Neste estudo foi avaliada a resistência à corrosão da liga 2024-T3 clad, anodizada em solução de ácido tartárico-sulfúrico (TSA) e pós-tratada em banhos contendo íons de cério (Ce(NO3)3) sem e com H2O2. O pós-tratamento visa aumentar a resistência à corrosão e conferir propriedades de auto regeneração à camada anodizada, sem, no entanto, causar o fechamento dos poros, mantendo assim as propriedades de adesão. Foram avaliados os efeitos da temperatura, do tempo de imersão e da porcentagem de H2O2 no banho de pós-tratamento sobre a microestrutura e resistência à corrosão. As observações por microscopia eletrônica de varredura (MEV) mostraram que não houve fechamento dos poros e que ocorre precipitação preferencial de oxihidróxidos de Ce nas proximidades dos defeitos da camada. A avaliação da resistência à corrosão em solução de NaCl 0,1 e 0,5 mol/L por espectroscopia de impedância eletroquímica (EIS) mostrou que a etapa de pós-tratamento em solução contendo 50 mM de Ce(NO3)3.6H2O e 10% vol. de H2O2 melhora o desempenho da camada, com o melhor resultado tendo sido obtido para a temperatura intermediária (50°C) de pós-tratamento. Os resultados dos ensaios de EIS mostraram também efeito negativo de altas temperaturas no pós-tratamento nas propriedades protetoras da camada anodizada. Esses resultados foram confirmados por fotos digitais e observação SEM das amostras após a conclusão dos experimentos de EIS. Já a caracterização composicional por meio de GDOES mostrou a incorporação de espécies de Ce dentro dos poros da camada anodizada após pós-tratamentos em solução contendo 50 mM de Ce(NO3)3.6H2O e 10% vol. H2O2 a 50°C para tempos de imersão de 2 e 5 minutos, resultados confirmados com a técnica RBS, que mostrou ainda a presença de Ce na superfície da camada e no interior dos poros mesmo após 15 dias de imersão em NaCl 0,1M. Medições de XPS mostraram que o Ce está presente na superfície das amostras nos estados de oxidação 3+ e 4+, e uma maior relação Ce3+/Ce4+ para as amostras pós-tratadas por 2 minutos. O ajuste dos diagramas de EIS com circuitos equivalentes mostrou que a selagem parcial dos poros tem papel importante na resistência à corrosão, e evidenciaram que os pós-tratamentos mais eficientes não afetam as propriedades protetoras da camada barreira. / This study evaluated the corrosion resistance of a 2024-T3 clad alloy anodized in tartaric-sulfuric acid solution (TSA) and post-treated in baths containing cerium ions, without or with H2O2. The post-treatment aims to increase the corrosion resistance and afford self-healing properties to the anodized layer, without, however, closing its porous structure, thus maintaining its adhesion properties. The effects of the temperature, immersion time and concentration of H2O2 in the post-treatment bath in the microstructure and in the corrosion resistance of the samples were evaluated. SEM observations showed that pores are not blocked and that preferential precipitation of Ce occurs in the vicinity of defective sites of the anodized layer. The evaluation of the corrosion resistance in 0.1 and 0.5 mol/L NaCl solution by means of electrochemical impedance spectroscopy (EIS) showed that the post-treatment in solutions containing 50 mM of Ce(NO3)3.6H2O and 10% vol. of H2O2 improves the corrosion resistance of the anodized samples, with the best result being obtained for the intermediary temperature (50°C) of the post-treatment bath. The results of the EIS tests also showed a negative effect of higher temperatures on the protective properties of the anodized layer. Digital photos and SEM observation of the samples after the completion of the EIS experiments confirmed these results. The compositional characterization by GDOES showed the incorporation of Ce species within the pores of the anodized layer after post-treatments in solution containing 50 mM Ce (NO3)3.6H2O and 10% vol. H2O2 at 50°C for 2 and 5 minutes, confirmed by the RBS technique, which also showed the presence of Ce both at the surface and within the pores of the layer, even after 15 days of immersion in 0.1M NaCl. XPS measurements showed the presence of Ce3+ and Ce4+ species at the post-treated samples surface and showed higher Ce3+ / Ce4+ ratio for the sample post-treated for 2 minutes. Fitting of the EIS diagrams with equivalent circuits showed that partial pore sealing plays an important role in corrosion resistance and evidenced that the most efficient post-treatments do not affect the protective properties of the barrier layer.

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Pour les structures aéronautiques, les zones sensibles à la corrosion sont principalement celles où le plan de protection de la structure peut être mis en défaut, comme à l’intérieur des joints de recouvrement (dénommé «lap joint» en anglais). Les assemblages de tôles métalliques réalisés par recouvrement en utilisant, par exemple le rivetage, peuvent présenter des défauts de contact et donc il peut exister un interstice entre les deux parties de l’assemblage. En général cet interstice est isolé de l’environnement extérieur par un mastic. Mais il y a un risque de piégeage d’humidité plus ou moins concentrée en ions agressifs qui peut provoquer des endommagements ou aggraver ceux initiés sur des défauts des revêtements. Le premier objectif de cette thèse est de développer une méthodologie permettant de reproduire, de manière contrôlée et de façon la plus représentative de cas réels, la corrosion d’un alliage d’aluminium 2024-T3 constituant un joint de recouvrement afin d’effectuer des observations complétées par des mesures chimiques et électrochimiques. Le deuxième objectif est de tester l’application de modèles de transport réactif (en milieu confiné) pour voir s’il est possible de simuler les réponses (chimiques ou électrochimiques) mesurées expérimentalement et donc de prédire sur le long terme l’évolution d’un assemblage. / For aircraft structures, corrosion sensitive areas are mainly those where the protection of the structure may suffer local breakdowns, as encountered inside lap joints. The assemblies of metal plates by overlapping (riveting) may present some defects in contact and consequently a gap can exist between the two parts of the assembly. Typically this gap is isolated from the outside environment by a sealant. But there is a risk of trapping of moisture more or less concentrated in aggressive ions which can induce corrosion or increase the damages initiated on coating defects. The first objective of this thesis is to develop a methodology to reproduce in a controlled manner and in the most representative way regarding actual cases, the corrosion of a lap joint made of aluminum alloy 2024- T3 plates, to perform not only observations but also chemical and electrochemical measurements. The second objective is to test the application of reactive transport models (in confined media) to check if it is possible to simulate the chemical or electrochemical changes recorded during experiments and thus to predict the long-term evolution of lap-joint in humid environment.

Manufacturing of aircraft parts is often complex and time-consuming, which has led to an increased interest in new manufacturing technologies in the Swedish industry such as additive manufacturing (AM). Additive manufacturing techniques could be a solution to meet the aircrafts’ demand since it contributes to an efficient manufacturing and allows a just-in-time production of complex metal parts in their final shape. However, the use of AM aluminum for aircraft applications is in a development phase and no surface treatment process exists. Thereby, it is of high interest to further investigate surface treatments for AM alloys. Currently at Saab AB, conventional aluminum alloys are generally anodized in tartaric sulphuric acid (TSA) to improve the corrosion resistance and adhesion properties of the metal. On the behalf of Saab AB, there is also an interest in establishing powder coating as a surface treatment. This master thesis’ purpose is to investigate the anodizing and adhesion properties for the two additive manufacturing alloys - AlSi10Mg and ScalmalloyⓇ, and compare it with the conventionally produced Al alloy 2024-T3. The anodization and the powder coating is examined by using following characterization techniques: profilometry, light microscopy, scanning electron microscopy and contact angle measurements. The results from the experimental part indicated successful anodizations for all the alloys and good adhesion properties for powder coating. This research is a first step in contributing to a better understanding of the anodic coating and adhesion properties for the AM samples ScalmalloyⓇ and AlSi10Mg

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Les couches de conversion actuellement utilisées dans l'industrie aéronautique, pour protéger le métal de la corrosion et favoriser l'adhérence de la peinture, contiennent du chrome hexavalent, composé toxique et cancérigène dont l'utilisation va prochainement être interdite par la réglementation européenne REACh. L'une des pistes envisagée pour remplacer ces couches chromatées est l'utilisation de couches de conversion TCP (Trivalent Chromium Protection). Ces travaux portent sur l'étude des couches de TCP et s'attachent à caractériser chaque étape du traitement de surface industriel, incluant les étapes de prétraitement et de post-traitement. Des techniques d'analyse de surface (XPS, ToF-SIMS, AFM, MEB et PM-IRRAS) ont été utilisées pour analyser la composition chimique et la morphologie de la surface après chaque étape du traitement. Cette étude a été réalisée sur un alliage d'aluminium AA 2024-T3, très utilisé en aéronautique pour ses propriétés mécanique, mais présentant une faible résistance à la corrosion. Les résultats obtenus ont notamment mis en évidence que la couche de TCP se forme sur toute la surface de l'alliage (composés intermétalliques et cavités), et ont permis de comprendre comment le post-traitement permet d'améliorer la résistance à la corrosion de la couche de TCP. Ces travaux s'intéressent également à des couches de conversion sans chrome, à base de zirconium, étudiées ici pour servir de point de départ au développement d'une conversion sans chrome qui respecterait les exigences de résistance à la corrosion. / Conversion coatings are used in aerospace industry to protect the metal from corrosion and to promote paint adhesion. Currently, chromate conversion coatings are used, but chromate is toxic and carcinogenic and its use will be forbidden by the European REACh regulation. TCP (Trivalent Chromium Protection) conversion coatings, are considered as a promising alternative to replace chromate conversion coating. This work focuses on the characterisation of the TCP layer and considers each step of the industrial surface treatment, including pre-treatment and post-treatment steps. Surface analytical techniques (XPS, ToF-SIMS, AFM, SEM and PM-IRRAS) were used to analyse the chemical composition and morphology of the surface after each step in the process. This work was done on an aluminium alloy AA 2024-T3, commonly used in the aerospace industry for its good mechanical properties, but poorly resistant to corrosion. The results obtained demonstrate, among other things, that the TCP layer totally covers the surface (intermetallic compounds and cavities) and enable to understand how the post-treatment can improve the corrosion resistance of the TCP coating. This work also focuses on conversion coating based on zirconium, which are studied here to be used as a starting point to develop a new conversion coating without chromium, meeting the corrosion resistance requirement.

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