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Design, Preparation, and Microstructural Characterization of High Entropy Materials
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Design, Preparation, and Microstructural Characterization of High Entropy Materials

A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Advanced Materials Characterization".

Deadline for manuscript submissions: closed (20 April 2026) | Viewed by 7917

Special Issue Editor

Dr. Wei Ren

E-Mail Website
Guest Editor
1. School of Science, Xi’an University of Posts & Telecommunications, Xi’an 710121, China
2. School of Physical Science and Technology, Northwestern Polytechnical University, Xi’an 710072, China
Interests: photovoltaic functional thin film materials; synthesis and characterization of gallium oxide films; thermal sensitive films; high entropy oxide films
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

High-entropy materials (high-entropy alloy, high-entropy oxide, high-entropy...) have attracted tremendous attention and have shown promise regarding exciting applications which have previously been unfathomable to achieve. Owing to their short-range disorder and long-range order nature, these materials maintain a high configuration entropy, which can still sustain phase stability, allowing various adjustment in the mechanical, electrical, optical, magnetic, and catalytic performances of the materials.

Previous research on high-entropy materials has focused on bulk samples. However, as the miniaturization of devices has evolved, there is a need to understand this multiple alloy system at the micro and nano levels. The development of high-entropy materials is as of now a debated issue that can be generally divided into two primary classes: coatings with bulk and thin films. Some of the major issues in bulk alloy-based material is the prevalence of brittle fracture upon deformation that leads to catastrophic fracture, which typically originates from a single, major shear band. The scientific community is also focusing on the following fields: 1) developing novel high-entropy alloy thin films with ideal strength and ductility in extreme conditions, such as cryogenic or acid environments; 2) developing novel high-entropy oxide thin films with various crystal structures, such as rocksalt, spinel, perovskite, fluorite, etc.; 3) developing a comprehensive prediction and screening methodology supported by machine learning technologies.

This Special Issue aims to bring together research papers, short communications, and review articles focused on the novel synthesis, device designs, fabrication, advanced characterization, and artificial intelligence design of various high-entropy materials in order to provide a comprehensive overview of the state of the art within this field

Dr. Wei Ren
Guest Editor

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Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • high-entropy alloy
  • high-entropy oxide
  • high-entropy nitride
  • high-entropy carbide

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Published Papers (5 papers)

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Research

15 pages, 13311 KB  
Article
Experimental Determination of Isothermal Sections in the Ni–Al–Cr–Ru Quaternary System: Implications for Ni-Based Superalloys and High-Entropy Alloys
by Jianping Huang, Dupei Ma, Zhi Li, Yan Liu, Ruihua Wang, Huayu Xiao and Qiang Zhang
Materials 2026, 19(8), 1669; https://doi.org/10.3390/ma19081669 - 21 Apr 2026
Viewed by 363
Abstract
The phase equilibria of the Ni–Al–Cr–Ru quaternary system were systematically investigated using the equilibrated alloy method combined with scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD). This study focuses on three key isothermal sections within the system: 55 at.% Al [...] Read more.
The phase equilibria of the Ni–Al–Cr–Ru quaternary system were systematically investigated using the equilibrated alloy method combined with scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD). This study focuses on three key isothermal sections within the system: 55 at.% Al at 1423 K, 55 at.% Ni at 1173 K, and 60 at.% Ni at 1423 K. In the 55 at.% Al section at 1423 K, a four-phase equilibrium region comprising Bcc(Cr), β-(Ni,Ru)Al, Al8Cr5, and Al2Ru, along with three three-phase regions, was identified. Complete mutual solubility between the NiAl and AlRu phases was achieved with approximately 10 at.% Cr. In the 55 at.% Ni section at 1173 K, two four-phase and seven three-phase equilibrium regions were observed. The addition of Cr was found to promote the emergence of the Fcc(Ni) + β-(Ni,Ru)Al + Ni3Al three-phase region and the Fcc(Ni) + β-(Ni,Ru)Al two-phase region. Critically, Cr addition enabled complete solubility between the β1 (NiAl) and β2 (AlRu) phases even at 1173 K. For the 60 at.% Ni section at 1423 K, while no four-phase equilibrium was found, two three-phase regions—(Ni,Ru)Al + Hcp(Ru) + Fcc(Ni) and (Ni,Ru)Al + Ni3Al + Fcc(Ni)—were confirmed. Notably, the (Ni,Ru)Al + Fcc(Ni) two-phase region exhibited a wide compositional range. This work provides essential experimental phase diagram data and insights for the design of Ni–Al–Cr–Ru-X high-entropy alloys and next-generation Ni-based superalloys. Full article
(This article belongs to the Special Issue Design, Preparation, and Microstructural Characterization of High Entropy Materials)
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15 pages, 2342 KB  
Article
Effect of Pre-Strain Induced Microstructure Evolution on Hydrogen Embrittlement Resistance of a CoCrNi Medium-Entropy Alloy
by Zening Wang, Sirui Jing and Yu Yan
Materials 2025, 18(21), 4915; https://doi.org/10.3390/ma18214915 - 27 Oct 2025
Cited by 2 | Viewed by 1055
Abstract
The effect of pre-strain-induced microstructural evolution on the hydrogen embrittlement (HE) resistance of an equiatomic CoCrNi medium-entropy alloy was systematically investigated by mechanical property testing, scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD) characterization. Three pre-strain levels (0%, 30%, and 50%) were [...] Read more.
The effect of pre-strain-induced microstructural evolution on the hydrogen embrittlement (HE) resistance of an equiatomic CoCrNi medium-entropy alloy was systematically investigated by mechanical property testing, scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD) characterization. Three pre-strain levels (0%, 30%, and 50%) were applied to produce distinct microstructures: dislocation-free and twin-free (P0), high dislocation density with few deformation twins (P30), and high densities of both dislocations and deformation twins (P50). Mechanical tests combined with hydrogen charging revealed that the P50 specimen exhibited the highest yield strength (1163.88 MPa) and the lowest HE-induced elongation loss (2.74%), indicating an improvement in HE resistance. By using SEM, detailed observations of the fracture morphology and crack propagation paths revealed that deformation twins can effectively reduce stress concentration, delay the nucleation and propagation rates of cracks, and suppress brittle intergranular fracture, thereby improving mechanical properties and resistance to hydrogen embrittlement. A detailed analysis was conducted of the HE resistance mechanism associated with the influence of deformation twins on hydrogen transport and distribution. Full article
(This article belongs to the Special Issue Design, Preparation, and Microstructural Characterization of High Entropy Materials)
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19 pages, 4269 KB  
Article
Effect of Synthesis and Processing Conditions on the Sintering Behavior and Total Conductivity of High-Entropy Fluorite/Bixbyite Oxides (RE-HEOs)
by Luca Spiridigliozzi, Viviana Monfreda, Antonello Marocco, Filippo Milano, Antonio Vendittelli and Gianfranco Dell’Agli
Materials 2025, 18(11), 2663; https://doi.org/10.3390/ma18112663 - 5 Jun 2025
Cited by 5 | Viewed by 1437
Abstract
This study explores the influence of two different synthesis methods on the sintering behavior of three novel high-entropy oxides possibly suitable for thermal barrier applications: (Ce0.2Zr0.2Yb0.2Er0.2Nd0.2)O2-δ, (Ce0.2Zr0.2Yb [...] Read more.
This study explores the influence of two different synthesis methods on the sintering behavior of three novel high-entropy oxides possibly suitable for thermal barrier applications: (Ce0.2Zr0.2Yb0.2Er0.2Nd0.2)O2-δ, (Ce0.2Zr0.2Yb0.2Er0.2La0.2)O2-δ, and (Ce0.2Nd0.2Yb0.2Er0.2La0.2)2O3+δ. Rare-Earth-based High-Entropy Oxides (RE-HEOs), recently known for their exceptional thermal stability and compositional flexibility, have gained increasing attention as potential candidates for many advanced technological applications. Thus, our current work focuses on the specific effects of synthesis techniques, namely co-precipitation and hydrothermal treatment, on the entropy-driven stabilization, microstructure, electrochemical properties, and sintering behavior of three novel RE-HEOs. The obtained results reveal significant differences in terms of densification yield and of the obtaining of the designed entropy-stabilized single phase depending on the adopted synthesis route, underscoring the critical role of synthesis in optimizing RE-HEOs for near-future technological applications. Full article
(This article belongs to the Special Issue Design, Preparation, and Microstructural Characterization of High Entropy Materials)
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12 pages, 3306 KB  
Article
Determination of the Entire Existence Composition Range of CrMnFeCoNi High-Entropy Alloys Using Sintered Diffusion Multiple Method
by Ryuta Yurishima, Ayako Ikeda and Teruyuki Ikeda
Materials 2025, 18(2), 295; https://doi.org/10.3390/ma18020295 - 10 Jan 2025
Cited by 2 | Viewed by 2045
Abstract
The sintered diffusion multiple (SDM) method, which has been developed in our research group, has been applied to determine the entire composition range of the CrMnFeCoNi high-entropy alloy stereoscopically and continuously over nearly the entire range. The samples were prepared by sintering mixed [...] Read more.
The sintered diffusion multiple (SDM) method, which has been developed in our research group, has been applied to determine the entire composition range of the CrMnFeCoNi high-entropy alloy stereoscopically and continuously over nearly the entire range. The samples were prepared by sintering mixed elemental powders and were annealed at 970 °C or 800 °C. Several hundreds of thousands of points were analyzed at random within the samples for chemical compositions using electron probe microanalysis. With the assumption that ideally, only chemical compositions of existing phases at the temperature of annealing are obtained, the compositional data thus obtained were analyzed to estimate the phase boundaries of the high-entropy phase, including the Cantor alloy composition, assuming local equilibrium within the samples. The analysis includes the determination of point densities and their slopes in the space of chemical composition. The results are shown in the tetrahedral compositional space, with vertices for the Cr, Mn, and Fe atomic fractions and the sum of the Co and Ni fractions. One of the features found in this work is that the high-entropy phase exhibits a wide compositional range in the Fe-CrMnCoNi direction. The estimated phase boundary compositions are found to be in good agreement, within an error range 3 at.%, with those obtained using samples prepared by the conventional method, where the samples with uniform compositions are equilibrated by annealing, and the compositions of their existing phases are analyzed using EPMA. Thus, the sintered diffusion multiple method is effective in providing an overview of the quinary phase diagrams. Full article
(This article belongs to the Special Issue Design, Preparation, and Microstructural Characterization of High Entropy Materials)
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9 pages, 3702 KB  
Article
Synthesis of β-Ga2O3:Mg Thin Films by Electron Beam Evaporation and Postannealing
by Weitao Fan, Sairui Li, Wei Ren, Yanhan Yang, Yixuan Li, Guanghui Liu and Weili Wang
Materials 2024, 17(19), 4931; https://doi.org/10.3390/ma17194931 - 9 Oct 2024
Cited by 5 | Viewed by 2054
Abstract
Doping divalent metal cations into Ga2O3 films plays a key role in adjusting the conductive behavior of the film. N-type high-resistivity β-Ga2O3:Mg films were prepared using electron beam evaporation and subsequent postannealing processing. Various characterization [...] Read more.
Doping divalent metal cations into Ga2O3 films plays a key role in adjusting the conductive behavior of the film. N-type high-resistivity β-Ga2O3:Mg films were prepared using electron beam evaporation and subsequent postannealing processing. Various characterization methods (X-ray diffraction, X-ray photoelectron spectroscopy, photoluminescence, etc.) revealed that the Mg content plays an important role in affecting the film quality. Specifically, when the Mg content in the film is 3.6%, the S2 film’s resistivity, carrier content, and carrier mobility are 59655.5 Ω·cm, 1.95 × 1014 cm3/C, and 0.53682 cm2/Vs. Also, the film exhibits a smoother surface, more refined grains, and higher self-trapped exciton emission efficiency. The Mg cation mainly substitutes the Ga+ cation at a tetrahedral site, acting as a trap for self-trapped holes. Full article
(This article belongs to the Special Issue Design, Preparation, and Microstructural Characterization of High Entropy Materials)
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