Microstructure and microhardness of high entropy alloys with Zn addition: AlCoFeNiZn and AlCoFeNiMoTiZn

High entropy alloys were designed from equiatomic multicomponent systems using powder metallurgy including mechanical alloying and sintering. The structure and morphology of the resulting alloys were characterized by means of X-ray diffraction, scanning electron microscopy, transmission electron microscopy techniques and their hardness values were also determined in the Vickers scale. The results indicate under the milling conditions used, the AlCoFeNiZn, AlCoFeNiMoTi and AlCoFeNiMoTiZn alloys crystallized forming BCC structures whereas the AlCoFeNi alloy presented two different phases, one with FCC structure and the other one with BCC. The synthesis method resulted in alloys with grain sizes in the nano scale having values between 4.1 and 9.4 nm on the powder form up to 40.1 nm after sintering phenomenon which lead to phase transformations which were more evident in the Mo-containing alloys. In addition, the AlCoFeNiZn and AlCoFeNiMoTiZn alloys did not show Zn traces after sintering as it was suggested by chemical analyses using energy dispersive spectroscopy, suggesting it is lost by evaporation during sintering process. Mo-containing systems exhibited the highest microhardness in both milled and sintered conditions.     

Elemental effect on formation of solid solution phase in CoCrFeNiX and CoCuFeNiX (X = Ti,Zn, Si,Al) high entropy alloys

The paper aims to investigate the effect of elements addition, its enthalpy of mixing, crystal structure and atomic size difference on the formation of solid solution phase during the synthesis of high entropy alloy (HEA) by mechanical alloying. For this CoCrFeNiX and CoCuFeNiX (where X?=?Ti, Zn, Si, Al), alloys were prepared by mechanical alloying. The phases formed during mechanical alloying were characterised by X-ray diffraction analysis, transmission electron microscopy and differential scanning calorimetry. Titanium and Aluminium addition facilitate solid solution formation during mechanical alloying. Formation of a BCC and FCC solid solution phase was observed for CoCrFeNiX and CoCuFeNiX system (where X?=?Ti, Al), respectively. Single solid solution phase was not observed for CoCrFeNiZn, CoCrFeNiSi, CoCuFeNiZn and CoCuFeNiSi HEA up to 20?hours of milling.     

Phase evolution in mechanical alloying and spark plasma sintering of AlxCoCrCuFeNi HEAs

ABSTRACT

Al_xCoCrCuFeNi high-entropy alloys were synthesised through mechanical alloying and spark plasma sintering. Different alloys were produced by varying the aluminium content (x?=?0.5, 1.5, 2.5 and 4). The influences of the milling duration on the evolution of microstructure, constituent phases and morphology were studied. Increasing milling time resulted in grain refinement and higher solid solution homogenisation characterised by a high internal strain. As a consequence of aluminium addition, the microstructure of materials evolved from face centered cubic (FCC) and body centered cubic (BCC) phases to FCC, BCC and ordered BCC phases. Both mechanical alloying and SPS conditions as well as aluminium content led to grain refinement and variations of mechanical properties. In particular, hardness increased with increasing aluminium content. The aluminium percentage and the evolution of consequent phases are responsible for the microstructural stability at high temperatures. In addition, with Al content increase, the further synergy of strength and ductility along with a more pronounced strain hardening was obtained.     

Effect of elemental composition on phase formation during milling of multicomponent equiatomic mixtures

Using mechanochemical synthesis through milling of equiatomic multicomponent mixtures of Cr, Fe, Co, Ni, Al, Ti, Mo, and Nb metals in various combinations, we have synthesized powder alloys with different phase compositions: amorphous phase (AP), AP + BCC phase, AP + BCC phase + MO, and FCC + BCC phases. The FCC phase has been shown to be a Ni-based solid solution. The presence of aluminum in a starting mixture helps to stabilize the BCC phase owing to the formation of a disordered B2 phase. Al dissolves in both the BCC and FCC solid solutions, increasing their lattice parameters. In Al-free starting mixtures, Cr is responsible for the formation of the BCC solid solution. The formation of an AP during milling of multicomponent mixtures is favored by the presence of transition metals with a large atomic radius: Ti, Mo, and Nb.     

Microstructure and mechanical properties of ultra-fine grained MoNbTaTiV refractory high-entropy alloy fabricated by spark plasma sintering

The MoNbTaTiV refractory high-entropy alloy(RHEA) with ultra-fine grains and homogeneous microstructure was successfully fabricated by mechanical alloying(MA) and spark plasma sintering(SPS).The microstructural evolutions,mechanical properties and strengthening mechanisms of the alloys were systematically investigated.The nanocrystalline mechanically alloyed powders with simple bodycentered cubic(BCC) phase were obtained after 40 h MA process.Afterward,the powders were sintered using SPS in the temperature range from 1500 ℃ to 1700 ℃.The bulk alloys were consisted of submicron scale BCC matrix and face-centered cubic(FCC) precipitation phases.The bulk alloy sintered at 1600℃ had an average grain size of 0.58 μm and an FCC precipitation phase of 0.18 μm,exhibiting outstanding micro-hardness of 542 HV,compressive yield strength of 2208 MPa,fracture strength of 3238 MPa and acceptable plastic strain of 24.9% at room temperature.The enhanced mechanical properties of the MoNbTaTiV RHEA fabricated by MA and SPS were mainly attributed to the grain boundary strengthening and the interstitial solid solution strengthening.It is expectable that the MA and SPS processes are the promising methods to synthesize ultra-fine grains and homogenous microstructural RHEA with excellent mechanical properties.     

放电等离子烧结制备AlCoCrFeNi高熵合金的组织演变与力学性能

采用放电等离子烧结方法(SPS)制备了AlCoCrFeNi高熵合金。通过差热分析、密度测试、X射线衍射、扫描电镜及力学性能测试,研究了SPS烧结温度对AlCoCrFeNi高熵合金的致密化行为、组织演变及力学性能影响。结果表明,随着SPS烧结温度的升高,材料的致密度与抗压缩强度明显提高。1200℃烧结后,AlCoCrFeNi高熵合金的致密度达到99.6%,抗压缩强度达到2195MPa,屈服强度达到1506MPa。在SPS烧结过程中,高熵合金从双相结构(BCC+B2)转变为三相结构(BCC+B2+FCC)。     

Nanocrystalline AlCoFeNiTiZn high entropy Alloy: Microstructural,Magnetic, and thermodynamic properties

AlCoFeNiTiZn high entropy alloy was successfully produced in powder form by the mechanical alloying process. The ball-milled alloyed product was characterized by X-ray diffractometry, scanning electron microscopy, energy dispersive spectroscopy, and transmission electron microscopy techniques, which indicated that after 120 h of milling, the solid solution was formed as predicted by thermodynamic calculations. Mechanical alloying began to form the BCC phase almost at 30 h and the FCC phase after about 30 h. Nucleation and growth were the processes involved in the formation of these phases, as shown by the Johnson-Mehl-Avrami kinetic model. Sintering was then used to fabricate the alloy in bulk metallic form. The powders were cold pressed and sintered after 120 h of mechanical alloying using a tube furnace with a controlled atmosphere at 500 °C. A similar FCC + BCC phase mixture was present after sintering. The sintered sample also contained minor amounts of Gahnite (ZnAl₂O₄) spinel material. DSC analysis revealed that recrystallization occurred at 280 °C. The as-milled and as-sintered alloys exhibit semi-hard magnetic properties measured by vibrating sample magnetometer (VSM), with saturation magnetization values of 39.14 and 65.78 emu/g, respectively.     

Structure,mechanical properties and grindability of dental Ti–10Zr–X alloys

This study aimed to investigate the structure, mechanical properties and grindability of a binary Ti–Zr alloy added to a series of alloying elements (Nb, Mo, Cr and Fe). The phase and structure of Ti–10Zr–X alloys were evaluated using an X-ray diffraction (XRD) for phase analysis and optical microscope for microstructure of the etched alloys. Three-point bending tests were performed using a desk-top mechanical tester. Grindability was evaluated by measuring the amount of metal volume removed after grinding for 1 min at each of the four rotational speeds of the wheel (500, 750, 1000 or 1200 m/min). Results were compared with c.p. Ti, which was chosen as a control. Results indicated that the phase/crystal structure, microstructure, mechanical properties and grindability of the Ti–10Zr alloy can be significantly changed by adding small amounts of alloying elements. The alloying elements Nb, Mo, Cr and Fe contributed significantly to increasing the grinding ratio under all grinding conditions, although the grinding rate of all the metals was found to be largely dependent on grinding speed. The Ti–10Zr–1Mo alloy showed increases in microhardness (63%), bending strength (40%), bending modulus (30%) and elastic recovery angle (180%) over those of c.p. Ti, and was also found to have better grindability. The Ti–10Zr–1Mo alloy could therefore be used for prosthetic dental applications if other conditions necessary for dental casting are met.     

Influences of Alloying Elements W, Mo, Cr and Nb on Retained Beta Phase in 47Al Based near γ-TiAl Alloys

The influences of alloying elements W, Mo, Cr, and Nb on retained β phase in 47Al based near γ-TiAI alloys have been studied.The results reveal that the amount of retained β phase is increased by the addition of Cr, Mo, W in rising rank, although the distribution of β phase in Cr-bearing alloys is different from that of Mo- or W-bearing alloys. For Nb-doped alloys, no retained β was found even when 5 at. pct Nb was added. The as-cast microstructural features and the distribution of the β phase in the different alloy families were compared and interpreted in terms of the different segregation behaviour of these elements in Ti.     

粉末冶金TiVNbTa难熔高熵合金的组织和力学性能

将机械合金化(MA)与放电等离子烧结(SPS)相结合制备了难熔TiVNbTa高熵合金,研究了这种合金的机械合金化过程、相组成和显微组织,以及烧结温度和O、N含量对其力学性能的影响。结果表明:机械合金化后高熵合金粉末为BCC结构,放电等离子烧结成的块体高熵合金由BCC基体和FCC析出相组成,其析出相为TiN+TiC+TiO的复合物。烧结温度为1100℃的高熵合金具有良好的综合力学性能,压缩屈服强度达到1506.3 MPa,塑性应变为33.2%。随着烧结温度的提高,合金发生了从准脆性到塑性再到脆性断裂的转变。O和N含量的提高对高熵合金强度的影响较小,但是使其塑性显著降低。     

放电等离子烧结对TiB_2/AlCoCrFeNi复合材料组织与性能的影响

采用放电等离子烧结方法(SPS),制备体积分数5%TiB_2的等摩尔AlCoCrFeNi高熵合金基复合材料。通过密度测试、X射线衍射、扫描电镜及力学性能测试等方法,研究SPS烧结温度及烧结压力对复合材料的微结构演变与力学性能影响。结果表明:随着SPS烧结温度及烧结压力的增加,复合材料的硬度及抗压强度得到明显提高。在1200℃/30MPa进行SPS烧结后,复合材料的致密度达99.6%,抗压强度达2416MPa,屈服强度达1474MPa,硬度超过470HB。烧结过程中,复合材料的基体高熵合金发生相变,1200℃及30~45MPa烧结时,复合材料由BCC,B_2,FCC,σ及TiB_2相组成。     

Effect of alloying elements on microstructure,mechanical and damping properties of Cr-Mn-Fe-V-Cu high-entropy alloys

A series of new Cr-Mn-Fe-V-Cu high-entropy alloys were prepared by arc melting and suction casting. It is found that with the addition of Cu, the structure of the alloys evolved from BCC?+?BCC1 phases to BCC?+?FCC phases. With increase of Cu, the volume fraction of the Cu-Mn-rich FCC phase increased, and the morphology of the FCC phase transformed from granular particles to long strips and blocks. Compared with other reported HEAs, the Cr-Mn-Fe-V-Cu HEAs exhibit a good balance between strength and ductility. The CrMn0.3FeVCu0.06 alloy with granular FCC particles exhibits the highest compressive yield strength (1273?MPa) and excellent ductility (ε_f?=?50.7%). Quantitative calculations for different strengthening mechanisms demonstrate that dislocation and precipitate strengthening are responsible for high strength of the CrMn0.3FeVCu0.06 alloy, while the solid solution strengthening effect is very low because of its small atomic-size difference. In addition, the CrMn0.3FeVCu0.06 alloy exhibits good damping capacity due to its high dislocation and interface damping effects. Therefore, the dislocation density and distribution of FCC phase are the crucial factors for improvement of both mechanical properties and damping capacity of the HEAs.     

多主元高熵合金FeCoNiCuxAl微观组织结构和性能

研究了不同Cu含量的FeCoNiCuxAl高墒合金的微观引织和性能特点,（x表示摩尔比,x=0、0．5、0．8、1．0、1．5、2）,分别用X衍射、扫描电镜和维氏硬度测试Cu含量的变化对合金组织和硬度的影响。研究表明,此合金体系容易形成简单FCC结构和BCC结构的固溶体,Cu含量增加会促进FCC固溶体的形成。Ca的含量的变化对合金硬度的影响较大。随着Cu含量的增加,合金的硬度显著降低,硬度的高低主要取决于显微组织形态和体系中BCC固溶体的含量的多少。     

Corrosion and in vitro biocompatibility properties of cryomilled-spark plasma sintered commercially pure titanium

Ti alloys, such as Ti6Al4V, are currently used in biomedical and dental implant applications. Ti alloys are used because they are stronger than commercially pure (CP) Ti due to the presence of alloying elements. However, toxicity of alloying elements during long-term use of implants is of concern. Another means of increasing the strength of materials is grain size refinement. In this study, ultrafine-grained (UFG, ~250 nm to 1 μm) CP Ti was produced by cryomilling followed by spark plasma sintering (SPS). Electrochemical impedance spectroscopy (EIS) and cell culture experiments were performed to compare the corrosion and biocompatibility properties of coarse grained (CG) Ti and UFG Ti. It was found that UFG Ti exhibited corrosion resistance comparable to CG Ti in Ringers solution. In addition, UFG Ti exhibited a reduced inflammatory response and enhanced cell adhesion compared to CG Ti. Investigation of surface roughness provided an explanation for enhanced cell adhesion.     

Strain-driven phase transition of molybdenum nanowire under uniaxial tensile strain

The phase transition processes of a single Mo nanowire under uniaxial tensile strains have been studied with molecular dynamics simulation. Two phase transitions were observed during the uniaxial tensile processes. The first one is the configuration of Mo nanowire transformed from BCC structure to FCC structure and the second one is that transformed from FCC-to-BCC. The phase structures have also been demonstrated with radial distribution function (RDF) analyses. A pseudoelasticity behavior was observed under large uniaxial tensile strain. Two average atomic energy curves of BCC and FCC structures as the function of the layer-space along [0 0 1] direction were obtained with embedded-atom method potential calculations, with which the strain-driven BCC-to-FCC and FCC-to-BCC phase transition mechanisms have been clarified clearly for Mo nanowire under uniaxial tensile strain.     

Tailoring mechanical and magnetic properties of AlCoCrFeNi high-entropy alloy via phase transformation

Phase constitutions,either changed by alloying or by phase transformation,are the key factors to determine the magnetic and mechanical performances of high-entropy alloys (HEAs).Using the AlCoCrFeNi HEA as a candidate alloy,this paper demonstrates the effect of phase transformation on both the mechanical and magnetic properties in the multi-phase system.With increasing heat treatment temperature,the sigma (σ) and face-centered-cubic (FCC) phases disappeared at 1000 ℃ and 1200 ℃,respectively.Such volume fraction changes ofσ,FCC and body-centered-cubic (BCC) phases have divergent effects on mechanical and magnetic properties.The excellent strength-ductility combination will be achieved as the disappearance of σ phase and formation of FCC phase.As for the magnetic properties,the volume fraction of BCC phase plays a major role in determining its saturation magnetization.When the volume fraction change of BCC phase is not evident,the higher volume fraction of FCC phase will influence its magnetization at 2 T.Our present work might provide insights into analyzing the evolution of both mechanical and magnetic properties of HEAs caused by complex phase transformation.     

Fabrication and properties of nanocrystalline Co0.5FeNiCrTi0.5 high entropy alloy by MA–SPS technique

Most of multi-component high entropy alloys were designed as equi-atomic or near equi-atomic and were mainly prepared by vacuum arc melting. The present paper reports synthesis of inequi-atomic Co_0.5FeNiCrTi_0.5 high entropy alloy by mechanical alloying and spark plasma sintering (MA–SPS). Alloying behavior, microstructure and properties of Co_0.5FeNiCrTi_0.5 alloy are investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and instron testing system, respectively. Both BCC and FCC crystal structure phases are observed after MA, while a FCC phase and additional sigma phase are noticed after SPS. Moreover, numerous nanostructured phases are founded in the alloy after consolidated by SPS. The alloy with a density of 99.15% after SPS exhibits excellent comprehensive mechanical properties. The yield stress, compressive strength, compression ratio and Vickers hardness of the alloy are 2.65 GPa, 2.69 GPa, 10.0% and 846 HV, respectively. The fracture mechanism of this alloy is observed as cleavage fracture and intergranular fracture.     

陶瓷颗粒增强Cr0.5MoNbWTi难熔高熵合金复合材料的制备及其力学性能

难熔高熵合金因其优异的力学性能、高温稳定性和抗氧化性能等,作为高温结构材料具有广阔的应用前景.为了进一步提升材料的力学性能,本研究利用原位反应烧结制备了陶瓷颗粒增强难熔高熵合金复合材料,并探讨了陶瓷增强相的生成机理及其对复合材料力学性能的影响.通过机械合金化制备了含有碳氮氧非金属元素的Cr0.5MoNbWTi过饱和体心...     

Fabrication of Ti–Nb–Ag alloy via powder metallurgy for biomedical applications

Ti and some of its alloys are widely used as orthopedic implants. In the present study, Ti–26Nb–5Ag alloys were prepared by mechanical alloying followed by vacuum furnace sintering or spark plasma sintering (SPS). The microstructure and mechanical properties of the Ti–Nb–Ag alloys were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDX), compressive and micro-hardness tests. The effect of different sintering methods on the microstructure and properties of Ti–Nb–Ag alloy was discussed. The results showed that the titanium alloy sintered by vacuum furnace exhibited a microstructure consisting of α, β and a small amount of α″ martensite phase; whilst the SPS sintered alloy exhibited a microstructure consisting of α, β and a small amount of α″ martensite phase, as well as a nanostructured Ag homogeneously distributed at the boundaries of the β phases. The Ti–Nb–Ag alloy sintered by SPS possessed fracture strength nearly 3 times of the alloy sintered by vacuum furnace.     

On the elemental effect of AlCoCrCuFeNi high-entropy alloy system

The AlCoCrCuFeNi high-entropy alloy system was synthesized using a well-developed arc melting and casting method. Their elemental effect on microstructures and hardness was investigated with X-ray diffraction, scanning electron microscopy and Vickers hardness testing. The alloys exhibit quite simple FCC and BCC solid solution phases. Co, Cu and Ni elements enhance the formation of the FCC phase while Al and Cr enhance that of the BCC phase in the alloy system. BCC phases form a spinodal structure during cooling. Copper tends to segregate at the interdendrite region and forms a Cu-rich FCC phase. Low copper content renders the interdendrite as a thin film and the as-cast structure like recrystallized grain structure. The formation of BCC phases significantly increases the hardness level of the alloy system. The strengthening mechanism is discussed.