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Modification of Chemical Vapor-Deposited Carbon Electrodes with Electrocatalytic Metal Nanoparticles through a Soft Nitriding TechniqueAmoah, Enoch 01 August 2019 (has links)
Metal nanoparticles have been widely used for many catalytic and electrocatalytic applications due to their larger surface area-to-volume ratios and higher densities of active sites compared to bulk materials. This has resulted in much interest in understanding the electrocatalytic behavior of metal nanoparticles with respect to their structure. However, most research on this topic has employed collections of nanoparticles. Due to difficulties in controlling and characterizing particle loading and interparticle distance in nanoparticle ensembles, single nanoparticles studies have recently become a topic of great interest. In this study, a soft nitriding technique was applied to chemical vapor-deposited carbon ultramicroelectrodes (UMEs) in order to immobilize ligand-free AuNPs onto the carbon substrate. The feasibility of this method is geared toward studying the properties of single AuNPs immobilized onto carbon nanoelectrodes. The ligand-free AuNPs immobilized onto the nitrided carbon UMEs were highly electrocatalytic toward methanol oxidation.
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Immobilization of Gold Nanoparticles on Nitrided Carbon Fiber Ultramicroelectrodes by Direct Reduction as a Platform for Measuring Electrocatalytic Properties.Affadu-Danful, George, Neequaye, Theophilus, Bishop, Gregory W. 04 April 2018 (has links)
Due to their small size and large surface area-to-volume ratios, nanoparticles (particles with limiting dimensions smaller than 100 nm) have been widely applied as catalysts. Metal nanoparticles are typically produced in suspensions from metal ion precursors, reducing agents, and organic ligands called capping agents. Capping agents help prevent particle agglomeration, fix nanoparticle size, and promote monodispersity. However, capping agents also affect the morphology and the physico-chemical surface properties of nanoparticles, which can influence catalytic properties in unpredictable ways. While there have been extensive studies focused on examining the relationship between nanoparticle size, shape, composition and catalytic activity, relatively few have investigated the effects of capping agent properties on catalysis, and most studies involving nanoparticle catalysts have been conducted on collections, ensembles, or arrays of particles rather than single nanoparticles. Results obtained for systems composed of multiple nanoparticles dispersed on solid surfaces can be difficult to interpret due to variations in particle loading and interparticle distance, which are often challenging or impossible to control and characterize. The complexity of these unavoidable experimental variables may explain some of the seemingly inconsistent conclusions that have been drawn between nanoparticle properties and catalytic activity in recent reports. Single nanoparticle studies should help overcome limitations associated with investigations based on collections of nanoparticles by helping uncover direct relationships between nanoparticle size, surface properties, and catalytic activity that are unobscured by complex factors such as interparticle distance and particle loading. In this work, we aim to use nitrided carbon fiber ultramicroelectrodes to examine electrocatalytic properties of bare (uncapped) and capped gold nanoparticles at the single nanoparticle level.
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Ion-Nitriding Of Maraging Steel (MDN 250A Grade) For Light Combat Aircraft ApplicationsShetty, Kishora 07 1900 (has links)
Maraging steels have got high strength and good toughness. Maraging steel MDN 250A grade is used for slat tracks on the leading edge of the wing of Light Combat Aircraft (LCA). This application requires high strength and good wear resistance. Required wear resistance for this application can be achieved by ion-nitriding (also called as Plasma nitriding or Glow discharge nitriding) process of case hardening. In conventional gas nitriding process the nitriding temperature is 500 – 550 0C, which is above the aging temperature of maraging steel. Ion-nitriding at temperatures lower than 480 0C is thought to be suitable for surface hardening for application of this material in slat tracks of the leading edge of the wing of LCA. Besides this ion-nitriding is stated to improve fatigue & wear resistance properties without significantly affecting other properties. Also this is a process where the thickness requirement is minimum for the wear properties accomplished. Further, no distortion, warpage and such other dimensional inhomogeneity problems are encountered.
In ion-nitriding method glow discharge technology is used to introduce nascent (elemental) nitrogen to the surface of a metal part for subsequent diffusion into the material. The plasma assisted surface modification techniques offer a great flexibility and are capable in tailoring desirable chemical and structural surface properties independent of the bulk properties. It has other advantages like nil or very thin white layer after nitriding and there is no machining or grinding involved for complex parts after the process. The hardened surface layers become an integral part of the basic material without any significant reduction in the properties of base material.
Aim of the present work is to study ion-nitriding process on Maraging steels, to carry out ion nitriding of Maraging steel MDN 250A grade at different temperatures and evaluation of properties. Presently, the ion-nitrided slat tracks have been cleared for limited usage instead of full expected life. Studies are also needed to understand the fatigue behavior upon nitriding. The main aspects considered in this study are, optimization of thickness of the ion-nitrided layer and properties required for aircraft applications like slat tracks on the leading edge of the wing where wear resistance, corrosion resistance, mechanical properties like tensile strength, impact strength and fatigue strength are important.
To establish the variation in the basic properties of maraging steel (MDN 250A Grade) because of ion nitriding.
Aging of Maraging steel is done at 480 ± 5 0C with very close temperature control. In industrial ion-nitriding furnaces the temperature control is of the order of ± 10 0C. As a part of this research work ion-nitriding at three different temperatures which are well below 480 0C were chosen. These temperatures are 435 0C, 450 0C and 465 0C and soaking time i.e., ion-nitriding duration is 10 hours. Microstructure is characterized using optical microscope, scanning electron microscope and X-ray Diffraction. Properties evaluated include Hardness, Case depth, Tensile, Low Cycle Fatigue, Impact and Corrosion by Salt Spray.
Optical microscopy and SEM examination don’t show change in core microstructure of the material after ion-nitriding. The iron compound formed in the hardened layer is Fe4N for all the three nitriding temperatures. Ion-nitrided specimens exhibit higher surface hardness and good case depth. Salt spray test results shows that there is animprovement in corrosion resistance after nitriding. The nitrided samples shown higher UTS and 0.2 % PS values than un nitrided ones, where as % Elongation and % Reduction in Area are lower for nitrided samples as compared to un nitrided samples. This can be attributed to the surface layer getting hardened because of ion nitriding. Impact strength of nitrided samples is lower compared to un nitrided samples. This is again due to the surface layer getting hardened because of ion nitriding. Low cycle fatigue properties obtained on ion-nitrided samples show improvement in the fatigue strength due to introduction of the residual compressive stresses.
The mechanical properties satisfy the design requirements. Thus ion-nitriding of this Maraging steel (MDN 250A Grade) is suitable for parts which are subjected to constant wear and are complex in shape.
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Process development for the removal of iron from nitrided ilmeniteSwanepoel, Jaco Johannes 11 July 2011 (has links)
The Council for Scientific and Industrial Research (CSIR) in South Africa is developing a process to produce titanium tetrachloride from a low-grade material such as ilmenite. Titanium tetrachloride can then be used as feed material for titanium metal or pigment-grade titanium dioxide production. Titanium tetrachloride is commercially produced by chlorinating synthetic rutile (<92% TiO2) or titanium dioxide slag (<85% TiO2) at ~900 ˚C. A drawback of chlorination at this temperature is that any constituents other than TiO2 will end up as hazardous waste material. A characteristic step in the CSIR’s proposed process is to nitride titanium dioxide contained in the feed material before it is sent for chlorination. The chlorination of the resulting titanium nitride is achieved at a much lower temperature (~200 ˚C) than that of the existing titanium dioxide chlorination reaction. An added advantage of the low-temperature chlorination reaction is that chlorine is selective mostly towards titanium nitride and metallic iron, which means that any other constituents present are not likely to react with the chlorine. The result is reduced chlorine consumption and less hazardous waste produced. The nitrided ilmenite must, however, be upgraded by removing all iron before it can be sent for chlorination. Commercial ilmenite upgrading processes, called synthetic rutile production, also require the removal of iron and other transition metals before chlorination. A literature review of existing ilmenite upgrading processes revealed four possible process options that could remove iron from nitrided ilmenite. Two of these process options, the Becher and Austpac ERMS SR processes, are proven process routes. The other two are novel ideas – one to passivate iron contained in the nitrided ilmenite against chlorination and the other to use ammonium chloride (as used in the Becher process) as a stoichiometric reactant to produce a ferrous chloride solution. A preliminary experimental evaluation of these process options indicated that the Austpac ERMS SR process is the most viable option for removing iron from nitrided ilmenite. The Austpac ERMS SR process was therefore selected as a template for further process development. A detailed Austpac ERMS SR process review found that two process units in the Austpac ERMS SR process could be used in a process that separates iron from nitrided ilmenite. These are the Enhanced Acid Regeneration System and the Direct Reduced Iron process units. The review also concluded that another leach unit would have to be developed. It was therefore necessary to further investigate the dissolution of nitrided ilmenite in hydrochloric acid. A detailed experimental evaluation of nitrided ilmenite dissolution in hydrochloric acid found that hydrochloric acid could be used as the lixiviant to selectively remove iron from nitrided ilmenite. The dissolution of metallic iron in 90 ˚C hydrochloric acid reached levels of at least 96% after only 60 minutes. An average “combined resistance” rate law was found that could be used to describe this dissolution reaction. The observed activation energy and Arrhenius pre-exponential factor were found to be equal to 9.45 kJ.mol-1 and 30.8 s-1 respectively. The Austpac ERMS SR process review and experimental results described above were then combined and used to propose a process that could be employed to remove iron from nitrided ilmenite. The proposed process was modelled using the Flowsheet Simulation module in HSC Chemistry 7.0 / Dissertation (MEng (Chemical Engineering))--University of Pretoria, 2010. / Chemical Engineering / MEng (Chemical Engineering) / unrestricted
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Immobilization of Gold Nanoparticles on Nitrided Carbon Fiber Ultramicroelectrodes by Direct ReductionAffadu-Danful, George 01 August 2018 (has links) (PDF)
Due to enhanced properties such as large surface area-to-volume ratio, metal nanoparticles are often employed as catalysts for various applications. However, most studies involving nanoparticle catalysts have been conducted on collections of particles rather than single nanoparticles. Results obtained for ensemble systems can be difficult to interpret due to variations in particle loading and interparticle distance, which are often challenging to control and characterize. In this study, two immobilization strategies for incorporating gold nanoparticles (AuNPs) on carbon fiber ultramicroelectrodes (UMEs) were compared with the goal of extending these techniques to nanoelectrodes for studies of single AuNPs. Both layer-by-layer deposition of AuNPs on natural carbon fiber UMEs and direct reduction of AuNPs on nitrided carbon fiber UMEs were explored. Although both methods proved feasible, the direct reduction method seemed to be more effective and should better enable direct comparisons of bare and capped AuNPs.
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Modeling Material Transformations in BiorefinementAgarwal, Vishal 01 September 2012 (has links)
Lignocellulosic biomass is a significant pool of energy resource, which can be harnessed to supplement or replace the dwindling fossil fuel reserves. This requires development of economically viable means to efficiently convert biomass to biofuels. A major requirement in biofuel industry is to develop highly active, selective and stable catalysts. Zeolites are an important class of micro-porous crystalline solids, and have proven to be effective and stable acid catalysts for a variety of petrochemical and fine-chemical processes. Nitrided zeolites -- i.e., those with Si-O-Si and Si-OH-Al groups substituted by Si-NH-Si and Si-NH2-Al -- have shown promise as shape-selective basic catalysts, and are potential candidates for biofuel production catalysts. In the first part of this dissertation, the stability and base characteristics of nitrided zeolites have been explored. The nitridation mechanism in HY and silicate type zeolites is computed by first time implementation of embedded-cluster procedure with nudged-elastic-band method of finding elusive transition states. The stability of nitrided sites is investigated by modeling the kinetics of nitridation in reverse, going back to untreated zeolite plus ammonia. Our calculations suggest that nitrided silicalite and HY zeolites require high temperatures to form, but once formed, they remain relatively stable, auguring well for their use as shape-selective base catalysts. In addition, a systematic study of base strength versus aluminium content or alkali cation of nitrided zeolites is also performed. Our studies suggest that K-N-Y (Si:Al = 11) optimizes the balance of activity, stability and cost. Pyrolysis of lignocellulosic biomass is a burgeoning technology to obtain renewable fuels. Commercializing pyrolysis would require efficient process design, especially reactors as they are one of the most energy intensive units in the whole process. This would in turn require detailed understanding of complex pyrolysis chemistries. Biomass is mainly composed of the biopolymer cellulose; therefore, understanding cellulose pyrolysis chemistries is important for efficiently modeling and optimizing pyrolysis reactors. In the second part of this dissertation, the mechanism(s) of conversion of crystalline cellulose to precursors of major products in cellulose pyrolysis have been explored. As the first step, the transformation of cellulose Iβ to a high-temperature (550 K) structure is modeled by computing infrared (IR) spectra as a probe of hydrogen bonding using constant-pressure classical molecular-dynamics simulations. To assist in the analysis of IR spectra, a novel synthesis of normal mode analysis and power spectrum methods is developed to assign the O-H stretches. Simulated IR spectra at elevated temperatures suggests a structural transformation above 450 K, a result in agreement with experimental IR results. The low-temperature (300-400 K) structure is found to be dominated by intrachain hydrogen bonds, whereas in the high-temperature structure (450- 550 K), many of these intrachain hydrogen bonds transform to longer, weaker interchain hydrogen bonds. Next, the subsequent decomposition of cellulose is modeled at 600 and 873 K using Car-Parrinello molecular- dynamics simulations and the metadynamics method. The computed nascent processes can explain the formation of precursors to major products observed during cellulose pyrolysis such as levoglucosan (LGA), hydroxy-methylfurfurral (HMF) and fragmentation products such as formic acid. LGA is found to be kinetically and thermodynamically favorable in comparison to other products, which explains why LGA is the major product observed during cellulose pyrolysis. The molecular insights presented in this part of the study will be helpful in developing detailed kinetic models for optimizing pyrolysis reactors.
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Approche thermomécanique de l’interface meule/pièce/lubrifiant lors de la rectification de dentures d'engrenage en acier nitruré : impacts sur l’intégrité du matériau rectifié / Thermomechanical approach of the interface wheel/workpiece/lubricant during a nitride steel gear grinding : impacts on the grinded material integrityLavisse, Bruno 19 October 2017 (has links)
La rectification est un procédé de fabrication permettant d’obtenir des états de surface avec une rugosité très faible. Elle est généralement utilisée sur des matériaux très durs pour lesquels les autres procédés d’usinage ne sont pas adaptés, cependant, ce procédé fait intervenir des mécanismes d’enlèvement matière complexes et difficiles à mettre en oeuvre. Lors du processus de rectification, l'énergie de rectification est principalement convertie en chaleur entre la pièce, la meule, le liquide d'arrosage et les copeaux. Les températures et les flux de chaleur à l'interface meule/pièce dépendent de la géométrie du contact, du matériau rectifié, de la meule (taille de grains, géométrie, densité, porosité, usure), de son dressage, des paramètres de rectification (profondeurs de passe, vitesse d'avance, vitesse de meule, conditions de dressage), des conditions d'arrosage et de lubrification. Les températures élevées peuvent engendrer des transformations métallurgiques superficielles, des gradients de contraintes résiduelles, ainsi que des variations dimensionnelles notables. D’une façon générale l’intégrité de surface peut être grandement modifiée par cette interaction. Les conditions de rectification doivent garantir les critères de qualité et d'intégrité du matériau tout en répondant aux besoins d’augmentation de la productivité en milieu industriel. L'objectif cette thèse a été l'étude mécanico-thermique de l'interface meule/pièce/lubrifiant, dans le but de réduire le risque d'endommagement lors de la rectification d’une denture d’engrenage en acier nitruré et de qualifier les transformations éventuelles impactant l’intégrité de la pièce qui lui est associé. Pour cela nous avons développé plusieurs axes de recherche. Nous avons proposé et vérifié expérimentalement à partir d’une méthode inverse et de mesures de température par thermocouple rectifiable, un modèle de flux thermique permettant, en utilisant une mesure d’effort de prédire le profil de température à l’interface meule/pièce/lubrifiant. Nous avons effectué un comparatif détaillé de meules dans le but de déterminer celle qui permettra pour un état de surface donné de limiter le risque d’endommagement thermique du matériau rectifié. Pour effectuer cette étude, nous nous sommes intéressés à la profondeur de passe maximale admissible de chaque meule avant brûlure. Ce comparatif a été mené à la fois en laboratoire et en milieu industriel. Nous avons ensuite étudié l’influence des endommagements thermiques provoqués par la rectification en étudiant et en qualifiant la microstructure de l’acier nitruré. L’utilisation de moyens de mesure classiques (dureté, MEB EBSD, DRX) ou inédits et peu utilisés sur les brûlures de rectification (bruit Barkhausen, spectroscopie Raman) nous a permis de définir les modifications du matériau endommagé en termes de contraintes résiduelles, de dureté, de tailles de grain et de création d’oxydes. Enfin, nous avons mené une étude détaillée sur l’influence de la lubrification lors de la rectification de notre acier nitruré. Nous avons pour cela modifié indépendamment les débits et vitesses d’arrosage en sortie de buse et observé les changements que cela engendrait sur le profil température dans la zone de rectification et sur le coefficient de répartition de la pièce / The grinding process is very useful to obtain a very precise surface finish. It is generally used on very hard materials which cannot be machined by other conventional machining processes. However grinding involves very complex material removal mechanisms and most of the time is difficult to set up. During the grinding process, the main grinding energy is converted into heat between chip, lubricant, wheel and workpiece. Temperature and heat flux in the grinding zone depend on the contact geometry, on the material, on the wheel (grit size, geometry, porosity, wear), on the dressing, on the grinding parameters (depth of cut, workpiece speed, wheel speed) and on lubrication conditions. High temperatures result in thermal damage such as metallurgical changes, stress gradients, and changes in workpiece dimensions. In general terms, because of this process, surface integrity may be seriously damaged. Grinding parameters have to guarantee the workpiece quality and have to respond to the productivity improvement in machining and cutting industry. The target of this thesis was the mechanical and thermal study of the grinding zone between workpiece, wheel and lubricant in order to reduce the burn risk during the grinding of a nitrided steel gear. The purpose was also to define possible transformations associated to this damage. To achieve it, we developed several research topics. We proposed an experimentally verified heat flux model, usable to predict accurately the nitrided steel temperature in the lubricated grinding zone. This model is based on an inverse method and temperature measurements with a workpiece/foil thermocouple. We made a grinding wheel comparative study in order to determine the wheel capable, for a given workpiece roughness, of limiting the risk of burn. To perform this study, we focused, for each wheel, on the maximum allowable depth of cut before burning. This comparative study was led both in laboratory and industrial conditions. We also studied the influence of thermal damages in grinding by studying and qualifying the nitrided steel microstructure. The use of classical measurement techniques such as: hardness, SEM, EBSD and DRX or original and underused techniques such as Barkhausen noise or Raman spectroscopy permitted to define changes in the burned grinded materials. Between the two states of materials (burned and no burned), we observed differences in hardness, grain size and ferrous oxides creation. At last, we made a detailed study on the lubrication efficiency during grinding of the nitrided steel. For this purpose we changed independently fluid flow and jet speed in outlet nozzle. Then we observed the modifications this could cause on the temperature distribution in the grinding zone and on the workpiece heat partition ratio
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Comportamento à fadiga por \"fretting\" de um aço inoxidável martensítico DIN X 90 nitretado por plasma / Fretting fatigue behaviour of plasma nitrided DIN X 90 martensitic stainless steelPereira, Luiz Edno 15 May 2000 (has links)
Neste trabalho, foram determinadas as propriedades de tração, fadiga convencional e fadiga por fretting, do aço DIN 1.4112 (DIN X 90 Cr Mo V 18) nitretado por plasma, usado na fabricação de anéis de pistão de motores de combustão interna. Os corpos de prova tratados a 500ºC durante 5 horas. O material nitretado não apresentou valores de alongamento e redução de área possíveis de serem medidos e, tanto o limite de escoamento como o limite de resistência à tração, tiveram valores próximos aos do material temperado e revenido. Os ensaios de fadiga convencional e fadiga por fretting foram realizados em temperatura ambiente, sob carregamento cíclico tração-tração com R=0,1 e freqüência de 30 Hz. O fretting foi conseguido pressionando blocos de contato, feitos a partir de um ferro fundido cinzento, contra o corpo de prova de fadiga, com uma força normal de 100 N. Com o levantamento das curvas S-N para os dois ensaios, foi obtido o fator de redução de resistência FRR=1,62, que o fenômeno de fretting causa na fadiga convencional. Nos ensaios de fadiga por fretting, o pico da força de atrito aumentou com a tensão axial cíclica aplicada, atingindo um valor mínimo de 28 N e no máximo de 76 N. A camada nitretada apresentou microdureza máxima 1288 HV100 e espessura da camada de 91 μm. A metalografia revelou na camada nitretada, uma camada de compostos, a zona de difusão e uma zona de transição para o subtrato bem definidas. Foram encontrados nitretos dos tipos ε (Fe2-3N) e γ\'(Fe4N) na superfície da camada nitretada. A análise fratográfica, revelou, em tração, o trincamento da superfície devido à baixa tenacidade da camada nitretada, além da programação de trincas por fadiga abaixo da camada nitretada, nos ensaios de fadiga convencional. Os ensaios de fadiga por fretting produziram acumulação de detritos e a formação de trincas secundárias na área ) na área de contato de fretting. / In the present work, the fretting and plain fatigue properties of plasma nitrided martensitic stainless steel, DIN 1.4112 (DIN X 90 Cr Mo V 18), used in piston rings, were investigated. Both fretting and plain fatigue specimens were treated at 500°C for 5 h. The fretting pads were made of gray cast iron. Both fretting and plain fatigue tests were carried out under a load-controlled condition under stress rate, R=0.1 and frequency of 30 Hz. The S-N curves generated with and without fretting showed the strength reduction factor SRF=1.62 when fretting was applied. In the fretting fatigue, frictional force increased with axial cyclic stress and reached a minimum value of 28 N and maximum value of 60 N. Microhardness measurements have shown that the nitrided case presented a maximum hardness of 1288 HV100 and thickness of 91 μm. X-ray diffraction techniques indicated that the compound layer consists of ε (Fe2-3N) and γ\' (Fe4N) phases. Fractographic observations showed superficial cracking in tensile specimens due to the low toughness of the nitrided case and fatigue crack growth below this layer in plain fatigue specimens. Fretting fatigue tests produced accumulation of debris and the formation of secondary cracks at the contact area.
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Comportamento à fadiga por \"fretting\" de um aço inoxidável martensítico DIN X 90 nitretado por plasma / Fretting fatigue behaviour of plasma nitrided DIN X 90 martensitic stainless steelLuiz Edno Pereira 15 May 2000 (has links)
Neste trabalho, foram determinadas as propriedades de tração, fadiga convencional e fadiga por fretting, do aço DIN 1.4112 (DIN X 90 Cr Mo V 18) nitretado por plasma, usado na fabricação de anéis de pistão de motores de combustão interna. Os corpos de prova tratados a 500ºC durante 5 horas. O material nitretado não apresentou valores de alongamento e redução de área possíveis de serem medidos e, tanto o limite de escoamento como o limite de resistência à tração, tiveram valores próximos aos do material temperado e revenido. Os ensaios de fadiga convencional e fadiga por fretting foram realizados em temperatura ambiente, sob carregamento cíclico tração-tração com R=0,1 e freqüência de 30 Hz. O fretting foi conseguido pressionando blocos de contato, feitos a partir de um ferro fundido cinzento, contra o corpo de prova de fadiga, com uma força normal de 100 N. Com o levantamento das curvas S-N para os dois ensaios, foi obtido o fator de redução de resistência FRR=1,62, que o fenômeno de fretting causa na fadiga convencional. Nos ensaios de fadiga por fretting, o pico da força de atrito aumentou com a tensão axial cíclica aplicada, atingindo um valor mínimo de 28 N e no máximo de 76 N. A camada nitretada apresentou microdureza máxima 1288 HV100 e espessura da camada de 91 μm. A metalografia revelou na camada nitretada, uma camada de compostos, a zona de difusão e uma zona de transição para o subtrato bem definidas. Foram encontrados nitretos dos tipos ε (Fe2-3N) e γ\'(Fe4N) na superfície da camada nitretada. A análise fratográfica, revelou, em tração, o trincamento da superfície devido à baixa tenacidade da camada nitretada, além da programação de trincas por fadiga abaixo da camada nitretada, nos ensaios de fadiga convencional. Os ensaios de fadiga por fretting produziram acumulação de detritos e a formação de trincas secundárias na área ) na área de contato de fretting. / In the present work, the fretting and plain fatigue properties of plasma nitrided martensitic stainless steel, DIN 1.4112 (DIN X 90 Cr Mo V 18), used in piston rings, were investigated. Both fretting and plain fatigue specimens were treated at 500°C for 5 h. The fretting pads were made of gray cast iron. Both fretting and plain fatigue tests were carried out under a load-controlled condition under stress rate, R=0.1 and frequency of 30 Hz. The S-N curves generated with and without fretting showed the strength reduction factor SRF=1.62 when fretting was applied. In the fretting fatigue, frictional force increased with axial cyclic stress and reached a minimum value of 28 N and maximum value of 60 N. Microhardness measurements have shown that the nitrided case presented a maximum hardness of 1288 HV100 and thickness of 91 μm. X-ray diffraction techniques indicated that the compound layer consists of ε (Fe2-3N) and γ\' (Fe4N) phases. Fractographic observations showed superficial cracking in tensile specimens due to the low toughness of the nitrided case and fatigue crack growth below this layer in plain fatigue specimens. Fretting fatigue tests produced accumulation of debris and the formation of secondary cracks at the contact area.
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Particules d'acier nitrurées : étude de la densification et caractérisations microstructurales des matériaux frittés à vocation tribologique / Nitrided steel particles : densification study and microstructural characterizations of sintered materials for tribological applicationJolly, William 28 May 2013 (has links)
L'objectif de ce travail de thèse consistait à développer d'une technologie de mise en forme de poudres d'aciers faiblement alliés nitrurées afin d'introduire le nitrure ε-Fe2-3N dans la masse de la pièce mécanique.Pour atteindre cet objectif, deux voies ont été étudiées :- réaliser des pièces frittées à partir de poudre d'acier nitrurée ou nitrurée-enrobée (contenant une teneur importante en nitrure ε),- nitrurer et densifier une poudre d'acier pendant l'étape de frittage.La nitruration d'une poudre d'acier 4140 lors du frittage en CIC s'est avérée insuffisante vis-à-vis des teneurs en nitrure ε nécessaires pour l'application industrielle.L'étude de la stabilité, en CIC, de la poudre d'acier 4140 nitrurée a démontré la conservation des nitrures γ' et ε en grande proportion jusqu'à des températures de 650°C, quel que soit la nature du cycle de CIC appliqué. L'étude de la stabilité, à 600°C, de poudres d'acier nitrurées placées en capsules scellées a montré une légère dénitruration de ces poudres pendant le traitement.Des essais de densification de ces poudres d'acier nitrurées ont ensuite été réalisés par frittage SPS puis CIC. Afin de densifier les particules d'acier nitrurées, nous avons choisi d'utiliser un liant. Les essais de frittage SPS ont permis de mettre en évidence les paramètres expérimentaux les plus pertinents pour l'obtention d'un matériau dense et comportant le nitrure ε, et de proposer des préconisations sur les compositions acier-liant. Ces compositions ont été testées en CIC avec succès. Deux d'entre elles ont ainsi permis l'obtention de matériaux denses aux propriétés tribologiques et mécaniques satisfaisantes pour l'application industrielle. / The aim of this Ph.D thesis was to develop a technology to shape nitrided low-alloyed steels powders to introduce the ε-Fe2-3N nitride in the volume of the mechanical component.To achieve this goal, two approaches were considered:- the sintering of coated nitrided steel powder or nitrided steel powder (containing a high content of ε nitride),- the simultaneous densification and nitriding of low-alloy steel powder during the sintering step.Nitriding 4140 steel powder during hot isostatic pressing (HIP) does not allow producing sufficient ε-phase content for industrial application.The stability study of nitrided 4140 steel powder during HIP shows that a huge proportion of nitrides (γ' and ε) is conserved at 650°C, regardless of the HIP cycle. The stability study, at 600°C, of nitrided steel powders placed in sealed evacuated glass tubes, shows a slight denitriding of these powders during the process.Thus, densification of these nitrided steel powders was made by spark plasma sintering (SPS) and HIP. To densify the nitrided steel particles, we have used a copper-phosphorous binder. From SPS experiments, we have deduced the most relevant experimental parameters to obtain a dense material containing ε-phase, and we have proposed recommendations on the composition of nitrided steel-binder mixture. The identified compositions were successfully sintered by HIP. Two of them allow obtaining dense materials with interesting tribological and mechanical properties for industrial application.
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