Doctor of Philosophy (PhD) / The evolution of atomistic-level nanostructure during the early stages of both standard, high-temperature T6 heat treatment, and low-temperature secondary ageing after interruption of the former (T6I4), has been investigated in rapid hardening Al-Cu-Mg alloys using a variety of microscopy and microanalytical techniques, including transmission electron microscopy (TEM), positron annihilation spectroscopy (PAS) and atom probe tomography (APT). In order to carry out this objective, quantitative data-analysis methods were developed with respect to new cluster-finding algorithms, specifically designed for use with three-dimensional APT data. Prior to this detailed characterisation work, the actual thermal impact from both heat treatment and quenching of small, lab-scale specimens was determined through correlation of both experimental results and calculations that modelled the heat transfer conditions using the lumped capacitance method. Subsequently, the maximum diffusion distance by random walk of the solute atoms was calculated for these periods, bearing significance on the propensity for these atoms to have the ability to cluster together, rather than segregate to the dislocation loops in the microstructure, which have a relatively larger interspacing distance. Age-hardening curves for the Al-1.1Cu-xMg (x = 0, 0.2, 0.5, 0.75, 1.0, 1.7 at.%) alloys at 150ºC show that the rapid hardening phenomenon (RHP) exists for Mg compositions ≥ 0.5Mg. Given that zone-like precipitate structures were unable to be detected by TEM or APT during the early stages of ageing at 150ºC, and that statistically significant dispersions of clusters were found in the APT data after ageing for 60 s, the RHP is attributed to these clustering reactions. Identification of clusters in the APT data has been achieved using the core-linkage algorithm and they have been found to be quite small, containing only a few atoms up to a couple of tens of atoms. The RHP is governed by some critical number density of both Mg clusters and Cu-Mg co-clusters of a critical size, whereas Cu clusters do not contribute significantly to the hardening mechanism. Significance testing indicates that Mg clusters are more significant at smaller clusters sizes and Cu-Mg co-clusters more important at larger cluster sizes. Hardness results also confirm the existence of rapid early hardening during secondary ageing at 65ºC in Al-1.1Cu-1.7Mg. The mechanism of secondary rapid hardening involves a combination of both secondary clustering from solute (mainly Mg atoms) residual in solution, and pre-existing amorphous primary clusters that have slower growth kinetics at the lower secondary ageing temperature. The latter occurs mainly by vacancy-assisted diffusion of Mg atoms as evidenced by the gradual increase of the Mg:Cu ratio of co-clusters. From an alloy design point of view it is important to fully understand the solute distribution in the microstructure to be able to subsequently optimise the configuration for enhanced material properties. The change in dispersion of solute atoms during ageing was determined by combining calculations of % vacancy-solute associations with detailed measurements of the dislocation loops to estimate the solute distribution within the microstructure. The implication of the balance of solute atoms segregated to the loops compared with that in the matrix is then discussed in the context of hardnening mechanisms.

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Three aluminium alloys from AA3003 series modified by zirconium were pre- pared by twin-roll casting. The role of composition, heat treatment and deforma- tion by cold-rolling or equal channel angular pressing on evolution of microstruc- ture and mechanical properties were studied. High density of α-Al(Mn,Fe)Si pre- cipitates formed during annealing between 300 ◦ C and 500 ◦ C. Coherent Al3Zr particles precipitated during annealing at 450 ◦ C with slow heating rate. Recrys- tallization resistance of deformed alloys was enhanced by either Al3Zr precipitates formed before deformation or by α-Al(Mn,Fe)Si particles nucleating simultane- ously with recrystallization. 1

Le soudage par faisceau d’électrons d’alliages à durcissement structural de la série7xxx induit des modifications importantes de leur microstructure, et par conséquent de leur comportement mécanique. Cette étude visait à formuler une loi de comportement incluant l’endommagement de structures soudées par une approche locale de la rupture. Pour cela, la microstructure de la soudure et les propriétés mécaniques résultantes sont caractérisées. Le lien est fait entre la distribution de précipités fins et les propriétés plastiques, ainsi qu’entre la précipitation grossière et les micromécanismes d’endommagement. Le modèle aux éléments finis proposé prend en compte le comportement plastique des différentes zones et reproduit le comportement en endommagement de la zone fondue, qui constitue le maillon faible de la structure à cause de l’évaporation d’éléments d’alliages durant le soudage. Ce modèle a été validé dans une gamme étendue de sollicitations mécaniques (géométrie,entaille). / The electron beam welding of 7xxx series alloys leads to modification of their microstructureand consequently of their mechanical behavior. This study aimed toformulate a constitutive law including damage for welded structures by a local approachof fracture. For this purpose, the weld microstructure and the resulting mechanicalproperties have been characterized. The relationship between fine scaleprecipitate distribution and plastic properties has been established, as well as therelationship between coarse precipitation and micro-mechanisms of damage. Thefinite elements model takes into account the plastic behavior of the different zonesand reproduces the damage behavior of the fusion zone, which is the weakest linkof the structure due to evaporation of alloying elements during welding. This modelhas been validated in a large variety of stress conditions (sample geometry, notch).

La décomposition de solutions solides sursaturées d'alliages multiconstitués Al-Cu- (Li, Mg) pose des défis théoriques et expérimentaux. La formation de fluctuations chimiques à température ambiante est analysée de façon critique en utilisant une combinaison de diffusion centrale (SAS), de calorimétrie différentielle à balayage (DSC), de sonde atomique tomographique (APT) et de micro-dureté. Une méthodologie pour l'interprétation combinée de données SAS d'expériences utilisant des neutrons et des rayons X est proposée et permet une comparaison avec les données de sonde atomique. Les résultats donnent la chimie et les dimensions sub-nanométriques des amas. L'effet du Mg sur les cinétiques de vieillissement naturel est discuté dans le contexte de son interaction avec les lacunes disponibles pour la diffusion. De courts traitements isothermes à températures relativement basses sont utilisés pour dissoudre les amas présents après vieillissement naturel et obtenir une solution solide avec moins de lacunes qu’après mise en solution. Lorsque du Mg est présent dans le système Al-Cu-Li, le soluté libéré après dissolution se regroupe avec une cinétique comparable à celle obtenue immédiatement après la trempe du traitement de mise en solution. L'augmentation immédiate de la cinétique de mise en amas quand une concentration quelconque de Mg est présente dans les alliages Al-Cu- (Li, Mg) est révélée avec couple de diffusion. / Decomposition of super saturated solid solutions of Al-Cu-(Li,Mg) alloys pose theoretical and experimental challenges. The chemical fluctuations - clusters - formed at room temperature are critically analysed using a combination of in-situ small angle scattering (SAS), differential scanning calorimetry (DSC), atom probe tomography (APT), and micro-hardness. A methodology for combined interpretation of SAS data from experiments using neutron and X-ray radiation is proposed and allows for comparison with standard analysis performed by APT. The results effectively capture the chemistry and sub-nanometer dimensions of clusters. The profound positive effect of Mg on clustering of Cu via excess vacancies available for diffusion is captured through the clustering kinetics over the course of natural ageing. Short isothermal treatments at relatively low temperatures are used to dissolve naturally aged clusters and obtain a solid solution with less expected vacancies. When Mg is present in the Al-Cu-Li system, released solute after dissolution exhibits clustering behaviour with kinetics comparable to those immediately after quench from solution treatment. The immediate increase of clustering kinetics when any concentration of Mg is present in Al-Cu-(Li,Mg) alloys is revealed through a composition graded sample.

The fatigue of materials and structures is a phenomenon in which surface condition plays an important role; specially in initiating the micro-cracks. Moreover, the structural components are also subjected to aggressive environments and hence are susceptible to corrosion phenomenon. Therefore, it is necessary to protect them against the corrosion phenomenon. For aluminium alloys used in aeronautical applications, anodization is widely used surface treatment to increase the corrosion resistance. Despite the benefits obtained in terms of enhanced corrosion resistance, the anodizing process has a damaging effect on the fatigue performance of the base material. One of the reasons for this decrease in fatigue life is associated to the degradation of surface condition during the anodizing process. In this work, we have studied the influence of machining and anodization on fatigue behaviour of aluminium alloys 2214 and 7050. We showed experimentally that for 2214 alloy the process of anodization-sealing reduced the fatigue life considerably while for 7050 alloy the process of pickling is the major cause in decreasing the fatigue life. We have also developed life prediction model for anodized alloys. The model is based on determination of concentration of stress ‘Kt’ generated by the surface condition. The developed model integrates the aspects of multi-site initiation, coalescence and regime of short crack propagation.

The desire to reduce weight in automotive products is driven by a need to improve efficiency. As such, to allow further weight reduction, higher performance aluminium alloys are in demand for sheet metal body structures. Due to their high strength to weight ratio 7xxx alloys are seen as an ideal candidate for this, however their use to date has been limited by poor formability. Previous work indicated that by moving to high temperatures (>350°C) or by using a soft temper (W), good formability could be achieved but the samples required further heat treatment post-forming. This work explored the warm forming temperature range to improve formability whilst developing the required properties during processing. The performance of a 7xxx candidate alloy, 7021, has been assessed in stretching and drawing operations, both at room temperature and over the elevated temperature range of 150-250°C. The microstructure and other properties of the alloy were investigated in W, T4 and T6 tempers, before and after testing, through a range of techniques, including DSC, DMTA, SEM, EBSD and TEM.In the T4 temper, UTS and proof stress increased with temperature up to 190°C, due to dynamic precipitation. Increasing temperature only provided a modest increase in strain to failure for both the T4 and T6 temper. Cup height was not significantly improved in the warm forming temperature range during Erichsen cup testing. By deep drawing at 250°C it was possible to fully draw a cup (with an LDR of 2.2) in both the T4 and T6 temper of 7021, with both tempers having comparable post-forming hardness. This indicates that at 250°C the starting condition has no impact on drawability. Although full drawability is achieved at 250°C the final product would require further heat treatment if it were to replace 6016. However, by deep drawing 7021-T4 at 190°C, a fully formed cup was produced with a hardness between that of the T4 and T6 temper. The microstructure of the formed cup showed no grain boundary precipitation and a fine distribution of the strengthening phase η', suggesting there is a dynamic effect on the precipitation during deep drawing at this temperature. In conclusion, the work has shown that warm forming does not significantly improve stretching behaviour of 7021, but by using warm forming temperatures deep drawing is improved.

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