[en] The interaction mechanisms between dislocations and semi-coherent, needle-shaped β′ precipitates in Al–Mg–Si alloys have been studied by High Resolution Transmission Electron Microscopy (HRTEM). Dislocation loops appearing as broad contrast rings around the precipitate cross-sections were identified in the Al matrix. A size dependency of the interaction mechanism was observed; the precipitates were sheared when the longest dimension of their cross-section was shorter than approximately 15 nm, and looped otherwise. A more narrow ring located between the Al matrix and bulk β′ indicates the presence of a transition interface layer. Together with the bulk β′ structure, this was further investigated by High Angle Annular Dark Field Scanning TEM (HAADF-STEM). In the bulk β′ a higher intensity could be correlated with a third of the Si-columns, as predicted from the published structure. The transition layer incorporates Si columns in the same arrangement as in bulk β′, although it is structurally distinct from it. The Z-contrast information and arrangement of these Si-columns demonstrate that they are an extension of the Si-network known to structurally connect all the precipitate phases in the Al–Mg–Si(–Cu) system. The width of the interface layer was estimated to about 1 nm. - Highlights: ► β′ is found to be looped at sizes larger than 15 nm (cross section diameter). ► β′ is found to be sheared at sizes smaller than 15 nm (cross section diameter). ► The recently determined crystal structure of β′ is confirmed by HAADF-STEM. ► Between β′ and the Al-matrix a transition layer of about 1 nm is existent. ► The β′/matrix layer is structurally distinct from bulk β′ and the aluminium matrix.

[en] The formation of the equilibrium precipitation phase during ageing treatment of Al-Mg-Si alloys is preceded by a series of metastable phases. Given longer ageing time, higher ageing temperature or elevated temperature service condition, β″, the main hardening phase, would be replaced by the more stable metastable phases such as β′, B′, U1 and U2. The post-β″ microstructure evolution, called “over-ageing”, leads to a steep drop in the hardness evolution curve. This paper aims to predict directly over-ageing in Al-Mg-Si alloys by extending a CALPHAD-coupled Kampmann-Wagner Numerical (KWN) framework towards handling the coexistence of several different types of stoichiometric particles. We demonstrate how the proposed modeling framework, calibrated with a limited amount of experimental measurement data, can aid in understanding the precipitation kinetics of a mix of different types particles. Simulation results are presented with some earlier reported transmission electron microscopy measurements [1,2] to shed light on how the alloy composition and ageing treatment influence the post- β″ phase selection.

[en] Precipitates in Al-Mg-Si alloys with Cu addition (∼0.1 wt%) and Zn addition (∼1 wt%) were investigated by aberration corrected high angle annular dark field scanning transmission electron microscopy (HAADF-STEM). Most precipitates had no overall unit cell but contained ordered network of Si atomic columns for both the Cu and the Zn containing precipitates. It was found that both Cu and Zn atomic columns are located at specific sites and producing characteristic local configurations on the Si atomic columns

[en] Solute atom nanoscale precipitates are responsible for the favourable mechanical properties of heat treatable aluminium alloys such as Al-Mg-Si (6xxx). The shape, structure and strengthening properties of age-hardening precipitates depend on alloy composition and thermo-mechanical history. We seek an improved understanding of the physics related to nucleation and precipitation on the atomistic level in these alloys. Once these mechanisms are sufficiently well described and understood, the hope is that 'alloy design' simulations can assist tailoring of materials with desired properties. In pure Al-Mg-Si we have determined the structure of nearly all the known metastable precipitate phases, by combining advanced TEM techniques (such as high resolution TEM and nano-beam diffraction) with atom probe tomography and density functional theory. We are now studying effects of additions /substitutions of Cu, Ag and/or Ge that promote formation of more disordered precipitates, employing aberration corrected high angle annular dark field scanning TEM. We find that all metastable precipitates contain variations of a widely spaced 'Si/Ge network'. In spite of disorder or defects, this network is surprisingly well ordered, with hexagonal projected sub-cell dimensions a = b ≅ 0.4 nm and c (along the fully coherent precipitate main growth direction) equal to 0.405 nm or a multiple of it.

[en] We have investigated the effect on precipitate microstructure and hardness upon adding small amounts of Ca to a base Al–Mg–Si alloy. The main investigative techniques were transmission and scanning electron microscopy. We found that large Ca-containing particles with composition CaAl₂Si₂ form during the production stages of the alloy. The particles leave less Si available in solid solution for the nucleation of hardening precipitates, leading to a coarser microstructure consisting of less coherent precipitates. The resulting hardness decrease is measurable for alloys containing more than 60 at ppm of Ca

[en] Highlights: • Isothermal ageing and unconventional thermomechanical processing are compared. • >2%IACS improvement in conductivity obtained using unconventional thermomechanical processing. • Transmission electron microscopy and atom probe tomography show different precipitate distributions after deformation. • Conductivity increase linked to reduced solute levels in the Al matrix. • Matrix solute level is the main factor determining conductivity. This work has examined an Al-0.54Mg-0.38Si (at.%) conductor alloy (6101) subjected to two different thermomechanical processing routes. Conventional solution treatment, quenching, and artificial ageing (170 °C) was compared to a process applying solution treatment, quenching, pre-ageing (7 h at 170 °C), 50% thickness reduction by cold-rolling, and re-ageing at 170 °C. Re-ageing after rolling caused a rapid increase in electrical conductivity. After 2 h re-ageing the rate of change in conductivity had slowed to a level comparable to that of the undeformed material after the same total ageing time. From this point on the deformed material maintained a 2–3%IACS gain in conductivity with further ageing. It is shown that the improvement in conductivity could largely be explained by two precipitate formation mechanisms, leading to increased solute depletion of the Al matrix in the deformed material, which was quantified by atom probe tomography. Clear differences between the deformed and undeformed material were also seen in precipitate distributions as shown by transmission electron microscopy results. The findings and the discussion presented are of importance to future alloy and process development for Al alloy conductor materials.

[en] Muon spin relaxation has the unique ability to detect very low concentrations of vacancies and vacancy–solute complexes in solids. In this work, we investigate quaternary Al-Mg-Si-Cu alloys and show that after quenching to room temperature from 848 K (575 °C), vacancies gradually become incorporated into clusters in the Al matrix. The total amount of vacancies in the material increases as small vacancy-rich clusters are formed, which is the opposite of the behavior in Cu-free Al-Mg-Si alloys.

[en] It is shown how size distributions of arbitrarily oriented, convex, non-overlapping particles extracted from conventional transmission electron microscopy (TEM) images may be determined by a variation of the Schwartz-Saltykov method. In TEM, particles cut at the surfaces have diminished projections, which alter the observed size distribution. We represent this distribution as a vector and multiply it with the inverse of a matrix comprising thickness-dependent Scheil or Schwartz-Saltykov terms. The result is a corrected size distribution of the projections of uncut particles. It is shown how the real (3D) distribution may be estimated when particle shape is considered. Computer code to generate the matrix is given. A log-normal distribution of spheres and a real distribution of pill-box-shaped dispersoids in an Al-Mg-Si alloy are given as examples. The errors are discussed in detail

[en] Aberration-corrected scanning transmission electron microscopy combined with electron energy loss spectroscopy has been used to determine the distribution of Cu and Ag atomic columns of precipitates in an Al–Mg–Si–Cu–Ag alloy. Cu columns were commonly part of C and Q′ phases, with the atomic columns having large projected separations. Columns containing Ag were more tightly spaced, in areas lacking repeating unit cells and at incoherent precipitate–host lattice interfaces. Cu-rich and Ag-rich areas were not found to intermix

[en] Highlights: • Significant differences in strength and ductility measured in alloys of similar alloying additions. • Material strength correlated well with a refinement of the precipitate microstructure. • Differences in ductility first appeared after moderate overageing of the alloys. • A large body of data on precipitate statistics and mechanical properties are presented. • Testing of three strengthening models, one showing excellent agreement with experiments. The mechanical properties of age hardenable Al alloys depend strongly on the precipitate microstructure. This work has investigated the relationship between properties such as strength and ductility and the distribution of precipitates, using three Al-Mg-Si(-Cu) alloys (Cu$\lesssim$0.1 at.%). A range of ageing conditions was examined in order to understand the effect of an evolving precipitate microstructure, and the results were used as input for strengthening models. The mechanical properties were obtained by tensile tests and microstructure characterisation was attained by transmission electron microscopy. The results showed that minor changes to the Si, Mg, and Cu additions – the total addition (at.%) kept approximately equal – had a significant impact on material properties, with corresponding changes in the precipitate microstructure. On the peak strength plateaus differences as large as 35 MPa in yield strength were measured between the strongest and the weakest alloy, obtained as 410 MPa and 375 MPa, respectively. Higher material yield strength correlated well with a refined precipitate microstructure comprising higher number densities of smaller precipitates. Differences with respect to material ductility first appeared after moderate overageing of the alloys, showing negative correlation with material strength. At significantly overaged conditions the differences in strength exceeded 100 MPa, demonstrating large differences with respect to the thermal stability of these materials, which has important consequences for alloys exposed to elevated temperatures under in-service conditions. The highly comprehensive body of data presented here should serve as a valuable reference in the development of precipitation and strengthening models for the Al-Mg-Si-Cu system and will hopefully incite further investigations on the topics covered.