3090 Microsc. Microanal. 27 (Suppl 1), 2021
doi:10.1017/S1431927621010709 © Microscopy Society of America 2021
Studying clusters and nano-precipitates in Aluminium alloys using SPED and ADF-
STEM
Elisabeth Thronsen
1
, Adrian Lervik
2
, Christoph Hell
3
, Calin D. Marioara
4
, Sigurd Wenner
5
, Ruben
Bjørge
6
, Jesper Friis
5
, SIgmund J. Andersen
5
and Randi Holmestad
3
1
Norwegian university of science and technology, United States,
2
NTNU, United States,
3
NTNU,
Trondheim, Sor-Trondelag, Norway,
4
SINTEF Industry, United States,
5
SINTEF, United States,
6
SINTEF, Norway
Age-hardenable aluminium (Al) – Al-Cu, Al-Mg-Si and Al-Zn-Mg - alloys are important structural materials for
construction and automotive applications due to properties like high strength/weight ratio and good formability.
These properties are caused by small precipitates which are volume (3D) defects in the Al fcc host lattice. The
crystal phases, morphologies and distributions of precipitates can be manipulated by chemical composition and
thermo-mechanical treatment. Our research group at NTNU and SINTEF in Trondheim has for decades worked
together with the Norwegian light metal industry on studies of precipitates and microstructure in these Al alloys
[1]. Precipitation starts out with nanoscale clustering of solute elements and vacancies from a supersaturated,
metastable solid solution in the Al host lattice. Solving the structure and quantifying the distribution of these
clusters are important for understanding the further precipitation and thus the design of better alloys.
Two TEM techniques are used to study the clusters. Annular dark field scanning transmission electron
microscopy (ADF-STEM) with different collection angles, using a double Cs corrected JEOL ARM200CF, gives
information about atomic structure and lattice strain. STEM simulations and quantitative analysis of column
intensities and spacings can enhance the information obtained from STEM imaging. The scanning (precession)
electron diffraction (S(P)ED) technique can be used for structure determination of a large number of clusters for
statistical and quantitative studies. [2]. Comparison between the unique PED patterns in the experimental data
stack with simulated nanobeam diffraction patterns allows for verification or modification of the atomic model
of the clusters initially deduced from STEM images. These models are subsequently assessed using density
functional theory (DFT). The SPED experiments are performed on a JEOL 2100F equipped with a Quantum
Detectors Merlin direct electron detector. Recently we have also started conducting quantitative convergent
beam electron diffraction (QCBED) experiments of the clusters which gives promising results [3].
We have recently proposed the structure of the main clusters, the so-called GPI zones, in Al-Zn-Mg alloys [4] and
found that they are composed of one fundamental basic unit. This is essentially a partial substitution by Mg and
Zn on an fcc unit cell and a surrounding truncated cube octahedral (TCO) shell with a possible interstitial at the
centre of the TCO. The TCO units arrange in certain directions according to simple principles to form larger
clusters, as shown in figure 1. The virtual dark-field image obtained from a SPED data stack in figure 2 shows a
fine dispersion of clusters in the Al-Zn-Mg alloy. Due to the small size of the clusters, the cluster/Al signal ratio in
the diffraction patterns is low. To increase the signal, the diffraction patterns in all pixels belonging to a single
cluster can be added, as shown in figure 2. From the virtual dark-field image, we are investigating the possibility
of extracting size and density of the clusters. In the Al-Mg-Si system, high angle ADF-STEM imaging is much
more challenging because of the similar Z contrast from all atoms. Additionally, the clusters are also smaller and
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