Influence of sintering time on microstructure and properties of hot oscillatory pressing sintered W–Cu refractory alloys

W–Cu refractory alloys are widely used in aerospace,aviation,electronics,power,and other fi elds.However,because of its large melting point diff erence between alloy elements,the conventional powder metallurgy method required a long time of high temperature sintering is very likely to cause low density and abnormal grain size growth.Therefore,90W-10Cu refractory alloys were successfully prepared by hot oscillatory pressing(HOP)under diff erent sintering time in this work.Then the infl uence of sintering time on the microstructure,grain size,density,Vickers hardness,room-tensile property,and electrical conductivity of the W–Cu refractory alloy was systematically invested.The results showed that during the short sintering time(30–90 min),the density,Vickers hardness,tensile strength,and electrical conductivity of the W–Cu refractory alloy increased signifi cantly to 98.7%,163.29 HV 30,507.3 MPa,and 14.2%International Annealed Copper Standard with the sintering time increasing,respectively,while its grain size showed no obvious change.When the sintering time further increased to 120 min,the density was basically consistent with the sintering time of 90 min.Nevertheless,the prolonged high temperature sintering resulted in the grain growth of the samples,which caused the deterioration of the Vickers hardness,room-tensile strength,and conductivity properties of the W–Cu refractory alloy.At the same sintering time,the density,Vickers hardness,and electrical conductivity of the HOP sintered W–Cu refractory alloy were signifi cantly higher than those of the HP sintered sample.It was indicated that high density,fi ne-grain,and excellent properties W–Cu refractory alloys could be prepared by hot oscillatory pressing under appropriate sintering time.

Spark plasma sintering of tungsten-based WTaVCr refractory high entropy alloys for nuclear fusion applications

W-based WTaVCr refractory high entropy alloys (RHEA) may be novel and promising candidate materials for plasma facing components in the first wall and diverter in fusion reactors. This alloy has been developed by a powder metallurgy process combining mechanical alloying and spark plasma sintering (SPS). The SPSed samples contained two phases, in which the matrix is RHEA with a body-centered cubic structure, while the oxide phase was most likely Ta2VO6through a combined analysis of X-ray diffraction (XRD),energy-dispersive spectroscopy (EDS), and selected area electron diffraction (SAED). The higher oxygen affinity of Ta and V may explain the preferential formation of their oxide phases based on thermodynamic calculations. Electron backscatter diffraction (EBSD) revealed an average grain size of 6.2μm. WTaVCr RHEA showed a peak compressive strength of 2997 MPa at room temperature and much higher micro-and nano-hardness than W and other W-based RHEAs in the literature. Their high Rockwell hardness can be retained to at least 1000°C.

Recent progresses on designing and manufacturing of bulk refractory alloys with high performances based on controlling interfaces

Refractory alloys such as tungsten and molybdenum based alloys with high strength,thermal/electrical conductivity,low coefficient of thermal expansion and excellent creep resistances are highly desirable for applications in nuclear facilities,critical components in aerospace and defense components.However,the serious embrittlement limits the engineering usability of some refractory alloys.A lot of research results indicate that the performances of refractory alloys are closely related to the physical/chemical status,such as the interface dimension,interface type,interface composition of their grain boundaries(GBs),phase boundaries(PBs)and other interface features.This paper reviewed the recent progress of simulations and experiments on interface design strategies that achieve high performance refractory alloys.These strategies include GB interface purifying/strengthening,PB interface strengthening and PB/GB synergistic strengthening.Great details are provided on the design/fabrication strategy such as GB interface controlling,PB interface controlling and synergistic control of multi-scaled interfaces.The corresponding performances such as the mechanical property,thermal conductivity,thermal load resistance,thermal stability,irradiation resistance,and oxidation resistance are reviewed in the aspect to the effect of interfaces.In addition,the relationships between these interfaces and material properties are discussed.Finally,future developments and potential new research directions for refractory alloys are proposed.

Microstructure and nano-mechanical property of cold spray Co-base refractory alloy coating

Co-base refractory alloy coating was prepared on carbon steel substrate by cold spray technology; microstructure and nano-mechenieal property were examined by scanning electron microscope （SEM） and nano indenter individually. The results showed that about 250 μm Co-base refractory alloy coating could be deposited o11 steel substrate by cold spray technique, interface between coating and substrate was combined well, and the refractory alloy particle had a significant plastic deformation during deposition process; mixing Ni powders into Co-base refractory alloy powders could increase the density and decrease the nano-hardness of coating, the nano-hardness and elastic modulus of refractory alloy coating was higher than 6 GPa and 160 GPa, respectively.

A review of refractory high-entropy alloys

This work reviews recent progress in the alloy design,microstructure,and mechanical properties of refractory high-entropy alloys(RHEAs).What’s more,the underlying strengthening mechanisms and deformation behavior are discussed.Composed mainly of near-equimolar refractory elements,RHEAs have superior mechanical properties,especially at high temperatures.However,many of them have limited room-temperature ductility.Much work has been done to solve this trade-off,and some of the RHEAs have the potential to be used for high-temperature applications in the future.In addition to their mechanical properties,RHEAs have other attractive properties,such as biocompatibility and wear resistance,which are discussed.Finally,current problems and future suggestions for RHEAs are discussed.

Research Progress of Refractory High Entropy Alloys:A Review

Owing to superior comprehensive performance than conventional superalloys at high temperature,refractory high entropy alloy(RHEA)is becoming a promising candidate for the next generation high-temperature material.Herein,contemporary aspects of corresponding development of RHEAs are reviewed to discuss various factors affecting the organization structure and service performance.It mainly covers alloying system and strengthening mechanism,the preparation method,plastic deformation and the related mechanism,as well as microstructure control by heat treatment.Firstly,the alloy systems and strengthening mechanism are introduced.This is followed by different preparation methods and the comparison of strengths and shortcomings based on different RHEAs.Then,hot deformation behavior and plastic deformation under different loadings are analyzed.Based on this,the influence of heat treatment on microstructures prior to and after the deformation is further summarized.Finally,some important research areas to be carried out in future are pointed out.This review will give a deep understanding of the effects of different factors on the service performance and provide scientific guide in designing RHEAs with improved performance.

Microstructure and mechanical properties of a low activation cast WTaHfTiZr refractory high-entropy alloy

In the face of the requirement that nuclear fusion reactor materials exhibit more excellent thermal,mechanical and physical properties,a novel refractory highentropy alloy,WTaHfTiZr was proposed.The constituent elements were selected in consideration of low activation,high melting point and high thermostability.The alloys were prepared by arc melting.The as-cast alloy shows a dendrite microstructure with two disordered BCC phases,which caused by the preferential nucleation of W and Ta with much higher melting points during solidification.It exhibits a high compressive yield strength of 1,900 MPa and fracture strain of 8.1% at room temperature,and its yield strengths are up to 612 MPa at 700 ℃ and 203 MPa at 1,000 ℃,respectively.The high strengths are attributed mainly to solid solution strengthening and second phase strengthening.This alloy shows great promise as one of the next-generation nuclear fusion reactor materials.

A Nitride-Reinforced NbMoTaWHfN Refractory High-Entropy Alloy with Potential Ultra-High-Temperature Engineering Applications

Refractory high-entropy alloys(RHEAs)have promising applications as the new generation of hightemperature alloys in hypersonic vehicles,aero-engines,gas turbines,and nuclear power plants.This study focuses on the microstructures and mechanical properties of the NbMoTaW(HfN)_(x)(x=0,0.3,0.7,and 1.0)RHEAs.The alloys consist of multiple phases of body-centered cubic(BCC),hafnium nitride(HfN),or multicomponent nitride(MN)phases.As the x contents increase,the grain size becomes smaller,and the strength gradually increases.The compressive yield strengths of the NbMoTaWHfN RHEA at ambient temperature,1000,1400,and 1800℃ were found to be 1682,1192,792,and 288 MPa,respectively.The high-temperature strength of this alloy is an inspiring result that exceeds the high temperature and strength of most known alloys,including high-entropy alloys,refractory metals,and superalloys.The HfN phase has a significant effect on strengthening due to its high structural stability and sluggish grain coarsening,even at ultra-high temperatures.Its superior properties endow the NbMoTaWHfN RHEA with potential for a wide range of engineering applications at ultra-high temperatures.This work offers a strategy for the design of high-temperature alloys and proposes an ultra-high-temperature alloy with potential for future engineering applications.

Phase,microstructure and compressive properties of refractory high-entropy alloys CrHfNbTaTi and CrHfMoTaTi

New refractory high-entropy alloys,CrHfNbTaTi and CrHfMoTaTi,derived from the well-known HfNbTaTiZr alloy through principal element substitution were prepared using vacuum arc melting.The phase components,microstructures,and compressive properties of the alloys in the as-cast state were investigated.Results showed that both alloys were composed of BCC and cubic Laves phases.In terms of mechanical properties,the yield strength increased remarkably from 926 MPa for HfNbTaTiZr to 1258 MPa for CrHfNbTaTi,whereas a promising plastic strain of around 15.0%was retained in CrHfNbTaTi.The morphology and composition of the network-shaped interdendritic regions were closely related to the improved mechanical properties due to elemental substitution.Dendrites were surrounded by an incompact interdendritic shell after Mo incorporation,which deteriorated yield strength and accelerated brittleness.

Hot deformation behavior of spray forming LSHR alloy using constitutive equation and processing map

Flow behaviors of spray forming low solvus high refractory (LSHR) alloy were investigated using hot compression tests performed on a Gleeble?3500 thermal mechanical simulator at temperatures of 1020?1150 °C and strain rates of 0.0003?1.0 s?1. The constitutive equation was established, power dissipation (η) maps and hot processing maps were plotted. The microstructure evolution and dislocation distribution of domains with different values of η in power dissipation maps were also observed. The results show that the flow stress increases with decreasing temperature and increasing strain rate. The activation energy of the spray forming LSHR alloy is 1243.86 kJ/mol. When the value of η is 0.36 at the strain of 0.5, the domain in the processing map shows characteristics of typical dynamic recrystallization (DRX) and low dislocation density. According to the microstructure evolution and processing maps, the optimum processing condition for good hot workability of spray forming LSHR alloy can be summed up as:temperature range 1110?1150 °C; strain rate range 0.01?0.3 s?1.

Phase evolution and mechanical properties of low-activation refractory high-entropy alloy Ti_(1.5)ZrV_(0.5)Ta_(0.5)

A novel low-activation Ti_(1.5)ZrV_(0.5)Ta_(0.5)refractory high-entropy alloy(RHEA)was designed as a potential candidate for nuclear reactor application.At room temperature,it had an elongation of 8.4%and a yield strength of 1096 MPa.The phase evolution of this alloy and its effect on properties was investigated.At 400℃,the solid solution bcc 1 transformed into the fcc phase and bcc 2 phase,and theωphase andαphase also appeared.At 600℃,theωphase andαphase disappeared,and the microstructure of the alloy was composed of the fcc phase and bcc 2 phase.When the temperature was up to 1200℃,the fcc phase and bcc 2 phase re-transformed into solid solution bcc 1 phase.The precipitation ofωphase andαphase caused a sharp increase in strength and a decrease in plasticity.Meanwhile,the appearance of the fcc phase led to a simultaneous decrease in strength and ductility,due to larger stress concentrations at the fcc/bcc interface.Besides,the formation mechanism of each phase in the alloy was discussed in detail.

Microstructure and Mechanical Properties of the Ti_(62)Nb_(12)Mo_(12)Ta_(12)W_(2)Refractory High Entropy Alloy Prepared through Spark Plasma Sintering

A refractory high entropy alloy Ti_(62)Nb_(12)Mo_(12)Ta_(12)W_(2)was prepared by mechanical alloying and spark plasma sintering.The microstructure and mechanical properties of the Ti_(62)Nb_(12)Mo_(12)Ta_(12)W_(2)alloy were analyzed.The experimental results show that the microstructure of the alloy is composed of two BCC phases,an FCC precipitated phase,and the precipitated phase which is a mixture of TiC,TiN and TiO.The alloy exhibits good room temperature compressive properties.The plasticity of the sample sintered at 1550℃can reach 10.8%,and for the sample sintered at 1600℃,the yield strength can be up to 2032 MPa,in the meantime the plasticity is 9.4%.The alloy also shows high strength at elevated temperature.The yield strength of the alloy exceeds 420 MPa at 900℃,and value of which is still above 200 MPa when the test temperature reaches 1000℃.Finally,the compressive yield strength model at room temperature is constructed.The prediction error of the model ranges from−7.9%to−12.4%,expressing fair performance.

Microstructure Modification and Ductility Improvement for TaMoNbZrTiAl Refractory High Entropy Alloys via Increasing Ti Content

Here, the composition of TaMoNbZrTiAl refractory high entropy alloy (RHEA) is optimized by increasing Ti content to improve its mechanical property especially the ductility, through comparing two RHEAs with different Ti content. The RHEAs contain two body-centered-cubic (BCC) phases. The BCC phase in the dendritic region is rich in Ta, Mo and Nb, and the BCC phase in the interdendritic region is enriched in Zr, Ti and Al. The as-cast RHEA with a higher Ti content remains dendritic microstructures, and Ti is mainly enriched in the interdendritic region. After annealing treatment at 1300 ℃ for 48 h, the dendritic microstructures change into equiaxed-grain morphology, accompanied by needle-like micron precipitates at grain boundaries in the RHEA with higher Ti content. For the as-cast RHEAs, the fracture strain increases by ~ 6.6% and the uniform plastic strain increases by ~ 5.9% at the compression test due to the increase of Ti content. Our work offers a reference for the composition design of RHEAs and makes a preliminary exploration of the optimization of the microstructures and mechanical properties.

Microstructure Recrystallization and Mechanical Properties of a Cold-Rolled TiNbZrTaHf Refractory High-Entropy Alloy

The equiatomic TiNbZrTaHf alloy was successfully rolled at room temperature with the reduction of ~ 85%. The microstructure and tensile properties were investigated after cold working and annealing. It was determined that the recrystallization temperature of the TiNbZrTaHf alloy between 850 and 900 ℃. Complete recrystallization and normal grain growth occurred, the high stability of single phase was maintained after annealing at 1000, 1200, and 1400 ℃. But the precipitated phase appeared after long term annealing, as seen after 500 h at 1000 ℃. After cold working, the tensile strength and the elongation of TiNbZrTaHf were 1137 MPa and 25.1%, respectively. The annealed alloy has a high tensile strength (σ_(b )= 863 MPa) and ductility (ε_(e )= 28.5%). Moreover, the oxidation of TiNbZrTaHf alloy at elevated temperatures has a significant impact on its mechanical properties. The poor oxidation resistance of TiNbZrTaHf can accelerate tensile failure by inducing fractures at grain boundaries.

D0_(22) precipitates strengthened W-Ta-Fe-Ni refractory high-entropy alloy

Refractory high-entropy alloys have recently emerged as promising candidates for high-temperature structural applications.However,their performance is compromised by the trade-off required between strength and ductility.Here,a novel W30Ta5(FeNi)65 refractory high-entropy alloy with an outstanding combination of strength and plasticity at both room and elevated temperatures is designed,based on the multi-phase transitions design strategy.The alloy comprises a body-centered cubic dendrite phase,a topologically close-packed μ rhombohedral phase,and a high-density coherent nano-precipitate γ"phase with the D0_(22)structure(Ni3Ta type)embedded in a continuous face-centered cubic matrix.Owing to pre-cipitation strengthening of D0_(22),the yield stress of the alloy is determined as high as 1450 MPa,which is a significant improvement(~100%)in comparison with the D0_(22)-free alloy,without a loss of ductil-ity.This alloy exhibits an excellent high-temperature strength,with the yield strengths of 1300 MPa at 600 ℃ and 320 MPa at 1000 ℃.Detailed microstructural characterization using transmission electron mi-croscopy,high-angle annular dark-field imaging,and three-dimensional atom probe tomography analyses indicated that this superior strength-plasticity combination stems from the synergy of a multiple-phase structure.These results provide a new insight into the design of RHEAs and other advanced alloys.

NbMoTiVSi_(x) refractory high entropy alloys strengthened by forming BCC phase and silicide eutectic structure

In order to improve mechanical properties of refractory high entropy alloys,silicide was introduced and NbMoTiVSi_(x)(x=0,0.1,0.2,0.3,and 0.4,molar ratio) refractory high entropy alloys are prepared by vacuum arc melting.Phase composition,micro structure evolution and mechanical properties were systematically studied.Results show that the silicide phase is formed in the alloys with addition of silicon,and the volume fraction of silicide increases from 0 to 8.3 % with increasing of silicon.Microstructure observation shows that the morphology of dendrite changes from columnar to near equiaxed,eutectic structure is formed at grain boundaries and composed of secondary BCC phase and silicide phase.The average length of the primary and second dendrites decreases with the increasing of silicon.Whereas,the ratio of eutectic structure increases from 0 to 19.8 % with the increment of silicon.The refinement of microstructure is caused by heterogeneous nucleation from the silicide.Compressive tests show that the yield and ultimate strength of the alloys increases from 1141.5 MPa to 2093.1 MPa and from 1700.1 MPa to 2374.7 MPa with increasing silicon content.The fracture strain decreases from 24.7 %-11.0 %.Fracture mechanism is changed from ductile fracture to ductile and brittle mixed fracture.The improvement of the strength is caused by grain bounda ry strengthening,which includes more boundaries around primary BCC phase and eutectic structure in grain boundary,both of them is resulted from the formation of silicide.

Microgravity Material Research in China:2012–2014

During 2012–2014, the main research activities from microgravity material research were focused on, which include study of microgravity effects on collagen fibrillogenesis and HAP crystallization, microgravity experiments using drop tube, and research of thermoelectric materials for space.This paper summarizes all these activities.

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 0.58μm and an FCC precipitation phase of 0.18μm,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.

Refractory high-entropy alloys:A focused review of preparation methods and properties

In recent years,high-entropy alloys(HEAs)have become prominent metallic materials due to their unique design strategies and excellent mechanical properties.The HEAs-inherent high-entropy,lattice-distortion,sluggish-diffusion,and cocktail effects make HEAs maintain high strength,oxidation resistance,corrosion resistance,wear resistance,and other excellent comprehensive properties,showing stronger competitiveness relative to traditional alloys.Refractory high-entropy alloys(RHEAs)are considered as a new kind of high-temperature materials with great application prospects due to their excellent mechanical properties and have the potential to replace nickel-based superalloy as the next generation of high-temperature materials.We reviewed the research status and preparation methods of RHEAs in recent years,including the metallurgical smelting,powder metallurgy,magnetron sputtering,and additive manufacturing technologies.The microstructure and phase-transformation process of RHEAs were analyzed.The mechan-ical properties and main strengthening and toughening mechanisms of RHEAs,such as solid-solution strengthening,precipitation strengthening,and the transformation-induced plasticity(TRIP),were discussed,and the deformation mechanism of RHEAs was revealed.The properties of RHEAs,including high strength,oxidation resistance,corrosion and wear resistance were reviewed.RHEAs will meet the huge market demand in the engineering materials field,but there are still many challenges,such as the tradeoff between high strength and high ductility,structural design,and performance optimization of RHEAs with brittle BCC structures.We believe that this combination of knowledge may shape the future of RHEAs and break through the mutually exclusive conundrum of high strength and high toughness for RHEAs.

Light-weight refractory high-entropy alloys: A comprehensive review

In recent years,high-entropy alloys(HEAs)have become a research hotspot in materials community,and great progress has been made in exploring various high-performance HEAs.As a special class,the light-weight refractory high-entropy alloys(RHEAs)own both excellent high-temperature comprehensive properties and low density and have accordingly attracted more and more attention.In this paper,we presented a comprehensive review of the recent progress and status in light-weight RHEAs.Based on an exhausting search of the literature reports,one strategy in terms of phase numbers after preparation was first proposed to classify the light-weight RHEAs into three categories.Then,the status on the fundamental thermodynamic and thermophysical data/databases,computational approaches for alloy designing,and preparation/fabrication techniques of light-weight RHEAs was introduced one after another.After that,the progress on mechanical properties and oxidation/corrosion/wear behaviors of light-weight RHEAs at room and high temperatures was summarized.Finally,the conclusions of this review were drawn.By pointing out the shortcomings of the current research,the follow-up development directions in the field of light-weight RHEAs were also given.