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The present work investigates the tribological properties of solid particles as lubricant additives in lubricants. Two types of solid particles, Ceria nanoparticles (CeO2) and Zinc borate ultrafine powders (ZB UFPs), were used as the lubricant additives in this study. The friction and wear behaviours of these lubricant additives in different base lubricants were identified. With an appropriate application of these solid lubricant additives, the friction reduction and wear resistance properties of the lubricant have been successfully improved. Without assistance of surfactant or surface modification, the two types of solid particles behave very differently. Evident performance was observed that pure ZB UFPs were capable of considerably reducing the friction coefficient of sunflower oil and liquid paraffin when they were used as a lubricant additive without further treatment. On the contrary, CeO2 nanoparticles did not show noticeable contribution to friction reduction when they were used as the only additive in water. Only when surfactant Sorbitan monostearate was employed to enhance the dispersibility of CeO2 nanoparticles in water, the application of this additive was capable of reducing friction coefficient of the water based lubricant effectively. Surface modification of the solid particles was carried out to improve the dispersibility of these particles in base lubricants. Oleic acid (OA) and Hexadecyltrimethoxysilane (HDTMOS) were selected as the modification agents. Modified CeO2 nanoparticles and ZB UFPs revealed outstanding wear resistance property. An improvement of up to 15 times was identified although this improvement on wear resistance, in this case, was often companied by a rise in friction coefficient. Tribo-films generated by tribo-chemical reaction were observed on most of the worn surfaces and the formation of this tribo-film appeared to have played an important role in the friction and wear behaviours of a system. A tenacious tribo-film with good surface coverage was only generated on the worn surface when HDTMOS modified solid particles were used as lubricant additives. The mechanical properties and elemental composition of the tribo-film were studied with nano-indentation and energy-dispersive X-ray spectroscopy (EDS). Finally, based on the experimental evidence, different functionalities of CeO2 nanoparticles and ZB UFPs as solid lubricant additives were recognized.

The purpose of this thesis was to compare graphene nanoplatelets (GNP) and WS2 as solid lubricant additives to aluminum in order to reduce friction and wear. The central hypothesis of this work relied on lubricating properties of 2D materials, which consist layers that slip under a shear force. Two aluminum composites were made (Al-2 vol.% GNP and Al-2 vol.% WS2) by spark plasma sintering. Tribological properties were evaluated by ball-on-disk wear tests at room temperature (RT) and 200°C. WS2 not only presented the lowest COF (0.66) but also improved the wear resistance of aluminum by 54% at RT. Al-2 vol.% GNP composite displayed poor densification (91%) and low hardness resulting in poor wear resistance. The wear rate of Al-2 vol.% GNP composite increased by 233% at RT and 48% at 200°C as compared to pure aluminum. GNP addition also resulted in lower COF (0.79) as compared to pure aluminum (0.87).

No / A comparison has been made between compaction, sintering, microstructural and mechanical properties of the 6061 aluminium alloy prepared via premixed elemental (EL) and prealloyed (PA) powders (as received and degassed) with and without additions of sintering aids and various solid and/or liquid lubricants. Both EL and PA powders were cold pressed at different pressures, ranging from 250 to 770 MPa, and sintered under vacuum in the range 580-640°C for 30-120 min. and then under pure nitrogen atmosphere for comparison. Vacuum degassing of the PA powder provided better compressibility and thus higher green densities than those for the as received PA or the premixed EL powder compacts pressed at compaction pressures ¿340 MPa. Near full sintered densities of ~98%TD were obtained for both EL and PA 6061 Al alloys. Degassed PA Al with 0·6 wt-% paraffin wax (PW) or with only 0·12 wt-%Pb addition as sintering aid and no lubricant, and premixed EL with only 0·12 wt-%Pb addition and no lubricant gave the best optimum properties. It became apparent that additions of some solid lubricants such as lithium stearate (LS) and acrawax to both the premixed EL and PA powders provided reasonable green densities, but had deleterious effect on sintered densities and microstructures, particularly under vacuum sintering. Heating data curves during the sintering cycle, revealed formation of both transient and persistent liquid phases for the EL and mainly supersolidus liquid phase sintering (SLPS) mechanism for the PA. Tensile properties of the degassed, vacuum or nitrogen sintered PA Al alloy in T6 condition were higher than those of the equivalent alloy prepared by EL mixing with the former giving a tensile strength of 330 MPa and 6-8% elongation to failure, which are similar to those of the commercial (wrought) 6061 Al alloys.

No / Physical and mechanical properties for prealloyed 6061 Al powder processed with and without additions of solid and/or liquid lubricants and sintering aids (Pb, Sn, Ag) are presented. For comparison, both vacuum and nitrogen sintering were carried out on as received (gas atomised) and degassed powder compacts pressed at 340 and 510 MPa. Vacuum degassing of the prealloyed powder provided better compressibility and thus higher green densities than those for the as received powder. Highest sintered densities of ~98-99% of theoretical were obtained for the prealloyed (and degassed) Al compacts by sintering under pure nitrogen with an addition of 0·6 wt-% paraffin wax as solid lubricant or 1·33 vol.-% liquid paraffin, or with a 0·12wt-%Pb addition as sintering aid and no lubricant. It was found that additions of solid lubricants such as lithium stearate and acrawax to both the premixed (elemental) and prealloyed powders provided reasonable green densities of ~94·5-95·5% TD, but had deleterious effect on sintered densities and microstructures, particularly under vacuum sintering. Other lubricants such as zinc stearate, stearic acid and liquid paraffin provided similar green densities, but higher sintered densities and less porous microstructures, particularly by sintering under pure nitrogen. The prealloyed compacts sintered under pure nitrogen consistently provided much higher sintered densities than elementally premixed compacts sintered under pure nitrogen or vacuum. It is therefore concluded that both lubricant type and sintering atmosphere will have a major effect on the sintered properties of the 6061 Al powder. Sintering under pure nitrogen resulted in higher sintered densities as compared with vacuum sintering for this grade of Al alloy. Tensile properties of the degassed and vacuum sintered (and T6 tempered) prealloyed powder compacts were higher than those of the equivalent alloy prepared by elemental mixing and comparable with those of the commercial (wrought) 6061 Al alloys.

Ces travaux de thèse portent sur l’élaboration et la caractérisation de revêtements sol-gel composites ≪ CSG ≫ sur acier inoxydable austénitique AISI 304. L’objectif de la thèse était de mettre au point le procédé d'élaboration et d'étudier les propriétés mécaniques et le comportement tribologique des revêtements. La première partie expérimentale présente l’optimisation des conditions de synthèse d’un sol d’alumine stable et l’influence du traitement thermique du gel sur les propriétés physico-chimiques et thermostructurales. Les paramètres étudiés sont : La stabilité chimique du sol et les conditions de traitement thermique (température et temps). Différentes techniques de caractérisations ont été utilisées pour l'optimisation des paramètres d'élaboration (rhéométrie, ATD/ATG, dilatométrie, DRX, MET, pynométrie hélium). Un dopage au nitrate de fer a permis d'améliorer les conditions de frittage de l'alumine sol-gel grâce à la formation d'une solution solide (Al,Fe)2O3. Cela reste cependant insuffisant pour une application du revêtement sur le substrat acier. La seconde partie concerne l’élaboration et la caractérisation mécanique de revêtements sol-gel composites ≪ CSG ≫ charges de particules d’α-Al2O3 et de h-BN. Ce procédé a permis d'obtenir par dip-coating des dépôts monocouches de 8,5 micromètres environ avec des taux de charge de 90% volumique. Cependant, un tel taux de charge provoque la création d’une porosité importante. Les couches CSG traitées thermiquement à 750°C ont par la suite été caractérisées mécaniquement par indentation instrumentée. Les résultats obtenus ont montré une trop faible dureté des couches pour pouvoir améliorer la résistance à l'usure. La dernière partie de la thèse concerne le renforcement des revêtements CSG après traitement à l'acide phosphorique et traitement thermique à 400°C. La formation de liaisons phosphates entre les grains d'alumine renforce l'architecture du composite qui est note CB-CSG ≪ Chemically Bonded Composite Sol-Gel ≫. Des essais d'indentation instrumentée montrent, pour des revêtements CB-CSG charges d’alumine, une amélioration de la dureté par rapport au substrat en acier. Des essais de frottements secs en configuration bille sur plan montrent une augmentation de la résistance aux frottements secs d’un facteur 5 et une diminution du coefficient de frottement par rapport au substrat. L’influence du nitrure de bore hexagonal dans les couches CB-CSG en plus de l'alumine a été étudiée en particulier en ce qui concerne les propriétés mécaniques et tribologiques. / This thesis focuses on the elaboration and the characterization of composite sol-gel coatings “CSG” on austenitic stainless steelAISI 304. The aim of the thesis is to develop the process and to study the mechanical properties and tribological behavior of thecoatings. The first experimental part presents the optimization of the synthesis conditions of a stable alumina sol and the influence of the thermal treatment of the gel on the physic-chemical and thermostructural properties. The studied parameters are: The chemical stability of the sol and the thermal treatment conditions (temperature and time). Various characterization techniques are used in order to optimize the elaboration parameters (rheometry, DTA / TGA, dilatometry, XRD, TEM, helium pycnometry). A Doping with iron nitrate has improved the sintering conditions of the sol-gel alumina through the formation of a solid solution (Al,Fe)2O3. However, this remains insufficient for an application of the coating on the steel substrate. The second part concerns the elaboration and the mechanical characterization of composite sol-gel coatings "CSG" filled with particles of α-Al2O3 and h-BN. This process enables the deposition by dip coating of monolayer coatings of 8.5 micrometers thickness with fill rate of 90% by volume. However, such filler content produces a high porosity. The CSG layers thermally treated at 750°C have been mechanically characterized by instrumented indentation. The results shown to low hardnesses in order to improve the wear resistance. The last part of the work presents the strengthening of CSG coatings with a treatment with phosphoric acid followed by a thermal treatment at 400°C. The formation of phosphate bonds between the alumina grains enhances the architecture of the composite which is denoted CB-CSG "Chemically Bonded Composite Sol-Gel". Instrumented indentation tests show, for CBCSG coatings filled with alumina, an improvement of hardness compared to the steel substrate. Dry friction tests, with ball on disc configuration, show an increase of resistance to dry friction by a factor of 5 and a decrease of the coefficient of friction relatively to the substrate. The influence of the hexagonal boron nitride and of the alumina in the CB-CSG layers on the mechanical and the tribological properties are particularly studied.

Conselho Nacional de Desenvolvimento Científico e Tecnológico / This work aims to study the tribological behavior of two solid lubricant materials used in different conditions: nanoparticles as additives for lubrication fluids and self-lubricating sintered steels. The synthetic base oil with different concentrations and kinds of nanoparticles (MoS2 particles, MoS2 nanoflowers, carbon nanotubes+MoS2, silver nanoparticles) was extensively evaluated through tribological tests: ball on disk scuffing; ball on disk constant load (250 N, 20min. duration) and constant load (2N, 20min. duration) reciprocating linear sliding tests assessing friction coefficient. None of the nanoparticles affected the friction coefficient in a significant way. The nanoparticles were found to be an aggregated state. On the other hand, the effect of sintering temperatures (1100, 1150 and 1200 °C) and precursor content (0-5%) on the tribological behavior of self-lubricating sintered steels, produced by metal injection molding (MIM), was analyzed by using linear reciprocating sliding tests (constant load 7N, 60 min. duration). Solid lubrication effect was produced by in situ formation of graphite nodules due to the dissociation of precursor (SiC particles) during sintering. It was shown that presence of the graphite nodules significantly improved the friction coefficient and the wear rate of the alloys and that the sintering temperature little affected these parameters. Chemical analyses of the wear scars by scanning electron microscopy (SEM-EDX) and auger electron spectroscopy (AES) showed the presence of a tribolayer composed predominantly by carbon and oxygen. The graphite on the samples contributed to the formation of the tribolayer on the contact interface. It is suggested that during sliding graphite foils are removed from the in situ generated graphite nodules and remain at the interface thus contributing to the formation of the protective tribolayer. This tribolayer breaks up and forms during sliding and it is continuously replenished by graphite. Analyses of the wear scars showed the presence of plastic deformation traces on the samples and counter-bodies and the predominance of the wear mechanism by abrasion. Study of the influence of roughness surface showed that polishing the surfaces closed the graphite sources due to plastic deformation. This fact has resulted in a friction coefficient higher than 0.2, which means that, in this condition, this material does not act anymore as solid lubricant. / Este trabalho tem como objetivo estudar o comportamento tribológico de dois materiais lubrificantes sólidos usados em diferentes condições: nanopartículas como aditivos de lubrificantes fluidos e aços sinterizados autolubrificantes. O óleo sintético, com diferentes concentrações e tipos de nanopartículas (partículas MoS2, nanoflores de MoS2, nanotubos de carbono + MoS2, nanopartículas de prata), foi extensivamente avaliado por meio de testes tribológicos: pino sobre disco sob carga variável (scuffing) e constante (250N, durante 20 minutos) e deslizamento linear alternado (2N, durante 20 minutos). O coeficiente de atrito não apresentou alterações significativas com a presença das nanopartículas no óleo, sendo esse comportamento atribuído ao estado de aglomeração das mesmas. Por outro lado, o efeito da temperatura de sinterização (1100, 1150 e 1200 ° C) e do teor de precursor (0-5%) no comportamento tribológico dos aços sinterizados autolubrificantes, produzidos por moldagem de pós por injeção (MIM), foram analisados por meio de testes de deslizamento linear alternado sob carga constante (7N, durante 60 minutos). O efeito de lubrificação sólida foi produzido pela formação in situ de nódulos de grafita devido à dissociação do precursor (SiC) durante a sinterização. Foi mostrado que a presença de nódulos de grafita melhorou significativamente o coeficiente de atrito e a taxa de desgaste das ligas, e que a temperatura de sinterização pouco afetou estes parâmetros. As análises químicas das marcas de desgaste por microscopia eletrônica de varredura (SEM-EDX) e espectroscopia por elétron auger (AES) mostraram a presença de uma tribocamada composta predominantemente por carbono e oxigênio. Sugeriu-se que durante o deslizamento as folhas de grafita são removidas dos nódulos gerados in situ e permanecem na interface contribuindo assim para a formação da tribocamada protetora. Esta, por sua vez, rompe-se e forma-se durante o deslizamento sendo continuamente reabastecida pela grafita. As análises das marcas de desgaste das amostras e dos contra-corpos mostraram a presença de sulcos produzidos por deformações plásticas e a predominância do mecanismo de desgaste por abrasão. Estudos da influência da rugosidade superficial mostraram que as superfícies polidas apresentaram o fechamento das fontes de grafita devido à deformação plástica. Este fato deu origem a um coeficiente de atrito superior a 0.2, o que significa que, nestas condições, o material deixa de atuar como lubrificante sólido. / Doutor em Engenharia Mecânica

In this research, a temperature dependent tribological investigation of selected ternary oxides was undertaken. Based on the promising results of previous studies on silver based ternary oxides, copper based ternary oxides were selected to conduct a comparative study since both copper and silver are located in the same group in the periodic table of the elements. Two methods were used to create ternary oxides: (i) solid chemical synthesis to create powders and (ii) sputtering to produce thin films. X-ray diffraction was used to explore the evolution of phases, chemical properties, and structural properties of the coatings before and after tribotesting. Scanning electron microscopy, Auger scanning nanoprobe spectroscopy, and X-ray photoelectron spectroscopy were used to investigate the chemical and morphological properties of these materials after sliding tests. These techniques revealed that chameleon coatings of copper ternary oxides produce a friction coefficient of 0.23 when wear tested at 430 °C. The low friction is due to the formation of copper tantalate phase and copper in the coatings. All sputtering coatings showed similar tribological properties up to 430 °C.

Os implantes cone morse apresentam um travamento e vedamento por meio de atrito entre as paredes do implante e do pilar protético. Nos sistemas convencionais do tipo Hexágono externo e interno, para reduzir o afrouxamento dos parafusos protéticos, são utilizados materiais de cobertura de superfície, como carbono e ouro. Não foram encontradas referências na literatura da utilização desse tipo de deposição em componentes do sistema cone morse. O propósito desse estudo é mensurar, registrar e avaliar os valores do torque de desaperto em pilares protéticos dos tipos sólido e parafuso passante do sistema cone morse com a deposição de carbono na zona de atrito do pilar protético. Foram utilizados 40 implantes cone morse com seus respectivos pilares divididos em 4 grupos (n=10): G1- pilar sólido; G2- pilar sólido com deposição de carbono na zona de atrito do sistema morse; G3- estudo somente do parafuso do pilar passante; G4- estudo somente do parafuso do pilar passante com deposição de carbono na ponta ativa; G5- estudo somente do pilar passante sem ação do parafuso; G6- estudo somente do pilar passante revestido em carbono na zona de atrito do sistema morse sem ação do parafuso. Cada pilar recebeu uma seqüência de 5 apertos e desapertos (20Ncm para o pilar sólido e 10Ncm para o parafuso passante). Os resultados mostraram no teste estatístico ANOVA para dois fatores de variação (desaperto e carbono), haver diferença estatística significante entre os grupos: G1 maior que G2 (p < 0,01); G4 maior que G3 (p < 0,01); G6 maior que G5 (p < 0,01). Esse estudo concluiu que o grupo controle G1 mostrou maior valor através da media aritmética (23,706 Ncm) em relação ao grupo experimental G2 (22,114 Ncm); o grupo experimental G4 mostrou maior valor através da media aritmética (8,218 Ncm) em relação ao grupo controle G3 (7,354 Ncm) e o grupo experimental G6 mostrou maior valor através da media aritmética (10,268 Ncm) em relação ao grupo controle G5 (6,906 Ncm), mostrou também que não houve diferença significativa (p > 0,01) para o fator desaperto em todos os grupos estudados, ou seja, não houve interferência da deformação do material com a repetição dos ciclos de aperto e desaperto. / The morse taper implants present a locking and sealing by means of the attrition between implants internal walls and the abutment. In the external and internal conventional hexagon system, to reduce the prosthetic screw loosing, its used covering surface materials, as carbon and gold. Literature reference using these kind of surface deposition were not found in morse taper abutment implants. The aim of this study is to measure, register and evaluate the removal torque values in morse taper solid abutment and passing screw abutment with carbon deposition in attrition zone. They were used 40 morse taper implants with their respective abutments divided in 4 groups (n = 10): G1 solid abutment; G2 - solid abutment with carbon deposition in attrition zone; G3 evaluation only in the screw of the passing abutment; G4 - evaluation only in the screw of the passing abutment with carbon deposition in the screw thread; G5 - evaluation only in the passing abutment without the screw action; G6 - evaluation only in the passing abutment with carbon deposition in attrition zone without the screw action. Each abutment received a sequence of 5 tightening and removal torque (20Ncm in solid abutment and 10Ncm in passant screw abutment). The results of ANOVA statistic test for two factors of variation (removal torque and carbon), showed that there is significant statistic difference between the groups: G1 higher than G2 (p < 0.01); G4 higher than G3 (p < 0.01); G6 higher than G5 (p < 0.01). This study concluded that control group G1 showed a higher value through the arithmetical media (23.706Ncm) in relation of the experimental group G2 (22.114Ncm); the experimental group G4 showed higher value through the arithmetical media (8.218Ncm) in relation of the control group G3 (7.354Ncm) and the experimental group G6 showed higher values through the arithmetical media (10.268Ncm) in relation of the control group G5 (6.906Ncm), and also showed that there was not significant difference (p < 0.01) to the removal torque factor in all the groups studied, that is, there was not a material deformation interference with the tightening and removal torque cycles repetition.