CN108220742A - A kind of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys and preparation method thereof - Google Patents

A kind of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys and preparation method thereof Download PDF

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CN108220742A
CN108220742A CN201810208569.5A CN201810208569A CN108220742A CN 108220742 A CN108220742 A CN 108220742A CN 201810208569 A CN201810208569 A CN 201810208569A CN 108220742 A CN108220742 A CN 108220742A
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alloy
melting
entropy
infusibility
infusibility high
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CN108220742B (en
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薛云飞
曹堂清
王本鹏
王富耻
王鲁
刘旭东
岳晗
才鸿年
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Beijing Zhongchen Zhigang Technology Co ltd
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Beijing Institute of Technology BIT
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting

Abstract

The present invention relates to a kind of microalloying Ti Zr Hf V Nb Ta infusibility high-entropy alloys and preparation method thereof, belong to technical field of metal material.The infusibility high-entropy alloy mainly by adjusting the proportioning of major components and adding a small amount of micro alloying element, makes infusibility high-entropy alloy have both good plasticity and higher intensity, and can adjust its density in a wider scope；In addition, in preparation process, high-melting-point Hf, Nb, Ta and the micro alloying element in addition to Al are first subjected to pre-alloyed melting, then addition Ti, Zr, V and Al carries out final alloying smelting, it is advantageously ensured that the uniform mixing of the huge several constituent elements of different melting points, ensures that prepared infusibility high-entropy alloy has excellent comprehensive performance.

Description

A kind of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys and preparation method thereof
Technical field
Present invention relates particularly to a kind of microalloying Ti-Zr-Hf-V-Nb-Ta infusibilities for having both high intensity and good plasticity High-entropy alloy and preparation method thereof belongs to technical field of metal material.
Background technology
High-entropy alloy is also referred to as multi-principal elements alloy, is a kind of novel alloy that developed recently gets up, is defined as by five kinds And Yi Shang element by wait atomic ratios or it is near wait former molecular alloy, the content of each major components is 5~35at.%；In addition, Other alloying elements can also be added and carry out alloying, additive amount is less than 5at.%.More pivot compositing characteristics of high-entropy alloy, no Being same as conventional alloys has specific matrix element (such as Fe based alloys, Ti based alloys, Al based alloys and Ni based alloys), so There is the very high entropy of mixing, and the high entropy of mixing can stablize solid solution phase, make this kind of conjunction under liquid or random solid solution state Gold utensil has better simply phase composition and microscopic structure.
Due to more pivot effects (high entropic effect, sluggish diffusion effect, distortion of lattice effect and cocktail effect), high entropy closes The metallurgical physical action mechanism of gold is different from conventional alloys, so as to show a series of excellent performances, such as prominent high temperature Intensity, good low-temperature flexibility, wear-resisting property, corrosion resistance and excellent anti-radiation performance etc..Therefore, high-entropy alloy has Wide application prospect, such as：The cutter and mold of high intensity, high rigidity；Wear-resistant corrosion-resistant coating；Turbo blade, welding pricker Material and heat exchanger heat proof material；High strength structure material；Bio-medical material etc..
The typical high-entropy alloy reported at present can be divided into four types：Using Co, Cr, Fe, Ni, Mn and Cu mainly to form The FCC configuration solid solution high-entropy alloy of element, typically there is CoCrFeNi, CoCrFeNiMn and CoCrFeNiCu；Co, Cr, The BCC structure solid solution high-entropy alloys that Al or/and Ti elements are formed are added on the basis of Fe, Ni, Mn and Cu, are typically had AlCoCrFeNi and AlCrFeCoNiTi0.5；The infusibility being made of high-melting-point element ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W is high The solid solution of entropy alloy, generally BCC structures；High entropy non-crystaline amorphous metal Zn with disordered structure20Ca20Sr20Yb20 (Li0.55Mg0.45)20, PdPtCuNiP and TiZrCuNiBe etc..Wherein, most commonly used FeCoCrNiMn high-entropy alloys tool is studied There is up to 60% stretching plastic, but yield strength is less than 300MPa.Infusibility high-entropy alloy has yield strength height, high temperatures The good advantage of energy has application prospect in high-temperature material field；However, there are the poor (rooms of plasticity for existing infusibility high-entropy alloy Temperature is almost without stretching plastic), the problems such as density is high (generally more than 8g/cm3).This significantly limits infusibility high-entropy alloy There is the good strong matched infusibility high-entropy alloy of plasticity to be of great significance for practical application, therefore, exploitation.
Invention content
For existing infusibility high-entropy alloy plasticity it is poor the problem of, the purpose of the present invention is to provide a kind of microalloying Ti- Zr-Hf-V-Nb-Ta infusibility high-entropy alloys and preparation method thereof, mainly by adjusting the proportioning of major components and adding a small amount of micro- Alloy element makes infusibility high-entropy alloy have both good plasticity and higher intensity, and can adjust in a wider scope Save its density；In addition, prepared using ripe molten alloy chemical industry skill, it is easy to operate.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys, the infusibility high-entropy alloy be by Ti, Zr, Hf, V, Nb, Ta and micro alloying element composition, chemical formula are denoted as TiaZrbHfcVdNbeTafMx；
Wherein, the M is one or more of Al, Cr, Mo, W, Mn, Fe, Co, Ni and Si；A=15~45, b=5~ When being 0 when 35, c=5~35, d=0~35, e=0~35, f=5~40, x=0.1~15,15≤b+c≤70, d with e difference 5≤d+e+f≤70。
A kind of preparation method of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys of the present invention, the method Include the following steps：
(1) under argon atmosphere, clean elemental metals Hf, Nb, Ta and M (except Al) is subjected to alloying and melted Refining, the aluminium alloy I that melting obtains is cooled down, obtains alloy pig I；Alloy pig I is overturn again, melting 2 times or more is repeated, obtains To pre-alloyed alloy pig；
(2) under argon atmosphere, clean elemental metals Ti, Zr, V, Al and pre-alloyed alloy pig are carried out The aluminium alloy II that melting obtains is cooled down, obtains alloy pig II by alloying smelting；Alloy pig II is overturn again, is repeated molten Refining 4 times or more, obtains the infusibility high-entropy alloy.
Wherein, alloying smelting is using vacuum melting.
In addition, according to the geomery of required product, it can be by prepared infusibility high-entropy alloy under argon atmosphere Remelting is heated, and the aluminium alloy after fusing is cast in corresponding mold and is molded, so as to obtain micro- conjunction of specific shape Aurification Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys.
Advantageous effect：
(1) infusibility high-entropy alloy of the present invention forms phase using BCC phases to be main, the valence electron numbers of major components compared with It is small, there is good plasticity, and the addition of micro alloying element, remain the feature of alloy high strength, thus the infusibility High-entropy alloy has both good plasticity and higher intensity.
(2) density of infusibility high-entropy alloy of the present invention is adjustable in a wider scope, between 5.5g/cm3~ 12g/cm3, the requirement of different use conditions can be met.
(3) preparation of infusibility high-entropy alloy of the present invention uses " the pre-alloyed melting of high-melting-point constituent element+final alloy Change melting " two steps are completed, it is advantageously ensured that the uniform mixing of the great several constituent elements of different melting points；In addition, using ripe conjunction Prepared by golden smelting technology, easy to operate.
Description of the drawings
Fig. 1 is Ti described in embodiment 132Zr30Hf5V10Nb13Ta5Al5XRD (X-ray diffraction) spectrogram of infusibility high-entropy alloy.
Fig. 2 is Ti described in embodiment 132Zr30Hf5V10Nb13Ta5Al5The quasi-static tensile mechanical property of infusibility high-entropy alloy Curve graph.
Fig. 3 is Ti described in embodiment 242Zr15Hf15Nb12Ta10Al6The XRD spectra of infusibility high-entropy alloy.
Fig. 4 is Ti described in embodiment 242Zr15Hf15Nb12Ta10Al6The quasi-static tensile mechanical property of infusibility high-entropy alloy is bent Line chart.
Fig. 5 is Ti described in embodiment 330Zr8Hf20Nb8Ta30Al4The XRD spectra of infusibility high-entropy alloy.
Fig. 6 is Ti described in embodiment 330Zr8Hf20Nb8Ta30Al4The quasi-static tensile mechanical property of infusibility high-entropy alloy is bent Line chart.
Fig. 7 is Ti described in embodiment 435Zr25Hf25Nb5Ta5Mo5The XRD spectra of infusibility high-entropy alloy.
Fig. 8 is Ti described in embodiment 435Zr25Hf25Nb5Ta5Mo5The quasi-static tensile mechanical property of infusibility high-entropy alloy is bent Line chart.
Fig. 9 is Ti described in embodiment 533Zr20Hf15Nb20Ta5Al5Mo2The XRD spectra of infusibility high-entropy alloy.
Figure 10 is Ti described in embodiment 533Zr20Hf15Nb20Ta5Al5Mo2The quasi-static tensile mechanical property of infusibility high-entropy alloy It can curve graph.
Figure 11 is Ti described in embodiment 628Zr25Hf28Ta17Al2The XRD spectra of infusibility high-entropy alloy.
Figure 12 is Ti described in embodiment 628Zr25Hf28Ta17Al2The quasi-static tensile mechanical curves of infusibility high-entropy alloy Figure.
Specific embodiment
The present invention is further elaborated with reference to the accompanying drawings and detailed description, wherein, the method is as without especially Explanation is conventional method, and the raw material can obtain unless otherwise instructed from open commercial sources.
1) reagent and equipment
Main agents information used in following embodiment refers to table 1, and key instrument facility information refers to table 2.
Table 1
Table 2
2) performance test and structural characterization
(1) density measurement：It is measured using Archimedes's drainage, concrete operation step is as follows：It will be difficult described in embodiment Molten high-entropy alloy is prepared into 3Cylindrical specimens, measure before be first put into the beaker for filling absolute alcohol In, sonic oscillation cleaning 10min is dried up after taking-up, then is weighed each sample using DT-100 precision balances (precision 0.1mg) and do Weight M1, each sample weighs 3 times, to reduce measurement error；Then, then the mass M of each sample in water is weighed2, each sample It weighs 3 times；Finally, density calculating is carried out as follows,
In formula, ρ0For the temperature of water, 0.9982g/cm3(20℃)；ρlFor atmospheric density, 0.0012g/cm3。
(2) material phase analysis：Material phase analysis is carried out using German Bruker AXS companies D8advance X-ray diffractometers, Operating voltage and electric current are respectively 40KV and 40mA, and x-ray source is CuK α (λ=0.1542nm) ray, and sweep speed is 0.2sec/step, scanning step be 0.02 °/step, 20 °~100 ° of scanning range.
(3) quasi-tensile test：Establishing criteria GB-T 228.1-2010, using the omnipotent examination of CMT4305 type computer electronics It tests machine and carries out room temperature axial direction quasi-tensile test, strain rate selected as 10-3s-1, test sample be nonstandard I-shaped part, sample Thick 1.0mm, wide 3.14mm, parallel segment length 10mm, gauge length 5mm.
Embodiment 1
Ti32Zr30Hf5V10Nb13Ta5Al5The specific preparation process of infusibility high-entropy alloy is as follows：
(1) it is first beaten using simple substance Ti, Zr, Hf, V, Nb, Ta and Al of more than purity 99.7wt% as raw material with grinding wheel The oxide skin for going to above-mentioned raw materials surface is abraded, absolute ethyl alcohol is reused and carries out ultrasonic oscillation cleaning, obtains clean raw material, and According to Ti:Zr:Hf:V:Nb:Ta:Al=32:30:5:10:13:5:5 atomic percent weigh gross mass for (80 ± 0.01) lustration raw material of g；
(2) load weighted simple substance Hf, Nb and Ta are put into the water jacketed copper crucible in high vacuum non-consumable arc-melting furnace, Then it vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, high-purity argon gas is filled with as protective gas；Melting is closed Before gold, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, then carries out alloying smelting, profit in fusion process Alloy is homogenized with electromagnetic agitation, melting 10min, cooling obtains alloy pig I, and alloy pig I is overturn, and repeats melting 2 times, obtains To pre-alloyed alloy pig；
(3) load weighted simple substance Ti, Zr, V, Al and the obtained pre-alloyed alloy pig of step (2) are put into high vacuum It in water jacketed copper crucible in non-consumable arc-melting furnace, then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3Pa Afterwards, high-purity argon gas is filled with as protective gas；Before molten alloy, first melting pure titanium metal ingot further reduces oxygen in furnace chamber and contains Amount, then carries out alloying smelting, homogenizes alloy using electromagnetic agitation in fusion process, and melting 10min, cooling is closed Ingot II overturns alloy pig II, repeats melting 4 times, obtains master alloy ingot；
(4) master alloy ingot is placed in high vacuum electric arc melting-turnover casting system, furnace chamber is vacuumized, treats vacuum degree Reach 2.5 × 10-3After Pa, it is filled with high-purity argon gas；Carry out melting under protection of argon gas, heated current by 20A incrementally increase to 500A, after master alloy ingot is completely melt by aluminium alloy be cast in copper-made mould (cavity dimension be Φ 10mm × 60mm) into Type obtains Ti32Zr30Hf5V10Nb13Ta5Al5Infusibility high-entropy alloy bar.
Fig. 1 is the XRD spectra of infusibility high-entropy alloy manufactured in the present embodiment, can be true according to lattice diffraction delustring rule Determine (110), (200), (211), (220) and (310) crystalline substance that five in collection of illustrative plates diffraction maximums correspond respectively to BCC structure phases Face shows that prepared infusibility high-entropy alloy is mainly made of BCC phases.As can be seen from FIG. 2, prepared infusibility high-entropy alloy Yield strength is 960MPa, tensile strength 980MPa, and elongation percentage is up to 37%.By measuring and calculation it is found that prepared high entropy The density of alloy is only 6.85g/cm3, with intensity is high, plasticity is good and the advantages such as density is low, comprehensive performance are superior.
Embodiment 2
Ti42Zr15Hf15Nb12Ta10Al6The specific preparation process of infusibility high-entropy alloy is as follows：
(1) grinder buffing is first used as raw material using simple substance Ti, Zr, Hf, Nb, Ta and Al of more than purity 99.7wt% The oxide skin on above-mentioned raw materials surface is removed, absolute ethyl alcohol is reused and carries out ultrasonic oscillation cleaning, obtain clean raw material, and press According to Ti:Zr:Hf:Nb:Ta:Al=42:15:15:12:10:It is (80 ± 0.01) g's that 6 atomic percent, which weighs gross mass, Lustration raw material；
(2) load weighted simple substance Hf, Nb and Ta are put into the water jacketed copper crucible in high vacuum non-consumable arc-melting furnace, Then it vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, high-purity argon gas is filled with as protective gas；Melting is closed Before gold, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, then carries out alloying smelting, profit in fusion process Alloy is homogenized with electromagnetic agitation, melting 10min, cooling obtains alloy pig I, and alloy pig I is overturn, and repeats melting 2 times, obtains To pre-alloyed alloy pig；
(3) that load weighted simple substance Ti, Zr, Al and the obtained pre-alloyed alloy pig of step (2) are put into high vacuum is non- It in water jacketed copper crucible in consumable arc-melting stove, then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, High-purity argon gas is filled with as protective gas；Before molten alloy, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, Then it carries out alloying smelting, homogenizes alloy using electromagnetic agitation in fusion process, melting 10min, cooling obtains alloy Ingot II overturns alloy pig II, repeats melting 4 times, obtains master alloy ingot；
(4) master alloy ingot is placed in high vacuum electric arc melting-turnover casting system, furnace chamber is vacuumized, treats vacuum degree Reach 2.5 × 10-3After Pa, it is filled with high-purity argon gas；Carry out melting under protection of argon gas, heated current by 20A incrementally increase to 500A, after master alloy ingot is completely melt by aluminium alloy be cast in copper-made mould (cavity dimension be Φ 10mm × 60mm) into Type obtains Ti42Zr15Hf15Nb12Ta10Al6Infusibility high-entropy alloy bar.
Fig. 3 is the XRD spectra of infusibility high-entropy alloy manufactured in the present embodiment, can be true according to lattice diffraction delustring rule Determine (110), (200), (211), (220) and (310) crystalline substance that five in collection of illustrative plates diffraction maximums correspond respectively to BCC structure phases Face shows that prepared infusibility high-entropy alloy is mainly made of BCC phases.As can be seen from FIG. 4, prepared infusibility high-entropy alloy Yield strength is 910MPa, tensile strength 930MPa, and elongation percentage is up to 33%.By measuring and calculation it is found that prepared high entropy The density of alloy is 7.42g/cm3, with intensity is high, plasticity is good and the more low advantage of density, comprehensive performance are superior.
Embodiment 3
Ti30Zr8Hf20Nb8Ta30Al4The specific preparation process of infusibility high-entropy alloy is as follows：
(1) grinder buffing is first used as raw material using simple substance Ti, Zr, Hf, Nb, Ta and Al of more than purity 99.7wt% The oxide skin on above-mentioned raw materials surface is removed, absolute ethyl alcohol is reused and carries out ultrasonic oscillation cleaning, obtain clean raw material, and press According to Ti:Zr:Hf:Nb:Ta:Al=30:8:20:8:30:It is the clean of (80 ± 0.01) g that 4 atomic percent, which weighs gross mass, Net raw material；
(2) load weighted simple substance Hf, Nb and Ta are put into the water jacketed copper crucible in high vacuum non-consumable arc-melting furnace, Then it vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, high-purity argon gas is filled with as protective gas；Melting is closed Before gold, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, then carries out alloying smelting, profit in fusion process Alloy is homogenized with electromagnetic agitation, melting 10min, cooling obtains alloy pig I, and alloy pig I is overturn, and repeats melting 2 times, obtains To pre-alloyed alloy pig；
(3) that load weighted simple substance Ti, Zr, Al and the obtained pre-alloyed alloy pig of step (2) are put into high vacuum is non- It in water jacketed copper crucible in consumable arc-melting stove, then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, High-purity argon gas is filled with as protective gas；Before molten alloy, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, Then it carries out alloying smelting, homogenizes alloy using electromagnetic agitation in fusion process, melting 10min, cooling obtains alloy Ingot II overturns alloy pig II, repeats melting 4 times, obtains master alloy ingot；
(4) master alloy ingot is placed in high vacuum electric arc melting-turnover casting system, furnace chamber is vacuumized, treats vacuum degree Reach 2.5 × 10-3After Pa, it is filled with high-purity argon gas；Carry out melting under protection of argon gas, heated current by 20A incrementally increase to 500A, after master alloy ingot is completely melt by aluminium alloy be cast in copper-made mould (cavity dimension be Φ 10mm × 60mm) into Type obtains Ti30Zr8Hf20Nb8Ta30Al4Infusibility high-entropy alloy bar.
Fig. 5 is the XRD spectra of infusibility high-entropy alloy manufactured in the present embodiment, can be true according to lattice diffraction delustring rule Determine (110), (200), (211), (220) and (310) crystalline substance that five in collection of illustrative plates diffraction maximums correspond respectively to BCC structure phases Face shows that prepared infusibility high-entropy alloy is mainly made of BCC phases.As can be seen from FIG. 6, prepared infusibility high-entropy alloy Yield strength is 930MPa, tensile strength 960MPa, and elongation percentage is up to 24%.By measuring and calculation it is found that prepared high entropy The density of alloy is 10.08g/cm3, have that intensity is high, plasticity is good and advantages, the comprehensive performance such as density height be superior.
Embodiment 4
Ti35Zr25Hf25Nb5Ta5Mo5The specific preparation process of infusibility high-entropy alloy is as follows：
(1) grinder buffing is first used as raw material using simple substance Ti, Zr, Hf, Nb, Ta and Mo of more than purity 99.7wt% The oxide skin on above-mentioned raw materials surface is removed, absolute ethyl alcohol is reused and carries out ultrasonic oscillation cleaning, obtain clean raw material, and press According to Ti:Zr:Hf:Nb:Ta:Mo=35:25:25:5:5:It is the clean of (80 ± 0.01) g that 5 atomic percent, which weighs gross mass, Net raw material；
(2) water jacketed copper crucible being put into load weighted simple substance Hf, Nb, Ta and Mo in high vacuum non-consumable arc-melting furnace In, it then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, high-purity argon gas is filled with as protective gas；It is molten Before refining alloy, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, then carries out alloying smelting, fusion process Middle to homogenize alloy using electromagnetic agitation, melting 10min, cooling obtains alloy pig I, and alloy pig I is overturn, and repeats melting 2 It is secondary, obtain pre-alloyed alloy pig；
(3) load weighted simple substance Ti, Zr and the obtained pre-alloyed alloy pig of step (2) are put into high vacuum non-consumable It in water jacketed copper crucible in arc-melting furnace, then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, it is filled with High-purity argon gas is as protective gas；Before molten alloy, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, then Alloying smelting is carried out, homogenizes alloy using electromagnetic agitation in fusion process, melting 10min, cooling obtains alloy pig II, Alloy pig II is overturn, melting 4 times is repeated, obtains master alloy ingot；
(4) master alloy ingot is placed in high vacuum electric arc melting-turnover casting system, furnace chamber is vacuumized, treats vacuum degree Reach 2.5 × 10-3After Pa, it is filled with high-purity argon gas；Carry out melting under protection of argon gas, heated current by 20A incrementally increase to 500A, after master alloy ingot is completely melt by aluminium alloy be cast in copper-made mould (cavity dimension be Φ 10mm × 60mm) into Type obtains Ti35Zr25Hf25Nb5Ta5Mo5Infusibility high-entropy alloy bar.
Fig. 7 is the XRD spectra of infusibility high-entropy alloy manufactured in the present embodiment, can be true according to lattice diffraction delustring rule Determine (110), (200), (211), (220) and (310) crystalline substance that five in collection of illustrative plates diffraction maximums correspond respectively to BCC structure phases Face shows that prepared infusibility high-entropy alloy is mainly made of BCC phases.As can be seen from FIG. 8, prepared infusibility high-entropy alloy Yield strength is 830MPa, tensile strength 860MPa, and elongation percentage is up to 10%.By measuring and calculation it is found that prepared high entropy The density of alloy is 7.96g/cm3。
Embodiment 5
Ti33Zr20Hf15Nb20Ta5Al5Mo2The specific preparation process of infusibility high-entropy alloy is as follows：
(1) it is first beaten using simple substance Ti, Zr, Hf, Nb, Ta, Al and Mo of more than purity 99.7wt% as raw material with grinding wheel The oxide skin for going to above-mentioned raw materials surface is abraded, absolute ethyl alcohol is reused and carries out ultrasonic oscillation cleaning, obtains clean raw material, and According to Ti:Zr:Hf:Nb:Ta:Al:Mo=33:20:15:20:5:5:2 atomic percent weigh gross mass for (80 ± 0.01) lustration raw material of g；
(2) water jacketed copper crucible being put into load weighted simple substance Hf, Nb, Ta and Mo in high vacuum non-consumable arc-melting furnace In, it then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, high-purity argon gas is filled with as protective gas；It is molten Before refining alloy, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, then carries out alloying smelting, fusion process Middle to homogenize alloy using electromagnetic agitation, melting 10min, cooling obtains alloy pig I, and alloy pig I is overturn, and repeats melting 2 It is secondary, obtain pre-alloyed alloy pig；
(3) that load weighted simple substance Ti, Zr, Al and the obtained pre-alloyed alloy pig of step (2) are put into high vacuum is non- It in water jacketed copper crucible in consumable arc-melting stove, then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, High-purity argon gas is filled with as protective gas；Before molten alloy, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, Then it carries out alloying smelting, homogenizes alloy using electromagnetic agitation in fusion process, melting 10min, cooling obtains alloy Ingot II overturns alloy pig II, repeats melting 4 times, obtains master alloy ingot；
(4) master alloy ingot is placed in high vacuum electric arc melting-turnover casting system, furnace chamber is vacuumized, treats vacuum degree Reach 2.5 × 10-3After Pa, it is filled with high-purity argon gas；Carry out melting under protection of argon gas, heated current by 20A incrementally increase to 500A, after master alloy ingot is completely melt by aluminium alloy be cast in copper-made mould (cavity dimension be Φ 10mm × 60mm) into Type obtains Ti33Zr20Hf15Nb20Ta5Al5Mo2Infusibility high-entropy alloy bar.
Fig. 9 is the XRD spectra of infusibility high-entropy alloy manufactured in the present embodiment, can be true according to lattice diffraction delustring rule Determine (110), (200), (211), (220) and (310) crystalline substance that five in collection of illustrative plates diffraction maximums correspond respectively to BCC structure phases Face shows that prepared infusibility high-entropy alloy is mainly made of BCC phases.As can be seen from FIG. 10, prepared infusibility high-entropy alloy Yield strength for 900MPa, tensile strength 917MPa, elongation percentage is up to 42%.By measuring and calculation it is found that prepared height The density of entropy alloy is 7.72g/cm3, with intensity is high, plasticity is good and the more low advantage of density, comprehensive performance are superior.
Embodiment 6
Ti28Zr25Hf28Ta17Al2The specific preparation process of infusibility high-entropy alloy is as follows：
(1) it is first removed using simple substance Ti, Zr, Hf, Ta and Al of more than purity 99.7wt% as raw material with grinder buffing The oxide skin on above-mentioned raw materials surface reuses absolute ethyl alcohol and carries out ultrasonic oscillation cleaning, obtains clean raw material, and according to Ti:Zr:Hf:Ta:Al=28:25:28:17:2 atomic percent weighs the lustration raw material that gross mass is (80 ± 0.01) g；
(2) load weighted simple substance Hf and Ta is put into the water jacketed copper crucible in high vacuum non-consumable arc-melting furnace, so After vacuumize, treat that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, high-purity argon gas is filled with as protective gas；Molten alloy Before, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, then carries out alloying smelting, is utilized in fusion process Electromagnetic agitation homogenizes alloy, melting 10min, and cooling obtains alloy pig I, and alloy pig I is overturn, and repeats melting 2 times, obtains Pre-alloyed alloy pig；
(3) that load weighted simple substance Ti, Zr, Al and the obtained pre-alloyed alloy pig of step (2) are put into high vacuum is non- It in water jacketed copper crucible in consumable arc-melting stove, then vacuumizes, treats that the vacuum degree in smelting furnace reaches 2.5 × 10-3After Pa, High-purity argon gas is filled with as protective gas；Before molten alloy, first melting pure titanium metal ingot further reduces oxygen content in furnace chamber, Then it carries out alloying smelting, homogenizes alloy using electromagnetic agitation in fusion process, melting 10min, cooling obtains alloy Ingot II overturns alloy pig II, repeats melting 4 times, obtains master alloy ingot；
(4) master alloy ingot is placed in high vacuum electric arc melting-turnover casting system, furnace chamber is vacuumized, treats vacuum degree Reach 2.5 × 10-3After Pa, it is filled with high-purity argon gas；Carry out melting under protection of argon gas, heated current by 20A incrementally increase to 500A, after master alloy ingot is completely melt by aluminium alloy be cast in copper-made mould (cavity dimension be Φ 10mm × 60mm) into Type obtains Ti28Zr25Hf28Ta17Al2Infusibility high-entropy alloy bar.
Figure 11 is the XRD spectra of infusibility high-entropy alloy manufactured in the present embodiment, can be true according to lattice diffraction delustring rule Determine (110), (200), (211), (220) and (310) crystalline substance that five in collection of illustrative plates diffraction maximums correspond respectively to BCC structure phases Face shows that prepared infusibility high-entropy alloy is mainly made of BCC phases；In addition, three weaker diffraction maximums near (110) peak (being indicated in figure with inverted triangle) is the corresponding diffraction maximums of HCP, shows that there are a small amount of HCP phases in the infusibility high-entropy alloy.Root According to Figure 12 it is found that the yield strength of prepared infusibility high-entropy alloy is 460MPa, tensile strength 800MPa, elongation percentage reaches 40%.By measuring and calculation it is found that the density of prepared high-entropy alloy is 9.16g/cm3, it is good and close with intensity height, plasticity Spend high advantage.
In conclusion the foregoing is merely a prefered embodiment of the invention, it is not intended to limit the scope of the present invention. All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's Within protection domain.

Claims (4)

1. a kind of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys, it is characterised in that：The infusibility high-entropy alloy Chemical formula is denoted as TiaZrbHfcVdNbeTafMx, one or more of M Al, Cr, Mo, W, Mn, Fe, Co, Ni and Si；
Wherein, a=15~45, b=5~35, c=5~35, d=0~35, e=0~35, f=5~40, x=0.1~15,15 5≤d+e+f≤70 when being 0 when≤b+c≤70, d with e difference.
2. a kind of preparation method of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys as described in claim 1, It is characterized in that：It the described method comprises the following steps,
(1) under argon atmosphere, clean elemental metals Hf, Nb, Ta and the M in addition to Al are subjected to alloying smelting, The aluminium alloy I that melting obtains is cooled down, obtains alloy pig I；Alloy pig I is overturn again, melting 2 times or more is repeated, obtains Pre-alloyed alloy pig；
(2) under argon atmosphere, clean elemental metals Ti, Zr, V and pre-alloyed alloy pig is subjected to alloying and melted Clean elemental metals Ti, Zr, V, Al and pre-alloyed alloy pig are carried out alloying smelting by refining, and melting is obtained Aluminium alloy II is cooled down, and obtains alloy pig II；Alloy pig II is overturn again, repeats melting 4 times or more, it is high to obtain the infusibility Entropy alloy.
3. a kind of preparation method of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys according to claim 2, It is characterized in that：The alloying smelting is using vacuum melting.
4. a kind of preparation method of microalloying Ti-Zr-Hf-V-Nb-Ta infusibility high-entropy alloys according to claim 2, It is characterized in that：Under argon atmosphere, the obtained infusibility high-entropy alloy is subjected to heating remelting, and will be after fusing Aluminium alloy is cast in mold and is molded, and the high entropy of microalloying Ti-Zr-Hf-V-Nb-Ta infusibilities for obtaining required shape closes Gold.
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