Al-Zn-Mg-Cu-Zr based AA7010 aluminum alloy belongs to the class of heat treatable alloys and the semi-finished products are generally produced by hot rolling, forging or extrusion processes. It is well known that the thermo-mechanical processing parameters strongly influence both the evolution of texture as well as microstructure in the material. As a result, the semi-finished products exhibit anisotropy in mechanical properties causing legitimate concerns on the applicability of the alloys. In the present thesis, a systematic study on the evolution of texture and microstructure and its implications on the mechanical properties anisotropy of AA7010 alloy has been attempted. A brief introduction on the development of texture and its influence on the anisotropy of the mechanical properties of 7xxx series aluminum alloys is presented first with a view to explore the scopes for further investigation. An overview of the relevant literature is described subsequently. The development of texture and microstructure in an Al-Zn-Mg-Cu-Zr based 7010 aluminum alloy during uneven, hot cross-rolling is presented. Materials processing involves three different types of uneven cross-rolling. The variations in relative intensity of the β-fibre components as a function of cross rolling modes have been investigated. It has been shown that the main attributes to the texture evolution in the present study are (a) cross-rolling and inter-pass annealing that reduce the intensity of Cu component following each successive pass, (b) recrystallization resistance of Bs oriented grains, (c) stability of Bs texture under cross-rolling, and (d) Zener pinning by Al3Zr dispersoids. The stability of the unique single, rotated Brass-{110}(556) component developed in the present alloy, during long term thermal annealing and cold rolling deformation has been systematically investigated further. Subsequently, the influence of development of microstructure and texture on the in-plane anisotropy (AIP) of yield strength, work hardening behavior and yield locus anisotropy has been presented. The AIP and work hardening behavior are evaluated by tensile testing at 0o, 45o and 90o to the rolling direction, whilst yield loci have been generated by Knoop hardness method. It has been observed that in spite of having strong rotated Brass texture, the specimens show low AIP especially in peak aged temper. The in-plane anisotropy (AIP) of yield strength, and work hardening behavior of a heat treated 7010 aluminum alloy sheet having strong, rotated Brass-{110}556 component with different texture intensity and volume fraction of recrystallization has been further evaluated. It is observed that the AIP increases with increase in texture intensity and volume fraction of recrystallization. In the subsequent chapter, the tensile flow and work hardening behavior are described using constitutive equations. Room temperature tensile properties have been evaluated as a function of tensile axis orientations in as-hot rolled as well as peak aged conditions. It has been found that both the Ludwigson and a generalized Voce-Bergström relation adequately describe the tensile flow behavior in all conditions compared to the Hollomon relation. The Voce-Bergström parameters define the slope of - plots in the stage-III regime when the specimens show a classical linear decrease in hardening. Further analysis of work hardening behavior throws light on the effect of texture on the dislocation storage and dynamic recovery. An overall summary of the experimental results and the scopes for future studies have been presented at the end.

No presente trabalho quatro ligas Al-Si hipereutéticas, três das quais foram produzidas por conformação por \"spray\" e a outra por fundição, foram caracterizadas quanto a textura, dureza, microestrutura e resistência à corrosão em meio de condensado sintético automotivo (CSA). Duas das ligas conformadas por \"spray\" foram retiradas de camisas de cilindro e a outra de um pré-formado obtido em laboratório. A conformação por \"spray\" envolve a atomização de uma liga e a deposição de gotículas em um substrato, antes mesmo que todas se encontrem no estado sólido. Este processo permite a obtenção de materiais que se caracterizam por uma microestrutura livre de macrossegregações e bastante refinada, implicando melhor trabalhabilidade a quente. A caracterização da microestrutura das quatro ligas hipereutéticas revelou a presença de porosidades na liga obtida em laboratório, e microestrutura com distribuição homogênea de precipitados primários nas três ligas conformadas por \"spray\". A microestrutura de uma das ligas apresentou-se muito diferenciada, com a presença de eutético, sugerindo que esta foi fabricada por fundição. Nas camisas de cilindro foram feitas medidas de rugosidade, e em todas as ligas foram realizados ensaios de microdureza. A liga conformada por \"spray\" e obtida em laboratório foi laminada a quente e a frio. Foram realizados também estudos de textura, para tentar estabelecer uma correlação entre todas as ligas quanto ao processo de fabricação. A avaliação da textura indicou que a presença de fases de silício primário, finamente distribuídas impedem o aparecimento de texturas típicas de deformação de ligas de alumínio, mesmo após severas deformações, como as necessárias para a transformação de pré-formados em tubos que originam as camisas de cilindro. As medidas de rugosidade indicaram características próprias do acabamento superficial usado para a produção das camisas, por brunimento ou por ataque químico. Os ensaios de microdureza apresentaram variações de acordo com as rotas de fabricação sendo que a liga eutética apresentou os maiores valores de microdureza em comparação às ligas conformadas por \"spray\". Todas as ligas foram avaliadas quanto a resistência à corrosão por ensaios de espectroscopia de impedância eletroquímica em dois meios, CSA com pH 3,3 e CSA com pH 11. As quatro ligas hipereutéticas estudadas apresentaram mecanismo de corrosão similar em condensado sintético automotivo (CSA) pH 3,3. Em todas ocorreu o ataque intenso da matriz de alumínio e as partículas de silício primário atuaram como regiões catódicas. A liga 2 apresentou maior resistência à corrosão entre todas as ligas ensaiadas, tanto em CSA pH 3,3 como em pH 11. Neste último meio, uma camada de produtos de corrosão formou-se sobre todas as ligas, e os resultados indicaram mecanismos diferentes para o ataque da matriz de Al e para o crescimento da camada depositada na superfície das ligas estudadas. O ataque da matriz da liga 2 neste meio foi aparentemente mais lento do que sobre as demais ligas, com a formação de uma camada mais compacta de produtos de corrosão, estabelecendo um controle por difusão dos processos interfaciais para maiores períodos de ensaio. A camada formada sobre as demais ligas neste meio apresentou-se mais defeituosa, e nestas ocorreu também menor controle da velocidade das reações interfaciais por processos difusionais. / In the present study four hypereutectic Al-Si alloys, three produced by spray forming and one by casting, were characterized for microhardness, roughness, microstructure, texture and corrosion resistance in a synthetic automotive condensed solution (SACS). Two of the spray formed alloys tested were obtained from cylinder liners and the other was laboratory made. Spray forming involves alloy atomization and droplets deposition on a substrate, previous to the solidification of all of the droplets. This process favours the production of materials with a fine microstructure free of macrosegregation that is related to improved hot workability. The microstructure characterization of the four alloys revealed the presence of porosities in the laboratory made alloy. All the three alloys produced by spray forming showed a homogeneous distribution of primary precipitates. The microstructure of one of the alloys showed eutectic microstructure, indicating that this alloy was fabricated by casting. In the cylinder liners, the surface roughness was measured and the microhardness of all the alloys was also evaluated. Furthermore, the laboratory made alloy was hot and cold rolled. Texture determinations were carried out to investigate the correlation between the alloy type and their fabrication process. The texture investigation indicated that the fine distribution of primary silicon phase in the alloy hindered the development of texture typical of aluminium alloys deformation, even after severe mechanical work, such as those used in the conversion of pre-formed in cylinder liners. The surface roughness results indicated typical characteristics of the surface finishing used, honing or chemical etching. The microhardness results were dependent on the fabrication process used, with higher microhardness associated to the eutectic alloy comparatively to the spray formed ones. All hypereutectic alloys were tested for corrosion resistance using electrochemical impedance spectroscopy in two electrolytes, SACS with pH 3.3 and SACS with pH 11. The four tested alloys showed similar corrosion mechanisms in the acid electrolyte (SACS pH 3.3). The intense attack of the aluminium matrix occurred in ali tested alloys and the primary silicon phase was unattacked and appeared as emerging from the surface after corrosion immersion test. The primary silicon particles acted as cathodic sites. The alloy 2 showed the highest corrosion resistance among the tested alloys in both electrolytes, SACS pH 3.3 and SACS pH 11. In this last medium, a layer of corrosion products formed on all the alloys, and the results indicated different mechanisms for the aluminium matrix corrosive attack and growth of the deposited layer on the alloys surface. The kinetics of aluminium matrix attack was apparently slower in the alloy 2 than for the other alloys, resulting in the formation of a more compact layer of corrosion products, leading to diffusion controlled interfacial processes for longer test periods. The layer of corrosion products on the other three alloys (1, 3, and 4) had more defects and for these alloys diffusional controlled interfacial processes were not as significant as for alloy 2.

Aluminium silicon alloy has been found to be advantageous in many automobile components like pistons, cylinders, brakes and clutches. The main objective in using these alloys is to obtain lightweight and low friction at a reasonable cost without sacrificing reliability and durability. Out of all the tribological components piston skirts, piston rings and cylinder liners, have to face the most hostile of environments in an internal combustion engine. Wear mechanism of these components have been identified as abrasion, scuffing and corrosion. Narrowing down the line of interest, cylinder wear is more important than ring wear to both the engine manufacturer and the user, as cylinders are more expensive to replace than piston rings. Wear of piston ring and cylinder combination have been studied using a wide range of techniques. It is difficult to predict the tribological performance of these parts in an engine, even with the most well designed laboratory tests, due to chemical, thermal and mechanical complexities in the operating environment. Therefore, a good correlation is sought from the wear behaviour of test bed engines and laboratory tests. This should form the basis of further development particularly in terms of efficiency, weight eduction and wear life improvement of the components. Many ASTM bench-wear tests are used to study wear, some of the common tests being ball-on-disc and pin-on-disc testing. From these tests, a large database of wear information can be achieved and they offer rapid and low cost means of comparison. The only drawback is that the real components are not tested. However, since the bench tests can never simulate the engine environment completely, engine tests are always required for final verification. This thesis work reports preliminary studies of machining damage and wear in actual engine bore to set a bench mark, followed by a set of unidirectional sliding bench tests to study the wear of aluminium alloy under lubricated conditions, to classify the different wear regimes in boundary lubrication zone under different pressure conditions, and to study the effect of a surface modification technique, etching, which improves wear properties. The investigation is divided into four parts. 1. Study of subsurface damage in an actual cylinder surface as introduced by prior machining and actual worn case: A study of the microstructure of bores, processed through a range of machining variables; feed and speed, are investigated in this part of the thesis. This work suggests that the first step of rough machining may be responsible for the microstructure of the finished bore even though subsequent processing steps are intended to remove all prior damages. This also includes some observations of worn surface of an actually run engine, locating the various worn spots and studying the cause of this damage 2. Bench wear test in pin-on-disc under dry and lubricated condition with varying load and lubricant: After setting a benchmark on wear in engine using actual worn cylinder bore, a set of bench tests were carried out on aluminium alloy. Here, steel pins are slid on aluminium silicon alloy discs in the boundary lubrication regime in the presence of one drop of oil. The effect of pure hexadecane and engine oil containing additives on friction and wear are analysed and the data are discussed in terms of the formation of a mechanically mixed layer at the interface. 3. Ultra-mild Wear in Lubricated Tribology of an Aluminium Alloy: To study the different wear regimes in boundary lubrication zone, flat faces of cylindrical steel pins were slid on an eutectic aluminium silicon alloy under lubricated condition in the 1-100 MPa mean contact pressure range and 0.2 m/s sliding speed. Two transitions in wear rate were observed, at 10 MPa and 70 MPa. The wear rate in the 1-10 MPa regime was found to be very small and within the measuring instrument resolution and also insensitive to contact pressure. The regime is designated ultra-mild wear. Lack of plastic flow, minimal fragmentation of silicon particles and the presence of undistorted voids on the fractured and unfractured silicon particles in the subsurface suggest that the state of stress in the near surface region is elastic. Contact mechanical calculations demonstrate that at contact pressures less that 13.7 MPa the system is likely to shakedown to an elastic state. 4.Ball-on-disc wear tests for etched and unetched samples: In the fourth part of the thesis, comparative studies have been done between the as polished and chemically treated samples. Formation of grooves in a ball-on-disc experiment is observed on etched and unetched flats as a function of normal load and sliding distance. The groove is initially formed by plastic flow, and then expanded by micro-abrasion as the ball continues to slide on the groove. However etching causes surface hardening of the alloy, but, more importantly, creates a surface topology that reduces the peak contact pressure, which inhibits further plastic flow in the subsurface.

Ο χαρακτηρισμός της ποιότητας των χυτών κραμάτων αλουμινίου , γίνεται μέχρι σήμερα μέσω του χαρακτηρισμού της ποιότητας της μικροδομής, μετρήσεων σκληρότητας και πειραμάτων κρούσης και σε μικρότερο βαθμό, δοκιμών εκφυλισμού. Στην παρούσα διατριβή, προτείνεται ένας νέος εμπειρικός δείκτης για τον ποσοτικοποιημένο χαρακτηρισμό της ποιότητας χυτών κραμάτων αλουμινίου. Ο προτεινόμενος δείκτης αξιολογεί την ποιότητα ενός υλικού από την πλευρά του μηχανικού που σχεδιάζει ένα κατασκευαστικό στοιχείο και επομένως την αξιολογεί ως την ικανότητα του υλικού για μηχανικές επιδόσεις. Για την αξιολόγηση αυτή ο προτεινόμενος δείκτης συνεκτιμά την αντοχή και την ολκιμότητα του υλικού σε εκφυλισμό. Παράλληλα, για το χαρακτηρισμό της ποιότητας, ο δείκτης παίρνει υπόψη τη δυσθραυσότητα του υλικού καθώς και τη διασπορά των μηχανικών ιδιοτήτων του υλικού. Η διατύπωση του δείκτη στηρίχτηκε σε έναν ευρείας έκτασης πειραματικό χαρακτηρισμό της μηχανικής συμπεριφοράς σε εφελκυσμό καθώς και της μικροδομής των κυριότερων αεροπορικών χυτών κραμάτων αλουμινίου σε συνάρτηση με τη μεταβολή α) της χημικής σύστασης, β) του ρυθμού στερεοποίησης και γ) της θερμικής κατεργασίας αυτών καθώς και στη διατύπωση εμπειρικών συναρτήσεων για την εξάρτηση των μηχανικών ιδιοτήτων των κραμάτων που εξετάστηκαν από τις παραπάνω μεταβολές των παραμέτρων χύτευσης. Προκειμένου να διευκολυνθεί η αξιοποίηση του δείκτη, διατυπώθηκαν απλουστευμένες προσεγγιστικές εκφράσεις που επιτρέπουν τον υπολογισμό του από δεδομένα των απλών πειραμάτων της σκληρομέτρησης και της κρούσης. Τέλος προτάθηκε μεθοδολογία δημιουργίας χαρτών ποιότητας με βάση τον προταθέντα δείκτη για την υποστήριξη της επιλογής υλικού όταν είναι γνωστές οι απαιτήσεις σε μηχανικές επιδόσεις συγκεκριμένων κατασκευαστικών στοιχείων. / Quality evaluation of cast aluminum alloys is currently made mainly by means of the met- allographic characterization of the alloy’s niicrostructure, hardness measurements, impact tests and, to a lesser extend, tensile tests, are involved, as well. Yet, the overall decision is not a straight forward procedure, relies heavily on the experience of the quality engineer and involves an appreciable amount of subjective judgment. In the present Thesis, a new empirical quality index for the quantitative evaluation of the quality of cast aluminum alloys is introduced. The proposed index evaluates quality which is regarded as the ability of a material for mechanical performance. The index evaluates the quality of a cast alloy on the basis of a balance between the material’s tensile strength and ductility with regard also to the material’s toughness. In the proposed index the scatter in mechanical properties is also accounted. The formulation of the index has been based on an extensive experimental characterization of the tensile behavior and the microstructural features of the main aircraft aluminum cast alloys by varying chemical composition, solidification rate and artificial aging treat- ment. To facilitate the wide spread use of the index, simplified approximate expressions of the index have been formulated as well. These expressions allow for the calculation of the proposed quality index based on hardness measurements and impact test results. The index has been also exploited to devise quality maps, which may be used to support material selection with regard to the mechanical properties required by the design office for a certain application.

Submitted by Mery Piedad Zamudio Igami (mery@ipen.br) on 2017-03-10T14:37:28Z No. of bitstreams: 1 22056.pdf: 6258956 bytes, checksum: 5b6bd2c4bc8c6f66cd739d2ef10fe810 (MD5) / Made available in DSpace on 2017-03-10T14:37:28Z (GMT). No. of bitstreams: 1 22056.pdf: 6258956 bytes, checksum: 5b6bd2c4bc8c6f66cd739d2ef10fe810 (MD5) / A soldagem por fricção (Friction Stir Welding - FSW) é um processo eficiente de unir ligas de alumínio de alta resistência evitando defeitos que são usualmente criados quando técnicas convencionais de soldagem são utilizadas. A indústria aeronáutica tem mostrado grande interesse neste método de soldagem, tanto para a união de ligas similares como dissimilares. Entretanto, este processo causa modificações microestruturais dependentes das condições de tratamento térmico ou termomecânico. Contato elétrico entre zonas de microestruturas diferentes, por sua vez, pode resultar em acoplamento galvânico. No presente estudo, a soldagem por FSW foi usada para unir duas ligas de alumínio dissimilares, AA2024-T3 e AA7475-T651 e o efeito desta soldagem na resistência à corrosão das juntas soldadas e na microestrutura das ligas foi avaliada. Na investigação da resistência à corrosão foram utilizados ensaios eletroquímicos, especificamente, medidas de potencial de circuito aberto (OCP) em função do tempo de exposição ao meio corrosivo, ensaios de polarização e de espectroscopia de impedância eletroquímica, global (EIS) ou local (LEIS), em duas soluções, seja 0,1 M Na2SO4 ou 0,1 M Na2SO4 + 1 mM NaCl. Os ensaios eletroquímicos evidenciaram efeito de acoplamento galvânico nas juntas soldadas. A caracterização microestrutural foi realizada por microscopia ótica, microscopia eletrônica de varredura, microscopia eletrônica de transmissão e por calorimetria diferencial. As zonas afetadas pela solda tiveram importantes modificações na microestrutura indicadas pela precipitação e dissolução de precipitados que afetam a resistência à corrosão localizada. A resistência à corrosão intergranular e a resistência à esfoliação das juntas soldadas também foram avaliadas e comparadas com as das ligas AA2024-T3 e AA7475-T651 não soldadas. Os resultados mostraram aumento da suscetibilidade das juntas soldadas a estas formas de corrosão em comparação com as ligas não soldadas sendo observado ataque mais severo na liga AA7475-T651. A identificação das áreas anódicas e catódicas resultantes do acoplamento galvânico nas juntas soldadas foi realizada por teste que consistiu na deposição de camada de gel (ágar-ágar) com indicador universal na superfície das ligas soldadas. A liga AA2024-T3 atuou como cátodo, enquanto a AA7475-T651, como ânodo no par galvânico. Além disso, evolução de hidrogênio foi observada na região de interface entre a zona termomecanicamente afetada e a termicamente afetada da liga AA7475-T651 mostrando que reações catódicas também ocorreram localmente nesta última liga. Resultados de LEIS obtidos nas diferentes zonas das duas ligas soldadas por FSW mostraram acoplamento galvânico na interface entre elas para tempos curtos de ensaio e deslocamento da região mais ativa com o tempo de ensaio para a liga AA7475-T651, mais precisamente para a interface entre a zona termomecanicamente afetada e a térmicamente afetada desta liga. / Tese (Doutorado em Tecnologia Nuclear ) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

No presente trabalho quatro ligas Al-Si hipereutéticas, três das quais foram produzidas por conformação por \"spray\" e a outra por fundição, foram caracterizadas quanto a textura, dureza, microestrutura e resistência à corrosão em meio de condensado sintético automotivo (CSA). Duas das ligas conformadas por \"spray\" foram retiradas de camisas de cilindro e a outra de um pré-formado obtido em laboratório. A conformação por \"spray\" envolve a atomização de uma liga e a deposição de gotículas em um substrato, antes mesmo que todas se encontrem no estado sólido. Este processo permite a obtenção de materiais que se caracterizam por uma microestrutura livre de macrossegregações e bastante refinada, implicando melhor trabalhabilidade a quente. A caracterização da microestrutura das quatro ligas hipereutéticas revelou a presença de porosidades na liga obtida em laboratório, e microestrutura com distribuição homogênea de precipitados primários nas três ligas conformadas por \"spray\". A microestrutura de uma das ligas apresentou-se muito diferenciada, com a presença de eutético, sugerindo que esta foi fabricada por fundição. Nas camisas de cilindro foram feitas medidas de rugosidade, e em todas as ligas foram realizados ensaios de microdureza. A liga conformada por \"spray\" e obtida em laboratório foi laminada a quente e a frio. Foram realizados também estudos de textura, para tentar estabelecer uma correlação entre todas as ligas quanto ao processo de fabricação. A avaliação da textura indicou que a presença de fases de silício primário, finamente distribuídas impedem o aparecimento de texturas típicas de deformação de ligas de alumínio, mesmo após severas deformações, como as necessárias para a transformação de pré-formados em tubos que originam as camisas de cilindro. As medidas de rugosidade indicaram características próprias do acabamento superficial usado para a produção das camisas, por brunimento ou por ataque químico. Os ensaios de microdureza apresentaram variações de acordo com as rotas de fabricação sendo que a liga eutética apresentou os maiores valores de microdureza em comparação às ligas conformadas por \"spray\". Todas as ligas foram avaliadas quanto a resistência à corrosão por ensaios de espectroscopia de impedância eletroquímica em dois meios, CSA com pH 3,3 e CSA com pH 11. As quatro ligas hipereutéticas estudadas apresentaram mecanismo de corrosão similar em condensado sintético automotivo (CSA) pH 3,3. Em todas ocorreu o ataque intenso da matriz de alumínio e as partículas de silício primário atuaram como regiões catódicas. A liga 2 apresentou maior resistência à corrosão entre todas as ligas ensaiadas, tanto em CSA pH 3,3 como em pH 11. Neste último meio, uma camada de produtos de corrosão formou-se sobre todas as ligas, e os resultados indicaram mecanismos diferentes para o ataque da matriz de Al e para o crescimento da camada depositada na superfície das ligas estudadas. O ataque da matriz da liga 2 neste meio foi aparentemente mais lento do que sobre as demais ligas, com a formação de uma camada mais compacta de produtos de corrosão, estabelecendo um controle por difusão dos processos interfaciais para maiores períodos de ensaio. A camada formada sobre as demais ligas neste meio apresentou-se mais defeituosa, e nestas ocorreu também menor controle da velocidade das reações interfaciais por processos difusionais. / In the present study four hypereutectic Al-Si alloys, three produced by spray forming and one by casting, were characterized for microhardness, roughness, microstructure, texture and corrosion resistance in a synthetic automotive condensed solution (SACS). Two of the spray formed alloys tested were obtained from cylinder liners and the other was laboratory made. Spray forming involves alloy atomization and droplets deposition on a substrate, previous to the solidification of all of the droplets. This process favours the production of materials with a fine microstructure free of macrosegregation that is related to improved hot workability. The microstructure characterization of the four alloys revealed the presence of porosities in the laboratory made alloy. All the three alloys produced by spray forming showed a homogeneous distribution of primary precipitates. The microstructure of one of the alloys showed eutectic microstructure, indicating that this alloy was fabricated by casting. In the cylinder liners, the surface roughness was measured and the microhardness of all the alloys was also evaluated. Furthermore, the laboratory made alloy was hot and cold rolled. Texture determinations were carried out to investigate the correlation between the alloy type and their fabrication process. The texture investigation indicated that the fine distribution of primary silicon phase in the alloy hindered the development of texture typical of aluminium alloys deformation, even after severe mechanical work, such as those used in the conversion of pre-formed in cylinder liners. The surface roughness results indicated typical characteristics of the surface finishing used, honing or chemical etching. The microhardness results were dependent on the fabrication process used, with higher microhardness associated to the eutectic alloy comparatively to the spray formed ones. All hypereutectic alloys were tested for corrosion resistance using electrochemical impedance spectroscopy in two electrolytes, SACS with pH 3.3 and SACS with pH 11. The four tested alloys showed similar corrosion mechanisms in the acid electrolyte (SACS pH 3.3). The intense attack of the aluminium matrix occurred in ali tested alloys and the primary silicon phase was unattacked and appeared as emerging from the surface after corrosion immersion test. The primary silicon particles acted as cathodic sites. The alloy 2 showed the highest corrosion resistance among the tested alloys in both electrolytes, SACS pH 3.3 and SACS pH 11. In this last medium, a layer of corrosion products formed on all the alloys, and the results indicated different mechanisms for the aluminium matrix corrosive attack and growth of the deposited layer on the alloys surface. The kinetics of aluminium matrix attack was apparently slower in the alloy 2 than for the other alloys, resulting in the formation of a more compact layer of corrosion products, leading to diffusion controlled interfacial processes for longer test periods. The layer of corrosion products on the other three alloys (1, 3, and 4) had more defects and for these alloys diffusional controlled interfacial processes were not as significant as for alloy 2.

Dans un contexte normatif toujours plus sévère concernant les rejets automobiles polluants, la substitution des aciers par des alliages d’aluminium dans les structures des véhicules est en plein essor. Ce projet de thèse, qui s’inscrit dans un programme de développement de la société Constellium, cible plus précisément les alliages d’aluminium de la série 7xxx (Al-Zn-Mg) qui, malgré leurs propriétés mécaniques élevées, peuvent présenter une sensibilité à la corrosion sous contrainte (CSC) liée au phénomène de fragilisation par l’hydrogène (FPH). La compréhension des mécanismes mis en jeu dans ce type d’endommagement constitue donc une première étape vers une optimisation métallurgique en vue d’une industrialisation future de ces alliages dans le secteur automobile. La première partie de ces travaux est consacrée à l’étude de l’influence de l’état métallurgique de l’alliage 7046 sur son comportement en CSC et à l’identification des mécanismes de dégradation. Un lien direct a pu être mis en évidence entre l’abattement des propriétés mécaniques et les modes de rupture actifs et la quantité d’hydrogène dans l’alliage. Les deux modes d’endommagement observés, intergranulaire-fragile et transgranulaire-fragile, ont respectivement été attribués à un enrichissement en hydrogène aux joints de grains et au piégeage de l’hydrogène au niveau des précipités intragranulaires. Les interactions entre l’hydrogène et les précipités fins d’une part et les dislocations d’autre part, identifiés comme deux hétérogénéités microstructurales critiques vis-à-vis de la FPH, ont été étudiées à une échelle plus locale dans la seconde partie du travail de thèse. Les essais ont été réalisés sur des échantillons modèles, chargés en hydrogène en milieu H2SO4 sous polarisation cathodique et la profondeur de pénétration de l’hydrogène a été évaluée par SKPFM (Scanning Kelvin Probe Force Microscopy). L’ensemble des résultats obtenus met en évidence : 1/ un effet « barrière » des précipités fins et des dislocations sur la diffusion de l’hydrogène en relation avec un abattement des propriétés mécaniques moins important, 2/ un transport possible de l’hydrogène par les dislocations et 3/ l’efficacité du SKPFM pour déterminer précisément des coefficients de diffusion apparents de l’hydrogène. Ces résultats ouvrent ainsi de nouvelles pistes vers la compréhension des mécanismes de CSC dans les alliages Al-Zn-Mg. / Automotive industry is increasingly affected by standards requiring a major cut of polluting emissions, leading R&D policies to focus on replacing steel by aluminum alloys. This thesis project, initiated by the manufacturer Constellium, focuses on 7xxx (Al-Zn-Mg) aluminum alloys known to have high mechanical properties but also to be susceptible to stress corrosion cracking (SCC) partly attributed to hydrogen embrittlement (HE). Understanding the mechanisms involved would be a first step towards a metallurgical optimization and a future industrialization of these alloys. The first part focuses on the SCC behavior of the 7046 aluminum alloy, related to its microstructure, and the identification of degradation mechanisms involved. A hydrogen amount – loss of mechanical properties relationship was highlighted. The damage observed was explained by the presence of hydrogen in the grain boundaries and by a trapping effect of the intragranular hardening precipitates, limiting the hydrogen diffusion to the grain boundaries. Interactions between hydrogen and hardening precipitates and dislocations, both identified as critical microstructural heterogeneities for HE, are studied at a local scale in a second part. The hydrogen effect was characterized by penetration depth measurements made by SKPFM (Scanning Kelvin Probe Force Microscopy) on “model” samples cathodically charged in H2SO4. The whole results finally highlight: 1/ a “shielding” effect of fine precipitates and dislocations on hydrogen diffusivity related to a lower susceptibility to HE, 2/ hydrogen transport by dislocations and 3/ the efficiency of SKPFM to precisely measure effective diffusion coefficients of hydrogen. These results lead to new opportunities to understand SCC mechanisms in Al-Zn-Mg alloys.

In most casting applications, dendritic microstructure morphology is not desired because it leads to poor mechanical properties. Forced convection causing sufficient shearing in the mushy zone of the partially solidified melt is one of the means to suppress this dendritic growth. The dendrites formed at the solid-liquid interface are detached and carried away due to strong fluid flow to form slurry. This slurry, consisting of rosette or globular particles, provides less resistance to flow even at a high solid fraction and can easily fill the die-cavity. The stated principle is the basis of a new manufacturing technology called “semi-solid forming” (SSF), in which metal alloys are cast in the semi-solid state. This technique has numerous advantages over other existing commercial casting processes, such as reduction of macrosegregation, reduction of porosity and low forming efforts. Among all currently available methods available for large scale production of semisolid slurry, the cooling slope is considered to be a simple but effective method because of its simple design and easy control of process parameters, low equipment and running costs, high production efficiency and reduced inhomogeneity. With this perspective, the primary objective of the present research is to investigate, both experimentally and numerically, convective heat transfer and solidification on a cooling slope, in addition to the study of final microstructure of the cast billets. Some key process parameters are identified, namely pouring temperature, slope angle, slope length, and slope cooling rate. A systematic scaling analysis is performed in order to understand the relative importance of the parameters in influencing the final properties of the slurry and microstructure after solidification. A major part of the present work deals with the development of an experimental set up with careful consideration of the range of process parameters involved by treating the cooling slope as a heat exchanger. Subsequently, a comprehensive numerical model is developed to predict the flow, heat transfer, species concentration solid fraction distribution of aluminum alloy melt while flowing down the cooling slope. The model uses a variable viscosity relation for slurry. The metal-air interface at the top during the melt flow is tracked using a volume of fluid (VOF) method. Solidification is modeled using an enthalpy based approach and a volume averaged technique. The mushy region is modeled as a multi-layered porous medium consisting of fixed columnar dendrites and mobile equiaxed or fragmented grains. In addition, the solidification model also incorporates a fragmentation criterion and solid phase movement. The effects of key process parameters on flow behavior involving velocity distribution, temperature distribution, solid fractions at the slope exit, and macrosegregation, are studied numerically and experimentally for aluminium alloy A356. The resulting microstructures of the cast billets obtained from the experiments are studied and characterized. Finally the experimental results are linked to the model predictions for establishing the relations involving interdependence of the stated key process parameters in determining the quality of the final cast products. This study is aimed towards providing the necessary guidelines for designing a cooling slope and optimizing the process parameters for desirable quality of the solidified product.

Les directives de l'Union Européenne conditionnent la R&D du secteur automobile concernant l'utilisation de matériaux plus légers ayant pour but de réduire la consommation de carburant et une diminution de l’émission de gaz d’échappement. L’objectif est de mettre au point des aciers allégés d’au moins 10% (ρmax ≈ 7g/cm3). Les alliages fer-aluminium possèdent des propriétés physiques et mécaniques prometteuses mais présentent des défauts de surface appelés roping, apparaissant après l’emboutissage à froid. Cette étude a consisté à mieux comprendre les conditions de recristallisation au cours du laminage à chaud afin de contrôler la microstructure et ainsi limiter ces défauts. Il est généralement admis, lors d’une déformation à chaud, que les alliages ferritiques, à haute énergie de défaut d’empilement, donnent lieu aux processus de recristallisation dynamique géométrique (RDG) et de recristallisation dynamique continue (RDC). Dans cette étude, l’existence d’une transition entre les mécanismes de RDC et de recristallisation dynamique discontinue (RDD) a été mise en évidence pour des températures comprises entre 900 et 1100°C et des vitesses de déformation comprises entre 0,1 et 50s 1. La recristallisation post dynamique a aussi été étudiée afin d’observer l’évolution de la microstructure lors de maintiens en température. Un modèle développé antérieurement pour la RDC de l’aluminium a ensuite été utilisé afin de simuler une passe de laminage. Bien que la comparaison des résultats expérimentaux et simulés fasse apparaître un certain nombre de différences, ce modèle permet de reproduire qualitativement les évolutions de la microstructure. / The instructions of the European Union pilot the R&D in the automotive industry regarding the use of lightweight materials which aims at reducing fuel consumption and emission of exhaust gases.The objective is to develop steels of density reduced by at least 10% (ρmax ≈ 7g/cm3). Iron aluminum alloys display promising physical and mechanical properties but they often exhibit surface defects, referred to as roping, appearing after the deep drawing process. This study was carried out to better understand the conditions of recrystallization during hot rolling to control the microstructure and thereby limit these defects.During hot deformation, it is generally agreed that geometric dynamic recrystallization (GDRX) and continuous dynamic recrystallization (CDRX) operate in ferritic alloys with high stacking fault energy. In this study, the existence of a transition between CDRX and the mechanism of discontinuous dynamic recrystallization (DDRX) has been brought into evidence in the temperature range 900 1100°C and strain rate range 0.1-50s-1. Post-dynamic recrystallization was also studied to observe the evolution of microstructure during holding temperatures.A model formerly developed for the CDRX of aluminum was then used to simulate a rolling pass. Comparison of computed and experimental results shows some differences but this model can reproduce microstructural changes qualitatively.

The aim of this thesis is to verify a possibility of controlling the crystallisation of aluminium alloys poured in shell moulds in order to achieve directional solidification. For this purpose, new cooling plant has been designed and fabricated. Several sample castings were produced under different initial conditions. Based on the evaluation of measured temperatures, a numerical simulation of heat transfer was created using the ProCAST software. Finally, the sample castings were sectioned into specimens that were, subsequently, metallographically polished and the evaluation of their structure with respect to the amount and types of defects was performed.