Sigurd Wenner

The effect of Zn on precipitation in Al–Mg–Si alloys

Effects of addition of Zn (up to 1 wt%) on microstructure, precipitate structure and intergranular corrosion (IGC) in an Al–Mg–Si alloys were investigated. During ageing at 185 °C, the alloys showed modest increases in hardness as function of Zn content, corresponding to increased number densities of needle-shaped precipitates in the Al–Mg–Si alloy system. No precipitates of the Al–Zn–Mg alloy system were found. Using high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), the Zn atoms were incorporated in the precipitate structures at different atomic sites with various atomic column occupancies. Zn atoms segregated along grain boundaries, forming continuous film. It correlates to high IGC susceptibility when Zn concentration is ~1wt% and the materials in peak-aged condition.

Phase stabilization principle and precipitate-host lattice influences for Al–Mg–Si–Cu alloy precipitates

In this work, we seek to elucidate a common stabilization principle for the metastable and equilibrium phases of the Al–Mg–Si–Cu alloy system, through combined experimental and theoretical studies. We examine the structurally known well-ordered Al–Mg–Si–Cu alloy metastable precipitates along with experimentally observed disordered phases, using high angle annular dark field scanning transmission electron microscopy. A small set of local geometries is found to fully explain all structures. Density functional theory based calculations have been carried out on a larger set of structures, all fully constructed by the same local geometries. The results reveal that experimentally reported and hypothetical Cu-free phases from the set are practically indistinguishable with regard to formation enthalpy and composition. This strongly supports a connection of the geometries with a bulk phase stabilization principle. We relate our findings to the Si network substructure commonly observed in all Mg–Al–Si(–Cu) metastable precipitates, showing how this structure can be regarded as a direct consequence of the local geometries. Further, our proposed phase stabilization principle clearly rests on the importance of metal-Si interactions. Close links to the Al–Mg–Si precipitation sequence are proposed.

Effect of room temperature storage time on precipitation in Al-Mg-Si(-Cu) alloys with different Mg/Si ratios

Abstract The effect of natural ageing time before artificial ageing has been investigated in four Al–Mg–Si(–Cu) alloys, with 0.4% Mg + 0.8% Si and 0.8% Mg + 0.4% Si, both with and without 0.14 at.% Cu. The precipitate microstructure was quantified by means of transmission electron microscopy. Varying the storage time before ageing for 170 min at 200°C, we observe an initial hardness increase after minutes, a decrease after several hours and another increase after weeks. The hardness decrease was most pronounced in the Mg-rich Cu-free alloy, caused by a reduced precipitate volume fraction. Adding Cu produces finer microstructures, higher hardness and reduces the negative effect of natural ageing regardless of the Mg/Si ratio of the alloy. With 1 week storage, an increase in the fraction of the Cu-containing precipitates L and Q′ was observed in the Cu-containing Si-rich and Mg-rich alloys respectively.

Optimising multi-frame ADF-STEM for high-precision atomic-resolution strain mapping

Annular dark-field scanning transmission electron microscopy is a powerful tool to study crystal defects at the atomic scale but historically single slow-scanned frames have been plagued by low-frequency scanning-distortions prohibiting accurate strain mapping at atomic resolution. Recently, multi-frame acquisition approaches combined with post-processing have demonstrated significant improvements in strain precision, but the optimum number of frames to record has not been explored. Here we use a non-rigid image registration procedure before applying established strain mapping methods. We determine how, for a fixed total electron-budget, the available dose should be fractionated for maximum strain mapping precision. We find that reductions in scanning-artefacts of more than 70% are achievable with image series of 20-30 frames in length. For our setup, series longer than 30 frames showed little further improvement. As an application, the strain field around an aluminium alloy precipitate was studied, from which our optimised approach yields data whos strain accuracy is verified using density functional theory.

Structural modifications and electron beam damage in aluminium alloy precipitate θ'–AL2

The –AlCu phase in an Al–4Zn–2Cu–1Mg–0.7Si (wt.%) alloy was investigated by means of scanning transmission electron microscopy. With our specific alloy composition, the phase is often formed with stacking faults on and planes. The stacking faults on planes are often regularly spaced and create a previously unreported superstructure. Structural damage by electron irradiation is observed, even at a low acceleration voltage of 80 kV. The damage is more pronounced in the precipitates with stacking faults, which agrees with theoretical calculations of knock-on scattering cross-sections. These two very different forms of disruptions of the structure are linked to its spacious interstitial sites and the ease at which Cu atoms diffuse into and between them.

Elemental electron energy loss mapping of a precipitate in a multi-component aluminium alloy.

The elemental distribution of a precipitate cross section, situated in a lean Al-Mg-Si-Cu-Ag-Ge alloy, has been investigated in detail by electron energy loss spectroscopy (EELS) and aberration corrected high angle annular dark field scanning transmission electron microscopy (HAADF-STEM). A correlative analysis of the EELS data is connected to the results and discussed in detail. The energy loss maps for all relevant elements were recorded simultaneously. The good spatial resolution allows elemental distribution to be evaluated, such as by correlation functions, in addition to being compared with the HAADF image. The fcc-Al lattice and the hexagonal Si-network within the precipitates were resolved by EELS. The combination of EELS and HAADF-STEM demonstrated that some atomic columns consist of mixed elements, a result that would be very uncertain based on one of the techniques alone. EELS elemental mapping combined with a correlative analysis have great potential for identification and quantification of small amounts of elements at the atomic scale.

μSR study of Al-0.67%Mg-0.77%Si alloys

Zero-field muon spin relaxation measurements were carried out with Al-0.67%Mg- 0.77%Si alloys in the temperature range from 20 K to 300 K. Observed relaxation spectra were compared with the relaxation functions calculated by a Monte Carlo simulation with four fitting parameters: the dipolar width, trapping rate, detrapping rate and fraction of initially trapped muons. From the fitting, the temperature variations of the trapping rates reveal that there are three temperature regions concerning muon kinetics. In the low temperature region below 120 K, muons appeared to be trapped in a shallow potential yielded by dissolved Mg atoms, and thus little effect of heat treatment of the samples was observed, while in the mid and high temperature regions, the trapping rates clearly depended on the heat treatment of the samples suggesting muon-cluster and/or muon-vacancy interactions.

Thermal migration of alloying agents in aluminium

The in situ thermal migration of alloying agents in an Al–Mg–Si–Li alloy is studied using surface sensitive photo-electron and electron diffraction/imaging techniques. Starting with the preparation of an almost oxide free surface (oxide thickness = 0.1 nm), the relative abundance of alloying agents (Mg, Li and Si) at the surface are recorded at various stages of thermal annealing, from room temperature to melting (which is observed at 550 ◦C). Prior to annealing, the surface abundances are below the detection limit 1%, in agreement with their bulk concentrations of 0.423% Si, 0.322% Mg and 0.101% Li (atomic %). At elevated temperatures, all three alloying agents appear at drastically increased concentrations (13.3% Si, 19.7% Mg and 45.3% Li), but decrease again with further elevation of the annealing temperature or after melting. The temperature at which the migration occurs is species dependent, with Li migration occurring at significantly higher temperatures than Si and Mg. The mechanism of migration also appears to be species dependent with Li migration occurring all over the surface but Mg migration being restricted to grain boundaries.

Atomic-Resolution Elemental Mapping of Precipitates in a 7449 Aluminium Alloy

The high-strength weldable 7xxx series of aluminium alloys are of great importance to the aeronautics industry. Only recently, the complex structures of the AlZnMg hardening precipitates have been solved by HAADFSTEM imaging and first-principles calculations. However, perfect models of precipitate structures are often insufficient as several elements may be mixed into precipitate compositions. We have investigated this effect by STEMEELS spectrum imaging with an aberration-corrected microscope. In a 7449 alloy, Cu and Al were found to replace atoms at certain sites in both metastable and equilibrium ZnMg precipitates.

Precipitate statistics in an Al-Mg-Si-Cu alloy from scanning precession electron diffraction data

The key microstructural feature providing strength to age-hardenable Al alloys is nanoscale precipitates. Alloy development requires a reliable statistical assessment of these precipitates, in order to link the microstructure with material properties. Here, it is demonstrated that scanning precession electron diffraction combined with computational analysis enable the semi-automated extraction of precipitate statistics in an Al-Mg-Si-Cu alloy. Among the main findings is the precipitate number density, which agrees well with a conventional method based on manual counting and measurements. By virtue of its data analysis objectivity, our methodology is therefore seen as an advantageous alternative to existing routines, offering reproducibility and efficiency in alloy statistics. Additional results include improved qualitative information on phase distributions. The developed procedure is generic and applicable to any material containing nanoscale precipitates.