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Synchrotron X-ray operando studies of atomic structure evolution of multi-component Al alloys in liquid state

Huang, Shi


Shi Huang



This research has studied one of the challenging scientific issues in materials science, i.e., in real time, understanding quantitatively the 3D atomic structures of multiple component alloys in the liquid state and how the atomic structures evolve with temperatures until the onset of crystal nucleation. Four Al-based alloys were used in the research: (1) Al-0.4Sc, (2) Al-1.5Fe, (3) Al-5Cu-1.5Fe and (4) Al-5Cu-1.5Fe-1Si alloy (all in weight percentage). All alloys were heated up to the liquid state and then cooled down with predefined cooling rates using a dedicated solidification apparatus. During cooling, synchrotron X-ray was used to illuminate onto the samples and the total scattering data were collected at the target temperatures. Based on the total scattering data, the empirical potential structure refinement (EPSR) method was used to model and reconstruct the 3D atomic structures in the liquid state at the selected temperatures for each alloy. The research has demonstrated that the EPSR is a computationally efficient tool for searching and finding the solutions of 3D atomic structures according to the measured total scattering data. For the studied alloys, the research reveals fully the temperature-dependent structure heterogeneity and their evolutions with temperature. The key findings of the research are:
(1) For the Al-0.4Sc alloy, at the short-range scale in the liquid state, Sc-centred Al polyhedrons form icosahedral type structures with the Al coordination number in the range of 10–12. As the melt is cooled down, the Sc-centred polyhedrons become more compacted, and the connections between adjacent polyhedrons change from more vertex connection to more edge and then more face-sharing connection. At the medium-range scale, the Sccentred clusters with face-sharing are proved to be the “precursors” for the L12 Al3Sc primary phase in the liquid-solid coexisting region.
(2) For the three Fe-containing alloys, atomic structural heterogeneities were found to exist in the 1st atomic shell and beyond. The degree of structural heterogeneities is related with the difference in atom radius, atomic bond length and the chemical preference between different atoms in each alloy. The competition resulted in that the Al-centred clusters expand, i.e., with larger bond length, while the solute atom-centred clusters contract, so with the reduced bond length.
(3) At the short-range scale, the structural heterogeneities were characterised by the co-existence and growth of the icosahedra-like (ICO-like) and crystal-like structures. During cooling, the Fe atoms show a higher degree of crystallinity than other atoms in the liquids. At the onset of crystal nucleation, relative percentage of the Fe-centred ICO-like and crystal-like Voronoi polyhedrons (VPs) reaches 8-10%, and the others in the range of 5.8-8.5%.
(4) The Fe-centred short-range orders (SROs) tend to connect together via five different modes to form larger Fe-centred medium-range orders (MROs). The percentage of the face-sharing increases almost linearly as the temperature is cooled down, approximately 18-20% at the onset of nucleation in the 3 melts. The Fe-centred MROs gradually approach to the structures of the Al13Fe4 primary phase (monoclinic structure) and are proved to be the nucleation precursors for the Al13Fe4 phases.
(5) For the quaternary Al-Cu-Fe-Si alloy melt, the research found that the liquid first transfers into a quasicrystal-like, metastable monoclinic Al13Fe4 phase. Such primary phase was confirmed to have a higher degree of five-fold and crystalline symmetry than the liquid. Upon cooling, the Fe-centred five-fold and crystalline symmetry both get enhanced in liquid, leading to a smaller Al13Fe4-liquid configuration entropy difference and interfacial free energy.


Huang, S. (2023). Synchrotron X-ray operando studies of atomic structure evolution of multi-component Al alloys in liquid state. (Thesis). University of Hull. Retrieved from

Thesis Type Thesis
Deposit Date Nov 14, 2023
Publicly Available Date Nov 15, 2023
Keywords Engineering
Public URL
Additional Information School of Engineering
University of Hull
Award Date Oct 12, 2023


Thesis (25.8 Mb)

Copyright Statement
© 2023 Shi Huang. All rights reserved. No part of this publication may be reproduced without the written permission of the copyright holder.

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