Mechanical alloying (MA) followed by sintering has been one of the most widely adopted routes to produce nanocrystalline high-entropy alloys (HEAs). Enhanced solid solubility, room temperature processing, and homogenous alloy formation are the key benefits provided by MA. Spark plasma sintering has largely been used to obtain high-density HEA pellets from milled powders. However, there are many challenges associated with the production of HEAs using MA, which include contamination during milling and high propensity of oxidation. The present review provides a comprehensive understanding of various HEAs produced by MA so far, with the aim to bring out the governing aspects of phase evolution, thermal stability, and properties achieved. The limitations and challenges of the process are also critically assessed with a possible way forward. The paper also compares the results obtained from high-pressure torsion, another severe plastic deformation technique.

The effect of severe warm rolling on microstructure and texture homogeneities was investigated in a lamellar (L12 + B2) AlCoCrFeNi2.1 eutectic high-entropy alloy (EHEA). The EHEA 90% warm-rolled at 400 °C showed disordering of the L12 phase and a remarkable increase in hardness. A much finer microstructure was observed on ND-RD (Normal Direction-Rolling Direction) plane as compared with that on the RD-TD (Rolling Direction-Transverse Direction) plane. The L12/Face Centered Cubic (FCC) phase developed α-fiber texture ND//〈110〉 with a particularly strong brass ({110}〈112〉) component, while the B2 phase developed the usual RD (//〈110〉) and ND (//〈111〉) fibers. Nevertheless, inhomogeneities in texture were noticed. Upon annealing at 800 °C, the ND-RD showed an ultrafine microduplex structure, while the RD-TD showed a retained lamellar structure. A rather uniform microduplex structure evolved after annealing at 1200 °C due to the accelerated kinetics of transformation at higher temperatures. The L12/FCC phase showed the retention of the α-fiber components, while the B2 phase showed stronger ND-fiber after annealing, although inhomogeneities in texture existed.

In the design of high-entropy alloys (HEAs) with desired properties, identifying the effects of elements plays an important role. HEAs with eutectic microstructure can be obtained by judiciously modifying the alloy compositions. In this study, the effect of Nb addition to FeCoNiCuNbx (x = 0.5, 5, 7.5, 11.6, 15) alloys was studied by varying the Nb concentration (at.%). FeCoNiCuNb0.5 HEA shows liquid phase separation to form Cu-rich and FeCoNiCu-rich phases. Detailed solidification paths are proposed for these alloys, which show eutectic, peritectic, and pseudo quasi-peritectic reactions. Increasing Nb content promotes the liquid phase separation tendency and causes the formation of Cu-rich spheres. The effect of Nb on the FeCoNiCu-rich phase was studied based on the nanoindentation and correlated with nanohardness. The compressive deformation properties of these alloys are studied at room temperature and high temperature and correlated with microstructure. Fractography results show the mode of fracture and are correlated with the microstructure obtained.

We assess the validity of criteria based on size mismatch and thermodynamics in predicting the stability of the rare class of high-entropy alloys (HEAs) that form in the hexagonal close-packed crystal structure. We focus on nanocrystalline HEA particles composed predominantly of Mo, Tc, Ru, Rh, and Pd along with Ag, Cd, and Te, which are produced in uranium dioxide fuel under the extreme conditions of nuclear reactor operation. The constituent elements are fission products that aggregate under the combined effects of irradiation and elevated temperature as high as 1200 °C. We present the recent results on alloy nanoparticle formation in irradiated ceria, which was selected as a surrogate for uranium dioxide, to show that radiation-enhanced diffusion plays an important role in the process. This work sheds light on the initial stages of alloy nanoparticle formation from a uniform dispersion of individual metals. The remarkable chemical durability of such multiple principal element alloys presents a solution, namely, an alloy waste form, to the challenge of immobilizing Tc.

Nanocrystalline (NC) and ultrafine-grained (UFG) CoCrCuFeNi high-entropy alloy (HEA) with grain size ranging between 59 and 386 nm was produced via powder metallurgy and heat treatment. The as-sintered HEA exhibited two face-centered cubic (FCC) phases (CoCrFeNi-rich and Cu-rich phases) and a small grain size (59 nm), whereas the alloy after heat treatment at 1000 °C exhibited a CoCuFeNi-rich phase with FCC structure and relatively larger grain size (386 nm). Moreover, the yield strength decreased from 1930 to 883 MPa, and plastic strain to failure increased by 8–32%. In terms of microstructural evolution, grain boundary strengthening coupled with lattice distortion was the dominant strengthening mechanism for NC HEAs. Furthermore, the coefficient for boundary strengthening was higher in the HEAs than in the corresponding pure elemental metals with FCC structure, possibly because of significant lattice distortion. The UFG HEAs exhibited high strength and good ductility because of the activation of dislocation.

Discs of CoCuFeMnNi face centered cubic high entropy alloy were subjected to monotonic and cyclic high pressure torsion (HPT) in a single step and multiple steps of 5° forward and reverse cycle for 100° and 360° twist, respectively, under 5 GPa pressure at room temperature. It was observed that the 100° cyclic HPT sample shows the highest hardness at the periphery comparable to 360° monotonic HPT sample, while the cyclic 360° HPT sample shows the lowest hardness throughout the sample. High hardness of 100° cyclic HPT sample can be attributed to finer grain size and unstable dislocation substructure by continuous change in strain path from initial compression to forward–reverse torsion, while stable dislocation structure corresponding to shear contributes to increase in hardness from 100° to 360° for monotonic HPT sample. The unstable dislocation substructure promotes grain boundary migration–enabled grain growth leading to low hardness throughout the 360° cyclic HPT sample.

In the present study, hot deformation behavior of a FCC high-entropy alloy CoCuFeMnNi has been investigated to explore the stress–strain response for a wide range of temperatures and strain rates. The deformation response has been examined by plotting a processing map and examining the evolution of microstructure and texture in each of the temperature–strain rate domain. Hot compression tests were carried out in the temperature range 850–1050 °C at strain rates varying from 0.001 s−1 to 10 s−1. Stress–strain curves indicate characteristic softening behavior due to dynamic recrystallization (DRX). DRX has been observed along grain boundaries, shear bands, as well as in the interior of deformed grains. The size of dynamically recrystallized grains shows a strong dependence on deformation temperature and increases with temperature. A high degree of twin formation takes place in the DRX grains evolved inside the shear bands, and the extent of twinning decreases at high temperatures. The optimal processing window has been estimated based on strain rate sensitivity and has been validated with detailed analyses of microstructure and texture. The best region for thermo-mechanical processing has been identified as in the temperature range 850–950 °C at strain rate 10−1 s−1.

In the present study, the phase evolution and microstructure of CrMoNbTiW, a new equi-atomic refractory high-entropy alloy, are studied. The alloy was synthesized through mechanical alloying (MA) followed by consolidation using spark plasma sintering. After MA, a major BCC solid solution along with residual Cr and Nb were observed. However, secondary phases such as Laves and carbides were also observed in addition to the major BCC solid solution after sintering. Unsolicited contamination from the milling media is found to be one of the reasons for the formation of secondary phases. The high hardness of 8.9 GPa after sintering was attributed to the presence of secondary phases along with the nanocrystalline nature of the alloy. To understand the phase evolution, calculation of phase diagram was carried out using CALPHAD. Further, binary phase diagram inspection and simple empirical parameters were also used to assess their effectiveness in predicting phases.

A novel series of nanocrystalline AlCuCrFeMnWx (x = 0, 0.05, 0.1, 0.5) high-entropy alloys (HEAs) were synthesized by mechanical alloying followed by spark plasma sintering. The phase evolution of the current HEAs was studied using X-ray diffraction (XRD), transmission electron microscopy, and selected area electron diffraction. The XRD of the AlCuCrFeMn sintered HEA shows evolution of ordered B2 phase (AlFe type), sigma phase (Cr rich), and FeMn phase. AlCuCrFeMnWx (x = 0.05, 0.1, 0.5 mol) shows formation of ordered B2 phases, sigma phases, FeMn phases, and BCC phases. Micro-hardness of the AlCuCrFeMnWx samples was measured by Vickers microindentation and the maximum value observed is 780 ± 12 HV. As the tungsten content increases, the fracture strength under compression increases from 1010 to 1510 MPa. Thermodynamic parameters of present alloys confirm the crystalline phase formation, and finally structure–property relationship was proposed by conventional strengthening mechanisms.

AlCoCrFeNi is among the promising high-entropy alloys (HEAs) that possess high strength with considerable ductility. Powder sintering is one of the competitive routes for the production of HEA powders. However, sintering of HEA powders under a pressureless condition is difficult. The present work aims to produce high-density components from mechanically alloyed AlCoCrFeNi HEA powders through the pressureless sintering method. Nearly full density was achieved at 1275 °C. Sintering was performed in the presence of a viscous phase in the temperature range of 1200–1250 °C, which was confirmed through differential scanning calorimetry and dilatometric measurements. This viscous phase was found have a Cr-rich composition, detected by interrupting the sintering and quenching of the sample. The powder initially contained the BCC phase with a small fraction of FCC and other phases. During sintering, a significant fraction of the FCC phase and nanosized B2 phase were formed. Sintered sample had a hardness of 679 ± 20 Hv.

In this investigation, we have reported the alloying behavior, phase evolution, and thermal stability of equiatomic AlCoCrFeNiTi high-entropy alloy (HEA). The 40 h milled powder shows good chemical homogeneity with agglomerated particles varying in the range of ∼3–18 μm. The formation of a nanostructured single-phase BCC (a = 2.85 ± 0.01 Å) was observed along with the minor tungsten carbide (WC) phase that formed due to contamination during milling. Thermal stability of the alloy has been studied using dynamic differential scanning calorimetry (DSC) thermogram and in situ X-ray diffraction. It has been found that this HEA is stable up to 600 °C (873 K). Consolidated samples at 1000 °C (1273 K) showed the transformation of body centered cubic (BCC) phase into the B2 (a = 2.87 ± 0.03 Å) phase co-existing with minor hexagonal WC (a = 2.90 Å, c = 2.83 Å) phase.

Cold-sprayed high-entropy alloy (HEA) coatings have been generated for the first time. Mechanically alloyed (MA) AlCoCrFeNi powder was chosen as feedstock, owing to the extensive literature on this alloy. Coatings were synthesized under various gas temperature and pressure conditions. Isothermal oxidation was conducted at 1100 °C for 25 h on the coating cold-sprayed at 400 °C and 10 bar on a Ni-base superalloy substrate. The as-sprayed coating retained the MA phases and formed a protective alumina layer upon oxidation. An interdiffusion zone at the interface and unanticipated Mo diffusion from the superalloy substrate into the coating were observed after oxidation. A comprehensive characterization at the coating–substrate interface suggests that diffusion in HEAs is not sluggish. The factors governing the coating’s oxidation are elucidated, and a plausible oxidation mechanism is discussed. These studies are aimed at developing oxidation-resistant HEA coatings for potential applications at high operating temperatures.

Three different high entropy-alloys consisting of six elements (Ti, Zr, V, Cr, Ni, and Fe) with varying Fe content were synthesized by using the RF induction melting technique. All the as-cast, slow-cooled, and rapidly quenched alloys exhibit C14 Laves phase, and it is found to be stable at high temperature. A lattice contraction has been observed with the addition of Fe. To the best of our knowledge, this is the first report on the synthesis of a single-phase high-entropy complex intermetallic compound in the hexanary alloy system. It has been shown that the thermodynamic calculations following Miedema’s approach and the parametric approach utilizing several descriptors comprising configurational entropy, mixing enthalpy, atomic size mismatch, electronegativity, and valence electron concentration favor the stability of the high-entropy multicomponent Laves phase.

CrFeNiTix (x = 0.2, 0.3, 0.4, 0.5, and 0.6 molar ratio) compositionally complex alloys were fabricated by vacuum arc melting to investigate the microstructure, hardness, and compressive properties. The results revealed that CrFeNiTix alloys consisted of the principal face-centered cubic (FCC) phase and body-centered cubic (BCC) solid solution, with an amount of (Ni, Ti)-rich hexagonal close-packed phase. CrFeNiTix alloys exhibited the typical dendrite. Ti0.2 and Ti0.3 alloys were composed of FCC and BCC solid solutions in the dendrite, as well as ε (Ni3Ti) and R (Ni2.67Ti1.33) phases in the inter-dendrite, simultaneously. For Ti0.4, Ti0.5, and Ti0.6 alloys, (Fe, Cr)-rich solid solution separated out and ε phase transformed into R phase gradually. Meanwhile, TEM analysis indicated that Ti0.4 alloy matrix consisted of the principal FCC phase containing (Ni, Ti)-rich intragranular nanoprecipitates. The hardness values of CrFeNiTix alloys were increased with the addition of Ti content and the high compressive strength of CrFeNiTix alloys was maintained, which was attributed to the solid solution strengthening and precipitation hardening.

FeCoNi(Mn–Si)x (x = 0.5, 0.75, 1.0) high-entropy alloys (HEAs) were successfully synthesized by mechanical alloying (MA), and the effect of Mn and Si in the ferromagnetic alloys on crystal structure and magnetic behavior was thoroughly investigated. XRD, SEM, and TEM were used to investigate the effect of Mn and Si content on the structure of HEAs. The high Mn and Si contents change the structure from the BCC phase to FCC phase. The evolution of surface morphology was discussed on the basis of MA time and content of Mn and Si. The magnetic hysteresis curve confirmed the highest magnetic saturation (Ms) value of 134.21 emu/g for FeCoNi(Mn–Si)1.0 alloy and an appreciably low coercivity (Hc) of 98.07 Oe for FeCoNi(Mn–Si)0.5 alloy. The finite element method (FEM), using COMSOL Multiphysics software, has been used for determining the magnetic flux density (B) on the surface and at the center of the transformer core to determine the performance of the proposed HEAs.

This study aims to investigate the sliding wear behavior of Al0.4FeCrNiCox (x = 0, 0.25, 0.5, 1.0 mol) high-entropy alloys (HEAs) under oil lubricating conditions at room temperature. Phase and microstructural characterizations of HEAs are performed by utilizing X-ray photoelectron spectroscopy (XRD) and scanning electron microscope (SEM). The compressive yield strength of Al0.4FeCrNiCox (x = 0, 0.25, 0.5, 1.0 mol) HEAs is observed to decrease from 1169.35 to 257.63 MPa. Plastic deformation up to 75% is achieved in the case of Al0.4FeCrNiCox=1 HEA. The microhardness of HEA samples is found to decrease from 377 to 199 HV after the addition of cobalt content from x = 0 to 1.0 mol. Thermal analysis is performed using a differential scanning calorimeter. It is confirmed that Al0.4FeCrNiCox (x = 0, 0.25, 0.5, 1.0 mol) HEAs do not undergo any phase change up to 1000 °C. The specific wear rate of Al0.4FeCrNiCox=1 HEA is observed to be highest in all wear conditions. The worn surfaces were analyzed by SEM with attached energy-dispersive spectroscopy, 3D profiling, and X-ray photoelectron spectroscopy (XPS).

In search of materials with better properties, polycrystalline materials are often found to be superior to their respective single crystalline counterparts. Reduction of grain size in polycrystalline materials can drastically alter the properties of materials. When the grain sizes reach the nanometer scale, the improved mechanical response of the materials make them attractive in many applications. Multicomponent solid-solution alloys have shown to have a higher radiation tolerance compared with pure materials. Combining these advantages, we investigate the radiation tolerance of nanocrystalline multicomponent alloys. We find that these alloys withstand a much higher irradiation dose, compared with nanocrystalline Ni, before the nanocrystallinity is lost. Some of the investigated alloys managed to keep their nanocrystallinity for twice the irradiation dose as pure Ni.

Herein, in order to research the crystalline behaviors of cyclotetramethylenetetranitramine-aluminum (HM-Al) composites in solvents, the modified attachment energy model was applied to predict the morphologies of HMX in vacuum, dimethyl sulfoxide (DMSO), and ethanol. Then HMX-Al composites with Al coated and noncoated were prepared via solvent–nonsolvent method, and the morphologies were characterized. Results show that HMX interacts with DMSO and ethanol mainly via van der Waals force and electrostatic force. HMX grows into polyhedral crystals in two solvents. However, the shapes and the crystalline surface area distributions of the polyhedrons are different for two solvents. There are many aluminum particles embedded in HMX crystals of HMX-Al composite particles prepared via solvent–nonsolvent method, but Al particles cannot embed in HMX crystals in the existence of fluoropolymer. The crystal morphology predicted is consistent with the experimental results.