Orientador: Carlos Roberto Grandini / Banca: Marize Varella de Oliveira / Banca: Nilson Tadeu Camarinho de Oliveira / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: Desde 1970, o titânio e algumas de suas ligas são vastamente usados na fabrição de próteses e dispositivos especiais nas áreas médica e odontológica devido às suas propriedades como baixos valores de módulo de elasticidade (Módulo de Young), resistência à corrosão e características de biocompatibilidade. A presença de elementos intersticiais (oxigênio, carbono, nitrogênio e hidrogênio) altera de maneira significativa as propriedades mecânicas da liga, principalmente suas propriedades elásticas, causando endurecimento ou fragilização da liga. As medidas de espectroscopia mecânica constituem uma ferramenta poderosa para o estudo da interação destes elementos substitucionais e intersticiais com a matriz metálica. O objetivo do trabalho foi prepararA LIGA Ti-15Mo por fusão a arco, e estudar a influência de tratamentos térmicos e do oxigênio presente em solução sólida, na estrutura, propriedades mecânicas, químicas, anelásticas e biocompatibilidade da liga. Os resultados de difração de raios X analisados pelo método de Rietveld permitiram quantificar as fases presentes na microestrutura, estando de acordo com as micrografias obtidas. Os resultados de dureza e módulo de elasticidade mostraram ser sensíveis à concentração de oxigênio e à microestrutura da liga. Nos ensaios de corrosão houve uma melhora significativa do potencial de corrosão após as dopagens com oxigênio. As medidas de espectroscopia mecânica apresentaram estruturas de relaxação e foram identificados os processos constituintes. Os ensaios de biocompatibilidade mostraram que a liga em questão pode ser considerada biocompatível / Abstract: Since 1970, titanium and some of its alloys have been widely used in the manufacture of special devices and prostheses in medical and dental areas due to properties which include low elasticity modulus values, corrosion resistance and characteristics of biocumpatibility. The presence of interstial elements (carbon, nitrogen, oxygen and hydrogen) significantly alters the alloy's mechanical properties, mainly its elastic properties, causing either a hardening or softening of the alloy. Mechanical spectroscopy measurements are a powerful tool to study the interaction of these substitutional and interstitial elements with a metallic matrix. The aim of this work was to prepare the Ti-15Mo alloy by arc-melting and study the influence of heat treatments and oxygen present in the solid solution of the structure, as well as the mechanical, chemical and anelastic properties, and biocompatibility of the alloys. The results of x-ray diffraction were analyzed by the Rietveld Method to allow the phases present in the microestructure to be quantified according to the obtained micrographies. The hardness and elasticity modulus results were sensitive to the oxygen concentration and the alloy microstructure. In corrosion tests there was a significant improvement of the corrosion potential after the oxygen dopyng. The mechanical spectroscopy measurements showed relaxation structures, and constituent relaxation processes were identified. The biocompatibility tests showed that the alloy in question can be considered biocompatible / Mestre

Made available in DSpace on 2016-12-23T14:08:13Z (GMT). No. of bitstreams: 1 Samuel Deoteronio da Silva - parte 1.pdf: 1190958 bytes, checksum: 08460415eb12294aa05f2834b78651da (MD5) Previous issue date: 2010-08-31 / Foram avaliadas a microestrutura, propriedades mecânicas e a resistência a corrosão de juntas soldadas de aço inoxidável duplex UNS S32304, submetidas a diferentes Tratamentos Térmicos Pós-Soldagem (TTPS). Fitas de aço inoxidável duplex UNS S32304, com 72 mm de largura e 1,8 mm de espessura, foram soldados pelo processo GTAW Gas Tungsten Arc Welding com corrente pulsada e sem metal de adição. Posteriormente foram tratadas termicamente por indução nas temperaturas de 950, 1050, e 1150°C durante 10 e 30 segundos. Através da microscopia ótica, utilizando-se diferentes ataques eletroquímicos, foram estudadas as microestruturas obtidas nas diferentes condições. As frações volumétricas de ferrita e austenita foram avaliadas por metalografia quantitativa e permeabilidade magnética. Foram realizados ensaios de tração para comparação das propriedades mecânicas. A resistência a corrosão foi investigada através de curvas de polarização anódica, medições dos potenciais de pite Ep e da temperatura crítica de pite (CPT). Os tratamentos térmicos pós-soldagem melhoraram tanto as propriedades mecânicas quanto a resistência a corrosão das juntas soldadas de aço inoxidável duplex UNS S32304. Evidenciou-se que fato citado está relacionado com a dissolução de precipitados de nitreto de cromo e o equilíbrio das frações volumétricas de ferrita e austenita no aço inoxidável duplex

Submitted by Jorge Silva (jorgelmsilva@ufrrj.br) on 2018-11-09T17:20:37Z No. of bitstreams: 1 2013 - Simone Alves do Nascimento Camilo.pdf: 363101 bytes, checksum: 552ddec128420b872fba894157546afe (MD5) / Made available in DSpace on 2018-11-09T17:20:39Z (GMT). No. of bitstreams: 1 2013 - Simone Alves do Nascimento Camilo.pdf: 363101 bytes, checksum: 552ddec128420b872fba894157546afe (MD5) Previous issue date: 2013-03-21 / CAPES / The soybean, besides containing protein of high biological value, presents oil with high content of polyunsaturated fatty acids, also having good emulsifying properties. Thus, soybean may be used for preparing creamy products. In spite of these advantages, its use is limited in Brazil due to its beany flavor. With the objective of developing a process to produce "soy-cream" with good sensory characteristics, dehulled soybean grains were boiled in water, as well as in NaHCO3 solution at three concentrations (0.25; 0.75 and 1.25%) at three cooking times (10, 25 and 40min), totaling 12 treatments. Then, the soybean grains were disintegrated with a paste of gelatinized starch, and subsequently, formulated to obtain the "soy-creams". These were submitted to a series of sensory evaluations (overall impression, sensory quality, quantitative descriptive analysis and preference), using a commercial milkcream for comparison. It was also carried out the analysis of proximate centesimal composition, as well as the determination of fatty acid profile. The results showed that a better boiling condition for dehulled soybean grains, used for preparing "soy-cream" with better sensory characteristics, was NaHCO3 at 0.75% for 25min using 40% of oil, although this was less preferred by the untrained panelists than the commercial milkcream. These two creams were submitted once more to consumer-type preference test, showing no significant difference between them. This "soy-cream" presented 84.85% of unsaturated fatty acids. Using this "soy-cream" and the commercial milkcream, two whipped cream (chantily) were prepared and submitted to consumer-type preference test. The results showed that the "soy-chantily? was more preferred than the one prepared with the commercial milkcream. Similarly, two ?spinach sauces? were prepared and submitted to consumer-type preference test. The results show that the "spinach sauce" prepared with the "soy-cream" was more preferred than that prepared with the commercial milkcream. / A soja, al?m de conter prote?na de alto valor biol?gico, apresenta ?leo com alto teor de ?cidos graxos poliinsaturados, tendo tamb?m boas propriedades emulsificantes. Desta forma, a soja pode ser usada para elabora??o do creme. Apesar destas vantagens, a sua utiliza??o no Brasil ? limitada devido ao sabor de feij?o cru (?beany-flavor?). Com objetivo de desenvolver um processo que permita obter um ?creme de soja? com boas caracter?sticas sensoriais, os gr?os de soja decorticados foram fervidos em ?gua e em solu??o de NaHCO3 a tr?s n?veis de concentra??o (0,25; 0,75 e 1,25%), durante tr?s intervalos de tempo (10, 25 e 40min), totalizando 12 tratamentos. Em seguida, os gr?os foram desintegrados com a pasta de amido gelatinoso, e formulados posteriormente, para obter os ?cremes de soja?. Estes foram submetidos a uma s?rie de avalia??es sensoriais (impress?o global, qualidade sensorial, an?lise descritiva quantitativa e prefer?ncia), usando-se o creme de leite comercial para a compara??o. Foi feita tamb?m a an?lise de composi??o centesimal aproximada, bem como a an?lise de perfil de ?cidos graxos. Os resultados indicam que, a melhor condi??o de fervura dos gr?os de soja decorticados para o uso em ?creme de soja? com melhores caracter?sticas sensoriais foi o emprego de NaHCO3 a 0,75% por 25min, usando-se 40% de ?leo, embora este tenha sido menos preferido por provadores n?o treinados do que o creme de leite comercial. Estes dois cremes foram submetidos novamente a teste massal de prefer?ncia com consumidores, mostrando que n?o houve diferen?a significativa entre essas duas amostras. O ?creme de soja? selecionado teve 84,85% de ?cidos graxos insaturados. Usando-se este ?creme de soja? e o creme de leite comercial, foram preparados dois chantilis, sendo submetidos a teste massal de prefer?ncia com consumidores. Os resultados mostram que o ?chantili de soja? foi mais preferido do que aquele preparado com o creme de leite comercial. Da mesma forma, foram preparados os dois ?molhos de espinafre? e submetidos a teste de consumidores. Os resultados indicam que o ?molho de espinafre? preparado com o ?creme de soja? foi mais preferido do que aquele preparado com o creme de leite comercial.

Garantir la qualité des produits sanguins est crucial. Les lysats plaquettaires (LP) riches en facteurs de croissance (FC) s’imposent comme le complément idéal pour l’expansion ex vivo des cellules souches, et comme produit thérapeutique pour la régénération cellulaire. L’intérêt est croissant pour les microparticules (MPs) extracellulaires, mais l’expression de phosphatidylsérine à leur surface peut induire des effets thrombotiques et inflammatoires. L’autre risque transfusionnel, la transmission de virus, dont le virus de l’hépatite C (VHC), est maîtrisable par traitements de réduction virale par solvant/détergent (S/D), chauffage, ou nanofiltration. Nous avons étudié des technologies de sécurisation des produits sanguins: (a) élimination des MPs par nanofiltration sur filtres de 75 nm et (b) traitements S/D, chauffage à 56°C ou nanofiltration pour inactiver ou éliminer le VHC. Les informations ont été utilisées pour développer des LP utiles en médecine régénérative. L’un d’eux destiné à la neurorégénération, a été préparé en émettant l’hypothèse qu’un lysat de culot plaquettaire (LCP) enrichi en facteurs neurotrophiques et dépourvu de protéines plasmatiques se montrerait efficace contre les maladies neurodégénératives. Nos résultats montrent que la nanofiltration sur des filtres de 75 nm préserve la composition en protéines plasmatiques, et le pouvoir hémostatique. La nanofiltration retire les MPs et évite, in vitro, la génération de thrombine. Par ailleurs le traitement S/D à 31°C pour 30 minutes élimine le pouvoir infectieux du VHC. Pris globalement les traitements de nanofiltration et S/D apparaissent donc comme des méthodes de choix pour l’amélioration de la sécurité du plasma vis à vis de risques thrombogènes et infectieux. Nous avons ensuite préparé un LCP appauvri en protéines plasmatiques (dont le fibrinogène) et enrichi en un mélange pléiotrope physiologique de FC destiné à l’administration cérébrale. Les analyses par ELISA et par protéomique ont montré qu’un chauffage de 56°C pour 30 min réduisait le contenu en protéines et modifiait favorablement la composition relative en facteurs neurotrophiques. Par ailleurs le chauffage améliore l’action neuroprotectrice et, associé aux traitements S/D et de nanofiltration, contribue à l’inactivation du VHC. Ce LCP exerce une neuroprotection élevée dans des modèles de la maladie de Parkinson (MP) tout à la fois (a) in vitro (cellules LUHMES différentiées en neurones dopaminergiques et exposées au MPP+) et (b) in vivo (souris intoxiquées par MPTP). L’expression de la tyrosine hydroxylase (TH) dans la Substantia nigra pars compacta montre que l’administration intracérébroventriculaire (ICV) ou intranasale (i.n.) apparait comme une option thérapeutique possible des maladies neuro-dégénératives. Les études cellulaires In vitro sur LUHMES et NSC34 ont montré que l’inhibition spécifique des voies signalétiques relayées par AkT et ERK altère l’activité neuroprotectrice du LC. Des événements neuro-inflammatoires pouvant aggraver l’évolution des maladies neurodégénératives, nous avons vérifié que le LCP n’induit pas de marqueurs inflammatoires (COX-2, iNOS) chez des cellules microgliales BV2, et pouvait même diminuer celle de COX-2 après exposition à des lipopolysaccharides. De plus, nous avons identifié que le LCP contenait 1.7 x 1012 MP/mL d’une taille moyenne de 160 nm. Isolées, ces MPs pourraient exercer un rôle neuroprotecteur des cellules LUHMES exposées à des agents neurotoxiques. En conclusion, nos résultats montrent la faisabilité technique à préparer des lysats plaquettaires viro-inactivés pour des usages dans le domaine de la médecine régénérative, y compris comme agent neuroprotecteur du système nerveux central. / Ensuring quality and safety of blood products is crucial. Platelet lysates (PL) rich in growth factors (GFs) have emerged as ideal clinical-grade supplement for ex vivo expansion of mesenchymal stromal cells, and as therapeutic product promote cellular regeneration. Interest for platelet extracellular microparticles (MPs) is growing but expression of phosphatidylserine on their surface may cause thrombotic and inflammatory side effects. Another transfusional risk, transmission of viruses, including hepatitis C virus (HCV), can be fully controlled by dedicated viral reduction methods as solvent/detergent (S/D) or heat treatments, or nanofiltration. We have evaluated technologies to secure therapeutic blood products: (a) removal of MPs by 75nm-nanofiltration and (b) inactivation/removal of HCV by S/D or 56°C heat treatments, or nanofiltration. Data have been used to develop LP of interest for regenerative medicine. In particular, one, targeting neuroregenerative applications, has been prepared based on the hypothesis that a platelet pellet lysate (PPL) enriched in multiple neurotrophic growth factors and depleted of plasma proteins could exert potent neuroprotective actions in neurodegenerative disease models. Our data show that 75 nm-plasma nanofiltration preserved plasma protein biochemical profile, and hemostatic power. Nanofiltration removes MPs and avoids in vitro the generation of thrombin. In addition, the S/D treatment at 31°C for 30 minutes fully inactivates HCV infectivity. Therefore, altogether, nanofiltration and S/D emerge as choice procedures to improve the safety of plasma for thrombogenic and infectious risks. We have then prepared a PPL depleted of plasma proteins (in particular fibrinogen), and rich in a physiological pleiotropic mixture of neurotrophins for brain administration. ELISA and proteomics studies revealed that the heat-treatment at 56°C for 30 min decreased the protein content and favorably modified the relative composition in neurotrophic factors. Heat-treatment improved the neuroprotective activity and, together with S/D and nanofiltration contributed to HCV inactivation. This PPL exerted strong neuroprotective effects in Parkinson’s disease (PD) models (a) in vitro, using LUHMES cells exposed to MPP+ neurotoxin, and (b) in vivo, in mice intoxicated by MPTP neurotoxin. Expression of tyrosine hydroxylase (TH) in the Substantia nigra pars compacta indicated that brain delivery by intracerebroventricular (ICV) or intranasal (i.n.) administration may be a therapeutic option for disease-modifying strategies of neurodegenerative diseases. In vitro studies in LUHMES and NSC34 cells showed that specific inhibition of signal transduction pathways through AkT and ERK influenced PPL neuroprotective function. Since neuro-inflammation detrimentally affects neurodegenerative disorders, we verified that the PPL did not stimulate the release of inflammatory markers (e.g. COX-2, iNOS) by BV2 microglial cells in culture, and could even restrict COX-2 expression when cells were exposed to LPS. In addition, the PPL was found to contain 1.7 x 1012 MP/mL with a mean size of 160 nm. These MPs may exert neuroprotective activity on LUHMES cells exposed to neurotoxins. Altogether, our data demonstrate the technical feasibility of developing virally-safe customized platelet lysate preparations with specific applications for cell therapy and regenerative medicine, in particular as neuroprotective agents of the central nervous system.

La micro fusion laser d'un lit de poudre (SLM) permet la réalisation de pièces complexes avec des microstructuresfines. Cette technologie présente de nombreux avantages mais se heurte encore à une faible disponibilité des poudres d'alliages. En SLM, la pièce est d'abord conçue par CAO (conception assistée par ordinateur), puis construite couche par couche avec un faisceau laser commandé par un ordinateur. Dans ce cadre, le travail effectué dans cette thèse a consisté à étudier et à développer une nouvelle méthode pour réaliser des pièces en alliages et en composites à partir de mélanges de poudres élémentaires, ouvrant ainsi la voie à une grande variété de compositions.Au niveau expérimental le choix s'est porté sur le système aluminium-silicium avec différentes teneurs en silicium (12, 18 et 50% en poids). L'effet de l'ajout d'un champ magnétique statique a aussi été proposé comme un outil supplémentaire de contrôle de la microstructure.Dans le processus de fabrication de pièces par SLM la puissance du laser et la vitesse de balayage déterminent au premier chef la densité, la microstructure, la composition des phases et les propriétés mécaniques du produit. Une analyse systématique de l'effet de ces paramètres sur l'alliage Al - Si fabriqué par SLM à partir de mélanges de poudres est présentée. Des alliages ont été ainsi obtenus pour plusieurs domaines de composition visés correspondant à des applications pratiques (structures légères, système tribologique, emballage électronique, ...).Les microstructures fines obtenues grâce à la solidification rapide des matériaux fondus conduit à des propriétés quise comparent de façon favorable à celles obtenues avec les techniques classiques d'élaboration et de mise en oeuvre. / As a new manufacturing technology, Selective laser melting (SLM) has a large potential in the manufacturing of complex parts with ultrafine microstructure.Selective laser melting has many significant advantages over traditional manufacturing methods but still faces a low availability of powder materials. With SLM, the part is firstly designed via 3D computer-aided design (CAD)), then built layer-by-layer with a high energy computer-controlled laser beam The work done in this study was therefore aiming at developing a new way to obtain alloys and composites directly from elemental powder mixtures with a large composition flexibility.Experimentally the choice was made of the aluminum-silicon system with several silicon contents (12, 18, 50 wt. %).Adding a static magnetic field was also considered as an additional way to control the microstructure. When parts are manufactured by SLM, laser power and scanning speed are the main parameters determining the density, microstructure, phase composition and mechanical properties. A systematic analysis of the role of these parameter on the manufacturing of Al - Si alloys by SLM from mixtures of powders was therefore conducted. Al - Si alloys with a very fine microstructure were thus obtained for several composition ranges corresponding to practical applications (lightweight structures, high wear resistance alloys, electronic packaging material, ...). The properties of the materials obtained in this way, according to the performed characterizations, compares favorably with those obtained via the conventional production technologies.

High chromium cast iron (HCCI) is considered as one of the most useful wear resistance materials and their usage are widely spread in industry. The mechanical properties of HCCI mainly depend on type, size, number, morphology of hard carbides and the matrix structure (γ or α). The hypereutectic HCCI with large volume fractions of hard carbides is preferred to apply in wear applications. However, the coarser and larger primary M7C3 carbides will be precipitated during the solidification of the hypereutectic alloy and these will have a negative influence on the wear resistance. In this thesis, the Ti-alloyed hypereutectic HCCI with a main composition of Fe-17mass%Cr-4mass%C is studied based on the experimental results and calculation results. The type, size distribution, composition and morphology of hard carbides and martensite units are discussed quantitatively. For a as-cast condition, a 11.2μm border size is suggested to classify the primary M7C3 carbides and eutectic M7C3 carbides. Thereafter, the change of the solidification structure and especially the refinement of carbides (M7C3 and TiC) size by changing the cooling rates and Ti addition is determined and discussed. Furthermore, the mechanical properties of hypereutectic HCCI related to the solidification structure are discussed. Mechanical properties of HCCI can normally be improved by a heat treatment process. The size distribution and the volume fraction of carbides (M7C3 and TiC) as well as the matrix structure (martensite) were examined by means of scanning electron microscopy (SEM), in-situ observation by using Confocal Laser Scanning Microscope (CLSM), Transmission electron microscopy (TEM) and electron backscattered diffraction (EBSD). Especially for the matrix structure and secondary M7C3 carbides, EBSD and CLSM are useful tools to classify the fcc (γ) and bcc (α) phases and to study the dynamic behavior of secondary M7C3 carbides. In conclusion, low holding temperatures close to the eutectic temperature and long holding times are the best heat treatment strategies in order to improve wear resistance and hardness of Ti-alloyed hypereutectic HCCI. Finally, the maximum carbides size is estimated by using statistics of extreme values (SEV) method in order to complete the size distribution results. Meanwhile, the characteristic of different carbides types will be summarized and classified based on the shape factor. / <p>QC 20130913</p>

Ett företag som tillverkar hydrauliska snabbkopplingar har genom regelbundna kvalitetsprover upptäckt att vissa låskulor till snabbkopplingarnas låsmekanism plötsligt fått en bristande kvalité och spricker vid belastning. Låskulorna är gjorda av rostfritt stål och har en viktig funktion i låsmekanismen. Om de spricker vid användning kan det leda till konsekvenser med materiella skador eller personskador. Företaget vill förekomma eventuella kvalitetsproblem och måste därför säkerställa att låskulorna har rätt hållfasthet. Låskulorna köps in från en underleverantör och företaget vill därför utveckla en provmetod som provar låskulornas materialegenskaper när de levereras till fabriken. Arbetet i denna rapport syftar till att hjälpa företaget utveckla en sådan provmetod. Ett första steg är att undersöka orsaken till att låskulorna spricker. Materialanalyser utförs av ett materiallaboratorium för att fastställa vilka faktorer i materialet som orsakar brott i låskulorna. Analyserna visar att låskulorna sannolikt spricker på grund av en ökad sprödhet i materialet. Sprödheten beror på att martensiten i materialet är dåligt anlöpt samt en stor mängd karbider. Med orsaken till sprickorna fastställd undersöks befintliga metoder för materialprovning. En provmetod måste prova materialet i färdigtillverkade låskulor eftersom låskulornas tillverkningsprocess påverkar materialegenskaperna. Många av de standardiserade provmetoderna är dock svåra att tillämpa på låskulorna med anledning av låskulornas geometri och små dimensioner. En form av slagprov och pressprov utförs på låskulorna. Ett av syftena med proven är att undersöka om de är lämpliga att använda som provmetod. Genom proven framträder olika materialegenskaper för olika låskulor. Resultaten är dock inte jämförbara låskulorna emellan och proven anses inte vara lämpliga som provmetod. Även ett utmattningsprov utförs på låskulorna genom en upprepande belastning i en snabbkoppling. Detta prov är inte heller lämpligt att använda som provmetod då provet är mycket tidskrävande samt att det finns vissa osäkerheter kring provresultatet. I detta arbete undersöks även två nyligen framtagna provmetoder för kulor till kullager och möjligheten att tillämpa dessa provmetoder på låskulorna. I undersökningen jämförs de båda provmetoderna med avseende på utförande samt framtagning av provkropp. Även en spänningsanalys av en låskula belastad i en snabbkoppling utförs för att ta reda på i vilket område av låskulan de maximala spänningarna uppstår. Undersökningen ger att enbart en provmetod är intressant för fortsatt arbete.   Den provmetod som föreslås i detta arbete kallas "the notched ball test" (NBT). Provmetoden innebär att en djup och smal skåra bearbetas i en låskula som sedan belastas med en tryckande kraft vinkelrätt mot skåran tills brott uppstår. Den maximala spänningen som verkar vid brottet beräknas med en enkel ekvation och används som mått för låskulans hållfasthet. Provmetoden är lämplig då den går att utföra med befintlig utrustning på företaget, den provar materialet i färdigtillverkade låskulor samt i samma område som de maximala spänningarna i en låskula belastad i en snabbkoppling uppstår. NBT nyttjar även dragspänningar vilket är fördelaktigt när sprödhet ska upptäckas i ett material. För att fastställa hur olika materialegenskaper samt geometrier för provkroppen påverkar provresultaten utförs en djupare analys av provmetoden. Analysen ger även vilka geometrier som bör användas vid utförandet av NBT samt värdet för den konstant som används vid beräkning av brottspänningen. Praktiska prov av NBT utförs inte i detta arbete men rapporten innefattar slutsatser om provmetoden och rekommendationer till företaget hur ett fortsatt arbete med NBT kan utföras. / A company that manufactures hydraulic quick-couplings has discovered through regular quality checks that the quality of some of the locking balls for the locking mechanism in the quick couplings suddenly has become insufficient and the locking balls rupture under load. The locking balls are made of stainless steel and if they rupture during usage the consequences can be material damage or even personal injury. The company wants to prevent any quality problems and must therefore ensure that the strength of the locking balls is sufficient. The locking balls are purchased from a subcontractor and the company would therefore like to develop a method for strength testing locking balls delivered to the factory. This thesis aims to help the company in developing such a method.  A first step is to investigate the cause of the locking balls rupture. Material analyses are executed by a material laboratory in order to determine what features in the material that causes the ruptures. The analyses shows that rupture is probably caused by an increased brittleness in the material and the brittleness is a consequence of less tempered martensite and a high amount of carbides. With the cause of rupture determined, existing methods for testing material properties is studied. It is important that strength testing is carried out with test specimens prepared from the actual locking balls. Otherwise the influence of the locking balls manufacturing process on the material properties is not taking into account. Many of the standardized methods for testing material properties, however, are hard to apply to the locking balls due to the geometry and small dimensions of the locking balls. A kind of impact test and compression test is performed. One of the purposes with the tests is to investigate if they are adequate for strength testing the locking balls. The results of the tests, however, are not suitable for comparison. Also, a fatigue test of the locking balls is performed by a repetitive loading of a quick coupling. The fatigue test is, however, time consuming and there are uncertainties in the test results. None of these tests is considered suitable as a strength testing method. In this thesis, two recently developed methods for strength testing ceramic balls and the possibility to apply these methods on the locking balls is studied. The study includes an analysis of the stress distribution in a locking ball under load to determine in which region the highest stresses occur. The study provides that only one of the methods is suitable for the locking balls due to differences in preparing the test specimen and which region of the locking ball that is tested in each method. The strength testing method that is proposed in this thesis is called the notched ball test (NBT). In NBT a long and narrow notch is cut in a locking ball which is then loaded in compression perpendicular to the notch until rupture occurs. The maximum stress acting at the rupture is calculated and used to determine the strength of the locking ball. NBT is suitable because it can be performed with existing equipment at the company, the test specimen is prepared from actual locking balls and the test uses tensile stresses which is an advantage when brittleness is to be detected in a material. An analysis of NBT is performed to determine how material properties and different notch geometries is affecting the test results. The analysis also gives some recommendations for notch geometries that should be used when performing NBT as well as a constant that is used when calculating the maximum stress. Practical experiments of NBT are not carried out in this thesis. Instead, conclusions regarding NBT and recommendations for the company on how they should proceed with NBT are given.

Die Temperaturverhältnisse beim Ziehen und Wärmebehandeln von Draht werden mit mathematisch-analytischen Methoden auf der Grundlage der FOURIERschen Wärmeleitungsgleichung eingehend untersucht. Insbesondere wird unter den spezifischen Wärmeübergangsbedingungen zwischen Draht und Ziehdüse sowie zwischen Draht und Ziehtrommel deren thermische Wechselwirkung analysiert. Ein Näherungsverfahren zur Berechnung der Drahttemperaturen in Zugfolgen unter Berücksichtigung des Ziehdüseneinflusses wird angegeben und mit einem Beispiel zum Nassziehen stark verzinkten Stahldrahts illustriert. Aus geschwindigkeitsabhängig gemessenen Änderungen des Drahtdurchmessers werden unter thermoelastischer Ziehringdurchmesserkorrektur Schmierfilmdicken bestimmt. Diffusionsgleichungen werden analysiert und ein Zusammenhang zur Reaktionskinetik wird hergestellt. Ein neues reaktionskinetisches Werkstoffmodell, das insbesondere auch im Falle stärker anisothermer Verhältnisse, also bei Kurzzeitwärmebehandlung anwendbar ist, wird vorgestellt.

Die vorliegende Arbeit beschäftigt sich mit der Entwicklung von Sol-Gel-Beschichtungen durch Optimierung der Ausgangszusammensetzung und der Applikations-Parameter für den Korrosionsschutz der Aluminium-Legierung AA7075. Verschiedene Arten von Silanen, z. B. Tetraethoxysilan (TEOS), Phenyltriethoxysilan (PTES) und Phenyltrim­ethoxysilan (PTMS) sind verglichen worden: Der Sol-Gel-Film aus PTMS präpariert, weist dabei die höchste Hydrophobizität auf, was sich insbesondere in den Barriere-Eigenschaften dieser Verbindung zeigte. Die Wirkung von Essigsäure als Katalysator in Sol-Gel-Prozessen wurden untersucht, um die optimale Katalysatorkonzentration für den Korrosionsschutz der beschichteten Proben zu ermitteln. Die Korrosionsbeständigkeit der beschichteten Proben sinkt bei höheren Konzentrationen des sauren Katalysators durch die Auflösung des Aluminiumoxids an der Substratoberfläche. Allerdings führten zu niedrige Konzentrationen des Katalysators zur Verlangsamung der Hydrolysereaktionen der Silane und es bildete sich poröse Sol-Gel-Schichten. Die Wärmebehandlung der beschichteten Aluminium-Proben ist für die Vernetzung des Films erforderlich. Eine Wärmebehandlung bei 300 ˚C für 2,5 Stunden ergab dabei den besten Korrosionsschutz. Höhere Temperaturen führten zu einer Verschlechterung der Eigenschaften der Filme, was mit der Zerstörung des organischen Teil des Films erklärt werden kann. Darüber hinaus verursachen zu niedrige Temperaturen einen geringeren Korrosionsschutz der beschichteten Aluminium-Proben. Vermutlich ist die geringe Vernetzung des Sol-Gel-Films bei Temperaturen was für als 300 ˚C verantwortlich. Die beschichteten Aluminium-Proben wuden mittels Raster-Elektronenmikroskopie (SEM), Energiedispersive Röntgenspektroskopie (EDX), Röntgen-Photoelektronenspektroskopie (XPS) und elektrochemischen Techniken charakterisiert. / The present work pertains to the development of sol-gel coatings by optimizing the composition and the application parameters for corrosion protection of aluminum alloy AA7075. Different kinds of silanes e.g. tetraethoxysilane (TEOS), phenyltriethoxysilane (PTES) and phenyltrimethoxysilane (PTMS) have been compared: the sol-gel film prepared from PTMS shows highest hydrophobicity manifested by the best barrier property of this compound. The effect of acetic acid as a catalyst on the chemistry of the sol is investigated in order to estimate the best catalyst concentration for better corrosion protection of the coated samples. The corrosion resistance of the coated samples is found to be decreasing at higher concentrations of the catalyst due to the dissolution of the aluminum oxide at the substrate surface in the acid sol. However, lower concentrations of the catalyst lead to low hydrolysis reactions of the silanes and non-dense sol-gel films have been formed. The heat treatment of the coated aluminum samples is required for cross-linking of the film. The heat treatment at 300 ˚C for 2.5 hours exhibits the best corrosion protection. Higher treatment-temperatures lead to degradation of the properties of the film which can be described in terms of destroying the organic part of the film. Moreover, low treatment-temperatures cause low corrosion protection of the coated aluminum samples which is presumably attributed to the low cross-linking of the sol-gel film at temperatures less than 300 ˚C. The coated aluminum samples are characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS) and electrochemical techniques.

[Truncated abstract] This study investigates the thermal stability of Plasma Enhanced Chemical Vapor Deposited (PECVD) silicon nitride thin films. Effects of heat-treatment in air on the chemical composition, atomic bonding structure, crystallinity, mechanical properties, morphological and physical integrity are investigated. The chemical composition, bonding structures and crystallinity are studied by means of X-ray Photoelectron Spectroscopy (XPS), Fourier Transform Infrared (FTIR) Spectroscopy and Transmission Electron Microscopy (TEM). The mechanical properties, such as hardness and Young’s modulus, are determined by means of nanoindentation. The morphological and physical integrity are analyzed using Scanning Electron Microscopy (SEM) . . . The Young’s modulus (E) and hardness (H) of the film deposited at 448 K were measured to have E=121±1.8 GPa and H=11.7±0.25 GPa. The film deposited at 573 K has E=150±3.6 GPa and H=14.7±0.6 GPa. For the film deposited at 573 K, the Young’s modulus is not affected by heating up to 1148 K. Heating at 1373 K caused significant increase in Young’s modulus to 180∼199 GPa. This is attributed to the crystallization of the film. For the film deposited at 448 K, the Young’s modulus showed a moderate increase, by ∼10%, after heating to above 673 K. This is consistent with the much lower level of crystallization in this film as compared to the film deposited at 573 K. In summary, low temperature deposited PECVD SiNx films are chemically and structurally unstable when heated in air to above 673 K. The main changes include oxidation to SiO2, crystallization of Si3N4 and physical cracking. The film deposited at 573 K is more stable and damage and oxidation resistant than the film deposited at 448 K.