CN108130470A - A kind of MoNbTaZrHf high-entropy alloys and preparation method thereof - Google Patents
A kind of MoNbTaZrHf high-entropy alloys and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of wear-resisting MoNbTaZrHf high-entropy alloys and preparation method thereof.The component MoaNbbTacZrdHfe of the high-entropy alloy, wherein, the mol ratio a of each element:b:c:d:e=1:1:1:1:1 or equimolar ratio.The present invention prepares high rigidity, the high entropy alloy material of good corrosion resistance by non-consumable vacuum arc melting technique, makes up the deficiency of conventional alloys, meets following high-hardness corrosion-resistant heat-resisting material application demand.
Description
Technical field
The present invention relates to technical field of novel materials, and in particular to a kind of MoNbTaZrHf high-entropy alloys and its preparation side
Method.
Background technology
High-entropy alloy (High Entropy Alloy) is a kind of new alloy design concept proposed the 1990s,
Also known as high randomness alloy, be alloy with the characteristics of multi-metal element equimolar ratio or nearly equimolar ratio breach with
The development framework of conventional alloys based on a kind or 2 kinds of metallic elements has dynamics, thermodynamics, tissue and configuration aspects and summarizes
Go out four big high-entropy alloy effects, i.e., sluggish diffusion effect, high entropic effect, distortion of lattice effect and cocktail effect.Due to having
High entropic effect thermodynamically, the distortion of lattice effect in structure, sluggish diffusion effect kinetically, the cocktail in performance
Effect is easy to get solid solution phase simple in structure, that thermal stability is high and nanostructured even non crystalline structure, have high intensity,
The performance characteristics such as wear-resisting, corrosion-resistant high rigidity, resistance to temper softening.
It such as can significantly be applied to make high intensity, obdurability, high temperature resistant, corrosion resistant cutter, mold and parts；Manufacture
The resistant material of chemical plant, ships etc.；By various process for treating surface, high-entropy alloy coating, which is made, improves substrate performance.
The application of high-entropy alloy is the high function of incision, the good opportunity of high added value specific alloy Material Field, therefore prepares high-performance
MoNbTaZrHf high-entropy alloys have very important significance.
At present, the research of high-entropy alloy is designed primarily with regard to alloy, phase composition and phase formation mechenism, main composition member
Influence of the element to alloy structure, mechanical property etc. is heat-treated the influence to high-entropy alloy tissue and performance, preparation and application etc..
And existing high entropy alloy material is mostly to lay particular emphasis on single performance (such as high rigidity, corrosion resistance, heat-resisting quantity), is lacked
Collect the alloy material of the matched well of high rigidity, corrosion resistance, heat-resisting quantity etc..
Invention content
The present invention is a kind of in order to which existing high-entropy alloy provides to have the heat safe high-entropy alloy of high-hardness corrosion-resistant and its system
Preparation Method.Make its application in high rigidity, corrosion-resistant, heat safe workpiece or material etc..
The used in order to solve the above problem technical solution of the present invention is：A kind of MoNbTaZrHf high-entropy alloys, feature
It is, the component of the high-entropy alloy is MoaNbbTacZrdHfe, wherein, the mol ratio a of each element:b:c:d:E=1:1:1:1:
1；Mass fraction degree, that is, purity of the materials such as Mo, Nb, Ta, Zr, Hf, Ti of use is more than 99.7%.
A kind of preparation method of MoNbTaZrHf high-entropy alloys, includes the following steps：
Step 1: Mo, Nb, Ta, Zr, Hf, Ti material are placed in container, then it is ultrasonically treated respectively, it is spare；
Step 2: according to the component, one obtained Mo, Nb, Ta, Zr, Hf material of the step of equimolar amounts matches is weighed
Material；
Step 3: processed Ti materials in step 1 is taken to be put into any melting kettle of water cooled copper mould, then by step
The two each material deciles of residue weighed are placed in the melting kettle of other 3~5 of water cooled copper mould, and each crucible is according to material
The sequence of fusing point from low to high from bottom to top is sequentially placed, spare；
Step 4: by the vacuum chamber inside smelting furnace to 6.6*10-3Pa is then charged with argon gas to 0.01Pa, should
Step repeats two and arrives three times with clean vacuum chambers；
Step 5: first acting on melting (also caning absorb the remnant oxygen in smelting furnace) by striking of Ti materials, then melt successively
Mo, Nb, Ta, Zr, Hf material in other crucibles are refined, pure Ti ingot bars A and alloy ingot B will be obtained after melting successively, will be closed
Golden ingot bar B melting 3~5 times again, overturn sample after each melting, carry out the melting of same method later, after furnace cooling, are made
MoNbTaZrHf high-entropy alloys.
Further, the method for the supersound process in step 1 is：After addition acetone floods material in container, ultrasound is clear
Wash 15~20min, the greasy dirt and impurity of the attachment of removal metal surface；Then again by remove impurity after Mo, Nb, Ta, Zr, Hf,
Ti materials are respectively placed in the container for adding in absolute ethyl alcohol, are cleaned by ultrasonic 15~20min, are subsequently placed in baking oven and dry, obtain
Mo, Nb, Ta, Zr, Hf, Ti material after supersound process.
In the step five of the present invention, melting is carried out using non-consumable vacuum arc melting technique, wherein, Ti materials 30~
Melting 2min under 50V voltages, 100~300A electric currents, obtains ingot bar A；Under identical voltage and current in other crucibles of melting
Mo, Nb, Ta, Zr, Hf material 2min, obtain alloy ingot B.
Compared with present technology, the advantage of the invention is that：
1. the present invention provides a kind of MoNbTaZrHf high-entropy alloys, the high-entropy alloy is mainly by simple BCC and HCP
Solid solution phase forms, and alloy structure is uniform.The alloy has high rigidity, good corrosion resistance, heat-resisting quantity, has wide answer
Use prospect.
2. the component element density of the high-entropy alloy of the present invention is larger, prepared by non-consumable vacuum arc melting technique
High rigidity, excellent corrosion-resistant, heat-resisting quantity high entropy alloy material make up the deficiency of conventional alloys, meet following high rigidity
Corrosion-resistant and high-temperature resistant material application demand.Melting vacuum degree, melting electric current and melting number are controlled during alloy melting, is prepared
MoNbTaZrHf high-entropy alloys.
3. in the present invention, elements Mo can promote alloy to be changed from FCC configuration to BCC structures, contribute to carrying for alloy strength
Height, and Mo is also corrosion resistant alloy common element, is easy to form dense oxidation film on surface, improves alloy corrosion resistance；Nb、Zr
(refractory metal) improves Impact Toughness of Alloy advantageous；Hf, Zr property are similar, not with dilute hydrochloric acid, sulfuric acid, highly basic the effects that, carry
The corrosion resistance of high alloy.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of MoNbTaZrHf high-entropy alloys prepared in embodiment
Specific embodiment
With reference to specific embodiment, the invention will be further described, so that those skilled in the art is better understood from
The present invention can be simultaneously practiced, but illustrated embodiment is not as a limitation of the invention.
First, a kind of MoNbTaZrHf high-entropy alloys, the component of the high-entropy alloy is MoaNbbTacZrdHfe, wherein, each element
Mol ratio a:b:c:d:E=1:1:1:1:1；The mass fraction percentage of the materials such as Mo, Nb, Ta, Zr, Hf, Ti of use
Content, that is, purity is more than 99.7%.
2nd, a kind of preparation method of MoNbTaZrHf high-entropy alloys, includes the following steps：
(1) it is ultrasonically treated：After addition acetone floods material in container, it is cleaned by ultrasonic 15~20min, removes metal surface
The greasy dirt and impurity of attachment；Then Mo, Nb, Ta, Zr, Hf, Ti material after removal impurity are respectively placed in again and add in anhydrous second
In the container of alcohol, it is cleaned by ultrasonic 15~20min, is subsequently placed in baking oven and dries, Mo, Nb, Ta, Zr after being ultrasonically treated,
Hf, Ti material；
(2) dispensing：Weigh the component, Mo, Nb, Ta after the supersound process for weighing step 1 and obtaining of equimolar amounts,
Zr, Hf material；
(3) high-entropy alloy melting：1. processed Ti materials in step 1 is taken to be put into any melting kettle of water cooled copper mould
It is interior, then each material decile of residue that step 2 weighs is placed in the melting kettle of other 3~5 of water cooled copper mould, each earthenware
Crucible is sequentially placed according to the fusing point sequence from low to high from bottom to top of material, spare；
2. by the vacuum chamber inside smelting furnace to 6.6*10-3Pa is then charged with argon gas to 0.01Pa, the step
Two are repeated to arrive three times with clean vacuum chambers；
3. melting (also caning absorb the remnant oxygen in smelting furnace) first is acted on by striking of Ti materials, then melting is another successively
Mo, Nb, Ta, Zr, Hf material in a little crucibles will obtain pure Ti ingot bars A and alloy ingot B after melting, by alloy ingot B successively
Melting 3~5 times again overturn sample after each melting, carry out the melting of same method later, after furnace cooling, are made
MoNbTaZrHf high-entropy alloys.
3rd, X-ray diffractometer (XRD) test and crystal species analysis：1. the ingot casting of acquisition is cut into 5mm using wire cutting
The square sample of × 5mm × 4mm sizes, then sample is beaten successively using the abrasive paper for metallograph of 600#, 800#, 1000# and 1500#
Mill, reuses diamond polishing cream and is polished.X-ray diffraction material phase analysis is penetrated in Rigaku Rigaku D/Max 2500X
It is carried out on line diffractometer.Equipment and technology specification：Using Cu as radiation source, graphite monochromator, operation voltage 40kV, electric current
250mA, rotation target.8 °/min of sweep speed, the selection angle of diffraction ranging from 2 θ=5-90 °.Using 6.0 softwares of MDI-Jade and
8.0 softwares of origin analyze experimental data, determine object phase.
2. as shown in Figure 1, the XRD test results of MoNbTaZrHf high-entropy alloys are shown, the main composition of alloy is mutually letter
Single BCC and HCP structure solid solution phases.
4th, microsclerometry and analysis：Ingot casting is cut into the rectangular of 5mm × 5mm × 4mm sizes using wire cutting machine
Sample, by sample successively using 600#, 800#, 1000# and 1500# abrasive paper for metallograph grind, reuse diamond polishing cream into
Row polishing.Using the hardness of HZr-1000 type microhardness testers test samples, the test force of the microhardness testers is 9.807N
(1kgf) loads 15s.Sample chooses 5~7 different locations and measures its microhardness, removes maximum hardness value and lowest hardness
Value, taking the mean values of remaining hardness number, the microhardness value for finally obtaining the alloy is as the microhardness value of sample
646HV。
5th, microscopic examination：The ingot casting of acquisition is cut into the rectangular sample of 5mm × 5mm × 4mm sizes using wire cutting
Sample using the abrasive paper for metallograph of 600#, 800#, 1000# and 1500# is ground, reuses the progress of diamond polishing cream by product successively
Polishing.It is mainly arborescent structure with scanning electron microscope observation sample tissue.
Claims (4)
1. a kind of MoNbTaZrHf high-entropy alloys, which is characterized in that the component of the high-entropy alloy is MoaNbbTacZrdHfe, each member
The mol ratio a of element:b:c:d:e=1:1:1:1:1 or equimolar ratio；The quality hundred of Mo, Nb, Ta, Zr, Hf, Ti material of use
It is more than 99.7% to divide than content, that is, purity；And the materials such as Mo, Nb, Ta, Zr, Hf, Ti are sheet, large grained.
2. prepare a kind of method of MoNbTaZrHf high-entropy alloys as described in claim 1, which is characterized in that including following step
Suddenly：
Step 1: Mo, Nb, Ta, Zr, Hf, Ti material are placed in container, then it is ultrasonically treated respectively, it is spare；
Step 2: according to the component, one obtained Mo, Nb, Ta, Zr, Hf material of the step of equimolar amounts matches is weighed；
Step 3: processed Ti materials in step 1 is taken to be put into any melting kettle of water cooled copper mould, then step 2 is claimed
Each material decile of residue taken is placed in the melting kettle of other 3 ~ 5 of water cooled copper mould, each crucible according to material fusing point
Sequence from bottom to top is sequentially placed from low to high, spare；
Step 4: by the vacuum chamber inside smelting furnace to 6.6*10-3Pa is then charged with argon gas to 0.01Pa, the step
Two are repeated to arrive three times with clean vacuum chambers；
Step 5: first melting is acted on by striking of Ti materials（Also the remnant oxygen caning absorb in smelting furnace）, then melting is another successively
Mo, Nb, Ta, Zr, Hf material in some crucibles will obtain pure Ti ingot bars A and alloy ingot B after melting successively, alloy will be cast
Block B melting 3 ~ 5 times again, overturn sample after each melting, carry out the melting of same method later, after furnace cooling, are made
MoNbTaZrHf high-entropy alloys.
3. a kind of preparation method of MoNbTaZrHf high-entropy alloys according to claim 2, it is characterised in that：In step 1
The method of supersound process be：After addition acetone floods material in container, it is cleaned by ultrasonic 15 ~ 20min, removal metal surface is attached
The greasy dirt and impurity；Mo, Nb, Ta, Zr, Hf, Ti material after removal impurity are then respectively placed in addition absolute ethyl alcohol again
Container in, be cleaned by ultrasonic 15 ~ 20min, be subsequently placed in baking oven and dry, Mo, Nb, Ta, Zr, Hf after being ultrasonically treated,
Ti materials.
4. a kind of preparation method of MoNbTaZrHf high-entropy alloys according to claim 2, it is characterised in that：Step 5
In, melting is carried out using non-consumable vacuum arc melting technique, wherein, Ti materials are under 30 ~ 50V voltages, 100 ~ 300A electric currents
Melting 2min obtains ingot bar A；Mo, Nb, Ta, Zr, Hf material 2min under identical voltage and current in other crucibles of melting,
Obtain alloy ingot B.
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Cited By (12)
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| CN109266880A (en) * | 2018-11-28 | 2019-01-25 | 湘潭大学 | High entropy alloy material and preparation method thereof that CuNbTaTiV is anti-corrosion |
| CN109338200A (en) * | 2018-11-07 | 2019-02-15 | 北京科技大学 | A kind of high temperature high-damping high-entropy alloy and preparation method thereof |
| CN109576519A (en) * | 2018-12-27 | 2019-04-05 | 中北大学 | A kind of preparation method of iron copper manganese nickel high-entropy alloy |
| CN110453131A (en) * | 2019-09-09 | 2019-11-15 | 沈阳工业大学 | A kind of high-entropy alloy and preparation method thereof with good thermal processability energy |
| CN111363964A (en) * | 2020-03-10 | 2020-07-03 | 中国人民解放军军事科学院国防科技创新研究院 | W-Ta-Mo-Nb-Hf-C high-temperature high-entropy alloy and preparation method thereof |
| CN112962011A (en) * | 2021-01-29 | 2021-06-15 | 佛山科学技术学院 | High-entropy alloy for corrosion-resistant nuclear power and preparation method thereof |
| CN114561621A (en) * | 2021-12-10 | 2022-05-31 | 吉林大学 | High-entropy metal glass film and preparation method and application thereof |
| CN114606424A (en) * | 2022-05-11 | 2022-06-10 | 北京科技大学 | High-strength high-toughness Mo-Nb-Ta-Hf-Zr refractory high-entropy alloy and preparation method thereof |
| CN114855049A (en) * | 2022-04-11 | 2022-08-05 | 北京科技大学 | TaNbHfZrTi series refractory high-entropy alloy and preparation method and application thereof |
| CN115627404A (en) * | 2022-10-21 | 2023-01-20 | 福建工程学院 | High-entropy alloy and preparation method of high-wear-resistant corrosion-resistant high-entropy alloy |
| CN115747604A (en) * | 2022-11-30 | 2023-03-07 | 太原理工大学 | Mo-based high-entropy alloy and application thereof |
| CN115745018A (en) * | 2021-01-08 | 2023-03-07 | 北京航空航天大学 | High-entropy MXene material, high-entropy MAX phase material, preparation methods of high-entropy MXene material and high-entropy MAX phase material, electrode and battery |
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Cited By (20)
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| CN109338200A (en) * | 2018-11-07 | 2019-02-15 | 北京科技大学 | A kind of high temperature high-damping high-entropy alloy and preparation method thereof |
| CN109338200B (en) * | 2018-11-07 | 2021-05-04 | 北京科技大学 | High-temperature high-damping high-entropy alloy and preparation method thereof |
| CN109266880A (en) * | 2018-11-28 | 2019-01-25 | 湘潭大学 | High entropy alloy material and preparation method thereof that CuNbTaTiV is anti-corrosion |
| CN109576519A (en) * | 2018-12-27 | 2019-04-05 | 中北大学 | A kind of preparation method of iron copper manganese nickel high-entropy alloy |
| CN109576519B (en) * | 2018-12-27 | 2020-10-30 | 中北大学 | Preparation method of iron-copper-manganese-nickel high-entropy alloy |
| CN110453131A (en) * | 2019-09-09 | 2019-11-15 | 沈阳工业大学 | A kind of high-entropy alloy and preparation method thereof with good thermal processability energy |
| CN111363964A (en) * | 2020-03-10 | 2020-07-03 | 中国人民解放军军事科学院国防科技创新研究院 | W-Ta-Mo-Nb-Hf-C high-temperature high-entropy alloy and preparation method thereof |
| CN111363964B (en) * | 2020-03-10 | 2021-08-20 | 中国人民解放军军事科学院国防科技创新研究院 | W-Ta-Mo-Nb-Hf-C high-temperature high-entropy alloy and preparation method thereof |
| CN115745018A (en) * | 2021-01-08 | 2023-03-07 | 北京航空航天大学 | High-entropy MXene material, high-entropy MAX phase material, preparation methods of high-entropy MXene material and high-entropy MAX phase material, electrode and battery |
| CN115745018B (en) * | 2021-01-08 | 2024-02-06 | 北京航空航天大学 | High-entropy MXene material, high-entropy MAX phase material, preparation methods of high-entropy MXene material and MAX phase material, electrode and battery |
| CN112962011A (en) * | 2021-01-29 | 2021-06-15 | 佛山科学技术学院 | High-entropy alloy for corrosion-resistant nuclear power and preparation method thereof |
| CN112962011B (en) * | 2021-01-29 | 2022-01-25 | 佛山科学技术学院 | High-entropy alloy for corrosion-resistant nuclear power and preparation method thereof |
| CN114561621A (en) * | 2021-12-10 | 2022-05-31 | 吉林大学 | High-entropy metal glass film and preparation method and application thereof |
| CN114561621B (en) * | 2021-12-10 | 2022-12-02 | 吉林大学 | High-entropy metal glass film and preparation method and application thereof |
| CN114855049A (en) * | 2022-04-11 | 2022-08-05 | 北京科技大学 | TaNbHfZrTi series refractory high-entropy alloy and preparation method and application thereof |
| CN114855049B (en) * | 2022-04-11 | 2023-03-07 | 北京科技大学 | TaNbHfZrTi series refractory high-entropy alloy and preparation method and application thereof |
| CN114606424A (en) * | 2022-05-11 | 2022-06-10 | 北京科技大学 | High-strength high-toughness Mo-Nb-Ta-Hf-Zr refractory high-entropy alloy and preparation method thereof |
| CN115627404A (en) * | 2022-10-21 | 2023-01-20 | 福建工程学院 | High-entropy alloy and preparation method of high-wear-resistant corrosion-resistant high-entropy alloy |
| CN115747604A (en) * | 2022-11-30 | 2023-03-07 | 太原理工大学 | Mo-based high-entropy alloy and application thereof |
| CN115747604B (en) * | 2022-11-30 | 2024-02-02 | 太原理工大学 | Mo-based high-entropy alloy and application thereof |
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