The evolution of precipitate crystal structures in an Al-Mg-Si(-Cu) alloy studied by a combined HAADF-STEM and SPED approach

This work presents a detailed investigation into the effect of a low Cu addition (0.01 at.%) on precipitation in an Al-0.80Mg-0.85Si alloy during ageing. The precipitate crystal structures were assessed by scanning transmission electron microscopy combined with a novel scanning precession electron diffraction approach, which includes machine learning. The combination of techniques enabled evaluation of the atomic arrangement within individual precipitates, as well as an improved estimate of precipitate phase fractions at each ageing condition, through analysis of a statistically significant number of precipitates. Based on the obtained results, the total amount of solute atoms locked inside precipitates could be approximated. It was shown that even with a Cu content close to impurity levels, the Al-Mg-Si system precipitation was significantly affected with overageing. The principal change was due to a gradually increasing phase fraction of the Cu-containing Q'-phase, which eventually was seen to dominate the precipitate structures. The structural overtake could be explained based on a continuous formation of the thermally stable Q'-phase, with Cu atomic columns incorporating less Cu than what could potentially be accommodated.Comment: 13 pages, 10 figures, 2 table

Stress Corrosion Cracking in an Extruded Cu-Free Al-Zn-Mg Alloy

Stress corrosion cracking (SCC) in Cu-free Al-Zn-Mg (7xxx) aluminium alloys limits its use in many applications. In this work, we study in detail the microstructure of a peak and slightly overaged condition in an AA7003 alloy using transmission- and scanning electron microscopy in order to provide a comprehensive understanding of the microstructural features related to SCC. The SCC properties have been assessed using the double cantilever beam method and slow strain rate tensile tests. Grain boundary particles, precipitate free zones, and matrix precipitates have been studied. A difference in the SCC properties is established between the two ageing conditions. The dominating difference is the size and orientation of the hardening phases. Possible explanations correlating the microstructure and SCC properties are discussed.</jats:p

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 hightemperature regions, the trapping rates clearly depended on the heat treatment of the samples suggesting muon-cluster and/or muon-vacancy interactions

Bonding in MgSi and AlMgSi Compounds Relevant to AlMgSi Alloys

The bonding and stability of MgSi and AlMgSi compounds relevant to AlMgSi alloys is investigated with the use of (L)APW+(lo) DFT calculations. We show that the $\beta$ and $\beta''$ phases found in the precipitation sequence are characterised by the presence of covalent bonds between Si-Si nearest neighbour pairs and covalent/ionic bonds between Mg-Si nearest neighbour pairs. We then investigate the stability of two recently discovered precipitate phases, U1 and U2, both containing Al in addition to Mg and Si. We show that both phases are characterised by tightly bound Al-Si networks, made possible by a transfer of charge from the Mg atoms.Comment: 11 pages, 30 figures, submitted to Phys. Rev.

Atomic Structure of Hardening Precipitates in Al-Mg-Si Alloys: Influence of Minor Additions of Cu and Zn

Shifting toward sustainability and low carbon emission necessitates recycling. Aluminum alloys can be recycled from postconsumer scrap with approximately 5% of the energy needed to produce the same amount of primary alloys. However, the presence of certain alloying elements, such as copper and zinc, as impurities in recycled Al-Mg-Si alloys is difficult to avoid. This work has investigated the influence of tiny concentrations of Cu (0.05 wt %) and Zn (0.06 wt %), individually and in combination, on the precipitate crystal structures in Al-Mg-Si alloys in peak aged and overaged conditions. To assess whether such concentrations can affect the hardening precipitate structures, atomic resolution high-angle annular dark-field scanning transmission electron microscopy and atom probe tomography were adopted. The results indicate that low levels of Cu or Zn have a significant influence. Both elements showed a relatively high tendency to incorporate into precipitate structures, where Cu occupies specific atomic sites, creating its own local atomic configurations. However, Zn exhibited distinct behavior through the formation of extended local areas with 2-fold symmetry and mirror planes, not previously observed in precipitates in Al-Mg-Si alloys. Incorporation of Cu and/or Zn will influence the precipitates' electrochemical potential relative to matrix- and precipitate-free zones and thus the corrosion resistance. Furthermore, the presence of Cu/Zn structures (e.g., β'Cu, Q'/C) enhances the thermal stability of these precipitates and, accordingly, the mechanical properties of the material. The results obtained from this work are highly relevant to the topic of recycling of aluminum alloys, where accumulation of certain alloying elements is almost unavoidable; thus, tight compositional control might be critical to avoid quality degradation

Aberration-corrected HAADF-STEM investigations of precipitate structures in Al–Mg–Si alloys with low Cu additions

Precipitates in a lean Al–Mg–Si alloy with low Cu addition (~0.10 wt.%) were investigated by aberration-corrected high angle annular dark field scanning transmission electron microscopy (HAADF-STEM). Most precipitates were found to be disordered on the generally ordered network of Si atomic columns which is common for the metastable precipitate structures. Fragments of known metastable precipitates in the Al–Mg–Si–(Cu) alloy system are found in the disordered precipitates. It was revealed that the disordered precipitates arise as a consequence of coexistence of the Si-network. Cu atomic columns are observed to either in-between the Si-network or replacing a Si-network column. In both cases, Cu is the center in a three-fold rotational symmetry on the Si-network. Parts of unit cells of Q′ phase were observed in the ends of a string-type precipitates known to extend along dislocation lines. It is suggested that the string-types form by a growth as extension of the B′/Q′ precipitates initially nucleated along dislocation lines. Alternating Mg and Si columns form a well-ordered interface structure in the disordered Q′ precipitate. It is identical to the interface of the Q′ parts in the string-type precipitate

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

Atomistic details of precipitates in lean Al–Mg–Si alloys with trace additions of Ag and Ge studied by HAADF-STEM and DFT

Bonding energies and volume misfits for alloying elements and vacancies in multicomponent Al–Mg–Si alloys have been calculated using density functional theory (DFT). A detailed atomic scale analysis has been done for characteristic precipitate structures, using high-angle annular dark-field scanning transmission electron microscopy. Two new stacking configurations of the important strengthening phase β′′ were discovered in the Ge-added alloy. All three stacking variations were found to be energetically favourable to form from DFT calculations. The second stacking configuration, β2′′, contains vacated columns in its unit cell, consequently requiring less solute to create the same volume fraction of precipitate needles. DFT suggests a lower formation enthalpy per atom for β2′′ when Si is exchanged with Ge. In the alloy containing Ag additions, a new Q’/C-like local configuration containing Ag instead of Cu was discovered, also this phase was deemed energetically favourable from DFT

Early Combination of Material Characteristics and Toxicology Is Useful in the Design of Low Toxicity Carbon Nanofiber

This paper describes an approach for the early combination of material characterization and toxicology testing in order to design carbon nanofiber (CNF) with low toxicity. The aim was to investigate how the adjustment of production parameters and purification procedures can result in a CNF product with low toxicity. Different CNF batches from a pilot plant were characterized with respect to physical properties (chemical composition, specific surface area, morphology, surface chemistry) as well as toxicity by &lt;em&gt;in vitro&lt;/em&gt; and &lt;em&gt;in vivo &lt;/em&gt;tests. A description of a test battery for both material characterization and toxicity is given. The results illustrate how the adjustment of production parameters and purification, thermal treatment in particular, influence the material characterization as well as the outcome of the toxic tests. The combination of the tests early during product development is a useful and efficient approach when aiming at designing CNF with low toxicity. Early quality and safety characterization, preferably in an iterative process, is expected to be efficient and promising for this purpose. The toxicity tests applied are preliminary tests of low cost and rapid execution. For further studies, effects such as lung inflammation, fibrosis and respiratory cancer are recommended for the more in-depth studies of the mature CNF product