High-entropy Alloy Powders Research Articles

Sample Preparation and Determination of Trace Elements in High-Entropy Alloys by Total Reflection X-Ray Fluorescence (TXRF)

High-entropy alloys (HEAs) have attracted significant attention in recent years owing to their exceptional material properties; however, trace impurities in these alloys can significantly affect their strength, toughness, and radiation resistance. This study employs total reflection X-ray fluorescence (TXRF) to determine the trace impurities in three common HEA powders prepared via suspension techniques. High-Z (Ca and Mn) and low-Z (Mg and Al) elements were quantified using the internal standard and calibration curve methods, respectively. The levels of high-Z elements are consistent with those determined using inductively coupled plasma – optical emission spectrometry (ICP-OES). Although the physical mechanisms exerted various effects on low-Z elements, qualitative and semi-quantitative analyses remained feasible, demonstrating the effectiveness of TXRF for impurities in HEAs. Additionally, the combination of suspension sample preparation and TXRF affords a nondestructive, rapid, and cost-effective methodology that requires minimal sample quantities. Consequently, TXRF is well suited for the rapid determination of impurities in HEAs.

Preparation process, surface properties and mechanistic study of HVAF-sprayed CoCrFeNiMo0.2 high-entropy alloy coatings

The objective of this study is to develop infrared reflective coatings with excellent service performance in extreme environments, aimed at reducing system energy consumption and enhancing service life. In this work, CoCrFeNiMo0.2 high-entropy alloy (HEA) powder was deposited on the 316 L stainless steel (SS) substrate using High-Velocity Air Fuel (HVAF) thermal spray technology. The microstructure, mechanical properties, infrared reflectivity, and corrosion resistance of the coatings under different spraying parameters were investigated and compared with those of the substrate. Computational Fluid Dynamics (CFD) simulation was employed to analyze the influence of HVAF spraying parameters on flame characteristics and particle flight behavior, providing guidance for optimizing the spraying process and explaining underlying mechanisms. Results demonstrated that adjusting parameters such as propane and air pressure, spraying distance, and powder feed rate could produce dense coatings with <1 % porosity. The microhardness of the coatings was approximately 1.8 times that of the substrate, and the bonding strength between the coating and the substrate is increased to 39.4 MPa. Additionally, the near-infrared reflectivity of the coatings was significantly higher than that of the substrate, with an enhancement of 18.7 %. Coatings sprayed under different parameters exhibited superior passivation and pitting corrosion resistance compared to the substrate in 3.5 wt% NaCl and 1 mol/L HCl solutions. Optimization of spraying parameters further enhanced the protective capability of the passivation film and corrosion resistance. Consequently, CoCrFeNiMo0.2 HEA coatings prepared by HVAF spraying technology demonstrate excellent comprehensive performance, holding promising potential for industrial applications.

Investigation of microstructural, hardness, and wear properties of AlCrCuFeNi high entropy alloys produced by hot-pressing with the enhancement of manufacturability through electroless Ag incorporation

This study involves the production of HEA materials using low-temperature and high-pressure principles by mechanical-alloying AlCrCuFeNi high-entropy alloy powders, followed by electroless Ag coating for enhanced interface properties and hot-pressing without additional sintering. The Ag interface significantly improved the bonding of HEA powders. While increasing temperature causes a 10 % weight gain due to oxidation in HEA samples, this rate is only 1.5 % in those produced with Ag-coated HEA. The Ag interface improved the hardness of the HEAs by 50 %. The wear rate was reduced by more than twofold due to the Ag-interfaces. Ag exhibited a self-lubricating effect due to the Ag layers that repeatedly emerge during sliding, resulting in a low friction coefficient of 0.19 and excellent wear resistance.

Powder metallurgical processing of novel Al0.5CoCrFeNiNb0.5-Si0.1 high entropy alloys: Phase evolution and nanomechanical properties

In this research, the high entropy alloy (HEA) of Al0.5CoCrFeNiNb0.5-Si0.1 was successfully synthesized through mechanical alloying utilizing a high-energy planetary ball mill. The synthesized HEA powder was subsequently pressed and sintered at 1400 °C with varying holding times. The phase evolution was investigated using X-Ray Diffraction (XRD) technique. Furthermore, the microstructural, morphological, and compositional characteristics of the powders were examined using Transmission Electron Microscopy (TEM) with Selected Area Electron Diffraction (SAED), as well as Scanning Electron Microscopy (SEM) in conjunction with Energy Dispersive Spectroscopy (EDS). The nano-mechanical properties of the HEA compact were evaluated through nanoindentation to determine nano-hardness and elastic modulus.The mechanical alloying process was conducted for a duration of 30 h, resulting in the formation of a single-phase BCC solid solution, as confirmed by XRD and SAED analyses. The study investigated the criteria for phase stability based on the minimum Gibbs free energy and Hume-Rothery rules, which were consistent with the observed microstructural characteristics. Furthermore, the sintering process resulted in porosity levels of 6.01 % and 4.71 %, with corresponding densities of 6.96 g/cm³ and 7.12 g/cm³ for holding times of 3 and 4 h, respectively. It was noted that extended holding times improved the mechanical properties, with the alloy achieving a maximum hardness of 546 HV, nano-hardness of 5.57 GPa, elastic modulus of 265.47 GPa, and yield stress of 1.89 GPa after a holding time of 4 h.

Optimization of Laser Welded Joints of Steel/Al with Pre-placed High-Entropy Alloy Powder

Optimization of Laser Welded Joints of Steel/Al with Pre-placed High-Entropy Alloy Powder

Microstructure Evolution and Formation of Dual-Phase AlCoCrFeNiSi0.5 High-Entropy Alloy Powders by Mechanical Alloying

Microstructure Evolution and Formation of Dual-Phase AlCoCrFeNiSi0.5 High-Entropy Alloy Powders by Mechanical Alloying

Microstructural, Electrochemical, and Hot Corrosion Analysis of CoCrFeCuTi High Entropy Alloy Reinforced Titanium Matrix Composites synthesized by Microwave Sintering

CoCrFeCuTi High Entropy Alloy (HEA) is reinforced in Ti6Al6V2Sn alloy through microwave sintering-assisted powder metallurgy and its corrosion behaviour is investigated under different conditions. The ball-milled CoCrFeCuTi HEA powder exhibits 17 μm average particle size of irregular fragments with a single-phase BCC structure and is added as reinforcement in Ti alloy at 3, 6, 9, and 12 wt%. As more reinforcement is added, the α-Ti decreases and β-Ti increases which enhances the interfacial bonding. The pinning effects from reinforcements inhibit grain growth contributing to improved properties including higher relative density with less porosity. The 12 wt% composite showed remarkable microhardness of 734 HV which is increased by 43.8% over Ti alloy. The 12 wt% composite also achieved finer grains (0.345 μm) due to uniform internal heat generation from the process. Corrosion behaviour is assessed through electrochemical corrosion and hot corrosion analysis, with 12 wt% composite demonstrating 59.5% better corrosion resistance compared to Ti alloy. The induced corrosion products, formation of passivation films, and their mechanism are examined by morphological analysis.

Microstructure and mechanical properties of Co31.5Cr7Fe30Ni31.5 high-entropy alloy powder produced by plasma rotating electrode process and its applications in additive manufacturing

Microstructure and mechanical properties of feedstock powders critically determine the quality of additive manufacturing (AM). The present study employs a plasma rotating electrode process (PREP) to produce non-equiatomic Co31.5Cr7Fe30Ni31.5 high-entropy alloy (HEA) powders and examines variations of their microstructure and mechanical properties with powder particle size in the range of 20–106 μm. It finds that the powders possess smooth surfaces, good sphericity, and equiaxed polycrystal grains under PREP electrode rod arc speed of 32000 r/min and main arc current of 760 A. A stable FCC structure is maintained regardless of the powder particle size. Moreover, the nano-hardness of the powders generally decreases with the increase of powder particle size except for that of 50–75 μm, which is positively correlated with the change of the grain size. The finest grain size is present for powders with particle sizes of 50–75 μm, which possess the highest average nano-hardness and reduced elastic modulus. Bulk alloys fabricated by cold spray (CS) and laser cladding (LC) AM maintain the FCC structure. The CSAM bulk alloy shows early brittle fracture due to the presence of pores and prior particle boundaries resulting from insufficient plastic deformation of the powder particles. The LCAM bulk alloy presents good tensile properties with the ultimate tensile strength (UTS) and elongation to failure being 481.2 MPa and 35.9%, respectively, which can be attributed to the good cohesion and grain characteristics. The present study shall provide the field of AM with useful information in the applications of non-equiatomic PREP HEA powders.

Unveiling Enhanced Properties via Microstructural Evolution in Stir‐Cast Al6061 Composite Reinforced with AlCrFeNiTi High‐Entropy Alloy Particles

The viability of reinforcing the Al 6061 matrix using AlCrFeNi and AlCrFeNiTi high entropy alloy (HEA) particles is investigated. Body‐centered cubic, A2, and TiC phases are observed in both alloys after 12 h of milling. In situ TiC formation happens during mechanical alloying in AlCrFeNiTi HEA powders. Selected area diffraction patterns are employed in transmission electron investigations to authenticate the presence of distinct phases, affirming their existence within the studied material. Fabricated composites exhibit evenly spaced grains with homogeneous particle dispersion. In comparison to its equivalent, a composite reinforced with AlCrFeNiTi‐C particles exhibits greater grain refinement. Benefiting from dispersion strengthening and grain refinement, both metal matrix composites (MMCs) showcase enhanced attributes. In the case of Al6061/AlCrFeNiTi‐C MMC, a remarkable 25% boost in ultimate tensile strength is achieved, accompanied by a substantial 141.6% improvement in hardness. The findings demonstrate the contribution of HEA particles in improving the characteristics of Al alloys.

Revealing the Microstructure Evolution and Mechanical Properties of Al2O3-Reinforced FCC-CoCrFeMnNi Matrix Composites Fabricated via Gas Atomization and Spark Plasma Sintering

In the present work, novel Al2O3 particles were used to reinforce heterogeneous CoCrFeMnNi high-entropy alloy (HEA) matrix composites with nano- (5.0 wt.%) and nano- + micro- (5.0 wt.% + 10.0 wt.%) specimens. Al2O3 particles were fabricated via gas atomization and spark plasma sintering. The microstructure evolution and properties, i.e., density, hardness, and room temperature compression, were systematically investigated. The results indicate that the concentration of the Cr element in the pure CoCrFeMnNi HEA and the HEA matrix composite can be effectively reduced by using a gas-atomized HEA powder as the matrix. The formation of an impurity phase can also be inhibited, while the distribution uniformity of matrix elements can be improved. The composites prepared via gas-atomized powders formed a network microstructure composed of continuous Al2O3-rich regions and isolated Al2O3-poor regions, exhibiting good plasticity and improved density. The relative densities of the pure HEA, nano- (5.0 wt.%), and nano- + micro- (5.0 wt.% + 10.0 wt.%) composites were 98.9%, 97%, and 94.1%, respectively. The results demonstrate a significant improvement in the relative densities compared to the values (97.2%, 95.7%, and 93.8%) of the composites prepared via mechanical alloying. In addition, compared to the compressive fracture strains of nano- (5.0 wt.%) and nano- + micro- (5.0 wt.% + 10.0 wt.%) composites based on the mechanically alloyed HEA powder, the values of the nano- (5.0 wt.%) and nano- + micro- (5.0 wt.% + 10.0 wt.%) specimens prepared via gas atomization and spark plasma sintering increased by 80% and 67%, respectively.

Synthesis and Characterization Study of Al10Cr25Co20Ni25Fe20 High-Entropy Alloy Powders through Mechanical Alloying

Synthesis and Characterization Study of Al10Cr25Co20Ni25Fe20 High-Entropy Alloy Powders through Mechanical Alloying

Devitrification-Induced Tailoring of Microstructure and Strength in Aluminum High-Entropy Alloy Powder for Cold Spray Deposition

Devitrification-Induced Tailoring of Microstructure and Strength in Aluminum High-Entropy Alloy Powder for Cold Spray Deposition

Effects of Selective Laser Melting Process Parameters on Structural, Mechanical, Tribological and Corrosion Properties of CoCrFeMnNi High Entropy Alloy

The structural, tribological, mechanical, corrosion, and other properties of materials produced by laser-based powder bed fusion additive manufacturing methods are significantly affected by production parameters and strategies. Therefore, understanding and controlling the effects of the parameters used in the manufacturing process on the material properties is extremely important for determining optimum production conditions and for saving time and materials. This study aimed to determine the optimal laser parameter values for CoCrFeMnNi high-entropy alloy powders using the selective laser melting (SLM) method. The layer thickness was kept constant during experimentation. 5 different laser powers and 10 varying laser scanning speeds were tested, with hatch spacing from 30 to 90%. After determining the optimal laser parameters for SLM, prismatic samples were fabricated in different build orientations (0°, 45°, and 90°), and subsequently, their structural, mechanical, tribological, and corrosion properties were compared. Melt pool morphology could not be obtained at 20—40 and 60W laser powers and at all laser scanning speeds used at these laser powers. At 100 W laser power, 600 mm/s laser scanning speed, and 70% hatch spacing parameters, an ultimate tensile stress of 550 MPa and elongation of 48% were obtained. Among the samples produced in different build orientations, the sample produced with a 0° build orientation exhibited the highest relative density (99.94%), the highest microhardness (201.2 HV0.1), the lowest friction coefficient (0.7025), and the lowest wear and corrosion rates (0.7875 mpy). Additionally, SLM parameters were evaluated to have a significant impact on the performance of all properties of the samples.Graphical

Microstructure and mechanical properties of Al0.5CoCrFeNi HEA prepared via gas atomization and followed by hot-pressing sintering

Pre-alloyed Al0.5CoCrFeNi high-entropy alloy (HEA) powders were prepared via gas atomization and followed by hot-pressing sintering (HPS) at 1200 °C for 1 h to fabricate bulk materials. The phase stability, microstructure evolution and mechanical properties of Al0.5CoCrFeNi HEA were mainly investigated. Results indicated that the atomized powders exhibited a fine-grained FCC + dendritic-like ordered BCC (B2) dual-phase structure. Rapid solidification was favorable to the metastable B2 phase formation during gas-atomization. Partial of the dendritic-like B2 phase dissolved after annealing (>600 °C), resulted in a homogeneous dual-phase structure with irregular B2 phase dispersed in the FCC matrix. The homogeneous structure was “inherited” in the sintered bulks and coarsened after HPS. Tensile test results suggested that the sintered bulks possessed excellent comprehensive mechanical properties with yield strength, ultimate tensile strength and elongation of 587.3 ± 18.7 MPa, 960.2 ± 23.6 MPa and 32.6 ± 5.1%, respectively. The excellent mechanical response during deformation was mainly attributed to the synergistic deformation of the FCC/B2 phase and considerable back stress hardening mechanism.

Computational insights into gas atomization of FeCoNiCrMoBSi high-entropy alloy: From droplet formation to rapid solidification

The intricate processes governing the gas atomization of molten metal droplets and their subsequent solidification hold paramount significance in materials science. Computational fluid dynamics simulations have emerged as indispensable tools for unraveling the complexities inherent in metal melt atomization. This study employed the volume of fluid method and the shear-stress transport k-ω turbulence model to simulate the primary atomization process of a FeCoNiCrMoBSi high-entropy alloy. Subsequently, the discrete phase model and Taylor analogy breakup model, based on the gas Weber number and incorporating primary atomization outcomes as initial conditions, were utilized to simulate droplet formation during the secondary atomization process. Analysis of the particle size distribution at the outlet of the geometric model demonstrated excellent agreement with experimental data for gas-atomized FeCoNiCrMoBSi high-entropy alloy powder. Furthermore, comprehensive characterization analyses were conducted to probe the phase constitution and structure of FeCoNiCrMoBSi powder produced by gas atomization. The results revealed that, irrespective of particle size, the powder exhibited a face-centered cubic structure and distinctive eutectic microstructural characteristics. The numerical simulation provided insights into the solidification process of secondary droplets by integrating inverse pole figure data for gas-atomized powder across varying particle sizes. The estimated cooling rate of secondary droplets ranged from 1.22 × 104 K/s to 2.64 × 105 K/s. These findings significantly advance the understanding of the gas atomization mechanism of the FeCoNiCrMoBSi high-entropy alloy, paving the way for the development of more efficient manufacturing processes for advanced materials.

Exploring Microstructural, Interfacial, Mechanical, and Wear Properties of AlSi7Mg0.3 Composites with TiMOVWCr High-Entropy Alloy Powder.

This study explored the impact of varying weight percentages of TiMoVWCr high-entropy alloy (HEA) powder addition on A356 composites produced using friction stir processing (FSP). Unlike previous research that often focused on singular aspects, such as mechanical properties, or microstructural analysis, this investigation systematically examined the multifaceted performance of A356 composites by comprehensively assessing the microstructure, interfacial bonding strength, mechanical properties, and wear behavior. The study identified a uniform distribution of TiMoVWCr HEA powder in the composition A356/2%Ti2%Mo2%V2%W2%Cr, highlighting the effectiveness of the FSP technique in achieving homogeneous dispersion. Strong bonding between the reinforcement and matrix material was observed in the same composition, indicating favorable interfacial characteristics. Mechanical properties, including tensile strength and hardness, were evaluated for various compositions, demonstrating significant improvements across the board. The addition of 2%Ti2%Mo2%V2%W2%Cr powder enhanced the tensile strength by 36.39%, while hardness improved by 62.71%. Similarly, wear resistance showed notable enhancements ranging from 35.56 to 48.89% for different compositions. Microstructural analysis revealed approximately 1640.59 grains per square inch for the A356/2%Ti2%Mo2%V2%W2%Cr processed composite at 500 magnifications. In reinforcing Al composites with Ti, Mo, V, W, and Cr high-entropy alloy (HEA) particles, each element imparted distinct benefits. Titanium (Ti) enhanced strength and wear resistance, molybdenum (Mo) contributed to improved hardness, vanadium (V) promoted hardenability, tungsten (W) enhanced wear resistance, and chromium (Cr) provided wear resistance and hardness. Anticipating the potential applications of the developed composite, the study suggests its suitability for the aerospace sector, particularly in casting lightweight yet high-strength parts such as aircraft components, engine components, and structural components, underlining the significance of the investigated TiMoVWCr HEA powder-modified A356 composites.

Fabrication of mechanically alloyed high entropy alloys (20-Fe-20Cr-20Ni-20Mn-20Ti) modified carbon paste electrode sensor for the cyclic voltammetric determination of methyl orange

We have successfully fabricated high entropy alloys (HEA) of composition 20-Fe-20Cr-20Ni-20Mn-20Ti by ball milling method for 20 h after optimizing the milling parameters. Generally, the HEAs are very popular for their multi-elemental cocktail effect and exhibit excellent high temperature oxidation resistance, high strength, electromagnetic, wear and corrosion resistance properties. But, HEAs also exhibit significant electrocatalytic properties due to their unique morphology, composition, and structure. Therefore, we have used planetary ball milled HEA powders for the electrochemical determination of methyl orange (MO). MO is recalcitrant and very difficult to degrade and can affect the humans as well as the environment. Therefore, we must determine the presence of MO. We have investigated the effect of scan rate, modifier and analyte concentration, and the pH variation on the anodic peak current (Ipa) of MO. The calculated active syrface area of bare carbon paste electrode (BCPE) and HEA-modified carbon paste electrode (HEA-MCPE) were found to be 0.041 cm2 and 0.137 cm2 respectively. We have obtained the maximum oxidation peak current for the 8 mg HEA-MCPE at a pH of 7.2 during the electrochemical oxidation of MO. The increased Ipa in basic medium is due to structural transformation of MO from quinoid form (in acidic medium) to azo structure (in basic medium). We have also calculated the number of electrons and the protons involved in the electrochemical reaction. The calculated values of detection limit (DL) and quantification limit (QL) of 8 mg HEA-MCPE was found to be 0.114 × 10−8 M and 0.38 × 10−8 M respectively.

Powder Synthesis and Characterization of Al0.5CoCrFeNi High-Entropy Alloy for Additive Manufacturing Prepared by the Plasma Rotating Electrode Process.

The Al0.5CoCrFeNi high-entropy alloy powder was produced by using a plasma rotating electrode process. The morphology, microstructure, and physical properties of the powder were characterized. The powder exhibited a smooth surface and a narrow particle size distribution with a single peak. The relationships between particle size and secondary dendrite arm space as well as cooling rate were evaluated as follows: λ = 0.0105d + 0.062 and vc = 4.34 × 10-5d-2 + 2.62 × 10-2d-3/2, respectively. The Al0.5CoCrFeNi powder mainly consisted of fcc + bcc phases. As the powder particle size decreased, the microstructure of the powder changed from dendritic to columnar or equiaxed, along with a decrease in the fcc content and an increase in the bcc content. The tap density (4.76 g cm-3), flowability (15.01 s × 50 g-1), oxygen content (<300 ppm), and sphericity (>94%) of the powder indicated suitability for additive manufacturing.

New insights on bonding mechanism of FCC and BCC high entropy alloy microparticles upon supersonic impact using micromechanical adhesion test

Coating buildup in cold spraying (CS) relies on particle bonding upon impact, thus making it a significant area of study. High entropy alloys (HEAs) are a class of materials with superior work-hardening ability and resistance to softening, making their particle impact and bonding particularly important to understand for their cold sprayability. In this study, the splat adhesion strength is measured with a scratch test for FCC CoCrFeMnNi and BCC AlCrFeMnNi HEA microparticles deposited on mirror-polished SS304 substrates. Nanoindentation tests were conducted to estimate the tensile and shear strengths of the HEA powders. The results showed that particle deformation and jetting were dominant in the FCC HEA/SS304 system, while substrate deformation was dominant in the BCC HEA/SS304 system. Focused ion beam cross sections of particles confirmed that the FCC HEA had good bonding and underwent significant deformation and grain refinement at the substrate/particle interface, while the BCC HEA had limited bonding only in the sheared zone of the particles.In spite of the very limited deformation of BCC splats, their average adhesion strength was measured to be 451 ± 141 MPa, which is significantly higher than that of FCC splats, with an average value of 308.7 ± 69.3 MPa. Fracture surface analysis revealed that FCC splats consistently exhibit ductile fracture, regardless of whether it occurs at the particle, substrate, or interface. In contrast, for BCC splats, fracture was ductile when occurring at the interface and substrate sides, while it was cleavage when occurring on the particle side. These findings suggest that the toughness and shear strength of the bonding developed at the interface were higher than those of the particle. It was found that the flattening ratio (FR) of the particles decreases for both FCC and BCC HEA splats with an increase in particle size, resulting in a decrease in adhesion strength. Metallurgical bonding has been identified as the primary factor contributing to the adhesion strength of both FCC and BCC HEA splats. Particle penetration, indicative of mechanical interlocking, appears to have little or no effect on adhesion strength. However, it does positively influence the increase in adhesion energy of the splats.

Phase transformation and strengthening of the gas-atomized FeCoCrNiMo0.5Al1.3 high-entropy alloy powder during annealing

Phase evolution and strengthening of the FeNiCoCrMo0.5Al1.3 powder alloy produced via inert gas atomization and annealed in the temperature interval of 300–800 °C have been studied by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and microhardness testing. It was found that annealing at 300–600 °C leads to an increase of the element segregations between the several solid solutions with a rise of the lattice misfit (ε) to 1.5 % and microhardness growth to 1070 HV. It was assumed that elastic stress caused by the element partitioning is the main strengthening mechanism: microhardness rises linearly with misfit rise with dHV/dε = 43400 MPa. Sigma arises after the maximum elastic deformation (in 1.5 %) was reached. Formation of the dispersed coherent sigma phase in the annealing interval 600–800 °C results in the microhardness rise. Oxidation that began at 800 °C in 27 h is accompanied with FCC formation due to a depletion of the B2 in Al caused by Al2O3 formation. Estimation of the activation energy of the initial stage of the solid solution decomposition gives a very low value in 0.65eV, apparently caused by the high concentration of quenched vacancies. The activation energy of sigma formation approximately coincides with the activation energy of self-diffusion in BCC metals (about 2.60 eV).