. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used for characterization of the microstructure after deposition. Tribological testing was done using a reciprocating pin-on-disk tribometer under dry sliding conditions at temperatures in the range between RT and 600°C. Bearing steel ball and a flat pin made of the same material were used as counterbodies. Wear volume loss was measured using a 3D optical interferometer. For identification of the wear mechanisms SEM/EDS techniqueswere used. Formation of a lubricious CrxSy phase was detected after deposition, additionally encapsulation of silver particles by CrxSy was also observed. Reduction of friction coefficient was observed for every self-lubricating hardfacing compared to the reference. Lowest friction coefficient (0.23-0.3) was observed when the testing temperature was set to 400°C using a pin-on-flat configuration. Lowest wear rate was observed at 400°C, with the coating containing Ag and WS2 having a specific wear rate of 3.04 · 10−5mm3/Nm. The lubricity of the self-lubricating hardfacings was attributed to the CrxSy phase observed on the worn surface. At low to moderate temperatures abrasive wear is the main wear mechanism. At the highest testing temperature, oxidative wear was dominant.

Solid lubricant coatings with controlled microstructures are good candidates in providing lubricity in moving mechanical assembly applications, such as orthopedics and bearing steels. Nanocrystalline ZnO coatings with a layered wurtzite crystal structure have the potential to function as a lubricious material by its defective structure which is controlled by sputter deposition. The interrelationships between sputtered ZnO, its nanocrystalline structure and its lubricity will be discussed in this thesis. The nanocrystalline ZnO coatings were deposited on silicon substrates and Ti alloys by RF magnetron sputtering with different substrate adhesion layers, direct current biases, and temperatures. X-ray diffraction identified that the ZnO (0002) preferred orientation was necessary to achieve low sliding friction and wear along with substrate biasing. In addition, other analyses such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) were utilized to study the solid lubrication mechanisms responsible for low friction and wear.

Currently available solid lubricants only perform well under a limited range of environmental conditions. Unlike them, oxides are thermodynamically stable and relatively inert over a broad range of temperatures and environments. However, conventional oxides are brittle at normal temperatures; exhibiting significant plasticity only at high temperatures (>0.5Tmelting). This prevents oxides' use in tribological applications at low temperatures. If oxides can be made lubricious at low temperatures, they would be excellent solid lubricants for a wide range of conditions. Atomic layer deposition (ALD) is a growth technique capable of depositing highly uniform and conformal films in challenging applications that have buried surfaces and high-aspect-ratio features such as microelectromechanical (MEMS) devices where the need for robust solid lubricants is sometimes necessary. This dissertation investigates the surface and subsurface characteristics of ALD-grown ZnO/Al2O3 nanolaminates and ZrO2 monofilms before and after sliding at room temperature. Significant enhancement in friction and wear performance was observed for some films. HRSEM/FIB, HRTEM and ancillary techniques (i.e. SAED, EELS) were used to determine the mechanisms responsible for this enhancement. Contributory characteristics and energy dissipation modes were identified that promote low-temperature lubricity in both material systems.

Fundação de Amparo a Pesquisa do Estado de Minas Gerais / The nickel-based superalloys have a high mechanical strength which remains at elevated temperature, high creep and fatigue resistances and excellent oxidation resistance. This makes these alloys highly recommended for use in high temperature working environments such as mechanical components for the aerospace industry. However, these characteristics are major problems when machining them, as it promotes high heat generation in the flow zone, resulting in the development of high wear rates on the cutting tools. In order to reduce the problems caused by the high temperatures generated, the application of a cutting fluid, when possible, is essential to reduce friction at the chip-tool-workpiece interfaces and lower the temperatures in the cutting zone. Seeking to further increase in the efficiency of cutting fluids during machining of nickel alloys, this work presents a study of the influence of solid lubricants, graphite and molybdenum disulphide (MoS2) mixed to a vegetal based cutting fluid, applied by conventional method (flooding) and minimal quantity of fluid - MQF in turning of Inconel 718 with carbide and ceramic (mixed, whisker and SiAlON) tools. When turning with cemented carbide tools the addition of graphite to the cutting fluid provided the best results, while with ceramic tools MoS2 presented the best performance. The life of the carbide tool had an average increase above 200% in conventional flooding application of cutting fluid when compared to MQF, regardless the addition of solid lubricant. The addition of solid lubricants promoted an increase in the life of whisker and SiAlON tools. The flank wear was dominant for cemented carbide tools and SiAlON ceramics, while for whisker and mixed ceramics the notch wear was predominant. Attrition and diffusion wear mechanism were observed in all evaluated conditions. The addition of solid lubricant to the cutting fluid provided significant improvements in the surface roughness values for most of the evaluated conditions. However, there were no significant changes in the machining forces and cutting temperature. The residual stress was tensile and compression, depending on the fluid application method. Overall, the addition of solid lubricant showed no significant differences. / As superligas à base de níquel apresentam alta resistência mecânica que se mantém em elevadas temperaturas, altas resistência à fluência e à fadiga e excelente resistência a oxidação. Isso torna estas ligas altamente recomendadas para utilização em ambientes que trabalham a altas temperaturas, como por exemplo na fabricação de componentes mecânicos para a indústria aeroespacial. Entretanto, esta característica representa um grande problema quando elas são usinadas, pois promove elevada geração de calor na zona de fluxo, implicando no desenvolvimento de altas taxas de desgaste da ferramenta de corte. A fim de reduzir os problemas causados pelas altas temperaturas geradas, a aplicação de um fluido de corte, quando possível, é essencial, proporcionando redução do atrito na interface cavaco-ferramenta-peça e menores temperaturas na zona de corte. Na busca de aumentar ainda mais a eficiência dos fluidos de corte na complexa usinagem das ligas de níquel, este trabalho apresenta um estudo da influência dos lubrificantes sólidos grafite e bissulfeto de molibdênio (MoS2) misturado a um fluido de corte de base vegetal, aplicados pelo método convencional (jorro) e mínima quantidade de fluído MQF, no torneamento do Inconel 718, com ferramentas de metal duro e cerâmicas (mista, whisker e SiAlON). No torneamento com ferramentas de metal duro a adição de grafite ao fluido de corte proporcionou os melhores resultados, enquanto que no torneamento com ferramentas cerâmicas, foi o MoS2 que apresentou melhor desempenho. A vida da ferramenta de metal duro teve um incremento acima de 200% na usinagem convencional (jorro) quando comparado com a usinagem por MQF, sem considerar a adição do lubrificante sólido. A adição de lubrificantes sólidos promoveu um incremento na vida das ferramentas whisker e SiAlON. O desgaste de flanco foi predominante para as ferramentas de metal duro e cerâmica SiAlON, enquanto que nas cerâmicas whisker e mista o desgaste de entalhe foi predominante. Os mecanismo de desgaste de attrition e difusão foram observados em todas as condições avaliadas. A adição de lubrificante sólido ao fluido de corte proporcionou melhorias significativas nos valores da rugosidade para a maioria das condições avaliadas. No entanto, não se observou mudanças significativas nas forças e temperatura de usinagem. As tensões residuais foram de tração e compressão, dependendo do método de aplicação do fluido. No geral, a adição do lubrificante sólido não apresentou diferenças significativas. / Doutor em Engenharia Mecânica

Les revêtements de carbone amorphe hydrogéné (a-C:H) avec incorporation de silicium et d’oxygène (a-C:H:Si:O) sont une catégorie de lubrifiants solides, de la famille des Diamond-Like Carbon (DLC), présentant aussi bien de bonnes propriétés mécaniques que tribologiques et une bonne stabilité thermique. Bien qu’il soit établi que le comportement tribologique de ces couches est moins dépendant de l’environnement que celui des couches a-C:H, sans éléments d’addition, l’origine physicochimique de ce comportement reste à élucider. Ce travail de thèse s’inscrit dans le cadre une collaboration internationale entre le Laboratoire de Tribologie et Dynamique des Systèmes de l’Ecole Centrale Lyon et le département de Génie Mécanique et Mécanique Appliquée de l’Université de Pennsylvanie, et a pour objectifs d’apporter des réponses à ces questions ouvertes. Un large éventail de techniques expérimentales complémentaires, notamment la nanoindentation, la microscopie à force atomique (AFM), la microscopie à mesure de force (FFM), la microscopie optique et électronique, le Raman, la spectroscopie de photoélectron X (XPS) et la spectroscopie de structure près du front d’absorption de rayons X (NEXAFS) a été mis en oeuvre pour non seulement établir une carte d’identité mécanique, structurale et chimique du revêtement initial, mais aussi comprendre les modifications structurelles induites par le frottement. Afin de contrôler l’environnement au cours des essais tribologiques, nous avons utilisé d’une part un tribomètre linéaire alternatif, que nous avons équipé d’un système de soufflage de gaz permettant de changer rapidement l’environnent au cours des essais, et d’autre part un tribomètre analytique à environnement contrôlé autorisant des expérimentations tant sous vide poussé qu’à pression élevée de gaz. Ainsi, nous avons pu montrer que le coefficient de frottement augmente avec le taux de vapeur d’eau dans l’environnement et cela est réversible lorsqu’on diminue brusquement l’humidité. En outre, la vapeur d’eau protège la couche de l’usure alors que la présence d’oxygène la favorise. Grace aux observations en microscopie électronique, nous avons pu prouver que le comportement tribologique des couches a- C:H:Si:O, lors d’un frottement contre de l’acier 100Cr6, est essentiellement contrôlé par la formation de jonctions adhésives dans l’interface. Sous vide poussé ou à faible pression de gaz (<1 mbar de vapeur d’eau, <10 mbar d’oxygène ou <50 mbar d’hydrogène), la rupture de ces jonctions adhésives a lieu dans l’acier, résultant en un transfert de matériau de l’acier vers l’a-C:H:Si:O s’accompagnant d’un coefficient de frottement élevé (μ≈1.2). Au delà de ces pressions seuils de gaz, les jonctions adhésives se rompent du côté du a-C:H:Si:O, le transfert de matière s’opérant alors dans la direction opposée, du revêtement vers l’acier. Des analyses NEXAFS ont révélé que ce phénomène s’expliquait par une réaction dissociative entre les éléments du gaz environnant et les liaisons carbone C–C contraintes, favorisée par la sollicitation mécanique en extrême surface de l’a-C:H:Si:O. Ceci résulte en une diminution drastique du coefficient de frottement à des valeurs d’un ordre de grandeur inférieures à celles obtenues dans la configuration précédente. L’ensemble de ces résultats nous a ainsi permis de développer un modèle expérimental expliquant les mécanismes fondamentaux d’interaction entre l’environnement et les lubrifiants solides du type a-C:H:Si:O. / Like Carbon (DLC) coatings that exhibit outstanding mechanical properties, thermal stability and tribological performance. It is well established that the frictional and wear performances of a-C:H:Si:O are less dependent on environment than that of pure hydrogenated amorphous carbon (a-C:H). However the fundamental mechanisms accounting for such excellent tribological behavior of a-C:H:Si:O are still not fully understood. The present work, which is part of a collaboration between the Laboratoire de Tribologie et Dynamique des Systèmes of Ecole Centrale de Lyon and the department of Mechanical Engineering and Applied Mechanics of University of Pennsylvania, consists in using a multi-scale, multidisciplinary and multi-technique experimental approach for understanding the influence of environment on the tribological response of a-C:H:Si:O. A wide rang of complementary techniques, including nanoindentation, Atomic Force Microscopy (AFM), Friction Force Microscopy (FFM), optical and electron microscopy, Raman, X-ray Photoelectron Spectroscopy (XPS) and near edge x-ray absorption fine structure spectroscopy (NEXAFS), have thus been used to fully characterize the structure, composition and mechanics of the studied material, as deposited as well as after tribological testing. Control of the environment has been achieved first thanks to an open air linear reciprocating tribometer that we equipped with a gas blowing system, thus allowing a quick change of the sliding environment, and a environment-controlled analytical tribometer operating from high vacuum to elevated pressures of desired gases. We were able to evidence the strong influence of the amount of water vapor in the environment on the friction behavior of a- C:H:Si:O, with a reversible behavior when abruptly changing the environment. Contrary to water vapor, oxygen promotes the wear of a-C:H:Si:O. SEM observations revealed that while sliding a-C:H:Si:O against 52100 steel, the frictional response is controlled by the build-up and the release of adhesive junctions within the interface. Under high vacuum and below a threshold pressure of water vapor (1 mbar), oxygen (10 mbar) and hydrogen (50 mbar), adhesive junctions are released in the steel, resulting in a transfer of material from steel to a-C:H:Si:O and in a high coefficient of friction (μ≈1.2). However, as the gas pressure is increased above the threshold, the adhesive junctions break on the a-C:H:Si:O side, leading to a material transfer in the opposite direction, from the a-C:H:Si:O to the steel. NEXAFS spectroscopy revealed that a dissociative reaction occurs between the gaseous species and the strained C–C atoms in the near surface region ofa-C:H:Si:O, thus resulting in a drastic decrease of the steady state coefficient of friction by at least an order of magnitude. In light of these observations, an analytical model has been proposed to describe the fundamental interaction mechanisms between the environment and the a-C:H:Si:O/steel tribopairs.

This thesis aims to investigate the coefficient of friction between steel on steel contacts with the addition of solid lubricants such as h-BN, WS2, MoS2 in powder form, in dry conditions and wet conditions. More specifically, the purpose is to enhance the sliding between the piston rings and cylinder block in a modern high temperature steam engine developed by RANOTOR. The friction test was carried out as a linear sliding test with determined loads and sliding speed. Hertzian contact theory was deployed to calculate contact pressure and shear stresses to make sure the contact was elastic, alternatively plastic. It was found that WS2 and  MoS2 lowered the coefficient of friction quite heavily in dry conditions, acting as a thin protective-lubricating film. h-BN performed rather poorly, increasing the coefficient of friction. In a water slurry, none of the powders managed to decrease the COF due to the particles not interacting with the surfaces.The solid lubricants tested should be further tested as coatings since they acted like it in dry conditions. / Denna rapport syftar till att undersöka friktionskoefficienten i stålkontakter med tillsats av fasta smörjmedel som  h-BN, WS2, MoS2 i pulverform, under torra och våta förhållanden. Mer specifikt är syftet att förbättra glidningen mellan kolvringarna och insidan av cylindern i en modern högtemperatur-ångmotor utvecklad av RANOTOR. Friktionstestet genomfördes som ett linjärt glidtest med bestämda belastningar och glidhastighet. Hertzian-kontaktteorin användes för att beräkna kontakttryck och skjuvspänningar för att säkerställa att kontakten var elastisk alternativt plastisk. Det visade sig att WS2och MoS2 kraftigt sänkte friktionskoefficienten under torra förhållanden genom att agera som en tunn skyddande-smörjfilm. h-BN presterade dåligt och ökade friktionskoefficienten. I vattenblandning lyckades inget av pulverna minska friktionskoefficienten eftersom partiklarna inte interagerade med ytorna. De testade fasta smörjmedlen bör vidare testas som beläggningar eftersom de fungerade som dessa under torra förhållanden.