Tratamentos de superfície são técnicas amplamente utilizadas com a finalidade de aumentar a resistência à corrosão de materiais metálicos. No caso específico do alumínio e ligas de alumínio, o tratamento com cromo hexavalente é um dos processos mais utilizados. Isso, em razão da eficiência e da facilidade de aplicação desse processo. Entretanto, em virtude de restrições ambientais e do elevado custo de tratamento de resíduos gerados neste processo, métodos alternativos para sua substituição vêm sendo avaliados. Neste contexto, o presente estudo investigou o processo de formação e proteção à corrosão fornecida por filmes de moléculas autoorganizáveis de compostos à base de fosfonatos sobre a liga de alumínio 1050. Para definir as condições do tratamento foram utilizadas medidas de condutividade e de ângulo de contato, juntamente com ensaios eletroquímicos. Técnicas eletroquímicas, especificamente: medidas de variação do potencial a circuito aberto (PCA), espectroscopia de impedância eletroquímica (EIE) e polarização potenciodinâmica foram utilizadas para avaliar a proteção à corrosão. Os diagramas experimentais de impedância foram interpretados utilizando circuitos elétricos equivalentes que simulam modelos do filme de óxido que se forma na superfície da liga. Os resultados fornecidos com a liga tratada com moléculas auto-organizáveis foram comparados com resultados obtidos em iguais condições com amostras da liga sem qualquer tratamento ou cromatizada com Cr(VI) e mostraram que o tratamento com moléculas auto-organizáveis aumenta significativamente a resistência à corrosão da liga e apresenta, em determinadas condições, desempenho próximo ao fornecido pelo processo de cromatização. / Surface treatments are widely used to increase the corrosion resistance of metallic materials. Specifically for aluminum and aluminum alloys, treatment with hexavalent chromium is one of the most used, due to its efficiency and ease of application. However, because of environmental restrictions and the high cost involved in the treatments of waste generated in this process, alternative methods for its replacement are necessary. In this context, this study investigated the effect of the surface treatment with self-assembling molecules (SAM) based on phosphonate compounds on the corrosion of the 1050 aluminum alloy. The conditions adopted for the SAM treatment were determined by conductivity and contact angle measurements, besides electrochemical experiments. Electrochemical techniques, specifically: measurement of the open circuit potential (OCP) variation with time, electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curves were used to evaluate the corrosion resistance of the 1050 aluminum alloy exposed to SAM treatment The experimental impedance diagrams were interpreted using equivalent electrical circuit models that simulate film that is formed on the alloy surface. The results of the samples treated with SAM were compared with those of samples either without any treatment or treated with chromatizing conversion coating with Cr(VI) and showed that the first treatment significantly increased the corrosion resistance of the aluminum alloy and approached that of chromatizing with Cr(VI) process.

A indústria aeronáutica está constantemente à procura de materiais que ofereçam benefícios em termos de redução de peso, desempenho e custo. Corrosão e fadiga em ligas de alumínio são questões importantes na avaliação da vida útil em estruturas de aeronaves e na gestão de frotas. O objetivo deste trabalho foi avaliar os processos de corrosão e corrosão-fadiga nas ligas 2198-T851 e 7081-T73511, que são promissoras substitutas das ligas 2524-T3 e 7050-T7451 normalmente utilizada pela indústria aeronáutica. As técnicas de potencial de circuito aberto (PCA), polarização potenciodinâmica, polarização potenciodinâmica em eletrodo cilíndrico rotatório, espectroscopia de impedância eletroquímica (EIE), eletrodo vibratório de alta resolução (SVET) e mapeamento de potencial (SKP) foram utilizadas para esclarecer e quantificar os mecanismos de corrosão destas ligas de alumínio. Os ensaios de fadiga e corrosão-fadiga foram realizados com uma razão de carga (R) de 0,1 e frequência de 15 Hz em ar e 0,1 Hz em meio de névoa salina. As amostras, antes e após os testes de corrosão e corrosão-fadiga foram analisadas usando microscopia eletrônica de varredura (MEV). As características localizadas das quatro ligas estão essencialmente relacionadas com a existência de compostos intermetálicos que, devido à sua natureza diferente, podem ser catódicos ou anódicos em relação à matriz de alumínio. Os resultados de corrosão-fadiga mostraram uma ligeira redução no limite de fadiga para as ligas da série 2XXX e 7XXX. Essa redução pode ser atribuída à formação de cavidades de corrosão (pites). Considerando o estágio de propagação de trinca, o ambiente salino aumentou a taxa de crescimento de trinca para um mesmo intervalo de fator de intensidade de tensão. / The aircraft industry is constantly looking for improved materials which offer benefits in terms of performance, weight and cost savings. Corrosion and fatigue of aluminium alloys are major issues in the service life assessment of aircraft structures and in the management of aging air fleets. The aim of this study was to evaluate the corrosion and corrosion fatigue processes of 2198-T851 and 7081-T73511 aluminium alloys, which are promising substitutes for the base line 2524-T3 and 7050-T7451 aluminium alloys normally used in aircraft fabrication. Open circuit potential monitoring (OCP), potentiodynamic polarization, potentiodynamic polarization in rotating cylindrical electrode, eletrochemical impedance spectroscopy (EIS), Scanning vibrating electrode technique (SVET) and Scanning Kelvin Probe (SKP) techniques have been used to clarify and quantify the corrosion mechanisms of these Al alloys. Fatigue and corrosion fatigue tests were carried out an applied stress ratio (R) of 0.1, 15 Hz frequency for air and 0.1 Hz frequency for salt spray using a sinusoidal wave form in all cases. The specimens, before and after corrosion and corrosion-fatigue testing were analyzed using scanning electron microscope (SEM). The localised features of all the four alloys are essentially related to the existence of intermetallics that, due to their different nature, may be cathodic or anodic sites in relation to the Al matrix. SEM and EDS analysis allowed to identify the intermetallics that are more active in determining the corrosion behavior of the specimens. The fatigue corrosion results show a slightly reduction in the fatigue life limit by chloride environment for the 2XXX and 7XXX aluminium alloys in each aged condition might be partially attributed to the formation of corrosion pits. Considering the crack propagation stage, the saline environment increased the fatigue crack growth rate for the same range of stress intensity factor.

A liga de alumínio 6063 possui um grande interesse industrial, apresentando características que justificam o seu uso mais freqüente quando comparadas às demais ligas de alumínio: a capacidade de endurecimento por precipitação (pois são termicamente tratáveis) aliada à facilidade de serem extrudadas. Estas ligas apresentam elevada ductilidade, que permite o seu uso em operações que acarretam elevados graus de deformação, como a extrusão. Por esse motivo, as ligas Al-Mg-Si apresentam a maior parte do volume de ligas extrudadas. Tendo em vista a freqüente utilização da liga de alumínio 6063, este trabalho estuda a caracterização e a recristalização da liga após a deformação plástica em diferentes graus de redução em área 20%, 50%, 70% e 90%, com tratamentos térmicos de 396ºC, 462ºC e 528ºC e com tempos de recozimento em 1minuto, 10 minutos e 100 minutos Tratamentos Termomecânicos. Observou-se como resultados de uma forma geral, que os tratamentos com 1minuto nas amostras de Al6063 houve pouca ou nenhuma alteração e ao aumentarmos o tempo de recozimento para 10 minutos e depois para 100 minutos os processos de recuperação/recristalização se tornam evidentes e o crescimento de também é observável para os tempos de tratamento em 100 minutos. / The aluminum 6063 alloy possesses a great industrial interest, presenting characteristics that justify its frequent use, when compared to the other aluminum alloys: the precipitation hardening and high cold work capacity. These alloys present high ductility, that allows their use in operations with high deformation degrees, as the cold work. The objective of this work is to show comparative analysis of the hardness Vickers of the commercial aluminum 6063 alloy, after cold work with different area reduction degree and thermal treatment. Considering the frequent utilization aluminium 6063 alloy, this work studies the caracterization and recristalization of this alloy, after the plastc deformation in different area reduction degrees, thermal treatment and convenient tratment times Termomechanic Tratments.

A liga de alumínio 6063 possui um grande interesse industrial, apresentando características que justificam o seu uso mais freqüente quando comparadas às demais ligas de alumínio: a capacidade de endurecimento por precipitação (pois são termicamente tratáveis) aliada à facilidade de serem extrudadas. Estas ligas apresentam elevada ductilidade, que permite o seu uso em operações que acarretam elevados graus de deformação, como a extrusão. Por esse motivo, as ligas Al-Mg-Si apresentam a maior parte do volume de ligas extrudadas. Tendo em vista a freqüente utilização da liga de alumínio 6063, este trabalho estuda a caracterização e a recristalização da liga após a deformação plástica em diferentes graus de redução em área 20%, 50%, 70% e 90%, com tratamentos térmicos de 396ºC, 462ºC e 528ºC e com tempos de recozimento em 1minuto, 10 minutos e 100 minutos Tratamentos Termomecânicos. Observou-se como resultados de uma forma geral, que os tratamentos com 1minuto nas amostras de Al6063 houve pouca ou nenhuma alteração e ao aumentarmos o tempo de recozimento para 10 minutos e depois para 100 minutos os processos de recuperação/recristalização se tornam evidentes e o crescimento de também é observável para os tempos de tratamento em 100 minutos. / The aluminum 6063 alloy possesses a great industrial interest, presenting characteristics that justify its frequent use, when compared to the other aluminum alloys: the precipitation hardening and high cold work capacity. These alloys present high ductility, that allows their use in operations with high deformation degrees, as the cold work. The objective of this work is to show comparative analysis of the hardness Vickers of the commercial aluminum 6063 alloy, after cold work with different area reduction degree and thermal treatment. Considering the frequent utilization aluminium 6063 alloy, this work studies the caracterization and recristalization of this alloy, after the plastc deformation in different area reduction degrees, thermal treatment and convenient tratment times Termomechanic Tratments.

One of the serious problems encountered in the use of various materials in technology is the occurrence of fatigue phenomena as an undesirable material damage under cyclic mechanical load. For aluminium alloys this issue is of extremely high importance in case of their utilisation for aircraft purposes, e.g., where a very wide spectrum of frequencies occur. Moreover, the cyclic loading may be joined by the presence of specific electrolyte media. Therefore, the material candidates must be thoroughly examined in view of their sensitivity to fatigue as well as to corrosion fatigue. Usually, the Cu-containing alloy EN-AW 2024 T3 is applied besides 7075 T6 in Airbus aircrafts, but the weldable alloy 6013 T6 is considered to be a potential alternative. Referring to former investigations on the environmental sensitivity (ES) in the fatigue behaviour /1-6/ this paper brings up experimental findings as well as expanded considerations about damaging mechanisms and modelling. The situation with the alloy 6013 T6 is emphasized. The propagation of cracks under cyclic load in different environments, such as vacuum, air or aqueous media, is described by means of fracture mechanics. This enables discrimination in view of the influence of environmental factors and, hence, the participation of corrosion processes.

There is a great need in the transportation industry for high strength, high stiffness and lightweight materials with excellent dimensional stability. The use of these materials reduces fuel consumption and greenhouse gas emission as well as malfunctioning of components when subjected to fluctuating temperatures. Metal matrix composites (MMCs) are designed to meet these needs of transportation and other industries. However, their use is limited by lack of information on their thermal behaviour. In addition, reactions that occur in MMCs alter their microstructure and properties. These reactions have been widely investigated using X-ray Diffractometry (XRD) and electron microscopy (EM). However, these techniques cannot provide information such as charge transfer and local elemental structures in materials. Synchrotron X-ray Absorption Spectroscopy (XAS) could be used to identify reaction products in MMCs as well as provide information which XRD and EM cannot provide.<p> The thermal behaviour of Al-Mg alloy A535 containing fly ash particles as well as charge transfer and reactivity in particulate aluminium alloy metal matrix composites (MMCs) were investigated in this work. The materials studied were (i) Al-Cu-Mg alloy AA2618 and its composites reinforced with 10 and 15 vol.% alumina (Al2O3) particles and (ii) Al-Mg alloy A535 and its composites reinforced with a mixture of 5 wt.% fly ash and 5 wt.% silicon carbide, 10 wt.% and 15 wt.% fly ash. The investigative techniques used included Differential Scanning Calorimetry (DSC), Thermomechanical Analysis (TMA), Optical Microscopy (OM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), and synchrotron X-ray Absorption Spectroscopy (XAS).<p> The results obtained showed that the coefficient of thermal expansion (CTE) of A535 decreased with the addition of fly ash and silicon carbide. Also, the addition of these particles improved the dimensional stability of the alloy in that the residual strain, åp, cycling strain, åc, and CTE decreased. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The addition of alumina particles into AA2618 increased the p-orbital population and also changed the surface chemistry of the matrix. It was also demonstrated that the XAS technique can be used to determine the presence of various oxides in industrial fly ash and spinel (MgAl2O4) in alumina and fly ash particles extracted from the MMCs.

There is a great need in the transportation industry for high strength, high stiffness and lightweight materials with excellent dimensional stability. The use of these materials reduces fuel consumption and greenhouse gas emission as well as malfunctioning of components when subjected to fluctuating temperatures. Metal matrix composites (MMCs) are designed to meet these needs of transportation and other industries. However, their use is limited by lack of information on their thermal behaviour. In addition, reactions that occur in MMCs alter their microstructure and properties. These reactions have been widely investigated using X-ray Diffractometry (XRD) and electron microscopy (EM). However, these techniques cannot provide information such as charge transfer and local elemental structures in materials. Synchrotron X-ray Absorption Spectroscopy (XAS) could be used to identify reaction products in MMCs as well as provide information which XRD and EM cannot provide.<p> The thermal behaviour of Al-Mg alloy A535 containing fly ash particles as well as charge transfer and reactivity in particulate aluminium alloy metal matrix composites (MMCs) were investigated in this work. The materials studied were (i) Al-Cu-Mg alloy AA2618 and its composites reinforced with 10 and 15 vol.% alumina (Al2O3) particles and (ii) Al-Mg alloy A535 and its composites reinforced with a mixture of 5 wt.% fly ash and 5 wt.% silicon carbide, 10 wt.% and 15 wt.% fly ash. The investigative techniques used included Differential Scanning Calorimetry (DSC), Thermomechanical Analysis (TMA), Optical Microscopy (OM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), and synchrotron X-ray Absorption Spectroscopy (XAS).<p> The results obtained showed that the coefficient of thermal expansion (CTE) of A535 decreased with the addition of fly ash and silicon carbide. Also, the addition of these particles improved the dimensional stability of the alloy in that the residual strain, åp, cycling strain, åc, and CTE decreased. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The results obtained from XAS measurements showed evidence of charge redistribution in the aluminium in AA2618 with the addition of alumina particles. The addition of alumina particles into AA2618 increased the p-orbital population and also changed the surface chemistry of the matrix. It was also demonstrated that the XAS technique can be used to determine the presence of various oxides in industrial fly ash and spinel (MgAl2O4) in alumina and fly ash particles extracted from the MMCs.

Al-Mg alloys were infiltrated into porous alumina preforms at temperatures greater than 950°C where significant amount of nitride forms in the matrix. The present work aims to obtain a process window for growing A1N rich composites over uniform thicknesses so that bulk fabrication of these composites could be carried out. Initial experiments were carried out in a thermo-gravimetric analyser (TGA) to establish suitable conditions for growing useful thicknesses. Al- 2wt% Mg alloy, alumina preforms of particle size 53-63μm and N2 - 2% H2 (5ppm O2) were used for the present study based on previous work carried out in the fabrication of MMCs at low temperatures. Experiments carried out in the TGA indicate that oxygen in the system has to be gettered for the growth of nitride rich composites. Infiltration heights of about 8mm were obtained using an external getter (Al - 5wt%Mg) alloy in addition to the base alloy used for infiltration. The above process conditions were subsequently employed in a tube furnace to fabricate bulk composites and to study the effect of temperature on the volume fraction of aluminium nitride in the matrix. The volume fraction of nitride in the composite varied between 30 and 95 vol % with increase in process temperature from 950°C to 1075°C. Microstructures of these composites indicate that A1N starts to form on the particle surface and tends to grow outwards. The metal supplied through channels adjacent to the particle surface nitride until a point is reached when the composite growing from the adjacent particles meet each other and isolate the melt underneath from nitrogen thereby leading to a metal rich region underneath. Increase in temperature results in an increased nitridation rate resulting in reduced metal pocket size. Composites fabricated at 975°C had a minor leak at the O-rings, which seal the tube. This led to infiltration under conditions of varying oxygen partial pressure leading to different nitride fractions in the composite. The above fact was confirmed by conducting an experiment with commercial purity nitrogen, which has an oxygen content of about 5000ppm. The composite had an A1N content of about 30% whereas the composite fabricated with N2 -2%H2 (5ppm oxygen) showed a nitride content of 64%. This suggests that one can vary the nitride content in the composite by varying the oxygen content in the system at a particular process temperature. The hardness of the matrix increases with increase in process temperature from 3.5 ± 0.7 GPa at 975°C to about 9.8 ± 0.9 GPa at 1075°C. Porosity was observed in the composite processed at 1075°C. This increased porosity leads to decreased hardness though the nitride content in the composite has increased by 11%. The scatter in the data is attributed to variations in the microstructure as well as due to interference from underlying metal pockets or particles as well as due to porosity introduced in the composite at high processing temperatures.

Friction Stir Welding (FSW) is an emerging solid state welding process. It has been a proven method for welding high strength aluminium alloys which were previously not recommended for conventional fusion welding. Since the invention of the process by The Welding Institute, United Kingdom, in 1991, a number of studies have been conducted on the material flow, microstructural evolution and mechanical properties of friction stir welds. However, there is not enough conceptual background available on FSW process for physical understanding of the mechanism of weld formation. In addition to that, FSW welds of high strength precipitation hardenable aluminium alloys suffer from reduced joint efficiency due to overaging in the heat affected zone. In the present investigation, experimental analysis has been carried out to understand the mechanism of weld formation and parameter optimization for aluminium alloys 7020-T6 and 6061-T6. For this purpose the investigations have been made on both the process aspects and the material aspects. The process aspects are analyzed with the objective of learning the mechanism to produce defect free welds. For this purpose experiments have been carried out to analyze the effect of FSW parameters, material flow and the frictional characteristics between the tool and base metal. Preliminary experiments are conducted on aluminium alloy 7020-T6 with different tool geometries to analyze the interaction of the tool with the base metal using a knee-type vertical milling machine. Then, the tool geometry which produced defect-free weld is used for further experimentation. The role of tool pin, shoulder and axial load on the formation of defect free weld is analyzed in an innovative experiment, where the tool and base metal interaction is continuously increased by continuously increasing the interference between the tool and base metal. In another experiment the initial abutting interface position with respect to the tool is continuously varied to study the interaction of the tool with the initial interface and to find the positional information where the initial interface is completely eliminated. Further, the tool metal interface condition is studied using a specially designed tribological experiment which simulates the FSW condition. From the base metal point of view, due to the strain, strain rate and temperature imposed on the base metal during the process, the microstructure is altered. In precipitation hardenable aluminium alloys the strengthening precipitates are dissolved or overaged in the weld region depending on the peak temperature in the region, which reduces the joint efficiency. However, the dissolution and overaging are kinetic process. In order to analyze this time dependant softening behavior of the base metal 7020-T6 and 6061-T6, isothermal annealing and differential scanning calorimetric studies are performed. In order to obtain FSW welds with maximum joint efficiency, the welding temperature should not exceed the “softening temperature” of the base metal. But, to produce defect free welds favorable material flow in the weld nugget is necessary. The material flow and consolidation depend on the process temperature. Hence, for a given tool to produce defect free weld there is a need for minimum temperature. If the weld formation temperature is less than the base metal softening temperature, the weld can be made with 100% joint efficiency. In order to optimize the FSW parameter which gives defect free weld with lowest possible temperature, an instrumented programmable FSW machine is designed and developed. The machine is designed in such a way that welding parameters – rotation speed, traverse speed and plunging depth – can be continuously varied from the start to end of the weld between given two values. This reduces the number of experimental trials, material and time. Based on the experimental results the following conclusions are derived. 1.The minimum diameter of the pin required for FSW depends on the base metal and tool material property for a given set of parameters. If the pin diameter is insufficient for a given set of welding parameters, it fails during plunging operation itself. 2.There is a minimum diameter of the shoulder for a given diameter of the pin which produces defect free weld. The ratio of pin to shoulder to produce a defect free weld is not a constant value. It changes with tool geometry and process parameters. 3.Increasing the area of contact between the tool and shoulder for a given set of parameters increases the heat input and results in increased weld nugget grain size. 4.Initial abutting interface of the base metal is eliminated at the leading edge of the tool. However, new surfaces are generated due to interaction with the tool and the newer surfaces are consolidated at the trailing edge of the tool. Importantly, the weld strength is controlled by the defects generated due the improper elimination of newly generated surfaces. 5.Optimal axial load is required to generate the required pressure to consolidate the transferred material at the trailing edge of the tool and should be equal to the flow stress of the material at the processing temperature. The optimal axial load is 8.1kN for a tool having 20mm diameter shoulder with 6mm diameter frustum shaped pin. 6.Only the material that approaches the tool at the leading edge on the advancing side is stirred and the remaining material is simply extruded around the tool. Further, the initial abutting interface is completely removed only when it is located in the stirring zone, otherwise the initial abutting interface is not eliminated. In the present study the interface is completely stirred when it is located on the advancing side of the tool between 0.5mm away from the centerline and edge of the tool. 7.The temperature and pressure at the tool–base metal interface is above the temperature and pressure required for seizure to occur for given tool material (H13) and base metal (7020-T6). Hence, it is clear that during FSW the base metal transfers on to the tool and interaction occurs between transferred layer on tool and base metal. The coefficient of friction between the given tool material and base metal in FSW condition is in the range of 1.2 – 1.4. 8.The minimum temperature requirement for FSW of 7020-T6 is 400oC and 6061-T6 is 430oC. However, 7020-T6 and 6061-T6 softens at lower temperatures than that of the minimum FSW temperature. 7020-T6 softens 30% in 7min at 250oC, 4min at 300oC, 2min at 350oC and 1min at 400oC. After softening 30%, there is 10% recovery in hardness and the hardness remains constant thereafter. Whereas 6061-T6 softens gradually up to 47% in 7min at 350oC and 400oC, below the temperature of 250oC for 7020-T6 and 350oC for 6061-T6 there is no softening observed in 7min. 9.The maximum joint efficiency of the 7020-T6 weld is 82% and 6061-T6 weld is 60%. 10. The reduction in joint efficiency is attributed to overaging of the material in the heat affected zone.

Made available in DSpace on 2014-10-09T12:27:16Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:57:06Z (GMT). No. of bitstreams: 0 / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP