CN107641751A - A kind of MoNbCrVTi infusibilities high-entropy alloy and preparation method thereof - Google Patents
A kind of MoNbCrVTi infusibilities high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to metal material and its preparation field, specially a kind of composition is MoNbCrVTi infusibility high-entropy alloys and preparation method thereof.The high-entropy alloy is made up of Mo, Nb, Cr, V and Ti, and preparation method is:Simple substance Mo, Nb, Cr, V and the Ti for taking purity to be not less than 99.5wt.%, chemical composition according to name is prepared, alloy is prepared by melting in vacuum arc furnace ignition to obtain, low melting point element is placed on below copper crucible during melting, high-melting-point is placed on above copper crucible, and electric arc furnaces working chamber is evacuated into 5 × 10‑4Pa, is subsequently passed the high-purity argon gas that purity is 99.99wt.%, and striking melting obtains MoNbCrVTi infusibility high-entropy alloys.Alloy of the present invention has simple single body-centered cubic structure, its excellent in mechanical performance, has very high intensity and preferable plasticity, the possibility with the potential application in hot environment.The inventive method 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 composition is MoNbCrVTi infusibility high-entropy alloys
And preparation method thereof.
Background technology
High-entropy alloy is a kind of new 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 expand the system of alloy design, breach traditional conjunction
The mentality of designing of pivot is used as using one or two element 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%.Due to alloy not
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 composition design, alloy tends to form solid solution
Body phase, such as:Face-centered cubic (fcc), body-centered cubic (bcc) or close-packed hexagonal (hcp), the phase formed is well below gibbs
The phase that phase rule is predicted, this is probably due to caused by the high entropic effect of high-entropy alloy, particularly in the event of high temperatures.
Infusibility high-entropy alloy turns into potential high-temperature structural material, but the high entropy of infusibility closes because its fusing point and intensity are high
Plasticity is poor at room temperature for gold, it is difficult to extensive use, has great importance so preparing a kind of single-phase infusibility high-entropy alloy.
This provides the thermo-mechanical processi for next step on good basis, to obtain having the alloy of more preferable combination property, low-density, height
The infusibility high-entropy alloy of fusing point, high intensity and good plasticity is with a wide range of applications.
The content of the invention
It is an object of the invention to provide a kind of MoNbCrVTi infusibilities high-entropy alloy and preparation method thereof, the high entropy of the infusibility closes
Gold utensil 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 infusibilities 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 are formed.
Described MoNbCrVTi infusibility high-entropy alloys, the component of the infusibility high-entropy alloy have identical crystal knot
Structure.
The preparation method of described MoNbCrVTi infusibility high-entropy alloys, comprises the following steps:
Step 1:Raw material is matched according to the chemical composition of alloy;
Step 2:By raw material according to low melting point under, high-melting-point is put into the copper crucible of vacuum arc furnace ignition in upper order;
Vacuum arc furnace ignition vacuum is 5 × 10-4After more than Pa, 0.03~0.05MPa high-purity argon gas is filled with, striking melting obtains
MoNbCrVTi infusibility high-entropy alloys.
Described MoNbCrVTi infusibility high-entropy alloys, when preparing the infusibility high-entropy alloy, raw material Mo and Cr to be discoid,
Nb is sheet, and V is dendroid, and Ti is titanium sponge, and the purity of each component is in 99.5 more than wt.%.
The preparation method of described MoNbCrVTi infusibility high-entropy alloys, in step 2, first among melting Mo-Nb- Ti
Alloy, raw material Mo, Nb and Ti is taken 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 described MoNbCrVTi infusibility high-entropy alloys, in step 2, in order to ensure that chemical composition is uniform
Property, alloy pig at least melting 5 times.
Described MoNbCrVTi infusibility high-entropy alloys, it is preferred that the vacuum arc furnace ignition vacuum ranges of step 3 be 1 ×
10-4~5 × 10-4Pa。
Described MoNbCrVTi infusibility high-entropy alloys, 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~
20min, then dried in drying box;Ti is directly dried in drying box.
Advantages of the present invention and beneficial effect are:
1st, for present invention selection five kinds of refractory elements of Mo, Nb, Cr, V and Ti as alloy constituent element, 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), fusing point it is high and the advantages that intensity is high, have extensive
Application prospect.
2nd, alloy of the present invention has simple single body-centered cubic structure, its excellent in mechanical performance, with very high intensity
While, also with preferable plasticity.So as to the possibility with the potential application in hot environment.
3rd, simple substance Mo, Nb, Cr, V and the Ti of purity not less than 99.5wt.% are mechanically removed table by the inventive method
The oxide skin in face, prepared according to the chemical composition of name, alloy prepare by melting in vacuum arc furnace ignition and must, during melting
Low melting point element is placed on below copper crucible, high-melting-point is placed on above copper crucible, electric arc furnaces working chamber is then evacuated to 5 ×
10-4Pa, it is subsequently passed the high-purity argon gas that purity is 99.99wt.%.This method is simple, easy, has broad application prospects.
Brief description of the drawings
Fig. 1 is the XRD spectrum of MoNbCrVTi infusibility high-entropy alloys.In figure, the θ of abscissa 2 (degrees) represents the angle of diffraction
(degree);Ordinate intensity represents intensity (a.u.).
Fig. 2 is the ESEM back scattering picture of MoNbCrVTi infusibility high-entropy alloys.
Fig. 3 is the room temperature compressive stress strain curve of MoNbCrVTi infusibility high-entropy alloys.
Embodiment
Present disclosure is described in detail below by way of specific embodiment.
Embodiment
1st, the preparation of MoNbCrVTi alloys, is comprised the following steps that:
1) raw material prepares:The infusibility high-entropy alloy component developed of the present invention is molybdenum (Mo), niobium (Nb), chromium (Cr),
Vanadium (V) and titanium (Ti).Alloy is higher than when preparing according to nominal chemical composition dispensing, selected 5 kinds of element material purities
99.5wt.%.Raw material Mo and Cr are discoid, and Nb is sheet, and V is dendroid, and Ti is titanium sponge.
Raw material is pre-processed first:Mechanically the oxide skin on Mo and Cr surfaces is removed, 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), drying (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:Alloy of the present invention prepares the instrument used to be had for Shenyang Scientific Instrument Development Centre, Chinese Academy of Sciences
The type tungsten electrode magnetic control arc stoves of WCE 300 of limit company production, crucible during melting is water jacketed copper crucible.
Raw material molybdenum (Mo), niobium (Nb), chromium (Cr), vanadium (V) and titanium (Ti) are put successively according to the order of fusing point from low to high
Enter 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 the type tungsten electrode magnetic control arc stoves of WCE 300.Treat that vacuum reaches 5 × 10-4After Pa, 0.05MPa high-purity argon gas is filled with.
Titanium ingot first in melting chamber, further reduces partial pressure of oxygen, prevents from aoxidizing during alloy melting.In order to ensure alloy
Chemical composition uniformity, each alloy pig melting 5 times.
Alloy melting is completed, and is filled with air after body of heater cooling, is opened cavity, take out alloy pig, obtain cast alloy, leads to
Cross wire cutting, quick saw and the method for mechanical polishing prepares organizational chart and sought peace the sample of mechanical property test.
2nd, the Characterization of constitutional structure of MoNbCrVTi alloys and Mechanics Performance Testing
1) phase structure of X-ray diffraction (XRD) analysis alloy
Taken from alloy pig using wire cutting and quick sawingDisk, successively using 240#, 600#,
1000# and 2000# silicon carbide paper polishing, alcohol washes, cold wind drying.XRD analysis are entered using X ' Pert Pro type diffractometers
Row analysis, 2 θ scopes are 20~100 °, 4 °/min of sweep speed.
As shown in figure 1, the diffraction maximum peak shape that XRD is can be seen that from test result is sharp, illustrate that the crystallinity of alloy is high.
It can show that the alloy has BCC crystal structures from four diffraction maximums, wherein crystal face corresponding to four diffraction maximums is respectively
(110), (200), (211) and (220), lattice constant is calculated as 3.1297nm.
2) ESEM (SEM) structure observation and analysis
The area's diameter 5mm cylinder from alloy cast ingot, diameter 5mm then is taken with quick sawing, the mm of thickness 2 disk, is made
For the sample of SEM observations.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, drying it is standby.SEM models
FEIXL30, backscatter mode is used during observation.
As shown in Fig. 2 contextual analysis of organization's test result shows, the alloy is made up of BCC solid solution, and tissue morphology is allusion quotation
The as cast condition pine-tree structure of type, the mutually rich high-melting-point element of dendrite is (such as:Mo and Nb), the mutually rich low melting point element in interdendritic is (such as:Cr and
Ti), specifically into being respectively in table 1.
Table 1 is the chemical composition (at.%) of MoNbCrVTi alloy branch crystals phase and interdendritic phase.
Region | Mo | Nb | V | Cr | Ti |
Overall composition | 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 that mutually main rich Mo, Nb enrichment degrees are lighter for dendrite.Interdendritic phase main rich Cr and Ti,
The substantially uniform distributions of V, are not substantially segregated.
3) the microhardness analysis of alloy
Size as the analysis of alloy microhardness be Φ 5mm × 2mm, sample pass through successively 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
The ultrasonic 30min of essence, drying are standby.Using the microhardness of MHVD-1000AP microhardness testers beta alloys, loading force during test
For 500g, retention time 15s gathers 7 significant figure strong points during test, their average value as last result, alloy
Micro-hardness testing result is 494.4 ± 7.7Hv.
4) room temperature Compressive Mechanical Properties are analyzed
Sample size for room-temperature mechanical property analysis is Φ 3mm × 6mm, and cylindrical side is polished with centerless grinder, end
Face is polished flat with abrasive paper for metallograph.Room temperature compression experiment uses equipment as Instron5582 electronic universal testers, strain rate
For 1 × 10-3/ s, test use 3 parallel samples.
As shown in figure 3, the yield strength of alloy is 1282MPa, compressive strength 1678MPa, strain as 7.8%, can be with
Find out that the alloy has excellent room-temperature mechanical property.
Claims (8)
1. a kind of MoNbCrVTi infusibilities high-entropy alloy, it is characterised 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 compositions.
2. MoNbCrVTi infusibilities high-entropy alloy according to claim 1, it is characterised in that the group of the infusibility high-entropy alloy
There is identical crystal structure into element.
A kind of 3. preparation method of the MoNbCrVTi infusibility high-entropy alloys described in claim 1 or 2, it is characterised in that including with
Lower step:
Step 1:Raw material is matched according to the chemical composition of alloy;
Step 2:By raw material according to low melting point under, high-melting-point is put into the copper crucible of vacuum arc furnace ignition in upper order;Vacuum
Electric arc furnaces vacuum is 5 × 10-4After more than Pa, 0.03~0.05MPa high-purity argon gas is filled with, striking melting obtains
MoNbCrVTi infusibility high-entropy alloys.
4. MoNbCrVTi infusibilities high-entropy alloy according to claim 3, it is characterised in that prepare the infusibility high-entropy alloy
When, raw material Mo and Cr are discoid, and Nb is sheet, and V is dendroid, and Ti is titanium sponge, and the purity of each component exists
More than 99.5wt.%.
5. the preparation method of MoNbCrVTi infusibilities high-entropy alloy according to claim 3, it is characterised in that in step 2,
Melting Mo-Nb-Ti intermediate alloys first, raw material Mo, Nb and Ti is taken 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 infusibilities high-entropy alloy according to claim 3, it is characterised in that in step 2,
In order to ensure chemical composition uniformity, alloy pig at least melting 5 times.
7. MoNbCrVTi infusibilities high-entropy alloy according to claim 3, it is characterised in that preferable, the vacuum of step 3
Electric arc furnaces vacuum ranges are 1 × 10-4~5 × 10-4Pa。
8. MoNbCrVTi infusibilities high-entropy alloy according to claim 3, it is characterised in that raw material is pre-processed:Mo and
Cr is removed the oxide skin on surface using mechanical means, and is cleaned, dried;Nb and V first cleans 10~20min with petroleum ether, then
10~20min is cleaned with EtOH Sonicate, is then dried in drying box;Ti is directly dried in drying box.
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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 |
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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 |
WO2022254919A1 (en) * | 2021-06-03 | 2022-12-08 | 株式会社日立製作所 | Alloy and structure |
CN113621861A (en) * | 2021-07-28 | 2021-11-09 | 中国科学院金属研究所 | MoNbTaTiVCrxHigh-entropy alloy and preparation method thereof |
CN113667875A (en) * | 2021-07-28 | 2021-11-19 | 中国科学院金属研究所 | MoNbTaTiVSix high-entropy alloy and preparation method thereof |
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