Este trabalho discutiu a relação entre o espaçamento inter-estrias , isto é, a taxa de propagação da trinca microscópica SL (local) e SP (projetada) e a taxa de propagação macroscópica , da/dN, obtido após o ensaio de propagação de trinca por fadiga. Corpos de prova compacto C(T) foram extraídos na orientação LT do centro de uma placa laminada de liga de alumínio SAE-AMS 7475 T7351 onde posteriormente foram realizados ensaios de fadiga sob carga ou &#916K constantes, à temperatura ambiente de acordo com a Norma ASTM-E647 (1993). Para o ensaio sob carga constante foram obtidos os dados do estágio II e III da curva da/dN vs. &#916K. Para o ensaio de fadiga sob &#916K constante, quatro níveis de &#916K foram utilizados com taxas de crescimento de trinca variando entre 0,15 à 2,4 &#956m/ciclo. Adicionalmente foram realizados ensaios de tenacidade à fratura, KIC nas direções LT e TL conforme a Norma ASTM-E1820 (1999). A análise fratográfica por microscopia eletrônica de varredura foi conduzida no ensaio de fadiga a &#916K constante para determinar os espaçamentos inter-estrias. As taxas de propagação macroscópica e microscópica foram comparadas e boas correlações foram obtidas para um intervalo entre 0,1 a 1,0 &#956m/ciclo. Através da técnica proposta por Berkovitz (1995), o espectro de carregamento foi estimado através da técnica de parametrização do fator K e os resultados foram comparados ao espectro de carregamento real imposto pela máquina de ensaio. Utilizando o espaçamento inter-estrias local, SL, e para valores de &#916K menores que 23 MPam 1/2 (região de Paris), a estimativa de carregamento exibiu um erro menor que 15%. As vidas estimadas em propagação fornecidas pelas taxas microscópicas de propagação de trinca foram comparadas à vida real de propagação obtida a partir da taxa de propagação de trinca macroscópica e o erro absoluto entre ambos os valores foi menor que 15,7 %. Estes resultados sugerem que a vida em fadiga e o espectro de carga podem ser adequadamente estimados utilizando o espaçamento inter-estrias local, SL. / This work discusses the relationship between striation spacing, i.e. the microscopic crack propagation rate, SL (local) e SP (projected), as measured in post-mortem fractographic inspection of fatigue fractured surfaces, and the macroscopic crack propagation rate, da/dN, as monitored during fatigue crack growth tests. Compact tensile specimens C(T) were extracted in LT orientation from the core of a laminated plate of a SAE-AMS 7475-T7351 Al alloy and subsequently fatigue tested either at constant load or at constant &#916K, at room temperature, according to ASTM-E647. For constant amplitude loading fatigue tests, da/dN- &#916K data points were obtained for Regions II and III of crack growth curve. For constant &#916K fatigue tests, four &#916K levels were selected to give crack growth rates typically ranging from 0.15 to 2.4 &#956m/cycle. Additionally, KIC fracture toughness tests were performed in both LT and TL directions, according to ASTM E1820. SEM fractographic analysis was conducted on constant &#916K fatigue specimens, in order to determine striation spacing created during the fatigue test. Macro- and microscopic crack growth rates were compared and good correlation have been obtained for data within the range from 0,1 to 1,0 &#956m/ciclo. Using the technique proposed by Berkovitz, loading history was estimated by the K-factor parametrization and the results were compared to the true loading spectrum imposed by the testing machine. Using the local striation spacing SL and for &#916K values lower than 23 MPam 1/2 (Paris region), the estimated loading exhibits an error less than 15%. Propagation life estimated by local striation spacing (microscopic crack growth rate) was compared to the true propagation life obtained from macroscopic crack growth rate values and the absolute difference between them was less than 15,7%. These results suggest that both life and loading history can be adequately estimated using the local SL striation spacing values.

Made available in DSpace on 2017-07-21T20:43:45Z (GMT). No. of bitstreams: 1 Natany Dayani de Souza Assai.pdf: 1950917 bytes, checksum: a6c8b87bcaabbbdbf5ca798360a90bcc (MD5) Previous issue date: 2014-08-27 / The residual stress may decrease and redistribute through a process called relaxation. The relaxation of the residual stress is an important phenomenon in relation to the estimated fatigue resistance of the material and can occur due to static mechanical loading, thermal, cyclical and extension fatigue effects. Residual stresses are usually harmful for overlapping the operating voltage, while the fatigue resistance of metals and alloys can be improved by compressive residual stresses present in the surface layer by means of shot peening surface. The fatigue life with the compressive residual stress field caused by shot peening or sophisticated models for modeling voltage field Compressive Residual (CTRC) usually does not take into account the possibility of this change during the cyclic loading, ie , place the relaxation process, which also changes the fatigue life. This study aimed to obtain the residual stress profile relaxation by cyclic loading on aluminum alloy samples 7050- T7541 with shot peening glass and ceramics subjected to axial fatigue test. The technique for determining the residual stress was the X-ray diffraction for measuring accurately the redistribution of residual stresses along the depth of fatigue produced by the process. The removal of layers of material was performed by electrolytic attack. Hereby, it was possible to establish the relationship between the maximum stress and number of cycles in relation to the greater or lesser relaxation test specimens in different regimes of cyclic peening conditions with spherical glass and ceramics in the longitudinal and transverse directions. The results showed that the samples with the longitudinal direction shot peening redistribution showed higher compressive residual stresses in the transverse direction along the depth. For the samples of shot peening ceramic was virtually no relaxation on the surface only in depth when compared to the original profile, samples of ceramic shot peening obtained relaxation in remote locations of the surface, due to the influence of roughness. The redistribution of stresses for samples of shot peening glass were higher than those with shot peening ceramic along the depth in all cyclic regimens studied in the L and T directions. The residual stress relaxation occurred in both directions did not compromise beneficial effect of shot peening increase the fatigue life thereof, in relation to the base material. / As tensões residuais podem diminuir e se redistribuir por meio de um processo chamado relaxação. A relaxação das tensões residuais é um fenômeno importante no que se refere à previsão da resistência à fadiga dos materiais e pode ocorrer devido a carga mecânica estática, térmica, cíclica como efeitos de extensão da fadiga. As tensões residuais geralmente são prejudiciais por se sobreporem às tensões de serviço, enquanto a resistência à fadiga dos metais e ligas pode ser melhorada por tensões residuais compressivas presentes nas camadas superficiais por meio do tratamento de superfície de shot peening. A vida em fadiga com o campo de tensão residual compressiva originada pelo shot peening ou modelos sofisticados para a modelagem do Campo de Tensão Residual Compressivo (CTRC), geralmente não leva em consideração, a possibilidade deste alterar-se durante o carregamento cíclico, ou seja, ocorrer o processo de relaxação, que também altera a vida em fadiga. Este trabalho teve como objetivo obter o perfil de tensão residual de relaxação por carregamento cíclico em amostras de liga de alumínio 7050- T7541 com shot peening de vidro e cerâmica submetidas a ensaio de fadiga axial. A técnica para determinação das tensões residuais foi a difração de raios X que permite medir com precisão a redistribuição de tensões residuais ao longo da profundidade produzidas pelo processo de fadiga. A remoção das camadas de material foi realizada por ataque eletrolítico. Por meio deste, foi possível constatar a relação entre a tensão máxima e quantidade de ciclos no que se refere à maior ou menor relaxação de corpos de prova em diferentes regimes cíclicos nas condições de shot peening com esfera de vidro e cerâmica nas direções longitudinal e transversal à laminação.Os resultados mostraram que as amostras com shot peening na direção longitudinal apresentaram redistribuição de tensões residuais compressivas maiores que no sentido transversal ao longo da profundidade. Para os corpos de prova de shot peening de cerâmica praticamente não houve relaxação na superfície apenas na profundidade quando comparado ao perfil original, as amostras de shot peening de cerâmica obtiveram a relaxação em posições mais afastadas da superfície, devido a influência da rugosidade. A redistribuição de tensões para as amostras de shot peening de vidro foram superiores em relação aquelas com shot peening de cerâmica ao longo da profundidade em todos os regimes cíclicos estudados nas direções L e T. A relaxação de tensão residual ocorrida em ambas direções não comprometeu o efeito benéfico do shot peening no aumento da vida em fadiga das mesmas em relação ao material base.

Made available in DSpace on 2017-07-21T20:43:48Z (GMT). No. of bitstreams: 1 JUAN CARLOS GALVIS.pdf: 4226266 bytes, checksum: 0eae227198c4da35bbd08f40e2f3a569 (MD5) Previous issue date: 2016-03-15 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / This study aimed to develop a detailed study of an alternative technique for surface coatings of components or structures made aluminum alloys, using the friction surfacing process. Thus, the influence of deposition process parameters was evaluated as: traverse speed and rotational speed of consumable rod in mechanical properties and metallurgical deposits made. Due to the fact that the machine used is conventional, the axial force as a process parameter was not obtained directly on the machine. To this was used as a control parameter deposition rate, which is calculated from the relationship between the manual displacements in the Z-axis (Dz) of the machine table with the total time (t) of deposition. The experiments were performed using a conventional milling machine KONE KFE-3 / BR available by machining center of SENAI Ponta Grossa-Paraná capable of generating rotational speeds up to 4200 RPM and traverse speed in the table up to 800 mm/min. aluminum alloy rods were deposited AA6351-T6 on AA5052-H32 aluminum alloy substrates using simple type layer deposition (CS) and overlay (S). After execution of the friction deposition process, the deposits obtained were characterized with regard to geometry (length, width and thickness), followed by macro- and microstructure by the techniques of stereoscopic microscopy (EM), optical microscopy (OM), scanning electron microscopy (SEM) and microanalysis by energy dispersive spectroscopy (EDS).Additionally, a microtexture analysis by EBSD technique in a scanning electron microscope with field emission (FEG-SEM) was carried out. In order to evaluate the mechanical properties along the thickness of deposits and especially the adhesion strength of the interface deposit /substrate and deposit / deposit microhardness tests and bending test at three points were conducted, respectively. The experimental results showed that the best combination of friction surfacing process parameters between traverse speed and rotational speed used had better interfacial adhesion strength of the deposits were: i) In the case of single layer deposits (CS),the deposit obtained with traverse speed of 240 mm/min and 3000 RPM rotational speed presented the best results and ii) In the case of the overlay type container (S), the best results were obtained with the traverse speed of 340 mm/min and 3000 RPM rotational speed / O presente trabalho teve como objetivo desenvolver um estudo detalhado de uma técnica alternativa para recobrimentos superficiais de componentes ou estruturas fabricadas em ligas de alumínio, utilizando o processo de união por Deposição Superficial por Atrito (Friction Surfacing FS). Assim, foi avaliada a influência dos parâmetros do processo de deposição como: velocidade de avanço da mesa da máquina e velocidade de rotação da haste consumível nas propriedades mecânicas e metalúrgicas dos depósitos realizados. Em virtude da máquina utilizada ser convencional, a força axial como parâmetro de processo não foi obtida diretamente na máquina. Para isto, foi utilizado como parâmetro de controle a taxa de deposição, sendo este calculado a partir da relação entre o deslocamento manual no eixo Z (Dz) da mesa da máquina com o tempo total (t) de deposição. Os experimentos foram realizados utilizando-se uma máquina fresadora KONE KFE-3/BR disponibilizada pelo Centro de Usinagem do SENAI Ponta Grossa - Paraná com capacidade de gerar velocidades de rotação de até 4200 RPM e velocidades de avanço na mesa de até 800 mm/min. Foram depositadas hastes de liga de alumínio AA6351-T6 sobre substratos de liga de alumínio AA5052-H32 realizando deposições de tipo camada simples (CS) e sobrecamada (S). Após execução do processo de deposição por atrito, os depósitos obtidos foram caracterizados quanto a geometria (comprimento, largura e espessura), seguido de análises macro e microestruturais por meio das técnicas de microscopia estereoscópica (ME), microscopia óptica (MO), microscopia eletrônica de varredura (MEV) e microanálise por espectroscopia de energia dispersiva (EDS). Adicionalmente, foi realizado uma análise de microtextura pela técnica de EBSD em microscópio eletrônico de varredura com emissão de campo (FEG-MEV). Com o intuito de avaliar as propriedades mecânicas ao longo da espessura dos depósitos e principalmente a resistência de adesão da interface depósito/substrato e depósito/depósito ensaios de microdureza e ensaios de dobramento em três pontos foram realizados, respectivamente. Os resultados experimentais mostraram que as melhores combinações de parâmetros de processo de deposição por atrito entre velocidade de avanço e velocidade de rotação usados que obtiveram melhor resistência de adesão interfacial dos depósitos foram: i) no caso dos depósitos de camada simples (CS), velocidade de avanço de 240 mm/min e velocidade de rotação de 3000 RPM e ii) no caso do depósito tipo sobrecamada (S), a velocidade de avanço de 340 mm/min e velocidade de rotação de 3000 RPM.

Le Cold spray est une technique de réalisation de dépôts épais par projection à haute vitesse de particules. Pour cette technologie, la température du gaz vecteur reste inférieure au point de fusion de poudres projetées. Dans ce cas, les mécanismes d’adhésion sont liés aux hautes déformations plastiques que subissent les particules lors de leur impact avec le substrat. Parmi la grande variété de poudres disponibles, trois compositions ont été retenues pour ce travail. Elles autorisent l’élaboration (i) d’alliage d’aluminium, (ii) d’acier inoxydable et (iii) de magnésium. L’ajout de particules de SiC (en fonction de leur quantité ou taille) aux poudres d’aluminium a également permis de modifier les propriétés mécaniques (telle que la dureté) des couches produites. En formant des couches denses et très peu poreuses, les revêtements cold spray présentent tous les atouts des revêtements anti-corrosion. Ce travail de thèse s’est attaché à comprendre les relations existantes entre les paramètres de projection de poudres (température et pression du gaz vecteur, concentration et tailles des particules de SiC) et la qualité du revêtement obtenu, de définir les interfaces substrat / revêtement en fonction de leur composition chimique et leurs influences sur les propriétés de protection vis-à-vis de la corrosion du substrat. D’un point de vu microstructural, les résultats obtenus montrent que l’augmentation de température du gaz améliore la densité des revêtements. En diminuant le nombre de défauts mais également en optimisant la qualité de l’interface substrat/revêtement, la résistance à la corrosion se trouve également améliorée. Sur la base des différences de potentiel entre le revêtement et le substrat, il est possible de classer la nature des couches selon (i) les revêtements sacrificiels et (ii) les revêtements cathodiques. Quel que soit leur nature, les revêtements obtenus par cold spray présentent tous de bonnes propriétés barrières. Toute fois le mode de dégradation des revêtements sacrificielles a pu être assimilé à de la corrosion intergranulaire en lien avec la morphologie du dépôt mais également la distribution et la taille de particule SiC (cas particulier du revêtement d’aluminium). Si les essais de corrosion longue durée ne permettent pas d’amorcer la corrosion du substrat après dissolution du revêtement (pour les couches sacrifielles), des essais de corrosion galvanique autorisent une discrimination rapide de l’efficacité de la couche barrière. Ces tests électrochimiques sont également l’occasion de discuter des effets de la rupture d’un revêtement sur les cinétiques de corrosion des matériaux qu’ils protègent. L’ensemble des caractérisations métallurgiques ainsi que les tests électrochimiques menés sur les différents assemblages substrat/revêtements indiquent que la technique de cold spray est une méthode de choix pour la protection des matériaux de structures vis-à-vis de la corrosion. / Cold spray is a relatively new coating technology in which coatings are produced by powders projected at high velocity. A significant feature of cold spray is that bonding is generated through severe plastic deformation at temperatures well below melting point of feedstock powders. In the present study, kinds of metallic coatings were produced by cold spray, including aluminum alloy coating, pure magnesium coating, magnesium alloy coating, stainless steel coating and SiC reinforced composite coatings. According to the manner in which the coating protects its substrate against corrosion, these cold sprayed coatings can be divided into two types, i.e. sacrificial anodic coating and noble barrier coating. The objective of this thesis is to verify the feasibility of producing both sacrificial anodic coating and noble barrier coating with high corrosion performance by cold spray, and meanwhile demonstrate the usefulness of electrochemical measurements for the characterization of corrosion protection properties of cold sprayed coatings. Besides material system, process parameters which influence corrosion performance of cold sprayed coatings were studied. Two factors, i.e. process gas temperature and process gas pressure were chosen. Results showed that higher process gas temperature leads to denser aluminum coating. Likely, higher process gas pressure improves denseness and corrosion resistance of stainless steel 316L coating. SiC reinforced aluminum based composite coatings were deposited on aluminum, stainless steel and magnesium substrate. Compared with aluminum coating, the addition of hard ceramic particle affects microstructure of coatings, and improves corrosion resistance by increasing denseness. Ceramic particle fraction and size affect coating microstructure in different ways and also influence corrosion behavior. In view of corrosion process, results indicate that corrosion protection of cold sprayed coating could be divided into two steps. In the first step, substrate is completely shielded by dense coating, no corrosion reaction occurs on substrate. In the second step, two types of coatings show totally different behavior. In the case of sacrificial anodic coating, substrate is under cathodic protection in galvanic couple; hence no corrosion (or weakened corrosion) happens on substrate. In contrast, when the coating is noble than substrate, the protection effect would be immediately interrupted once corrosive electrolyte penetrates through coating to interface. The overall results indicate that cold spray is a highly reliable alternative for production of coatings in anti-corrosion applications. Electrochemical measurements are useful tools for quality evaluation of corrosion behavior of cold sprayed coatings.

A multi-analytical approach based on in-situ and ex-situ local probing techniques was employed to investigate localized corrosion mechanisms of some aluminum alloys in chloride containing solutions, focusing on the influence of intermetallic particles (IMPs) in the alloys. In the EN AW-3003 alloy, SEM-EDS analysis revealed constituent and dispersoid IMPs. There are two types of constituent IMPs, with size ranging from 0.5 to several μm, and composition typically Al6(Fe,Mn) or Al12(Mn,Fe)3Si, respectively,having a Mn/Fe ratio of about 1:1. Fine dispersoids of 0.5 μm or less in size normally have the composition Al12Mn3Si1-2. Scanning Kelvin probe force microscopy (SKPFM measurements showed that the constituent IMPs have a higher Volta potential compared to the matrix, and the Volta potential difference increased with particle size, probably related to the composition of the IMPs. The SKPFM results also showed a Volta potential minimum in the boundary region adjacent to some larger IMPs. The open-circuit potential and electrochemical impedance spectroscopy measurements indicated local electrochemical activities occurring on the surface, and active-like dissolution in the acidic solutions, but a passive-like behavior in the near-neutral solutions. Infrared reflection-absorption spectroscopy measurements after exposure and thermodynamic calculations suggested the formation of mixtures of aluminum oxyhydroxide and acetate on the surface in acetic acid solutions. The formation and fraction of dominant species of the corrosion products depend on the pH of the solution, and aluminum chloride compounds may form at very low pH. Moreover, an integrated in-situ atomic force microscopy (AFM) and scanningelectrochemical microscopy (SECM) set-up was used to investigate the localized activities on the surface. With a dual mode probe, acting as both AFM tip and SECM microelectrode, concurrent topography and electrochemical current images were obtained on the same area of the surface. Numerical simulations of the SECM suggested a micrometer lateral resolution under favorable conditions and the ability to resolve μmsized active sites with a separation distance of about 3 μm or larger. The simulations were verified by SECM mapping of the aluminum alloys in the chloride solutions. The AFM/SECM measurements revealed enhanced cathodic activity on some larger IMPs and local anodic dissolution around larger IMPs. In-situ AFM monitoring confirmed preferential dissolution in the boundary region adjacent to some of these IMPs. The results elucidate the micro-galvanic effect and size effect of the IMPs during the initiation of localized corrosion of the Al alloys. Furthermore, differences in corrosion properties between EN AW-3003 and a newly developed Al–Mn–Si–Zr alloy were studied with a similar approach. Compared to EN AW-3003, the new alloy had a smaller number of particles with a large Volta potential difference relative to the matrix. In slightly corrosive solutions extensive localized dissolution and deposition of corrosion products occurred on EN AW-3003, whereas only a small number of corroding sites and “tunnel-like” pits occurred on the Al–Mn–Si–Zr alloy. The lower corrosion activity and the smaller tunnel-like pits resulted in lower material loss of the Al–Mn–Si–Zr alloy, which is beneficial for applications using a thin material. / QC 20100702

The need for clean and renewable fuel such as hydrogen is driven by a growing worldwide population and increasing air pollution from fossil fuels. One of the major barriers for the use of hydrogen in automotive industry is the storage of hydrogen. Physisorption is the most promising storage technique due to its high storage density, reversibility and rapid sorption kinetics besides being safe and volume-efficient. A major challenge for physisorption is the need to manage the heat of adsorption at cryogenic temperatures. In this thesis, a 6061 aluminum microchannel cooling plate is designed to remove the equivalent heat flux required by the adsorption of hydrogen within an adsorption bed. Therefore, the objective of this thesis is to determine whether laser welding and heat treating strategies can be developed for a 6061 aluminum microchannel cooling plate as part of a larger hydrogen storage thermal management system. Key manufacturing process requirements include controlling the hermeticity, strength and dimensional stability of the heat-treated weld joint. A hermetic microchannel cooling plate was successfully laser welded and heat treated using free convection in air to quench the solution heat treatment. The weld strength and warpage obtained were within acceptable limits. Experimental testing of the fabricated microchannel cooling plate showed acceptable percent error with an experimental heat removal rate within 13.4% of computational fluid dynamics (CFD) analyses and an average pressure drop error of 25%. Calculations show that the cooling plate developed could support a hydrogen storage thermal management system taking up 5.0% and 10.3% of the system displacement volume and mass, respectively. / Graduation date: 2013

The continuing quest for higher performance levels of modern gas turbine engines has been accompanied by the demand for higher engine operating temperatures. The use of Thermal Barrier Coatings (TBCs) enabled gas turbines to operate at higher temperatures by protecting the blade material (nickel superalloy) while operating in extreme environments. The TBC system typically consists of a bond coat for protection of the nickel–based superalloy against oxidation followed by a top coat consisting of a thermally insulating zirconia-yttria. In addition to the complex gradation in phases, the coatings are subjected to continuous oxidation with service exposure, mechanical loading on rotating parts, fatigue, thermal mis-match and temperature gradients. Hence, the study of failure mechanisms of TBCs become important in deciding operational reliability and service life of the coating. As there are many systems in which the operating temperatures are not high enough to warrant the use of the top coat (ceramic layer), the study of failure mechanisms in superalloys coated with only the bond coat continue to be of great interest. The present work concentrates on the fracture behavior of NiAl bond coats on nickel superalloy and seeks to evaluate the fracture toughness of the coating through the use of micro-machined samples. A review of the relevant literature indicated that while a considerable body of work exists on bulk tests of failure (spalling, splitting, etc.), not much has been reported in the open literature on the evaluation of basic quantities such as the toughness of the coating itself. The present thesis seeks to establish a protocol for the evaluation of toughness and crack propagation mechanisms in coatings through a combination of micro-sample testing that allows fracture to be correlated with location in the film and the use of an analytical model to quantitatively evaluate stress intensity factors in a bi-material system. A system of NiAl coating produced by pack aluminizing is studied for the fracture properties of the coating. Specimen geometries are optimized to enable micro-cracks to be machined and propagated in a low load testing system, such as a depth sensing indenter, so that crack lengths (and position relative to the interface) can be correlated with load. To enable linear elastic theory to be used, dimensions are determined that allow fracture before general yielding. A three point bending test using miniaturized micro-beam specimens of ~ 4 X 0.3 X 0.3 mm is found to be suitable for the above purpose. The technique is a challenging one that requires focused ion beam machining (FIB) along with careful handling and alignment of small samples. The coatings are characterized for their microstructure by electron microscopy to identify compositional variation across the thickness and to determine the thickness of the coating and inter diffusion zone (IDZ). The crack advancement is monitored with increments of loading and the stress intensity factor is evaluated using a program written in “MAPLE” for an edge crack subjected to bending in a bilayered material. Surprisingly, fracture in this system is found to be stable owing to a gradual increase in toughness from the coating surface to the interface. Such an increase from less than 2 to more than 9 MPa m0.5 may be due to the increasing Ni/Al ratio across the thickness of the bond coat. Crack branching is observed as the crack approaches the IDZ and the reasons for such behaviour are not fully understood. This work establishes the viability of this technique to determine fracture properties in highly graded coated systems and may be readily extended to more complex coating architectures and other forms of loading such as cyclic, mixed mode, etc.

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.

Fundação de Amparo a Pesquisa do Estado de Minas Gerais / The main objective of the present work is to study the effect of the input variables: mechanical properties of the workpiece (tensile strength, hardness and elongation) and cutting conditions (cutting speed, feed rate, depth of cut and lubri-cooling system) over the output variables: cutting forces, power consumption, cutting temperature, surface roughness (Ra, Rz and Rq parameters) and toolholder vibration in turning of aluminum alloys: 1350-O, 6082-T4, 6262-T6,7075-T73 e 7075-T6. This set of alloys covers a large range of properties of the aluminum alloys. A 2k factorial planning and a Central Composite Design (CCD) were used to determine the machining test conditions. After ANOVA and Regression analysis of the results, 2nd order models were generated, relating the input and the output variables for each aluminum alloy and also globally (considering the properties of the alloys). Surface Response Method SRM, level curves and gradient vector generated after the models were used to present and analyze the influence of the input variables and their interactions on the output parameters. Validated models used in a multi-response optimization process (genetic algorithm) identified the levels of the input variables that simultaneously optimize all the output parameters. The most important contribution of this work on the machining of aluminum alloys lies on its efficiency of describing the behavior of each machining characteristic (output variable) as a function of the input variable interactions within the range studied. Many researches on machining of aluminum alloys describe, in an isolated form, the behavior of the machining characteristics (output parameters) as functions of a few or only one factor, limiting the conclusions about the machinability of these alloys. In the present work it was observed that generally the machining output parameters varied individually according to the literature, however, new behavior, due to the interaction of the input variables, so far not described by previous work was presented. / Este trabalho objetiva estudar o efeito das variáveis de entrada: propriedades mecânicas da peça (resistência mecânica, dureza e alongamento) e condições de corte (velocidade de corte, avanço, profundidade de corte e sistema de lubri-refrigeração) sobre as variáveis de saída (respostas): forças de usinagem; potência de usinagem; temperatura de corte; parâmetros de rugosidade: Ra, Rz e Rq e vibração do suporte da ferramenta no torneamento das ligas de alumínio: 1350-O, 6082-T4, 6262-T6, 7075-T73 e 7075-T6. Estas ligas cobrem uma larga faixa de propriedades das ligas de alumínio. Para este estudo foi utilizado o planejamento fatorial 2k completo e o planejamento composto central (PCC), para determinar as condições de ensaios de usinagem. A partir de análise de variância e de regressão dos resultados foram gerados modelos de 2ª ordem, relacionando, em cada liga de alumínio, e também de forma global (considerando as propriedades das ligas), as respostas com as entradas. Superfícies de respostas, curvas de níveis e vetor gradiente gerados a partir desses modelos foram utilizados para apresentar e analisar as influências das entradas, por interação entre fatores, sobre as respostas. Modelos validados foram utilizados em um processo de otimização multiresposta (algoritmo genético), que identificou os níveis das entradas que otimizassem, simultaneamente, todas as respostas. A grande contribuição deste trabalho, relacionado com a usinabilidade das ligas de alumínio, repousa em sua capacidade de descrever o comportamento da característica de usinabilidade (resposta) em função das interações das entradas em sua região de variação. Muitas pesquisas envolvendo a usinagem das ligas de alumínio descrevem de forma isolada o comportamento das características de usinabilidade em função de alguns fatores ou apenas um único fator, o que limita grandemente as conclusões sobre a variação das características de usinabilidade. Neste trabalho se observou, de maneira geral, que as características de usinabilidade variaram de forma isolada com os fatores, de acordo com o registrado na literatura, mas novos comportamentos das características de usinabilidade, ainda não descritos na literatura, devido à interação entre fatores foram presenciados. / Doutor em Engenharia Mecânica

Este trabalho discutiu a relação entre o espaçamento inter-estrias , isto é, a taxa de propagação da trinca microscópica SL (local) e SP (projetada) e a taxa de propagação macroscópica , da/dN, obtido após o ensaio de propagação de trinca por fadiga. Corpos de prova compacto C(T) foram extraídos na orientação LT do centro de uma placa laminada de liga de alumínio SAE-AMS 7475 T7351 onde posteriormente foram realizados ensaios de fadiga sob carga ou &#916K constantes, à temperatura ambiente de acordo com a Norma ASTM-E647 (1993). Para o ensaio sob carga constante foram obtidos os dados do estágio II e III da curva da/dN vs. &#916K. Para o ensaio de fadiga sob &#916K constante, quatro níveis de &#916K foram utilizados com taxas de crescimento de trinca variando entre 0,15 à 2,4 &#956m/ciclo. Adicionalmente foram realizados ensaios de tenacidade à fratura, KIC nas direções LT e TL conforme a Norma ASTM-E1820 (1999). A análise fratográfica por microscopia eletrônica de varredura foi conduzida no ensaio de fadiga a &#916K constante para determinar os espaçamentos inter-estrias. As taxas de propagação macroscópica e microscópica foram comparadas e boas correlações foram obtidas para um intervalo entre 0,1 a 1,0 &#956m/ciclo. Através da técnica proposta por Berkovitz (1995), o espectro de carregamento foi estimado através da técnica de parametrização do fator K e os resultados foram comparados ao espectro de carregamento real imposto pela máquina de ensaio. Utilizando o espaçamento inter-estrias local, SL, e para valores de &#916K menores que 23 MPam 1/2 (região de Paris), a estimativa de carregamento exibiu um erro menor que 15%. As vidas estimadas em propagação fornecidas pelas taxas microscópicas de propagação de trinca foram comparadas à vida real de propagação obtida a partir da taxa de propagação de trinca macroscópica e o erro absoluto entre ambos os valores foi menor que 15,7 %. Estes resultados sugerem que a vida em fadiga e o espectro de carga podem ser adequadamente estimados utilizando o espaçamento inter-estrias local, SL. / This work discusses the relationship between striation spacing, i.e. the microscopic crack propagation rate, SL (local) e SP (projected), as measured in post-mortem fractographic inspection of fatigue fractured surfaces, and the macroscopic crack propagation rate, da/dN, as monitored during fatigue crack growth tests. Compact tensile specimens C(T) were extracted in LT orientation from the core of a laminated plate of a SAE-AMS 7475-T7351 Al alloy and subsequently fatigue tested either at constant load or at constant &#916K, at room temperature, according to ASTM-E647. For constant amplitude loading fatigue tests, da/dN- &#916K data points were obtained for Regions II and III of crack growth curve. For constant &#916K fatigue tests, four &#916K levels were selected to give crack growth rates typically ranging from 0.15 to 2.4 &#956m/cycle. Additionally, KIC fracture toughness tests were performed in both LT and TL directions, according to ASTM E1820. SEM fractographic analysis was conducted on constant &#916K fatigue specimens, in order to determine striation spacing created during the fatigue test. Macro- and microscopic crack growth rates were compared and good correlation have been obtained for data within the range from 0,1 to 1,0 &#956m/ciclo. Using the technique proposed by Berkovitz, loading history was estimated by the K-factor parametrization and the results were compared to the true loading spectrum imposed by the testing machine. Using the local striation spacing SL and for &#916K values lower than 23 MPam 1/2 (Paris region), the estimated loading exhibits an error less than 15%. Propagation life estimated by local striation spacing (microscopic crack growth rate) was compared to the true propagation life obtained from macroscopic crack growth rate values and the absolute difference between them was less than 15,7%. These results suggest that both life and loading history can be adequately estimated using the local SL striation spacing values.