Pulsed laser ablation of ultra-hard structures: generation of tolerant freeform surfaces for advanced machining applications

This thesis covers the laser generation of novel micro-cutting arrays in ultra-hard super-abrasive composites (e.g. polycrystalline diamond, PCD and polycrystalline cubic boron nitride, PCBN). Pulsed laser ablation (PLA) has been used to manufacture repeatable patterns of micro cutting/abrasive edges onto micro structurally different PCD/PCBN composites. The analysis on the influence of microstructural factors of the composite materials in the use of laser ablation technology has been carried out via a novel technique (Focused Ion Beam/High Resolution Transmission Electron Microscopy/Electron Energy Loss Spectroscopy) to identify the allotropic changes occurring in the composite as a consequence of PLA allowing the laser ablated PCD/PCBN surfaces to be characterized and the nanometric changes evaluated. The wear/failure characteristics/progression of the ultra-hard laser generated micro cutting/abrasive arrays has been studied in wear tests of Silicon Dioxide workpiece shafts and the influence of the microstructural factors in the wear properties of the super-abrasive micro cutting edges has been found. Opposing to these highly-engineered micro cutting/abrasive arrays, conventional electroplated abrasive pads containing diamond and CBN abrasives respectively have been chosen as benchmarks and tested under the same conditions. Contact profiling, Optical Microscopy and Environmental Scanning Electron Microscopy have been employed for the characterization of the abrasive arrays/electroplated tools before/during/after the wear/cutting tests. In the PCD abrasive micro-arrays, the type of grain and binder percentage proved to affect the wear performances due to the different extents of compressive stresses occurring at the grain boundaries. Mixed grained PCD arrays performed 25% better than fine grained arrays. All of the PCD laser manufactured arrays showed an increase up to 60% in the tool life when compared to the benchmarked pads. As for the PCBN abrasive micro-arrays, the laser manufactured arrays proved to perform 50% better than the electroplated ones in terms of wear resistance. This eThesis was first deposited on 6 November 2014

Small-scale testing of micromechanical response of cemented carbides

Tesi per compendi de publicacions, amb diferents seccions retallades per drets de l'editorCemented carbides are composite materials widely used in different industry fields within applications involving wear, due to their outstanding wear resistance. The most commonly used are WC-Co grades, for Co wettability with the carbide and adhesion characteristics. Emergence of new applications, the existence of advanced characterization techniques, economic and environmental aspects, among others, encourages the development of a new cemented carbides generation containing other binding phases as Ni and Fe or alloys of them. Furthermore, Co powder has been classified as very toxic for the human health and the combination carbide-cobalt hardmetals dust has shown to be even more toxic than both pure cobalt and tungsten. The success of substitution of the main constituents of cemented carbides, have been commonly measured in terms of their final mechanical properties at macroscale such as hardness, toughness and transverse rupture strength; and structural integrity under service-like conditions, such as corrosion resistance, thermal shock and fatigue resistance. In this sense, general framework of microstructural effects – carbide mean grain size, volume fraction and chemical nature of constitutive phases - on the mechanical response of cemented carbides is well established at the macroscale. However, assessment of the individual role of the binder and carbide phases at local scale i.e. microscale, is yet to be studied in depth. Within micromechanical testing, special attention has being paid to the micropillar compression approach because its advantages: the stress-state is nominally uniaxial, allowing a straight conversion of the measured load-displacement data into flow curves; sample preparation by means of Focused Ion Beam (FIB) milling is a relatively easy machining route; it involves the use of a conventional nanoindenter with a flat-end tip; and, it can be performed ex-situ or in-situ by using Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM) techniques. However, attention have to be paid to sample sizes since it has been well established that intrinsic properties of crystalline materials such as yield stress and strength, can be greatly influenced by extrinsic factors such as volume. For instance, results have evidenced an inverse relation between hardness and the indentation depth at the micro- and nanometric length scales. Regarding cemented carbides, recent studies showed that changes in volume fraction of binder and carbides in samples can lead to wide scatter in results of Young’s modulus measured at the microscale. Following the above ideas, in this PhD thesis uniaxial compression of micropillars and nanoindentation have been selected to evaluate the role of binder and carbides regarding their chemical nature and microstructural dimensions, i.e. carbide mean grain size and binder mean free path, in the mechanical properties and response of cemented carbides at local scales. This thesis is presented by a compendium of scientific publications in which several specific objectives are studied individually. In the first and second publications the sample size and the volume fraction of constitutive phases within the micropillar are studied respectively. Results allowed to overcome the size effect issue – usually found when testing in the micro or nanometer regime – by selecting an appropriate sample size, to accomplish reliability on the mechanical properties evaluated at local length scales. Third and fourth publications are devoted to investigating the mechanical properties of cemented carbides with partial or total substitution of WC or Co as main constitutive phases based on their intrinsic mechanical properties and behavior. Outcomes evidence that small scale testing of complex composite materials such as cemented carbides by means of uniaxial compression of micropillars and nanoindentation, allows to evaluate the role of each constitutive phase on their mechanical behavior.Los carburos cementados son materiales compuestos ampliamente utilizados en diferentes campos de la industria dentro de aplicaciones que implican desgaste, debido a su excelente resistencia al mismo. Los más utilizados son los grados WC-Co, debido a la buena mojabilidad del Co con el carburo. La aparición de nuevas aplicaciones, la existencia de técnicas avanzadas de caracterización, y aspectos económicos y ambientales, fomenta el desarrollo de una nueva generación de carburos cementados que contiene otras fases ligantes como Ni y Fe o sus aleaciones. Además, el polvo de Co ha sido clasificado como muy tóxico para la salud humana y la combinación de polvo de metal duro de carburo y cobalto ha demostrado ser aún más tóxico que el cobalto y el tungsteno puros. El éxito en la sustitución del Co y WC en carburos cementados es medido comúnmente en términos de sus propiedades mecánicas finales a escala macro, como dureza, tenacidad y resistencia; y de su integridad estructural en condiciones de servicio, como resistencia a la corrosión, choque térmico y resistencia a fatiga. En este sentido, los efectos microestructurales (tamaño medio de WC, fracción de volumen y naturaleza química de las fases constitutivas) sobre la respuesta mecánica de estos materiales están bien establecidos a macroescala. Sin embargo, el papel individual cada fase a escala local, es decir, microescala, aún no se ha estudiado en profundidad. Dentro de los ensayos micromecánicos, se ha prestado especial atención a la compresión de micropilares debido a sus ventajas: estado de tensión nominalmente uniaxial, permitiendo la conversión directa de los datos medidos de desplazamiento y carga en curvas de flujo; la preparación de la muestra mediante fresado con haz de iones focalizados (FIB) es una ruta de mecanizado relativamente fácil; implica el uso de un nanoindentador convencional con punta plana; y, puede realizarse ex situ o in situ utilizando técnicas de microscopía electrónica de barrido (SEM) o microscopía electrónica de transmisión (TEM). Sin embargo, se debe prestar atención a los tamaños de muestra, ya que las propiedades intrínsecas de los materiales cristalinos, como el límite elástico y la resistencia, pueden verse muy influidas por factores extrínsecos como el volumen. Por ejemplo, resultados han evidenciado una relación inversa entre la dureza y la profundidad de indentación en las escalas de longitud micro y nanométrica. Con respecto a los carburos cementados, estudios recientes mostraron que cambios en la fracción de volume de ligante y carburos conducen a una amplia dispersión en los resultados del módulo de Young medido a microescala. Siguiendo las ideas anteriores, en esta tesis doctoral se ha seleccionado la compresión uniaxial de micropilares y nanoindentación para evaluar el papel del ligante y los carburos con respecto a su naturaleza química y dimensiones microestructurales, es decir, el tamaño medio del grano de carburo y el camino libre medio del ligante, en las propiedades y respuesta mecánica de carburos cementados a escalas locales. Esta tesis es presentada por un compendio de publicaciones científicas en los que varios objetivos específicos se estudian individualmente. En la primera y segunda publicación se estudia el efecto del diámetro del micropilar y la fracción volumétrica de las fases constitutivas dentro del mismo para superar el problema del efecto del tamaño de la muestra, seleccionando un tamaño apropiado para lograr confiabilidad en las propiedades mecánicas evaluadas localmente. Las publicaciones tercera y cuarta se dedican a investigar las propiedades mecánicas de los carburos cementados con sustitución parcial o total de WC o Co, en función del comportamiento mecánico intrínseco de las fases constitutivas. Los resultados demuestran que las pruebas a pequeña escala de materiales compuestos complejos – como los carburos cementados – mediante compresión uniaxial de micropilares y nanoindentación, permiten evaluar el papel de cada fase constitutiva en su respuesta y propiedades mecánicas. Al hacerlo, se debe seleccionar un tamaño de muestra apropiado para obtener resultados confiables del comportamiento general del material.Els carburs cimentats – també coneguts com a metalls durs – són materials compostos àmpliament usats a diversos camps industrials en aplicacions que comporten desgast, com en eines de tall, mecanitzat o trepat, a causa de la seva excepcional resistència al mateix. Els carburs cimentats més comunament usats són graus de WC-Co, per les característiques d’humectabilitat de cobalt (Co) amb el carbur de tungstè (WC) i la seva adhesió. L’aparició de noves aplicacions, l’existència de tècniques de caracterització avançades, aspectes econòmics i ambientals, entre d’altres, fomenta a el desenvolupament d’una nova generació de carburs cimentats que continguin altres fases d’unió com níquel (Ni) i ferro (Fe) o els seus aliatges. A més, la pols de Co ha estat classificada com a molt tòxica per a la salut humana i la combinació de pols de metall dur carbur-cobalt ha demostrat ser encara més tòxica que el Co o el W purs. L’èxit de la substitució dels constituents principals dels carburs cimentats es mesura habitualment en termes de propietats mecàniques finals, com la duresa, la tenacitat de fractura Palmqvist i la resistència a fractura transversal (TRS) a escala macroscòpica; i en termes d’integritat estructural en condicions similars a servei, com ara la resistència a corrosió, resistència a xocs tèrmics i fatiga, etc. En aquest sentit, el marc general dels efectes de les característiques microestructurals – mida mitjana dels carburs i fracció de volum i naturalesa química de les fases constitutives – en la resposta mecànica dels carburs cimentats està ben establerta en l’escala macroscòpica. No obstant això, encara cal estudiar en profunditat el paper individual de la fase lligant i dels carburs en l’escala local, és a dir, a l’escala micromètrica. Pel que fa als assajos micromecànics, s’ha prestat especial atenció a la compressió de micropilars gràcies als seus avantatges: l’estat de tensions és nominalment uniaxial, permetent una conversió directa de les mesures càrrega-desplaçament a corbes de flux; la preparació de mostres mitjançant un microscopi de feix de ions (FIB) és una tècnica de mecanitzat relativament senzilla; implica l’ús d’un nanoindentador convencional amb una punta plana; i es pot realitzar ex-situ o in-situ mitjançant un microscopi electrònic de rastreig (SEM) o de transmissió (TEM). Tot i això, cal parar atenció a les dimensions de les mostres, ja que està ben establert que les propietats intrínseques dels materials cristal·lins, com ara la tensió i la resistència, poden estar molt influïdes per factors extrínsecs com ara el volum. Per exemple, els resultats han evidenciat una relació inversa entre la duresa i la profunditat d’indentació a les escales micro- i nanomètriques. Respecte als carburs cimentats, estudis recents han demostrat que canvis en la fracció volumètrica de lligant i carburs comporta una àmplia dispersió en els resultats de mòdul de Young mesurat a la microescala. Seguint aquestes idees, en aquesta tesi doctoral s’ha seleccionat la compressió uniaxial de micropilars i nanoindentació per avaluar el paper del lligant i els carburs respecte la seva naturalesa química i dimensions microestructurals, és a dir, grandària mitjana del carbur i camí lliure mig del lligant, en les propietats mecàniques dels carburs cimentats i la seva resposta mecànica a escales locals. Aquesta tesi es presenta com a compendi de publicacions científiques en les quals s’estudien objectius específics individualment. La primera publicació té com a objectiu avaluar l’efecte del diàmetre del micropilar en la resposta micromecànica del WC-Co. A la segona publicació, s’investiguen l’efecte de la mitja mitjana del gra de WC i la fracció de volum de les fases de carbur i lligant. Els resultats han permès superar el problema de l’efecte de mida – habitual quan s’assaja a escales micro- i nanomètrica – seleccionant una mida de mostra adequada per tal d’aconseguir propietats mecàniques fiables avaluades a escales locals. La tercera i quarta publicacions estan dedicades a investigar les propietats mecàniques dels carburs cimentats amb substitució parcial o total de WC o Co com a fase constitutiva principal. En aquest sentit, en la tercera publicació s’usa la tècnica de nanoindentació per avaluar la duresa intrínseca de les fases constitutives i la tensió de flux del lligant constret en un carbur cimentat WC-(W,Ti,Ta,Nb)C-Co. Finalment, en el quart treball s’han estudiat tres materials, un amb Co i dos amb substitució parcial o total de Co com a lligant, respectivament, per tal d’investigar la influència de la naturalesa química del lligant en la resposta mecànica global dels carburs cimentats, segons fenòmens de deformació plàstica i mecanismes de fallada induïts per compressió uniaxial de micropilars. Els resultats derivats de la investigació realitzada durant aquesta tesi doctoral demostren que els assajos a escala petita de materials compostos complexos com ara els carburs cementats mitjançant compressió uniaxial de micropilars i tècniques de nanoindentació permeten avaluar el rol de cada fase constitutiva en les propietats i resposta mecàniques. Per fer-ho, cal seleccionar una mida de mostra adequada per tal d’obtenir resultats fiables del comportament global del material.Postprint (published version

Investigation on micro-cutting mechanics with application to micro-milling

This thesis was submitted for the award of Doctor of Philosophy and was awarded by Brunel University LondonNowadays technology development places increasing demands on miniature and micro components and products, and micro-milling is one of the most flexible machining processes in manufacturing 3D structures and complex structured surfaces. A thorough and scientific understanding on fundamentals of the micro-milling process is essential for applying it in an industrial scale. Therefore, in-depth scientific understanding of the micro-cutting mechanics is critical, particularly on size effect, minimum chip thickness, chip formation, tool wear and cutting temperature, etc. so as to fulfil the gap between fundamentals and industrial scale applications. Therefore, three key fundamental research topics are determined for this research, and a comprehensive study on those topics is conducted by means of modeling, simulation, experiments. The topics include chip formation process in micro-milling, novel cutting force modeling in multiscale and study on the tool wear and process monitoring. The investigation into chip formation process in micro-milling consists of three stages; the micro-cutting process is firstly simulated by means of FEA with a primary focus on finding the minimum chip thickness for different tool/material pair and explaining the size effect; the simulation results are then validated by conducting micro-cutting experiment on the ultra-precision lathe. Experiments are carried out on aluminium 6082-T6 with both natural diamond and tungsten carbide tool. By knowing the minimum chip thickness for different tool/material pair, the chip formation process is investigated by performing comparative study by using the diamond and tungsten carbide micro-milling tools. As the minimum chip thickness for diamond micro-milling tool is smaller than that for tungsten carbide tool compared to nominal chip thickness, MCT is ignored in diamond micro-milling. Thus the comparative study is conducted by utilizing both tools with perfectly sharpened cutting edge and tools with the rounded cutting edge in micro-milling. The chips are inspected and associated with cutting force variations in the micro-milling process. The findings are further consolidated by comparing with research results by other researchers. The cutting force modeling is developed in three different aspects, e.g. cutting force on the unit length or area and cutting force on the unit volume in order to better understand the micro-cutting mechanics in aspects of size effect, tool wear mechanism and the cutting energy consumption. The mathematical modeling firstly starts with a novel instantaneous chip thickness algorithm, in which the instantaneous chip thickness is computed by taking account of the change of tool geometry brought about by the tool runout; then the collected cutting forces are utilized to calibrate the model coefficients. For accurate measurement on cutting forces, the Kalman Filter technique is employed to compensate the distortion of the measured cutting force. Model calibration is implemented using least-square method. The proposed cutting force model is then applied in micro-milling to represent the conditions of tool wear and the cutting energy consumption. Further study on the surface generation simulation is based on force model and its comparison with the machined surface is also performed. Cutting experiments using the new tungsten carbide tool are carried out and the tool wear is monitored offline at different machining stages. The dominant tool wear types are characterised. Tool wear is investigated by mainly analysing cutting force at different tool wear status. Frequency analysis by Fourier Transform and Wavelet Transform are carried out on the force signals, and features closely related to the tool wear status are identified and extracted. The potential of applying these features to monitoring the tool wear process is then discussed. Experimental studies to machine the structured surface and nano-metric level surface roughness are presented, the machining efficiency, dimensional accuracy and tool-path strategies are optimised so as to achieve the desired outcomes. Moreover, investigation on cutting temperature in micro-cutting is also studied to some extent by means of simulation; the influence of cutting edge radius on cutting temperature is particularly investigated. Investigation on above aspects provides systematic exploration into the micro-milling process and can contribute substantially to future micro-milling applications.China Scholarship Council and Korean Institute of Machinery and Material

Tooling performance in micro milling: Modelling, simulation and experimental study

This thesis was submitted for the degree of Doctor of Philosophy and awarded by Brunel University.With the continuing trend towards miniaturization, micro milling plays an increasingly important role in fabrication of freeform and high-accuracy micro parts or components directly and cost-effectively. The technology is in kinematics scaled down from the conventional milling, however, existing knowledge and experiences are limited and comprehensive studies on the micro tooling performance are essential and much needed particularly for the process planning and optimization. The cutting performance of micro tools is largely dependent on the dynamic performance of machine tools, tooling characteristics, work material properties and process conditions, and the latter three aspects will be focused in the study. The state of the art of micro milling technology with respect to the tooling performance has been critically reviewed, together with modelling work for performance prediction as well as metrology and instrumentation for the performance characterization. A novel 3D finite element method taking into account the geometry of a micro tool, including the tool diameter, rake angle, relief angle, cutting edge radius and helix angle, has been proposed for modelling and simulation of the micro milling process. Validation through well-designed micro milling trials demonstrates that the approach is capable of characterizing the milling process effectively. With the support of FEM simulation developed, the tooling geometrical effects, including those from helix angle, rake angle and cutting edge radius with influences on cutting forces, tool stresses, tool temperatures, milling chip formation and temperatures have been comprehensively studied and compared for potential micro tool design and optimization purposes. In an effort to prolong the tool life and enhance the tooling efficiency, DLC and NCD coatings have been deposited on micro end mills by PE-CVD and HF-CVD processes respectively. Corresponding cutting performance of these coated tools have been assessed and compared with those of WC micro tools in both dry and wet cutting conditions so as for better understanding of the coating influence on micro tools. Furthermore, the cutting characteristics of the DLC coated and uncoated tools have been analysed through verified plane-strain simulations. The effects of coating friction coefficient, coating thickness and UCT have been determined and evaluated by design of simulation method. Mechanical, chemical and physical properties of a work material have a direct influence on its micro-machinability. Five most common engineering materials including Al 6061-T6, C101, AISI 1045, 304 and P20, have been experimentally investigated and their micro milling behaviours in terms of the cutting forces, tool wear, surface roughness, and micro-burr formation have been compared and characterized. Feed rate, cutting speed and axial depth of cut constitute the complete set of process variables and they have significant effects on the tooling performance. Fundamental understanding of their influences is essential for production engineers to determine optimum cutting parameters so as to achieve the maximum extension of the tool life. 3D FE-based simulations have been carried out to predict the process variable effects on the cutting forces, tool stresses, tool temperatures as well as micro milling chip formation and temperatures. Furthermore, experimental approach has been adopted for the surface roughness characterization. Suggestions on selecting practical cutting variables have been provided in light of the results obtained. Conclusions with respect to the holistic investigation on the tooling performance in micro milling have been drawn based on the research objectives achieved. Recommendations for future work have been pointed out particularly for further future research in the research area.This study is funded by Brunel University and the UK Technology Strategy Board (TSB)

Advanced Powder Metallurgy Technologies

Powder metallurgy is a group of advanced processes used for the synthesis, processing, and shaping of various kinds of materials. Initially inspired by ceramics processing, the methodology comprising the production of a powder and its transformation to a compact solid product has attracted attention since the end of World War II. At present, many technologies are availabe for powder production (e.g., gas atomization of the melt, chemical reduction, milling, and mechanical alloying) and its consolidation (e.g., pressing and sintering, hot isostatic pressing, and spark plasma sintering). The most promising methods can achieve an ultra-fine or nano-grained powder structure, and preserve it during consolidation. Among these methods, mechanical alloying and spark plasma sintering play a key role. This book places special focus on advances in mechanical alloying, spark plasma sintering, and self-propagating high-temperature synthesis methods, as well as on the role of these processes in the development of new materials

Tungsten Carbide

Tungsten Carbide - Processing and Applications, provides fundamental and practical information of tungsten carbide from powder processing to machining technologies for industry to explore more potential applications. Tungsten carbide has attracted great interest to both engineers and academics for the sake of its excellent properties such as hard and wear-resistance, high melting point and chemically inert. It has been applied in numerous important industries including aerospace, oil and gas, automotive, semiconductor and marine as mining and cutting tools, mould and die, wear parts, etc., which also has a promising future particularly due to enabling to resist high temperature and are extremely hard

Pulsed laser ablation of ultra-hard structures: generation of tolerant freeform surfaces for advanced machining applications

This thesis covers the laser generation of novel micro-cutting arrays in ultra-hard super-abrasive composites (e.g. polycrystalline diamond, PCD and polycrystalline cubic boron nitride, PCBN). Pulsed laser ablation (PLA) has been used to manufacture repeatable patterns of micro cutting/abrasive edges onto micro structurally different PCD/PCBN composites. The analysis on the influence of microstructural factors of the composite materials in the use of laser ablation technology has been carried out via a novel technique (Focused Ion Beam/High Resolution Transmission Electron Microscopy/Electron Energy Loss Spectroscopy) to identify the allotropic changes occurring in the composite as a consequence of PLA allowing the laser ablated PCD/PCBN surfaces to be characterized and the nanometric changes evaluated. The wear/failure characteristics/progression of the ultra-hard laser generated micro cutting/abrasive arrays has been studied in wear tests of Silicon Dioxide workpiece shafts and the influence of the microstructural factors in the wear properties of the super-abrasive micro cutting edges has been found. Opposing to these highly-engineered micro cutting/abrasive arrays, conventional electroplated abrasive pads containing diamond and CBN abrasives respectively have been chosen as benchmarks and tested under the same conditions. Contact profiling, Optical Microscopy and Environmental Scanning Electron Microscopy have been employed for the characterization of the abrasive arrays/electroplated tools before/during/after the wear/cutting tests. In the PCD abrasive micro-arrays, the type of grain and binder percentage proved to affect the wear performances due to the different extents of compressive stresses occurring at the grain boundaries. Mixed grained PCD arrays performed 25% better than fine grained arrays. All of the PCD laser manufactured arrays showed an increase up to 60% in the tool life when compared to the benchmarked pads. As for the PCBN abrasive micro-arrays, the laser manufactured arrays proved to perform 50% better than the electroplated ones in terms of wear resistance. This eThesis was first deposited on 6 November 2014

Focused ion beam machining of hard materials for micro engineering applications

The Focused Ion Beam (FIB) milling of single crystal diamond was investigated and the beam drift and mill yield were quantified. The effect of water assistance on the milling of diamond was found to double the yield. The surface morphology that spontaneously forms during milling was measured and the mechanisms behind its formation investigated. The effect of gallium implantation on the diamond crystal structure was measured by x-ray diffraction. Chemical vapour deposited polycrystalline diamond (PCD) has been machined into micro scale turning tools using a combination of laser processing and FIB machining. Laser processing was used to machine PCD into rounded tool blanks and then the FIB was used to produce sharp cutting edges. This combines the volume removal ability of the laser with the small volume but high precision ability of the FIB. Turning tools with cutting edges of 39µm and 13µm were produced and tested by machining micro channels into oxygen free high conductivity copper (OFHCC). The best surface quality achieved was 28nm Sq. This is compared to a Sq of 69nm for a commercial PCD tool tested under the same circumstances. The 28nm roughness compares well to other published work that has reported a Ra of 20nm when machining OFHCC with single crystal diamond tools produced by FIB machining. The time taken to FIB machine a turning tool from a lasered blank was approximately 6.5 hours. Improvements to the machining process and set up have been suggested that should reduce this to ~1 hour, making this a more cost effective process. PCD tools with sinusoidal cutting prongs were produced using FIB. The dimensions of the prongs were less than 10µm. The tools were tested in OFHCC and the prongs survived intact. Changes to the machining conditions are suggested for improved replication of the prongs into metal. Sapphire was FIB machined to produce nano and micro patterns on a curved surface. The sapphire is part of a micro injection mould for replication of polymer parts. The comparative economics of hot embossing and injection moulding have been studied. Injection moulding was found to be the more cost effective process for making polymer parts at commercial production levels.EThOS - Electronic Theses Online ServiceGBUnited Kingdo

Tribossistemas de revestimentos multicamada de diamante CVD micro/nanocristalino

Doutoramento em Ciência e Engenharia de MateriaisA combinação das características do diamante microcristalino (MCD) e nanocristalino (NCD), tais como elevada adesão do MCD e a baixa rugosidade superficial e baixo coeficiente de atrito do NCD, é ideal para aplicações tribológicas exigentes. Deste modo, o presente trabalho centrou–se no desenvolvimento de revestimentos em multicamada MCD/NCD. Filmes com dez camadas foram depositados em amostras de cerâmicos de Si3N4 pela técnica de deposição química em fase vapor assistida por filamento quente (HFCVD). A microestrutura, qualidade do diamante e adesão foram investigadas usando técnicas como SEM, AFM, espectroscopia Raman, DRX, indentação Brale e perfilometria ótica 3D. Diversas geometrias para aplicações distintas foram revestidas: discos e esferas para testes tribológicos à escala laboratorial, e para testes em serviço, anéis de empanques mecânicos e pastilhas de corte para torneamento. Nos ensaios tribológicos esfera–sobre–plano em movimento recíproco, sob 10–90% de humidade relativa (RH), os valores médios dos coeficientes de atrito máximo e em estado estacionário são de 0,32 e 0,09, respetivamente. Em relação aos coeficientes de desgaste, observou–se um valor mínimo de cerca de 5,2×10–8 mm3N–1m–1 para valores intermédios de 20–25% de RH. A humidade relativa tem um forte efeito sobre o valor da carga crítica que triplica a partir de 40 N a 10% RH para 120 N a 90% de RH. No intervalo de temperaturas 50–100 ° C, as cargas críticas são semelhantes às obtidas em condições de baixa RH (~10–25%). A vida útil das ferramentas com revestimento de dez camadas alternadas MCD/NCD e 24 μm de espessura total no torneamento de um compósito de matriz metálica Al– 15 vol% Al2O3 (Al–MMC) é melhor do que a maioria das ferramentas de diamante CVD encontradas na literatura, e semelhante à maioria das ferramentas de diamante policristalino (PCD). A formação de cratera ocorre por desgaste sucessivo das várias camadas, atrasando a delaminação total do revestimento de diamante do substrato, ao contrário do que acontece com os revestimentos monocamada. Os anéis de empanque testados com biodiesel apresentaram coeficientes de desgaste (4,1x10–10 mm3N–1m–1) duas ordens de grandeza menores do que em ensaios esfera–sobre–plano em movimento recíproco (k = 5,0x10–8 mm3N–1m–1), mas não foi possível obter vedação completa devido a sobreaquecimento do fluido. Esta condição foi obtida com água sob pressão, para condições P.V na gama 0,72–5,3 MPa.ms–1. Um coeficiente de atrito em estado estacionário de ~ 0,04 e um valor de coeficiente de desgaste de 6,0x10–10 mm3N–1m–1, característico de um regime desgaste ultra–suave, revelam o alto desempenho deste tribossistema.The combination of the characteristics of microcrystalline diamond (MCD) and nanocrystalline diamond (NCD) varieties, such as high adhesion of MCD and low surface roughness and low friction coefficient of NCD, is ideal for highly–demanding tribological applications. The main objective of this study was thus the development of multilayered MCD/NCD coatings for such purpose. Single layer and tenfold multilayer coatings were grown onto Si3N4 ceramic samples by the hot–filament CVD (HFCVD) process and their microstructure, diamond quality and adhesion were investigated using SEM, AFM, Raman spectroscopy, XRD, Brale indentation and 3D optical profilometry. Several geometries for distinct applications were then coated: discs and balls for lab–scale tribological testing, mechanical seal rings and cutting inserts for in–service testing. For the ball–on–flat reciprocating tests in the 10–90% relative humidity (RH) range the average values of the maximum and steady–state friction coefficients are 0.32 and 0.09, respectively. Regarding the wear coefficient of the discs, a valley–shaped evolution is observed within the same RH range, with a minimum of about 5.2×10–8 mm3N–1m–1. Humidity has a strong effect on the value of the critical load that triples from 40 N at 10% RH to 120 N at 90% RH. In the 50–100 °C range the critical loads are similar to those attained under dry conditions ( 25% RH). The tool life of a 24 μm thick tenfold multilayered MCD/NCD coated insert in the turning of an Al–15 vol.% Al2O3 metal matrix composite (Al–MMC) is better than most reported CVD diamond systems, behaving as well as most PCD tools. Crater wear occurs by successive wear of the layers, delaying total delamination of the diamond coating from the substrate, unlike what would happen with monolayer coatings. Under biodiesel lubrication seal rings present wear coefficients (4.1x10–10 mm3N–1m–1) two orders of magnitude lower than the reciprocating sliding ball–on–flat experiments (k = 5.0x10–8 mm3N–1m–1), but no full sealing was possible due to overheating of the fluid. This condition was only attained with pressurized water, for P.V conditions in the range 0.72–5.3 MPa.ms–1. A steady state friction coefficient value of ~0.04 and a wear coefficient value of 6.0x10–10 mm3N–1m–1, characteristic of an ultra–mild wear regime, reveal the high performance of this tribosystem

Systematic characterization of the micromechanical behaviour of inorganic matrix composites

El nitrur de bor cúbic (cBN) policristal·lí és un material ceràmic compost que pertany a la família dels materials súper durs. La informació sobre el comportament mecànic a escales micromètriques d’aquests materials és normalment escassa. En aquest sentit, la present investigació desenvolupa un estudi sistemàtic de les propietats micro mecàniques d’un material compost de cBN amb matriu ceràmica de nitrur de titani (TiN). L’estudi complert es divideix entres lots de caracterització ben interrelacionats entre ells: 1. Anàlisis composicional i microstructural. S’han desenvolupat anàlisis de composicions químiques mitjançant EDS i EMPA. A més s’ha realitzat l’estudi microstructural mitjançant tres metodologies diferents i s’han comparat els resultat i la precisió reportada per cadascuna d’elles. 2. Assaig micromecànic. S’ha implementat la metodologia de nanoindentació massiva, aconseguint extreure les propietats intrínseques de cadascuna de les fases del material a més del seu comportament com a material compost. Les dureses que s’han obtingut han estat de 32,82 i 55 GPa per a el TiN, cBN i el material compost respectivament. 3. Anàlisi per elements finits d’un volum representatiu de material extret mitjançant la reconstrucció d’una tomografia realitzada amb la tècnica de Canó d’ions focalitzat (FIB). Per últim també s’han mecanitzat pilars de mida micromètrica fi de poder comparar la resposta mecànica del material compost predita per la simulació amb la resposta física d’un pilar de material compost en ser comprimit