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Processing of Bulk Nanocrystalline Metals at the US Army Research Laboratory

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Published on: March 7, 2018

In Situ Visualization of Electron Beam-Driven High-Entropy Alloy Crystallization.

Azadeh Amiri¹, Reza Shahbazian-Yassar¹

¹Department of Mechanical and Industrial Engineering, University of Illinois Chicago, Chicago, IL, 60607, USA.

Advanced Science (Weinheim, Baden-Wurttemberg, Germany)

|October 21, 2025

Summary

Electron beam crystallization creates uniform high-entropy alloy (HEA) nanoparticles. This method offers superior control over composition and morphology compared to traditional heating, enabling new synthesis routes.

Keywords:

high entropy alloy nanoparticles in situ transmission electron microscopy

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Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

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Quantitative Atomic-Site Analysis of Functional Dopants/Point Defects in Crystalline Materials by Electron-Channeling-Enhanced Microanalysis

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Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Published on: June 7, 2018

Area of Science:

Materials Science
Nanotechnology
Solid-state Chemistry

Background:

Achieving uniform high-entropy alloy (HEA) nanoparticles via reduction-based synthesis is difficult due to elemental variations.
Controlling elemental reduction, diffusion, and phase stability is crucial for HEA synthesis.

Purpose of the Study:

To visualize and understand the electron beam-induced crystallization of amorphous high-entropy glycerolate (HE-glycerolate) films.
To investigate the mechanism of forming single-phase face-centered cubic (fcc) HEA nanoparticles with controlled morphology.

Main Methods:

In situ transmission electron microscopy (TEM) was used to observe the crystallization process.
Amorphous HE-glycerolate films (Mg, Mn, Co, Ni, Zn) were subjected to electron beam irradiation.

Main Results:

Electron beam irradiation induced crystallization via phase separation, radiolytic reduction, and atomic rearrangement.
This process yielded single-phase fcc HEA nanoparticles with uniform cuboidal morphology and dominant {100} facets.
The electron beam pathway provided finer control over composition and morphology than thermal annealing by limiting atomic mobility.

Conclusions:

Electron beam-driven crystallization offers a novel, low-temperature route for synthesizing uniform HEA nanoparticles.
Controlling atomic mobility is essential for achieving stable, compositionally homogeneous multielement solid solutions.
The findings provide a foundation for designing scalable synthesis strategies for advanced HEA materials.