CN107641751B - A kind of MoNbCrVTi infusibility high-entropy alloy and preparation method thereof - Google Patents
A kind of MoNbCrVTi infusibility high-entropy alloy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 89
- 239000000956 alloy Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 27
- 230000008018 melting Effects 0.000 claims abstract description 27
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 18
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 15
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000010891 electric arc Methods 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 241000555268 Dendroides Species 0.000 claims description 3
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical group C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 238000005275 alloying Methods 0.000 claims description 2
- 229910020012 Nb—Ti Inorganic materials 0.000 claims 1
- 239000004615 ingredient Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 239000007769 metal material Substances 0.000 abstract description 3
- 239000010955 niobium Substances 0.000 description 14
- 239000011651 chromium Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 210000001787 dendrite Anatomy 0.000 description 3
- 229910000967 As alloy Inorganic materials 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000005502 phase rule Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to metal material and its preparation field, specially a kind of ingredient is MoNbCrVTi infusibility high-entropy alloy and preparation method thereof.The high-entropy alloy is made of Mo, Nb, Cr, V and Ti, the preparation method comprises the following steps: simple substance Mo, Nb, Cr, V and Ti for taking purity to be not less than 99.5wt.%, it is prepared according to the chemical component of name, alloy preparation is obtained by melting in vacuum arc furnace ignition, low melting point element is placed below copper crucible when melting, high-melting-point is placed on above copper crucible, and electric arc furnaces working chamber is evacuated to 5 × 10‑4Pa, is subsequently passed the high-purity argon gas that purity is 99.99wt.%, and striking melting obtains MoNbCrVTi infusibility high-entropy alloy.Alloy of the present invention has simple single body-centered cubic structure, and excellent in mechanical performance has very high intensity and preferable plasticity, has a possibility that potential application in the high temperature environment.The method of the present invention is simple, easy, has broad application prospects.
Description
Technical field
The present invention relates to metal material and its preparation field, specially a kind of ingredient is MoNbCrVTi infusibility high-entropy alloy
And preparation method thereof.
Background technique
High-entropy alloy is a kind of novel metal material, and the design concept of alloy is existed by TaiWan, China scholar Ye Junwei
The 1990s proposes.This novel alloy design concept greatly expands the system of alloy design, breaches traditional conjunction
Using one or two element as the mentality of designing of pivot in gold design.Sensu lato high-entropy alloy refer to the constituent element number of alloy >=
5, the constituent element of alloy is matched with equimolar ratio, and the mole percent of every kind of element is between 5%~35%.Not due to alloy
Based on some element, high-entropy alloy is also referred to as multi-principal elements alloy.
Although the constituent element of high-entropy alloy is more, after rationally meticulous ingredient design, alloy tends to form solid solution
Body phase, such as: face-centered cubic (fcc), body-centered cubic (bcc) or close-packed hexagonal (hcp) are formed by mutually well below gibbs
The phase that phase rule is predicted, this may be as caused by the high entropy effect of high-entropy alloy, especially in the event of high temperatures.
Infusibility high-entropy alloy becomes potential high-temperature structural material, but the high entropy of infusibility closes since its fusing point and intensity are high
Plasticity is poor at room temperature for gold, it is difficult to be widely applied, have great importance so preparing the single-phase infusibility high-entropy alloy of one kind.
This will provide good basis for the thermo-mechanical processi of next step, to obtain having the alloy of more preferable comprehensive performance, low-density, height
The infusibility high-entropy alloy of fusing point, high intensity and good plasticity is with a wide range of applications.
Summary of the invention
The object of the present invention is to provide a kind of MoNbCrVTi infusibility high-entropy alloy and preparation method thereof, the high entropy of the infusibility is closed
Fitting has low-density, high-melting-point, high intensity and good plasticity, while its structure should be single-phase body-centered cubic (bcc) structure.
The technical scheme is that
A kind of MoNbCrVTi infusibility high-entropy alloy, the high-entropy alloy by 18.0~22.0at.% of Mo, Nb 17.6~
18.0~22.0at.% of 22.4at.%, Ti, 17.8~22.2at.% of V 18.0~22.0at.% and Cr composition.
The MoNbCrVTi infusibility high-entropy alloy, the component of infusibility high-entropy alloy crystal knot having the same
Structure.
The preparation method of the MoNbCrVTi infusibility high-entropy alloy, comprising the following steps:
Step 1: raw material is matched according to the chemical component of alloy；
Step 2: by raw material according to low melting point under, high-melting-point is in the copper crucible that upper sequence is put into vacuum arc furnace ignition；
Vacuum arc furnace ignition vacuum degree is 5 × 10-4After Pa or more, it is filled with the high-purity argon gas of 0.03~0.05MPa, striking melting obtains
MoNbCrVTi infusibility high-entropy alloy.
The MoNbCrVTi infusibility high-entropy alloy, when preparing the infusibility high-entropy alloy, raw material Mo and Cr be it is discoid,
Nb is sheet, and V is dendroid, and Ti is titanium sponge, and the purity of each component is in 99.5 wt.% or more.
The preparation method of the MoNbCrVTi infusibility high-entropy alloy, in step 2, among melting Mo-Nb- Ti first
Alloy takes raw material Mo, Nb and Ti to match melting intermediate alloy according to alloying component；It is then placed in other elements, melting to 5 kinds of members
Plain consolute.
The preparation method of the MoNbCrVTi infusibility high-entropy alloy, in step 2, in order to guarantee that chemical component is uniform
Property, alloy pig at least melting 5 times.
The MoNbCrVTi infusibility high-entropy alloy, it is preferred that the vacuum arc furnace ignition vacuum ranges of step 3 be 1 ×
10-4~5 × 10-4Pa。
The MoNbCrVTi infusibility high-entropy alloy, raw material are pre-processed: Mo and Cr uses mechanical means by surface
Oxide skin is removed, and cleans, dries；Nb and V first cleans 10~20min with petroleum ether, then 10 are cleaned with EtOH Sonicate~
Then 20min is dried in drying box；Ti is directly dried in drying box.
The invention has the advantages and beneficial effects that:
1, the present invention selects five kinds of refractory elements of Mo, Nb, Cr, V and Ti as alloy constituent element, and a kind of Gao Rong is prepared in melting
The single-phase infusibility high-entropy alloy of point, the alloy have the low (7.304g/cm of density3), the advantages that fusing point is high and intensity is high, have extensive
Application prospect.
2, alloy of the present invention has simple single body-centered cubic structure, and excellent in mechanical performance is very high-intensitive having
While, also there is preferable plasticity.To have a possibility that potential application in the high temperature environment.
3, simple substance Mo, Nb, Cr, V and the Ti of the method for the present invention by purity not less than 99.5wt.% mechanically remove table
The oxide skin in face is prepared according to the chemical component of name, and alloy preparation is by melting in vacuum arc furnace ignition, when melting
Low melting point element is placed below copper crucible, high-melting-point is placed on above copper crucible, electric arc furnaces working chamber is then evacuated to 5 ×
10-4Pa is subsequently passed the high-purity argon gas that purity is 99.99wt.%.This method is simple, easy, has broad application prospects.
Detailed description of the invention
Fig. 1 is the XRD spectrum of MoNbCrVTi infusibility high-entropy alloy.In figure, 2 θ of abscissa (degrees) represents the angle of diffraction
(degree)；Ordinate intensity represents intensity (a.u.).
Fig. 2 is the scanning electron microscope back scattering picture of MoNbCrVTi infusibility high-entropy alloy.
Fig. 3 is the room temperature compressive stress strain curve of MoNbCrVTi infusibility high-entropy alloy.
Specific embodiment
The contents of the present invention are described in detail below by way of specific embodiment.
Embodiment
1, the preparation of MoNbCrVTi alloy, the specific steps are as follows:
1) raw material preparation: the infusibility high-entropy alloy component developed of the present invention is molybdenum (Mo), niobium (Nb), chromium (Cr),
Vanadium (V) and titanium (Ti).According to nominal chemical component ingredient when prepared by alloy, 5 kinds of selected element raw material purity is highs in
99.5wt.%.Raw material Mo and Cr be it is discoid, Nb is sheet, and V is dendroid, and Ti is titanium sponge.
Raw material is pre-processed first: mechanically removing the oxide skin on the surface Mo and Cr, and cleans, dry.
Nb and V first cleans 15min with petroleum ether, then cleans 15min with EtOH Sonicate, then dried in drying box (80 DEG C of temperature, when
Between 2 hours), dry (80 DEG C of temperature, time 2 h) in titanium sponge convection drying case.After pretreatment, according to equimolar than essence
Really weigh the quality of each element.
2) prepared by alloy: the instrument that alloy preparation of the present invention uses has for Shenyang Scientific Instrument Development Centre, Chinese Academy of Sciences
The 300 type tungsten electrode magnetic control arc furnace of WCE of limit company production, crucible when melting are water jacketed copper crucible.
Raw material molybdenum (Mo), niobium (Nb), chromium (Cr), vanadium (V) and titanium (Ti) are successively put according to the sequence of fusing point from low to high
Into in water jacketed copper crucible, the raw material of low melting point is placed on lower section, dystectic raw material is placed over, then to electric arc stove evacuation,
Smelting equipment is 300 type tungsten electrode magnetic control arc furnace of WCE.Reach 5 × 10 to vacuum-4After Pa, it is filled with the high-purity argon gas of 0.05MPa.
The indoor titanium ingot of melting chamber first, further decreases partial pressure of oxygen, prevents from aoxidizing during alloy melting.In order to guarantee alloy
Chemical component uniformity, each alloy pig melting 5 times.
Alloy melting is completed, and is filled with air after furnace body is cooling, is opened cavity, take out alloy pig, obtain cast alloy, leads to
It crosses wire cutting, quickly saw and the method for mechanical polishing prepares the sample of Characterization of constitutional structure and mechanical property test.
2, the Characterization of constitutional structure of MoNbCrVTi alloy and Mechanics Performance Testing
1) phase structure of X-ray diffraction (XRD) analysis alloy
It is taken from alloy pig using wire cutting and quick sawingDisk, successively using 240#,
The silicon carbide paper of 600#, 1000# and 2000# are polished, alcohol washes, cold wind drying.XRD analysis is spread out using X ' Pert Pro type
It penetrates instrument to be analyzed, 2 θ ranges are 20~100 °, 4 °/min of scanning speed.
As shown in Figure 1, the diffraction maximum peak shape that can be seen that XRD from test result is sharp, illustrate that the crystallinity of alloy is high.
From four diffraction maximums it can be concluded that the alloy has BCC crystal structure, wherein the corresponding crystal face of four diffraction maximums is respectively
(110), (200), (211) and (220), lattice constant is calculated as 3.1297nm.
2) scanning electron microscope (SEM) structure observation and analysis
The cylinder of area's diameter 5mm from alloy cast ingot, then takes diameter 5mm with quick sawing, and the disk of 2 mm of thickness is made
For the sample of SEM observation.Sample successively by 240#, 600#, 1000#, 2000# and 3000# abrasive paper for metallograph polishing after, with 2.5
μm and 1.0 μm of diamond polishing cream mechanical polishing, then sample alcohol ultrasound 30min dry up spare.SEM model
FEIXL30 uses backscatter mode when observation.
As shown in Fig. 2, contextual analysis of organization's test result shows that the alloy is made of BCC solid solution, tissue morphology is allusion quotation
The as cast condition pine-tree structure of type, dendrite mutually rich high-melting-point element (such as: Mo and Nb), interdendritic mutually rich low melting point element (such as: Cr and
Ti), specifically at being respectively in table 1.
Table 1 is the chemical composition (at.%) of MoNbCrVTi alloy branch crystal phase and interdendritic phase.
| Region | Mo | Nb | V | Cr | Ti |
| Whole ingredient | 20.8 | 22.3 | 18.1 | 18.2 | 20.7 |
| Dendrite phase | 26.5 | 22.7 | 17.0 | 15.4 | 18.4 |
| Interdendritic phase | 16.5 | 21.0 | 17.8 | 21.6 | 23.1 |
EDAX results show dendrite, and mutually main richness Mo, Nb enrichment degree are lighter.The main richness Cr and Ti of interdendritic phase,
The substantially uniform distribution of V, is not obviously segregated.
3) the microhardness analysis of alloy
As alloy microhardness analysis size be Φ 5mm × 2mm, sample successively pass through 240#, 600#, 1000#,
After the polishing of 2000# and 3000# abrasive paper for metallograph, mechanically polished with 2.5 μm and 1.0 μm of diamond polishing cream, then sample wine
Smart ultrasound 30min, dries up spare.Using the microhardness of MHVD-1000AP microhardness testers beta alloy, loading force when test
For 500g, retention time 15s, when test, acquires 7 significant figure strong points, their average value is as last as a result, alloy
Micro-hardness testing result is 494.4 ± 7.7Hv.
4) room temperature Compressive Mechanical Properties are analyzed
Sample for room-temperature mechanical property analysis having a size of Φ 3mm × 6mm, polished with centerless grinding machine by cylindrical side, end
Face is polished flat with abrasive paper for metallograph.Room temperature compression experiment uses equipment for Instron5582 electronic universal tester, strain rate
It is 1 × 10-3/ s, test use 3 parallel samples.
As shown in figure 3, the yield strength of alloy is 1282MPa, compressive strength 1678MPa, straining is 7.8%, can be with
Find out that the alloy has excellent room-temperature mechanical property.
Claims (8)
1. a kind of MoNbCrVTi infusibility high-entropy alloy, which is characterized in that the high-entropy alloy is by 18.0~22.0at.% of Mo, Nb
17.6~22.4at.%, 18.0~22.0at.% of Ti, 17.8~22.2at.% of V 18.0~22.0at.% and Cr composition.
2. MoNbCrVTi infusibility high-entropy alloy according to claim 1, which is characterized in that the group of the infusibility high-entropy alloy
At element crystal structure having the same.
3. a kind of preparation method of MoNbCrVTi infusibility high-entropy alloy of any of claims 1 or 2, which is characterized in that including with
Lower step:
Step 1: raw material is matched according to the chemical component of alloy；
Step 2: by raw material according to low melting point under, high-melting-point is in the copper crucible that upper sequence is put into vacuum arc furnace ignition；Vacuum
Electric arc furnaces vacuum degree is 5 × 10-4After Pa or more, it is filled with the high-purity argon gas of 0.03~0.05MPa, striking melting obtains
MoNbCrVTi infusibility high-entropy alloy.
4. the preparation method of MoNbCrVTi infusibility high-entropy alloy according to claim 3, which is characterized in that prepare the hardly possible
When molten high-entropy alloy, raw material Mo and Cr be it is discoid, Nb is sheet, and V is dendroid, and Ti is titanium sponge, each component it is pure
Degree is in 99.5wt.% or more.
5. the preparation method of MoNbCrVTi infusibility high-entropy alloy according to claim 3, which is characterized in that in step 2,
Melting Mo-Nb-Ti intermediate alloy first takes raw material Mo, Nb and Ti to match melting intermediate alloy according to alloying component；It is then placed in
Other elements, melting to 5 kinds of element consolutes.
6. the preparation method of MoNbCrVTi infusibility high-entropy alloy according to claim 3, which is characterized in that in step 2,
In order to guarantee chemical component uniformity, alloy pig at least melting 5 times.
7. the preparation method of MoNbCrVTi infusibility high-entropy alloy according to claim 3, which is characterized in that step 2
Vacuum arc furnace ignition vacuum ranges are 1 × 10-4~5 × 10-4Pa。
8. the preparation method of MoNbCrVTi infusibility high-entropy alloy according to claim 3, which is characterized in that raw material carries out
Pretreatment: Mo and Cr is removed the oxide skin on surface using mechanical means, and is cleaned, dried；Nb and V first clean 10 with petroleum ether
~20min, then 10~20min is cleaned with EtOH Sonicate, then dried in drying box；Ti is directly dried in drying box.
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| CN108342635A (en) * | 2018-03-28 | 2018-07-31 | 广西大学 | A kind of hexa-atomic high-entropy alloy CoCrFeNiVAl of high intensity infusibilityxAnd preparation method thereof |
| CN108950351A (en) * | 2018-08-15 | 2018-12-07 | 北京理工大学 | A kind of high temperature resistant VNbMoTa high-entropy alloy and preparation method thereof |
| CN110358964B (en) * | 2019-07-24 | 2021-11-05 | 中国科学院金属研究所 | MoVNbTiCr for nuclear powerxHigh-entropy alloy and preparation method thereof |
| CN110331322B (en) * | 2019-07-24 | 2021-01-08 | 中国科学院金属研究所 | MoVNbTiZr for nuclear powerxHigh-entropy alloy and preparation method thereof |
| JP2022185832A (en) * | 2021-06-03 | 2022-12-15 | 株式会社日立製作所 | Alloy and structure |
| CN113621861B (en) * | 2021-07-28 | 2022-06-07 | 中国科学院金属研究所 | MoNbTaTiVCrxHigh-entropy alloy and preparation method thereof |
| CN113667875B (en) * | 2021-07-28 | 2022-07-12 | 中国科学院金属研究所 | MoNbTaTiVSix high-entropy alloy and preparation method thereof |
| CN116024480A (en) * | 2023-01-10 | 2023-04-28 | 昆明理工大学 | High-entropy alloy material and preparation method thereof |
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| CN104120325A (en) * | 2014-07-04 | 2014-10-29 | 北京科技大学 | Low thermal expansion coefficient NaMxAlySiz high entropy alloy and preparation method thereof |
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| CN104120325A (en) * | 2014-07-04 | 2014-10-29 | 北京科技大学 | Low thermal expansion coefficient NaMxAlySiz high entropy alloy and preparation method thereof |
| CN105296836A (en) * | 2015-11-17 | 2016-02-03 | 北京科技大学 | NxMy high-entropy alloy with shape memory effect and preparing method thereof |
| CN106048374A (en) * | 2016-07-19 | 2016-10-26 | 中南大学 | Refractory high-entropy alloy/titanium carbide composite and preparation method thereof |
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