CN105886805A - High-plasticity five-element refractory high-entropy alloy and preparation method thereof - Google Patents
High-plasticity five-element refractory high-entropy alloy and preparation method thereof Download PDFInfo
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- CN105886805A CN105886805A CN201610329339.5A CN201610329339A CN105886805A CN 105886805 A CN105886805 A CN 105886805A CN 201610329339 A CN201610329339 A CN 201610329339A CN 105886805 A CN105886805 A CN 105886805A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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Abstract
The invention relates to high-plasticity five-element refractory high-entropy alloy and a preparation method thereof and belongs to the field of metal materials. The high-entropy alloy is prepared from zirconium, titanium, hafnium, vanadium and niobium, wherein the molar weights of the zirconium, the titanium, the hafnium, the vanadium and the niobium are equal. The preparation method of the high-plasticity five-element refractory high-entropy alloy comprises the steps that the zirconium, the titanium, the hafnium, the vanadium and the niobium are placed in a water-cooling metal crucible in a melting point progressively-decreasing sequence, the element with the lowest melting point is placed at the bottom, and the element with the highest melting point is placed at the top; and arc striking smelting is conducted in an oxygen-free environment till the five elements are fully mixed, and the high-entropy alloy is obtained. The high-entropy alloy is of a single body-centered cubic structure, the yield strength of the high-entropy alloy is higher than 800 MPa, the tensile strength is over 1100 MPa, and the plastic strain is larger than 55%; and the large solid solubility between the elements is obtained, and a simple solid-solution phase is formed. The preparation method has the advantages that the power is high, the performance is table, operation is convenient, the melting point is high, the vacuum degree is high, and the quantity of impurities is small.
Description
Technical field
The present invention relates to a kind of five yuan of infusibility high-entropy alloys of high-ductility and preparation method thereof, belong to metal material field.
Background technology
High-entropy alloy is to take the lead in the alloy design concept of a kind of novelty that proposes by TaiWan, China scholar Ye Junwei in the nineties in 20th century, and its theory varies with conventional alloys, enriches the research contents of alloy material greatly.It requires that alloy at least contains five kinds of essential elements, and mole percent shared by every kind of alloying element atom is close, no more than 35%, and minimum also it is not less than 5%, i.e. there is no any element as dominant element, therefore also can be many pivots high-entropy alloy.
High-entropy alloy design concept is since proposing, just cause the common concern of scientific circles and try to explore, the research of high-entropy alloy is shown by scholars, because metallic element in alloy is many, the randomness of element is big, substantial amounts of intermetallic compound not only will not be formed as conventional alloys after alloy graining, on the contrary because high entropic effect promotes the mixing between element, many pivots high-entropy alloy is formed simply and crystallizes phase, i.e. multiple element confusing array forms body-centered cubic phase or face-centered cubic the most even amorphous phase, inhibit again the formation of the intermetallic compound of fragility simultaneously.Be easily formed this feature of single solid solution phase make high-entropy alloy show excellence performance: (1) high rigidity；(2) good corrosion resistance；(3) good wearability；(4) good heat-resisting quantity；(5) high work hardening ability.
Compared with conventional alloys, high-entropy alloy has uniqueness and the structure of excellence and performance.But the development of high-entropy alloy is still in initial stage, formation mechenism and performance study to high-entropy alloy are the most plain, and theoretical research or experimental studies results are the most fewer.High-entropy alloy is as a kind of novel alloy material, and its mechanical behavior under shock environment and deformation fracture mechanism research are the most extremely limited.The especially plasticity of high-entropy alloy is not fine, because high-entropy alloy constituent element element is more, and each constituent content is more or less the same, in high-entropy alloy system, all atoms can regard that solute atoms can regard again solvent atom as, these atomic radiuses are not of uniform size, and the solid solution also resulting in formation has bigger distortion of lattice.Meanwhile, the diffusion of atom needs the mutually coordinated of various Elements Atom in alloy, and high-entropy alloy constituent element number is more, and there is the serious distortion of lattice hindering atomic motion so that the diffusion of high-entropy alloy is difficult to.Therefore, in general the diffusion velocity in high-entropy alloy is slower than conventional alloys.So the plasticity of the high-entropy alloy formed is not typically the most fine.The compression plastic strain of major part high-entropy alloy is 5%～7%, and the compression plastic strain of part high-entropy alloy is 25%～33%.
Plasticity, refers under external force, and material can stably occur permanent deformation not destroy the ability of its integrity.Directly reflection ground is the machinability of material, and this has the widest application in the industrial production.And high-entropy alloy has high intensity and high rigidity concurrently, can be with existing high intensity if one can be worked out, high rigidity, have again the high-entropy alloy of high-ductility concurrently, that will have the brightest prospect at Material Field.
Summary of the invention
For defect present in prior art, an object of the present invention there are provided a kind of five yuan of infusibility high-entropy alloys of high-ductility；The two of the purpose of the present invention there are provided the preparation method of a kind of five yuan of infusibility high-entropy alloys of high-ductility.
For achieving the above object, technical scheme is as follows.
A kind of five yuan of infusibility high-entropy alloys of high-ductility, described high-entropy alloy is made up of the zirconium (Zr) of equimolar amounts, titanium (Ti), hafnium (Hf), vanadium (V) and niobium (Nb), i.e. ZrTiHfVNb；The purity of the most described component is all more than 99%；The most described component has identical crystal structure.
The preparation method of five yuan of infusibility high-entropy alloys of a kind of high-ductility of the present invention, described method step is as follows:
Raw material zirconium (Zr), titanium (Ti), hafnium (Hf), vanadium (V) and niobium (Nb) are successively put in water-cooled metal crucible according to fusing point order from low to high successively, the element that fusing point is minimum is placed on bottom, and the element that fusing point is the highest is placed on the top；Striking melting under oxygen-free environment, to five kinds of abundant consolutes of element, obtains a kind of five yuan of infusibility high-entropy alloys of high-ductility of the present invention.
Non-consumable fine vacuum arc-melting furnace can be used, raw material is put into water jacketed copper crucible and carries out striking melting.
Oxygen-free environment can use and be evacuated down to more than or equal to 10-4MPa, is then charged with noble gas to more than or equal to 0.05MPa.
Preferably striking smelting parameter is as follows:
Unit weight (raw material weight): 10g～100g/ melting pond, 3 melting pond dress raw materials, 1 melting pond striking；
Working gas: Ar gas or He gas；
The type of cooling: water-cooled/automatic alarm；
Vacuum: > 2 × 10-3Pa (molecular pump)；
Starting the arc mode: contacting ignition arc；
Alr mode: manual cantilever stirring；
Maximum current: 550A.
Beneficial effect
1. the invention provides a kind of five yuan of infusibility high-entropy alloys of high-ductility, described high-entropy alloy is by the high-entropy alloy having single body-centered cubic structure of five kinds of element meltings of Zr, Ti, Hf, V and Nb, its yield strength is more than 800MPa, tensile strength is more than 55% more than 1100MPa, plastic strain.Compared with the high-entropy alloy of existing research, described high-entropy alloy presents fabulous plasticity；
2. the invention provides a kind of five yuan of infusibility high-entropy alloys of high-ductility, the element that described high-entropy alloy is selected has identical crystal structure, and Atomic radiuses difference is little, and lattice paprmeter is close with electronegativity, so can make to obtain bigger solid solubility between element, form simple solid solution phase.
3. the invention provides the preparation method of a kind of five yuan of infusibility high-entropy alloys of high-ductility, melting is carried out with the non-consumable vacuum arc melting furnace alloy to being configured, this smelting furnace is made up of high-melting-point conductive materials, keep stable a kind of electrode as far as possible, so its method of smelting to have power big, stable performance, easy to operate；Fusing point is high, and vacuum is high, the advantage that impurity is few.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the five yuan of infusibility high-entropy alloys of high-ductility prepared in embodiment 1.
Fig. 2 is the five yuan of infusibility high-entropy alloys of high-ductility prepared in embodiment 1 metallographs after corrosion treatmentCorrosion Science.
Fig. 3 is the five yuan of infusibility high-entropy alloy room temperature Static Compression true stress-strain curves of high-ductility prepared in embodiment 1.
Fig. 4 is the true stress and strain curve of the five yuan of infusibility high-entropy alloy room temperature dynamic compression of high-ductility prepared in embodiment 1.
Detailed description of the invention
The present invention is described in detail below by specific embodiment.
In following example, the preparation method of a kind of five yuan of infusibility high-entropy alloys of high-ductility uses the SKY08K-102 type non-consumable fine vacuum arc-melting furnace that Shenyang Scientific Instrument Research & Mfg. Center Co., Ltd., C.A.S produces, and the crucible of melting uses water jacketed copper crucible.
Embodiment 1
A kind of five yuan of infusibility high-entropy alloys of high-ductility, described high-entropy alloy is made up of the zirconium (Zr) of equimolar amounts, titanium (Ti), hafnium (Hf), vanadium (V) and niobium (Nb), i.e. ZrTiHfVNb, wherein, the purity of described component is all more than 99%, and has identical crystal structure.
Raw material with ten thousand/scales/electronic balance weighing to reduce experimental error, it is followed successively by titanium (Ti), zirconium (Zr), vanadium (V), hafnium (Hf), niobium (Nb) according to fusing point order from low to high, put in the water jacketed copper crucible of non-consumable fine vacuum arc-melting furnace, the element titanium (Ti) that fusing point is minimum is placed on bottom, and the elemental niobium (Nb) that fusing point is the highest is placed on the superiors side.It is evacuated down to 10-4MPa, is then charged with argon to 0.05MPa, striking melting；Melt back 6 times, to guarantee five kinds of abundant consolutes of element in raw material, obtains as cast condition ZrTiHfVNb, for a kind of five yuan of infusibility high-entropy alloys of high-ductility of the present invention.
Wherein, striking melting design parameter is as follows:
Unit weight (raw material weight): 50g/ melting pond, 3 melting pond dress raw materials, 1 melting pond striking；
Working gas: Ar gas；
The type of cooling: water-cooled；
Vacuum: > 2 × 10-3Pa (molecular pump)；
Starting the arc mode: contacting ignition arc；
Alr mode: manual cantilever stirring；
Maximum current: 550A.
It is as follows that the five yuan of infusibility high-entropy alloys of high-ductility (i.e. as cast condition ZrTiHfVNb alloy) preparing the present embodiment carry out test:
1. use Bruker AXS company of Germany D8advance x-ray diffractometer to carrying out material phase analysis
From described high-entropy alloy, cut the blockage of a size of 4mm × 4mm × 2mm, with sand papering light before test, obtain sample removing surface impurity；Running voltage and electric current are respectively 40KV and 40mA, and x-ray source is CuKα(λ=0.1542nm) ray, sweep limits: 20 °～90 °, scanning speed: 0.2sec/step, scanning step: 0.02 °/step.
Test obtains result as it is shown in figure 1, the XRD figure that Fig. 1 is sample is composed, and diffraction maximum peak shape is sharp-pointed, illustrates that degree of crystallinity is high；2 θ that in Fig. 1,4 diffraction maximums are corresponding are respectively as follows: 2 θ1=37.798 °, 2 θ2=54.303 °, 2 θ3=68.139 ° and 2 θ4=80.374 °, therefore sin2(θ1): sin2(θ2): sin2(θ3): sin2(θ4)=1:1.9850:2.9913:3.9890, close to 1:2:3:4, and first peak is the strongest in the first two diffraction maximum, thus may determine that sample is simple single-phase body-centered cubic structure, diffraction crystal face corresponding to 4 diffraction maximums is (110), (200), (211) and (220), and lattice paprmeter isOwing to the atomic radius of Zr and the Hf element atomic radius than Ti is big, therefore when after the atomic substitutions Ti atom of Zr and Hf, Ti structure cell can occur a certain degree of distortion, and lattice paprmeter becomes big, and therefore the diffraction maximum of solid solution phase can offset slightly to the left relative to the base peak of Ti.
2. use Carl Zeiss Inc. of Germany Axio observer A1m type research grade metallurgical microscope to carry out metallurgical microstructrue observation
From described high-entropy alloy, the cylinder obtaining a size of diameter (Φ) 4mm × 4mm is cut with line cutting, after 100# sand paper is roughly ground, the sand paper using 400#, 800#, 1000#, 1500#, 2000#, 3000# and 5000# the most successively refines, and uses Cr subsequently2O3Suspension mechanically polishes, after being polished to can't see surface scratch completely under 100 times of optical microscopes, corrode with corrosive liquid, obtain sample and carry out metallographic observation, obtain metallograph as in figure 2 it is shown, by Fig. 2 it can be seen that etching pit uniform not, some is local it is observed that there is obvious crystal boundary, thick intra-die has the dendrite of prosperity, and organizational structure is the finest and close and there is network structure；Dendrite continues to grow secondary dendrite and three dendrite in growth process, one time between dendrite and secondary dendrite, between secondary dendrite with three dendrite the most each other 90 ° vertical, dendrite is more and more tiny.There is the state of long-range order in whole organizational structure.
3. use Archimedes's drainage to measure density
Line cutting processing from described high-entropy alloy is used to obtain the cylinder 3 of a size of Φ 6mm × 9mm as density measure sample.First being put into by described sample before measurement and fill submergence in the beaker of acetone, sonic oscillation cleans 30min, and taking-up dries up.Concrete measurement process is: use ten thousand/balance to weigh sample dry weight M1, each sample weighing 3 times, to reduce measurement error；Weigh sample mass M in water2, each sample weighing 3 times.The density of described high-entropy alloy (1) as follows calculates:
Wherein, ρ0For the density of water, it is 0.9962g cm when 28 DEG C-3, ρlFor atmospheric density, for 0.0012g cm-3.Experimental result is as shown in table 3.According to formula D=ρActual/ρTheoreticalMeasuring the consistency of described high-entropy alloy, can calculate described high-entropy alloy consistency is: D=99.85%.
Density (the g cm of table 3 high-entropy alloy-3)
4. compression verification
Use line cutting that described high-entropy alloy is processed into the cylinder of Φ 4mm × 6mm, and with sand paper described cylindrical end face polished and obtain sample and be used as compression verification.Compression verification uses U.S.'s Instron Instron5569 electronic universal tester, at room temperature carries out, loading speed 0.36mm/min, and strain rate is 10-3s-1, test load 4500kg.Obtain the room temperature compression performance data of described high-entropy alloy, finally make load-deformation curve as shown in Figure 3 with Origin software.Compression experiment is applying pressure axial to sample, measures intensity and the plasticity of specimen material in it deforms even fracture process.Shown high-entropy alloy compression performance is had a significant impact by crystal structure, because face-centred cubic structure has more slip system, thus polyphyly sliding easily occurs, so for face-centered cubic high-entropy alloy is relative to body-centered cubic high-entropy alloy, having more preferable plasticity and toughness.Therefore the high-entropy alloy of body-centered cubic structure is more easy to cleavage fracture when normal temperature compressed.ZrTiHfVNb alloy shows the plasticity of excellence, until losing efficacy and the most not rupturing in compression process.Its yield strength reaches 856MPa, and comprcssive strength reaches 1123MPa, and plastic strain is more than 55%.
5. CS-4D Split Hopkinson Bar (SHPB) experimental provision using Bei Dai River electronic machine to produce carries out room temperature axial mechanical dynamic compression property performance test
In experimentation, with line cutting, described high-entropy alloy is processed into the cylinder of Φ 4mm × 4mm；Choose tetra-pressure of 0.3MPa, 0.4MPa, 0.5MPa and 0.55MPa it is tested.For improving experimental precision, test front sand paper and cylindrical two end faces are polished, obtain two end faces and be parallel to each other and be perpendicular to the sample of side.Tungsten carbon (WC) pad is placed, it is desirable in experimentation, depression bar and the contact surface of sample must keep smooth and be parallel to each other between the depression bar of sample and described experimental provision.Owing to ZrTiHfVNb alloy plasticity is preferable, when strain rate reaches 4433s-1Time, just there is the fracture of alloy.Fig. 4 is the true stress and strain curve of described high-entropy alloy room temperature dynamic compression, raising along with strain rate, the comprcssive strength of sample is almost unchanged with yield strength, show that described high-entropy alloy does not exist strain rate hardening effect under room temperature dynamic compression, but amount of plastic deformation improves with strain rate and increases.Under four strain rates the most first there is elastic deformation in sample, and a certain degree of plastic deformation, last failure damage occur after exceeding yield point.
In sum, these are only presently preferred embodiments of the present invention, be not intended to limit protection scope of the present invention.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (8)
1. five yuan of infusibility high-entropy alloys of a high-ductility, it is characterised in that: described high-entropy alloy is by equimolar amounts
Zirconium, titanium, hafnium, vanadium and niobium composition.
A kind of five yuan of infusibility high-entropy alloys of high-ductility the most according to claim 1, it is characterised in that: institute
State in high-entropy alloy the purity of component all more than 99%.
A kind of five yuan of infusibility high-entropy alloys of high-ductility the most according to claim 1, it is characterised in that: institute
State component in high-entropy alloy and there is identical crystal structure.
A kind of five yuan of infusibility high-entropy alloys of high-ductility the most according to claim 1, it is characterised in that: institute
State in high-entropy alloy the purity of component all more than 99%, and there is identical crystal structure.
5. the preparation side of the five yuan of infusibility high-entropy alloys of high-ductility as described in any one of Claims 1 to 4
Method, it is characterised in that: described method step is as follows:
Successively zirconium, titanium, hafnium, vanadium and niobium is put into water-cooled metal earthenware successively according to fusing point order from low to high
In crucible, the element that fusing point is minimum is placed on bottom, and the element that fusing point is the highest is placed on the top；At oxygen-free environment
Lower striking melting, to five kinds of abundant consolutes of element, obtains five yuan of infusibility high-entropy alloys of described high-ductility.
The preparation method of five yuan of infusibility high-entropy alloys of a kind of high-ductility the most according to claim 5, it is special
Levy and be: oxygen-free environment is by being evacuated down to more than or equal to 10-4MPa, is then charged with noble gas to being more than
Realize in 0.05MPa.
The preparation method of five yuan of infusibility high-entropy alloys of a kind of high-ductility the most according to claim 5, it is special
Levy and be: use non-consumable fine vacuum arc-melting furnace, raw material is put into water jacketed copper crucible and carries out striking melting.
The preparation method of five yuan of infusibility high-entropy alloys of a kind of high-ductility the most according to claim 5, it is special
Levy and be: striking smelting parameter is as follows:
Raw material weight: 10g～100g/ melting pond, 3 melting pond dress raw materials, 1 melting pond striking；
Working gas: Ar gas or He gas；
The type of cooling: water-cooled/automatic alarm；
Vacuum: > 2 × 10-3Pa；
Starting the arc mode: contacting ignition arc；
Alr mode: manual cantilever stirring；
Maximum current: 550A.
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Cited By (11)
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| CN106636845A (en) * | 2016-12-01 | 2017-05-10 | 中国人民解放军国防科学技术大学 | HfZrTiTax high-entropy alloy, and preparation method and application thereof |
| CN107267842A (en) * | 2017-06-26 | 2017-10-20 | 北京理工大学 | A kind of high-melting-point high-entropy alloy and preparation method thereof |
| CN107619982A (en) * | 2017-11-03 | 2018-01-23 | 北京理工大学 | Hexa-atomic the infusibility high-entropy alloy and its verification method of a kind of high-ductility high intensity |
| CN109252082A (en) * | 2017-07-13 | 2019-01-22 | 山东理工大学 | A kind of multi-element alloyed infusibility high-entropy alloy and preparation method thereof |
| CN109402482A (en) * | 2018-12-10 | 2019-03-01 | 北京理工大学 | It is a kind of to have both high-intensitive and high-ductility lightweight high-entropy alloy and preparation method thereof |
| CN110541103A (en) * | 2019-08-27 | 2019-12-06 | 北京工业大学 | High-strength high-plasticity quaternary refractory high-entropy alloy and preparation method thereof |
| CN111014616A (en) * | 2019-12-26 | 2020-04-17 | 爱柯迪股份有限公司 | HfZrWMoVNbN/CrSiN high-entropy alloy nano composite coating die-casting aluminum die and preparation method thereof |
| CN111945033A (en) * | 2020-07-30 | 2020-11-17 | 东北大学 | High-entropy alloy with neutron poison characteristic and preparation method thereof |
| CN112466409A (en) * | 2020-11-19 | 2021-03-09 | 江苏科技大学 | Five-element high-entropy amorphous alloy component design method based on combination of two quaternary amorphous alloy elements |
| CN113088785A (en) * | 2021-03-31 | 2021-07-09 | 北京科技大学 | Body-centered cubic high-entropy alloy and preparation method thereof |
| CN113373366A (en) * | 2021-06-17 | 2021-09-10 | 西北工业大学 | Multi-element refractory high-entropy alloy and preparation method thereof |
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| CN106636845B (en) * | 2016-12-01 | 2018-11-20 | 中国人民解放军国防科学技术大学 | HfZrTiTaxHigh-entropy alloy and its preparation method and application |
| CN106636845A (en) * | 2016-12-01 | 2017-05-10 | 中国人民解放军国防科学技术大学 | HfZrTiTax high-entropy alloy, and preparation method and application thereof |
| CN107267842A (en) * | 2017-06-26 | 2017-10-20 | 北京理工大学 | A kind of high-melting-point high-entropy alloy and preparation method thereof |
| CN109252082A (en) * | 2017-07-13 | 2019-01-22 | 山东理工大学 | A kind of multi-element alloyed infusibility high-entropy alloy and preparation method thereof |
| CN107619982A (en) * | 2017-11-03 | 2018-01-23 | 北京理工大学 | Hexa-atomic the infusibility high-entropy alloy and its verification method of a kind of high-ductility high intensity |
| CN107619982B (en) * | 2017-11-03 | 2019-05-17 | 北京理工大学 | A kind of hexa-atomic infusibility high-entropy alloy and its verification method of high-ductility high intensity |
| CN109402482B (en) * | 2018-12-10 | 2022-07-05 | 北京中辰至刚科技有限公司 | Light high-entropy alloy with high strength and high plasticity and preparation method thereof |
| CN109402482A (en) * | 2018-12-10 | 2019-03-01 | 北京理工大学 | It is a kind of to have both high-intensitive and high-ductility lightweight high-entropy alloy and preparation method thereof |
| CN110541103A (en) * | 2019-08-27 | 2019-12-06 | 北京工业大学 | High-strength high-plasticity quaternary refractory high-entropy alloy and preparation method thereof |
| CN111014616A (en) * | 2019-12-26 | 2020-04-17 | 爱柯迪股份有限公司 | HfZrWMoVNbN/CrSiN high-entropy alloy nano composite coating die-casting aluminum die and preparation method thereof |
| CN111014616B (en) * | 2019-12-26 | 2022-12-02 | 爱柯迪股份有限公司 | HfZrWMoVNbN/CrSiN high-entropy alloy nano composite coating die-casting aluminum die and preparation method thereof |
| CN111945033A (en) * | 2020-07-30 | 2020-11-17 | 东北大学 | High-entropy alloy with neutron poison characteristic and preparation method thereof |
| CN112466409A (en) * | 2020-11-19 | 2021-03-09 | 江苏科技大学 | Five-element high-entropy amorphous alloy component design method based on combination of two quaternary amorphous alloy elements |
| CN112466409B (en) * | 2020-11-19 | 2023-09-22 | 江苏科技大学 | Five-membered high-entropy amorphous alloy component design method based on combination of two quaternary amorphous alloy elements |
| CN113088785A (en) * | 2021-03-31 | 2021-07-09 | 北京科技大学 | Body-centered cubic high-entropy alloy and preparation method thereof |
| CN113373366A (en) * | 2021-06-17 | 2021-09-10 | 西北工业大学 | Multi-element refractory high-entropy alloy and preparation method thereof |
| CN113373366B (en) * | 2021-06-17 | 2022-08-30 | 西北工业大学 | Multi-element refractory high-entropy alloy and preparation method thereof |
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Application publication date: 20160824 |