CN117089754A - Nanoscale ultrafine lamellar eutectic high-entropy alloy and preparation method thereof - Google Patents
Nanoscale ultrafine lamellar eutectic high-entropy alloy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 84
- 239000000956 alloy Substances 0.000 title claims abstract description 84
- 230000005496 eutectics Effects 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 238000003723 Smelting Methods 0.000 claims abstract description 44
- 239000000126 substance Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000010791 quenching Methods 0.000 claims abstract description 6
- 230000000171 quenching effect Effects 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 230000006698 induction Effects 0.000 abstract description 5
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000010891 electric arc Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 6
- 238000007711 solidification Methods 0.000 description 6
- 230000008023 solidification Effects 0.000 description 6
- 239000000155 melt Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910001325 element alloy Inorganic materials 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/003—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals by induction
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/20—Arc remelting
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- 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
- C22C1/023—Alloys based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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Abstract
A nanoscale superfine lamellar eutectic high-entropy alloy and a preparation method thereof relate to a nanoscale superfine lamellar eutectic high-entropy alloy and a preparation method thereof. The invention aims to solve the problems that the eutectic high-entropy alloy has larger alloy grain size and wider lamellar spacing, so that high strength and high plasticity can not be obtained at the same time, and the chemical formula of the nano-scale ultrafine lamellar eutectic high-entropy alloy is Al 1.25 CoCrFeNi 3 . The preparation method comprises the following steps: firstly, smelting an ingot by using an electric arc furnace, obtaining an alloy bar by using wire cutting, and then, after induction smelting by using a Bridgman smelting furnace, instantly entering Ga-In liquid for quenching to obtain the ultra-fine eutectic high-entropy alloy. The eutectic high entropy alloy prepared by the inventionThe hardware has a layer sheet with nano-scale thickness and has excellent strength and plasticity, and the invention is applied to the field of metal materials and preparation thereof.
Description
Technical Field
The invention relates to a nanoscale superfine lamellar eutectic high-entropy alloy and a preparation method thereof.
Background
Along with the progress of science and society, the requirements on high-performance materials are becoming more severe, and the materials are required to have corrosion resistance, abrasion resistance, oxidation resistance and the like on the premise of meeting the strength and the plasticity. The design concept of conventional metal materials has therefore been difficult to follow the development of the era.
The high-entropy alloy breaks through the design concept of the traditional alloy, and is designed by adding trace elements instead of one to two elements as principal elements, and is composed of five or more elements, wherein each element can be used as principal element, so that the alloy is also called as multi-principal element alloy. Due to the cocktail effect of the high-entropy alloy, the high-entropy alloy has the excellent properties of each element. However, single-phase solid solutions, such as face-centered cubic high-entropy alloys, have low plastic properties and low body-centered cubic strength, and the mismatch of such strong plastic properties makes it difficult to further develop engineering applications for the single-phase high-entropy alloys.
The eutectic high-entropy alloy generally consists of soft and hard phases, and has the advantages of the strength and the plasticity of face-centered cubic and body-centered cubic high-entropy alloys. However, the existing preparation method of the eutectic high-entropy alloy is mainly focused on methods such as arc melting, plasma sintering and the like, and the prepared alloy has larger grain size and wider lamellar spacing, and is difficult to improve strength and plasticity at the same time. Due to the limitation of the preparation method, the component design of the existing eutectic high-entropy alloy can consider ensuring certain plasticity, and the strength of the alloy is difficult to further improve.
Disclosure of Invention
The invention aims to solve the problems that the eutectic high-entropy alloy cannot obtain high strength and high plasticity at the same time due to larger alloy grain size and wider lamellar spacing, and provides a nanoscale superfine lamellar eutectic high-entropy alloy and a preparation method thereof.
The invention relates to a kind of deviceThe chemical formula of the nano superfine lamellar eutectic high-entropy alloy is Al 1.25 CoCrFeNi 3 。
The invention relates to a preparation method of a nanoscale superfine lamellar eutectic high-entropy alloy, which comprises the following steps:
1. weighing raw materials according to an atomic ratio to obtain raw materials;
2. putting the raw materials into a tungsten electrode non-consumable vacuum melting furnace for ingot casting melting to obtain an ingot casting;
3. cutting the cast ingot into metal bars, and then cleaning to obtain cleaned metal bars;
4. and placing the metal rod into a ceramic tube, then placing the ceramic tube into a vacuum smelting furnace, heating and smelting, and immediately entering Ga-In liquid for quenching to obtain the eutectic high-entropy alloy with the nanoscale superfine lamellar.
The invention has the following beneficial effects:
1. the invention provides a novel method for preparing a nanoscale superfine lamellar eutectic high-entropy alloy, which combines induction smelting and quenching, and utilizes a smelting and solidification mode combining the induction smelting and the quenching, so that the solidification speed is high, the prepared alloy has small grain size, the eutectic lamellar thickness can reach nanoscale, the remarkable fine-grain strengthening effect is realized, and the strength and plasticity of the alloy are further improved on the basis of alloy components. The invention has simple preparation process, low preparation cost and high production efficiency. The method can also be applied to the preparation of other eutectic high-entropy alloys, and is a preparation process with great development prospect.
2. Designed novel Al 1.25 CoCrFeNi 3 The high content of Al and Ni promotes the formation of high-strength BCC phases in the alloy, and the high content of BCC phases further improves the strength of the alloy.
3. The novel preparation method provided by the invention prepares Al 1.25 CoCrFeNi 3 The eutectic high-entropy alloy has excellent performance at room temperature. The tensile strength is 826.91MPa, and the elongation is 19.08%. The compression strain exceeds 55%, and the compression strength exceeds 2.8GPa.
Drawings
FIG. 1 is a nano-scale ultrafine platelet Al in example 1 1.25 CoCrFeNi 3 A longitudinal section microstructure map of the eutectic high-entropy alloy;
FIG. 2 is a nano-scale ultrafine platelet Al in example 1 1.25 CoCrFeNi 3 Electron back scattering diffraction pattern of eutectic high entropy alloy;
FIG. 3 is a nano-scale ultrafine platelet Al in example 1 1.25 CoCrFeNi 3 A tensile stress-strain curve of the eutectic high-entropy alloy;
FIG. 4 shows the nanoscale ultrafine platelet Al in example 1 1.25 CoCrFeNi 3 A compressive stress-strain curve of the eutectic high entropy alloy;
FIG. 5 shows Al prepared by the directional solidification method in example 2 1.25 CoCrFeNi 3 Microstructure map of eutectic high entropy alloy;
FIG. 6 shows Al prepared by the directional solidification method in example 2 1.25 CoCrFeNi 3 A tensile stress-strain curve of the eutectic high-entropy alloy.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments. The first embodiment is as follows: the chemical formula of the nano-scale ultra-fine lamellar eutectic high-entropy alloy in the embodiment is Al 1.25 CoCrFeNi 3 。
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the Al is 1.25 CoCrFeNi 3 The high-entropy alloy consists of 17.25% Al, 13.79% Co, 13.79% Cr, 13.79% Fe and 41.38% Ni in atomic percent. The other is the same as in the first embodiment.
And a third specific embodiment: the preparation method of the nanoscale superfine lamellar eutectic high-entropy alloy comprises the following steps of:
1. weighing raw materials according to an atomic ratio to obtain raw materials;
2. putting the raw materials into a tungsten electrode non-consumable vacuum melting furnace for ingot casting melting to obtain an ingot casting;
3. cutting the cast ingot into metal bars, and then cleaning to obtain cleaned metal bars;
4. and placing the metal rod into a ceramic tube, then placing the ceramic tube into a vacuum smelting furnace, heating and smelting, and immediately entering Ga-In liquid for quenching to obtain the eutectic high-entropy alloy with the nanoscale superfine lamellar.
In the embodiment, the diameter of the metal rod is equal to or similar to the inner diameter of the ceramic tube, so that the metal rod is ensured to be contacted with the inner wall of the ceramic tube.
The specific embodiment IV is as follows: the third difference between this embodiment and the third embodiment is that: vacuumizing a tungsten electrode non-consumable vacuum smelting furnace to 6 multiplied by 10 before smelting -3 Pa, then argon is introduced to 0.1MPa. The other is the same as in the third embodiment.
Fifth embodiment: this embodiment differs from the third or fourth embodiment in that: the smelting times are 7 times. The other is the same as in the third or fourth embodiment.
Specific embodiment six: this embodiment differs from one of the third to fifth embodiments in that: the cleaning method of the metal rod in the melting step III comprises the following steps: and (5) polishing by using sand paper, and then ultrasonically cleaning. The others are the same as in one of the third to fifth embodiments.
Seventh embodiment: this embodiment differs from one of the third to sixth embodiments in that: the sand paper is 400-2000 meshes. The others are the same as in one of the third to sixth embodiments.
Eighth embodiment: this embodiment differs from one of the third to seventh embodiments in that: and step four, vacuumizing to 20Pa before smelting, then introducing protective gas to 0.1MPa, and repeating gas washing for 3 times. The others are the same as in one of the third to seventh embodiments.
Detailed description nine: this embodiment differs from one of the fifth to eighth embodiments in that: the shielding gas is argon. The others are the same as in one of the fifth to eighth embodiments.
Eleventh embodiment: this embodiment differs from one of the fifth to ninth embodiments in that: and step four, raising the temperature to 2000 ℃ and then preserving the heat for 50 minutes to perform smelting. The others are the same as in one of the fifth to ninth embodiments.
The following examples are used to verify the benefits of the present invention:
example 1
The chemical formula of the nano-scale ultra-fine lamellar eutectic high-entropy alloy is Al 1.25 CoCrFeNi 3 。
The preparation process is as follows:
step one, according to atomic Al 1.25 CoCrFeNi 3 The metal simple substance particles with the purity of 99.5% are weighed, wherein the metal simple substance particles are calculated according to the mass ratio, and the metal simple substance particles comprise 8.96% of Al, 15.65% of Co, 13.81% of Cr, 14.83% of Fe and 46.75% of Ni;
wherein, considering the burning loss during smelting, the weighing mass is weighed according to 103 percent of the nominal component mass, and the mass is accurate to 0.01 gram;
and secondly, carrying out ingot casting smelting by using a tungsten electrode non-consumable vacuum smelting furnace, and placing Al metal particles with the lowest density and the lowest melting point at the bottommost part in a crucible of the smelting furnace, wherein Al, ni, co, fe, cr is arranged in sequence from bottom to top. Vacuum is required to be pumped to 6 multiplied by 10 before smelting -3 Pa, then introducing argon of 0.1MPa as shielding gas, and repeatedly smelting for 7 times to ensure that the components are uniformly distributed;
cutting the cast ingot into bars with the diameter of 8mm, polishing impurities on the surface by using 400-2000 meshes of sand paper, and cleaning by using ultrasonic waves;
and fourthly, placing the metal rod into a ceramic tube with the inner diameter of 8mm, and placing into a vacuum Bridgman smelting furnace. The smelting mode of the vacuum Bridgman smelting furnace is vacuum induction smelting, ga-In liquid is arranged below the melt, and carbon felt is used for isolating the temperature. Before smelting by using a vacuum Bridgman smelting furnace, vacuumizing to 20Pa, and then introducing argon as a protective gas to 0.1MPa, thus finishing primary gas washing. Three scrubbing operations are repeated. After the start of melting, the temperature was raised to 2000℃and the mixture was kept at that temperature for 50 minutes. After the alloy is completely melted, the alloy melt is instantly quenched In Ga-In liquid, and the eutectic high-entropy alloy of the nanoscale superfine lamellar layer is obtained.
Experimental test analysis:
the embodiment is manufactured intoPrepared nano superfine lamellar Al 1.25 CoCrFeNi 3 As can be seen from the scanning tissue diagram of FIG. 1, the thickness of the lamellar structure of the longitudinal section of the eutectic high-entropy alloy prepared by the method is nano-scale. FIG. 2 is a nano-scale ultrafine platelet Al 1.25 CoCrFeNi 3 Electron back scattering diffraction pattern of eutectic high entropy alloy; the alloy composition of this example obtained a high content of BCC phase, which was about 42% in content, improving the strength of the alloy.
FIG. 3 is a tensile engineering stress-strain curve of the alloy, the tensile strength of the alloy is 826.91MPa, and the elongation is 19.08%. FIG. 4 is a graph showing the compressive engineering stress-strain curve of the alloy having extremely excellent compressive plasticity, the alloy still being unbroken at a compressive strain exceeding 55%, the compressive strength of the alloy exceeding 2.8GPa at a strain of 55%. Therefore, the eutectic high-entropy alloy prepared by the method has a nanoscale superfine lamellar structure and has excellent strength and plasticity.
Example 2
This example is Al prepared by the directional solidification method 1.25 CoCrFeNi 3 The process of eutectic high entropy alloy is as follows:
step one, according to atomic Al 1.25 CoCrFeNi 3 The metal simple substance particles with the purity of 99.5% are weighed, wherein the metal simple substance particles are calculated according to the mass ratio, and the metal simple substance particles comprise 8.96% of Al, 15.65% of Co, 13.81% of Cr, 14.83% of Fe and 46.75% of Ni;
wherein, considering the burning loss during smelting, the weighing mass is weighed according to 103 percent of the nominal component mass, and the mass is accurate to 0.01 gram;
and secondly, carrying out ingot casting smelting by using a tungsten electrode non-consumable vacuum smelting furnace, and placing Al metal particles with the lowest density and the lowest melting point at the bottommost part in a crucible of the smelting furnace. Vacuum is required to be pumped to 6 multiplied by 10 before smelting -3 Pa, and then argon of 0.1MPa was introduced as a shielding gas. Repeatedly smelting for 7 times, and ensuring the uniform distribution of the components.
Cutting the cast ingot into bars with the diameter of 8mm, polishing impurities on the surface by using 400-2000 meshes of sand paper, and cleaning by using ultrasonic waves;
and fourthly, placing the metal rod into a ceramic tube with the inner diameter of 8mm, and placing into a vacuum Bridgman smelting furnace. The smelting mode of the vacuum Bridgman smelting furnace is vacuum induction smelting, ga-In liquid is arranged below the melt, and carbon felt is used for isolating the temperature. Before smelting by using a vacuum Bridgman smelting furnace, vacuumizing to 20Pa, and then introducing argon as a protective gas to 0.1MPa, thus finishing primary gas washing. Three scrubbing operations are repeated. After the start of melting, the temperature was raised to 2000℃and the mixture was kept at that temperature for 50 minutes. After ensuring that the alloy is completely melted, slowly drawing the melt into Ga-In liquid at a drawing speed of 5 mu m/s to obtain the directionally solidified eutectic high-entropy alloy.
Experimental test analysis:
al prepared by directional solidification in this example 1.25 CoCrFeNi 3 As can be seen from the scanning structure diagram of fig. 5, the lamellar structure of the eutectic high-entropy alloy prepared by the method is obviously coarsened relative to the nano lamellar structure in fig. 1. As can be seen from the engineering stress strain curve of FIG. 6, the strength of the directionally solidified eutectic high-entropy alloy is similar to that of the eutectic high-entropy alloy with the thickness of the nano-scale sheet, but the elongation is 14.22%, which is obviously lower than that of the eutectic high-entropy alloy obtained by the novel preparation method. From this, the eutectic high-entropy alloy obtained by the preparation method of example 1 has a nano-scale ultrafine lamellar structure, and can improve the strength and plasticity of the alloy.
Claims (10)
1. A nanoscale ultrafine lamellar eutectic high-entropy alloy is characterized in that the chemical formula of the high-entropy alloy is Al 1.25 CoCrFeNi 3 。
2. The nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 1, characterized in that the Al 1.25 CoCrFeNi 3 The high-entropy alloy consists of 17.25% Al, 13.79% Co, 13.79% Cr, 13.79% Fe and 41.38% Ni in atomic percent.
3. The method for preparing the nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 1, which is characterized by comprising the following steps:
1. weighing raw materials according to an atomic ratio to obtain raw materials;
2. putting the raw materials into a tungsten electrode non-consumable vacuum melting furnace for ingot casting melting to obtain an ingot casting;
3. cutting the cast ingot into metal bars, and then cleaning to obtain cleaned metal bars;
4. and placing the metal rod into a ceramic tube, then placing the ceramic tube into a vacuum smelting furnace, heating and smelting, and immediately entering Ga-In liquid for quenching to obtain the eutectic high-entropy alloy with the nanoscale superfine lamellar.
4. The method for preparing a nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 3, wherein the tungsten electrode non-consumable vacuum melting furnace is vacuumized to 6×10 before the second melting step -3 Pa, then argon is introduced to 0.1MPa.
5. The method for preparing a nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 3, wherein the smelting times are 7 times.
6. The method for preparing the nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 3, wherein the method for cleaning the metal rod in the third step is as follows: and (5) polishing by using sand paper, and then ultrasonically cleaning.
7. The method for preparing a nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 6, wherein the abrasive paper is 400-2000 meshes.
8. The method for preparing a nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 3, wherein the vacuum is pumped to 20Pa before smelting in the fourth step, then protective gas is introduced to 0.1MPa, and the gas washing is repeated for 3 times.
9. The method for preparing a nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 8, wherein the shielding gas is argon.
10. The method for preparing a nanoscale ultrafine lamellar eutectic high-entropy alloy according to claim 3, wherein the temperature is raised to 2000 ℃ in the fourth step, and then the mixture is kept for 50 minutes for smelting.
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