Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / No presente trabalho, foram realizados ensaios de tribocorrosão no aço inoxidável AISI 304L, no titânio comercialmente puro (CPTi) e na liga de titânio Ti6Al4V em solução aquosa de 0,90% m/v NaCl. Amostras de ligas de titânio com tratamento térmico superficial de refusão a laser também foram utilizadas. Um tribômetro do tipo pino-no-disco com contracorpo de alumina foi usado. Técnicas eletroquímicas in situ de monitoramento em circuito aberto, espectroscopia de impedância eletroquímica, curvas de polarização e amperimetria de resistência nula foram empregadas. Os resultados obtidos indicam que o desgaste tribocorrosivo das ligas de titânio é mais intenso do que o observado no aço inoxidável, apresentando perfis de superfície mais irregulares. A análise da impedância eletroquímica mostrou que todos os materiais utilizados apresentam uma rápida recuperação da camada passiva, exibindo módulos e fases um pouco menores do que os medidos antes do desgaste. Sob atrito, os diagramas de impedância apresentam uma forte redução do módulo. Sob desgaste, o expoente α do elemento de fase constante (CPE) atinge seu valor mais baixo, enquanto o parâmetro γ é máximo. As curvas de polarização exibem potenciais menores e densidades de corrente de corrosão maiores durante o desgaste. O tratamento de refusão a laser, embora mude a microestrutura e a dureza superficial das amostras, não indica uma mudança aparente nos parâmetros eletroquímicos sob tribocorrosão, bem como do coeficiente de atrito. Nos ensaios de amperimetria de resistência nula, foi possível estimar a corrente mensurada no ARN por meio do emprego de um circuito elétrico equivalente. A densidade espectral de potência dos sinais de potencial e de corrente exibe a frequência de rotação (1,25 Hz) e seus harmônicos. Para baixas frequências (abaixo de 10 mHz), o decaimento obedece à relação 1 ⁄ e 1⁄ para os sinais de potencial e corrente, respectivamente. / In this study, tribocorrosion tests were performed in stainless steel AISI 304L, commercially pure titanium (CPTI) and Ti6Al4V titanium alloy in 0.9% m/v NaCl aqueous solution of. Titanium alloy sample with laser remelting treatments were also tested. A pin-on-disc tribometer with alumina counterbody was used. In situ electrochemical techniques of open circuit monitoring, electrochemical impedance spectroscopy, polarization curves and zero resistance ammeter were employed. Results indicate tribocorrosion wear of titanium alloys is more intense than that observed in stainless steel, presenting more irregular surface profiles. Analysis of electrochemical impedance spectroscopy showed all materials used have a fast recovery of the passive layer, showing modulus and phase slightly smaller than those measured prior to wear. Under friction, impedance diagrams show a strong reduction of the modulus. Under rubbing, exponent α of the constant phase element (CPE) reaches its lowest value, while γ parameter is maximum. Polarization curves show lower corrosion potential and higher corrosion current density during rubbing. Laser remelting treatments, although changes microstructure and surface hardness of the samples, does not indicate an apparent change in electrochemical parameters under tribocorrosion, as well as in coefficient of friction. In zero resistance ammeter tests, it was possible to estimate the current measured in ZRA using an electrical equivalent circuit. Power spectral density of the potential and current signals exhibits the rotation frequency (1.25 Hz) and its harmonics. For lower frequencies (below 10 mHz), the decay follows 1⁄ and 1⁄ roll-off for signals of potential and current, respectively.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / No presente trabalho, foram realizados ensaios de tribocorrosão no aço inoxidável AISI 304L, no titânio comercialmente puro (CPTi) e na liga de titânio Ti6Al4V em solução aquosa de 0,90% m/v NaCl. Amostras de ligas de titânio com tratamento térmico superficial de refusão a laser também foram utilizadas. Um tribômetro do tipo pino-no-disco com contracorpo de alumina foi usado. Técnicas eletroquímicas in situ de monitoramento em circuito aberto, espectroscopia de impedância eletroquímica, curvas de polarização e amperimetria de resistência nula foram empregadas. Os resultados obtidos indicam que o desgaste tribocorrosivo das ligas de titânio é mais intenso do que o observado no aço inoxidável, apresentando perfis de superfície mais irregulares. A análise da impedância eletroquímica mostrou que todos os materiais utilizados apresentam uma rápida recuperação da camada passiva, exibindo módulos e fases um pouco menores do que os medidos antes do desgaste. Sob atrito, os diagramas de impedância apresentam uma forte redução do módulo. Sob desgaste, o expoente α do elemento de fase constante (CPE) atinge seu valor mais baixo, enquanto o parâmetro γ é máximo. As curvas de polarização exibem potenciais menores e densidades de corrente de corrosão maiores durante o desgaste. O tratamento de refusão a laser, embora mude a microestrutura e a dureza superficial das amostras, não indica uma mudança aparente nos parâmetros eletroquímicos sob tribocorrosão, bem como do coeficiente de atrito. Nos ensaios de amperimetria de resistência nula, foi possível estimar a corrente mensurada no ARN por meio do emprego de um circuito elétrico equivalente. A densidade espectral de potência dos sinais de potencial e de corrente exibe a frequência de rotação (1,25 Hz) e seus harmônicos. Para baixas frequências (abaixo de 10 mHz), o decaimento obedece à relação 1 ⁄ e 1⁄ para os sinais de potencial e corrente, respectivamente. / In this study, tribocorrosion tests were performed in stainless steel AISI 304L, commercially pure titanium (CPTI) and Ti6Al4V titanium alloy in 0.9% m/v NaCl aqueous solution of. Titanium alloy sample with laser remelting treatments were also tested. A pin-on-disc tribometer with alumina counterbody was used. In situ electrochemical techniques of open circuit monitoring, electrochemical impedance spectroscopy, polarization curves and zero resistance ammeter were employed. Results indicate tribocorrosion wear of titanium alloys is more intense than that observed in stainless steel, presenting more irregular surface profiles. Analysis of electrochemical impedance spectroscopy showed all materials used have a fast recovery of the passive layer, showing modulus and phase slightly smaller than those measured prior to wear. Under friction, impedance diagrams show a strong reduction of the modulus. Under rubbing, exponent α of the constant phase element (CPE) reaches its lowest value, while γ parameter is maximum. Polarization curves show lower corrosion potential and higher corrosion current density during rubbing. Laser remelting treatments, although changes microstructure and surface hardness of the samples, does not indicate an apparent change in electrochemical parameters under tribocorrosion, as well as in coefficient of friction. In zero resistance ammeter tests, it was possible to estimate the current measured in ZRA using an electrical equivalent circuit. Power spectral density of the potential and current signals exhibits the rotation frequency (1.25 Hz) and its harmonics. For lower frequencies (below 10 mHz), the decay follows 1⁄ and 1⁄ roll-off for signals of potential and current, respectively.

L’apparition d’inclusions exogènes demeure un problème majeur pour les élaborateurs de titane. Afin d’améliorer la propreté inclusionnaire des lingots élaborés par le procédé de refusion à l’arc sous vide (Vacuum Arc Remelting), une étude numérique et expérimentale a été réalisée. La partie numérique de la thèse consiste à modéliser le comportement d’un défaut hard-α provenant de l’électrode consommable et tombant dans le puits liquide du lingot. Un modèle décrivant le processus de dissolution prédit l’évolution de la taille d’une inclusion durant son séjour dans le puits liquide. La trajectoire est déterminée à l’aide d’un modèle lagrangien tenant compte de la turbulence de l’écoulement en modifiant le coefficient de trainée. Les deux modèles ont été couplés et implémentés dans le logiciel SOLAR, qui simule la croissance d’un lingot VAR.Les résultats mettent en évidence la difficulté d’éliminer une inclusion hard-α avec une seule refusion, principalement à cause de la croissance d’une couche de phase β pendant les premiers moments de l’immersion. Le comportement global du défaut dépend fortement de l’hydrodynamique du puits et des caractéristiques de l’inclusion.Pour étudier la dissolution expérimentalement, des défautssynthétiques (hard-α et HDI) ont été immergés dans un bain de titane liquide chauffé dans un four à bombardement électronique. Les vitesses de dissolution ont été déterminées en mesurant les dimensions des défauts avant et après les expériences et ont été ensuite utilisées pour valider les modèles numériques. Par ailleurs, nous avons mis en évidence la grande influence de la température et de la vitesse de l’écoulement sur les cinétiques de dissolution / The presence of exogeneous inclusions has always been a major concern for the titanium industry. To help improve the inclusional cleanliness of VAR (Vacuum Arc Remelting) titanium ingots, a numerical and experimental study was undertaken.The numerical model is capable of predicting the motion and dissolution of a hard-α defect falling from the electrode tip into the ingot melt pool during vacuum arc remelting. It is implemented in SOLAR, a CFD code that simulates the ingot growth and solidification. The dissolution of the inclusion is governed by nitrogen diffusion from the defect towards the surrounding molten metal. A model describing this phenomenon predicts the particle size evolution and the nitrogen profile at each moment. The motion of the spherical particle is tracked using a Lagrangian model and the influence of turbulence is accounted for by a modification of the drag coefficient.Results show that inclusion removal is difficult with a single melt since the growth of a β-phase layer leads to an initial increase in the defect size. The inclusion behaviour is highly dependent on the pool hydrodynamics and on inclusion characteristics.In order to clarify dissolution aspects of these defects and to measure their dissolution kinetics, synthetically processed defects were introduced into molten titanium heated in an electron beam melting furnace. Dissolution rates were calculated by measuring the size of the defects before and after the experiments and the results were used to validate the numerical models. Furthermore, the experiments show that dissolution kinetics highly depend on fluid motion and temperature

Thermal barrier coatings (TBCs) are commonly used for thermal protection of components in modern gas turbine application and typically consisting of ceramic top coat and CoNiCrAlY bond coat (BC), both thermally sprayed. Nanostructured CoNiCrAlY bond coatings were deposited onto Ni-based alloy (Inconel 718) by both HVOF and CGDS spraying techniques. Subsequently the deposits were remelted by electron beam up to depth of about 100 m which resulted in removal of defects on the substrate to the bond coat interface. The primary objective of this thesis was to investigation of the influence of parameters used for EB remelting, including multiple remelting on the microstructural changes, phase modification and final state of the coatings. The amount of porosity in the coatings and surface roughness has been evaluated. Scanning electron microscopy and X-Ray diffraction were performed in order to characterize the phase modification before and after the applied treatment. The results indicated that multiple remelting process improved the coating properties in terms of porosity, smooth surface, strength and chemical homogeneity and at last but not least this study demonstrate that low-temperature processing of CoNiCrAlY bond coat represents an interesting and promising alternative for their manufacturing.

The master thesis is dealing with characterization of the structure and properties of the YSZ thermal barrier coating deposited by water hybrid plasma spray technology on the CoNiCrAlY bond coats modified by using electron beam and vacuum annealing. Deposition of the bond coats was performed via high velocity oxy-fuel technology and cold spray. In case of experimental evaluation, the microstructure and chemical composition of the ceramic top coat deposited with powder and suspension feedstock was analyzed. The same analysis procedure was used also for bond coats after electron beam remelting by using two sets of parameters. Furthermore, the changes in microstructure and chemical composition of the remelted and annealed bond coats was evaluated. Eventually, the micromechanical properties of the top coats and the bond coats were measured. The ceramic top coats deposited with powder feedstock exhibited the structure composed by splats, while the top coats deposited in form of suspension showed fine structure with columnar grains. The dendritic structure was observed on remelted bond coats. The annealing process had an influence on the structure in form of coarsened phases and the chemical composition was changed due to diffusion of the elements.

Hypoeutectic Fe-C and Fe-C-Si model alloys were produced at different solidification conditions. Copper mold casting yields low cooling rates promoting the formation of a eutectic microstructure characterized by two morphologies: elongated cementite plates and a rod structure growing perpendicular to the plates, i.e. austenite rods in a cementite matrix. Electron beam surface remelting generates a mainly plate-like eutectic due to rapid solidification. The microstructures were characterized by light-optical microscopy and electron backscatter diffraction (EBSD). The latter allows for a spatially resolved investigation of the growth crystallography of the eutectic phases. Thereby, a possible existence of crystallographic orientations relationships between cementite and austenite within the plate-like eutectic was assessed experimentally. The eutectic phases were found to grow largely crystallographically independently. Moreover, ferrite and eutectic cementite within the decomposed eutectic microstructure comply frequently with the Bagaryatsky or the Pitsch-Petch orientation relationship. Complementary X-ray diffraction (XRD) analysis reveals a pronounced cementite {002} texture in the microstructure produced by mold casting. Characteristic changes in the lattice parameters indicate that as-cast cementite is non-stoichiometric.

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