CN110576185A - Nanocrystalline high-entropy alloy powder and preparation method thereof - Google Patents
Nanocrystalline high-entropy alloy powder and preparation method thereof Download PDFInfo
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- CN110576185A CN110576185A CN201910888130.6A CN201910888130A CN110576185A CN 110576185 A CN110576185 A CN 110576185A CN 201910888130 A CN201910888130 A CN 201910888130A CN 110576185 A CN110576185 A CN 110576185A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/04—Nanocrystalline
Abstract
The invention discloses nanocrystalline high-entropy alloy powder and a preparation method thereof, relating to the technical field of powder metallurgy and comprising the nanocrystalline high-entropy alloy powder; a preparation method of nanocrystalline high-entropy alloy powder; the nanocrystalline high-entropy alloy powder comprises cobalt powder, chromium powder, iron powder, nickel powder, manganese powder, aluminum powder and titanium powder; the preparation method of the nanocrystalline high-entropy alloy powder directly mixes the metal element powder by a high-energy mechanical ball milling method, and the nanocrystalline high-entropy alloy powder is prepared according to specific steps. According to the invention, through high-speed impact and grinding of the grinding medium, the reaction activation energy is reduced, the powder activity is improved, the solid diffusion among element powder is promoted, the low-temperature chemical reaction is induced, and finally the alloy powder with uniformly distributed components and tissues is obtained, so that the problems of element volatilization and non-uniform components of the smelted powder are solved. The technology has simple equipment, simplifies the working procedures and reduces the manufacturing cost compared with the traditional method, and is suitable for industrial large-scale preparation.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, relates to nanocrystalline high-entropy alloy powder and a preparation method thereof, and particularly relates to high-entropy alloy powder prepared by mixing cobalt powder, chromium powder, iron powder, nickel powder, manganese powder, aluminum powder and titanium powder and then performing mechanical ball milling and a preparation method thereof.
Background
the traditional metal alloy generally refers to that one or two metal elements are used as a matrix, and a small amount of other metal or nonmetal elements are added to adjust the metal characteristics of the material. However, the traditional design concept also makes the metal material unable to obtain a great breakthrough. In recent years, the high-entropy alloy is proposed, the high mixed entropy concept is applied to alloy design, and the development of metal materials is brought into a new era. The high-entropy alloy is a disordered solid solution alloy discovered in the amorphous research process, has random disordered arrangement of atoms of each element, simple structure, no tendency of forming intermetallic compounds and other complex ordered phases, and has the characteristics of nano precipitates and amorphous structures. Definition of high entropy alloy: the alloy is a single-phase solid solution alloy which is generally composed of five or more main elements according to equal atomic ratio or nearly equal atomic ratio, the content of each main element is between 5 and 35 at.%, and the mixed entropy is more than 1.5R. The high-entropy alloy has high strength, high room temperature toughness, excellent wear resistance, oxidation resistance, corrosion resistance and thermal stability, and has potential application in heat-resistant and wear-resistant coatings, magnetic materials, die linings, high-temperature alloys, hard alloys and the like.
With the development of powder metallurgy forming technology, 3D printing, metal powder injection molding and other near-static forming technologies, the preparation of high-entropy alloy powder is paid more attention and researched. The conventional method for preparing powder is to obtain a block by a casting method, and then heat the metal block in an inert gas such as Ar, He or the like at a low pressure by a gas phase method such as an inert gas evaporation condensation method, so that the metal block is evaporated and then rapidly condensed to form powder. Or by atomization, blowing off with inert gas, pulverizing, and condensing to obtain powder. The method has the advantages that: controllable grain diameter, higher purity, capability of preparing nano metal powder, clean surface and less powder agglomeration. However, elements are easily segregated during the melting process, and the components are difficult to be uniformly distributed, which requires long-time homogenization treatment. Meanwhile, the vapor pressure of elements such as Al, Mg, Li, Mn and the like is high, and elements prepared by smelting are easy to volatilize, so that the components are unstable and equipment is damaged. In addition, the method has complex steps, large equipment investment and high manufacturing cost.
Disclosure of Invention
In view of the above-mentioned defects of the conventional technology, the technical problem to be solved by the present invention is to provide a novel process for preparing a nanocrystalline high-entropy alloy powder, so as to overcome the defects of the prior art, and to obtain the following effects:
The complex process for preparing the high-entropy alloy powder is simplified, and a simple and feasible alternative method is adopted; the bottleneck in industrial large-scale production and use is overcome, and the high-entropy alloy powder is produced in a large scale through simple procedures; the problems of high energy consumption and large equipment investment of the traditional production process are solved, and the high-entropy alloy powder is prepared by using simple mechanical ball milling equipment.
In order to achieve the purpose, the invention provides nanocrystalline high-entropy alloy powder and a preparation method thereof. The specific technical scheme is as follows:
The invention discloses a preparation method of nanocrystalline high-entropy alloy powder, which comprises the following steps:
placing and drying a mixture of cobalt powder, chromium powder, iron powder, nickel powder, manganese powder, aluminum powder and titanium powder in a vacuum drying oven;
Secondly, putting the dried mixture into a ball milling tank in a glove box filled with argon;
Filling inert gas into the ball milling tank, mixing powder at a low rotating speed, and then performing high-energy ball milling at a high rotating speed;
And step four, after the high-energy ball milling is finished, opening the ball milling tank in the glove box, then transferring the alloy powder to a transition bin, vacuumizing, filling air, standing for many times, repeating the steps to slowly passivate the alloy powder in the air, and taking out the prepared nanocrystalline high-entropy alloy powder after passivation.
furthermore, in the mixture, the mass ratio purity of each metal powder is more than 99.5 wt.%, the particle size of the powder is 100-300 meshes, and the atomic percentage of each element is 5-35 at.%.
further, the drying time is 1-12 hours, and the temperature of the vacuum drying oven is 30-120 ℃.
further, in the glove box, the oxygen content is less than 1000 ppm.
Further, the parameters of the high-energy ball mill are as follows: the mass ratio of the ball material is 1:1-50: 1.
further, the rotation speed of the mixed powder is 50-200rpm, and the time duration is 0.5-6 h; the rotation speed of the high-energy ball mill is 200-500rpm, and the time duration is 6-84 h.
further, the mixed powder may be selected from one of a planetary ball mill, a stirred ball mill, or a vibratory ball mill.
Furthermore, the high-energy ball mill uses a planetary ball mill, and the grinding balls are high-chromium steel balls or stainless steel balls with the diameter of 5-25 mm.
The invention also discloses nanocrystalline high-entropy alloy powder obtained according to the preparation method of the nanocrystalline high-entropy alloy powder, wherein the nanocrystalline high-entropy alloy powder is one of CoCrFeNiMn, CoCrFeNi, AlCoCrFeNi, CoCrFeNiTi, CoCrFeNiMnTi and CoCrFeNiAlTi high-entropy alloy powder.
Furthermore, the appearance of the nanocrystalline high-entropy alloy powder is irregular polygon, the particle size distribution is 10-500 mu m, and the grain size distribution is 10-200 nm.
The invention has the beneficial effects that: various metal powders are uniformly mixed in a high-energy ball milling mode, and the high-speed impact and grinding of a grinding medium reduce the reaction activation energy, improve the powder activity, promote the solid diffusion among the element powders, induce the low-temperature chemical reaction, and further refine the microstructure to the nanometer level, so that the nanocrystalline high-entropy alloy powder with higher value is obtained. Under high-speed impact, the metal powder particles repeatedly undergo high-strain and high-strain-rate plastic deformation, fracture, cold welding and other behaviors, so that the grains in the particles are effectively refined. By using such powder as a raw material, it is possible to obtain an ultrafine structural material profile and parts having excellent properties such as high strength, good toughness and plasticity and having high value by thermo-mechanical consolidation such as hot forging and hot extrusion of a pre-sintered powder compact. In addition, the technical equipment is simple, compared with the traditional method, the working procedure is simplified, the manufacturing cost is reduced, and the method is suitable for industrial large-scale preparation.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a flow chart of a method for preparing nanocrystalline high-entropy alloy powder according to the present invention;
FIG. 2 is a scanning electron micrograph of the nanocrystalline CoCrFeNi high-entropy alloy powder obtained in example 1;
FIG. 3 is an XRD pattern of the nanocrystalline CoCrFeNi high-entropy alloy powder obtained in example 1;
FIG. 4 shows nanocrystalline Al obtained in example 20.3Scanning electron microscope photos of the CoCrFeNi high-entropy alloy powder;
FIG. 5 shows nanocrystalline Al obtained in example 20.3XRD pattern of CoCrFeNi high entropy alloy powder.
Detailed Description
the invention is described in further detail below with reference to the figures and specific embodiments. It should be understood that the embodiments are illustrative of the invention and are not to be construed as limiting the scope of the invention in any way. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
The invention discloses a preparation method of nanocrystalline high-entropy alloy powder, which comprises the following steps of:
100. Placing and drying a mixture of cobalt powder, chromium powder, iron powder, nickel powder, manganese powder, aluminum powder and titanium powder in a vacuum drying oven;
200. putting the dried mixture into a ball milling tank in a glove box filled with argon;
300. Filling inert gas into the ball milling tank, mixing powder at a low rotating speed, and then performing high-energy ball milling at a high rotating speed;
400. And after the high-energy ball milling is finished, opening a ball milling tank in a glove box, transferring the alloy powder to a transition bin, vacuumizing, filling air, standing, repeating for many times to slowly passivate the alloy powder in the air, and taking out the prepared nanocrystalline high-entropy alloy powder after passivation.
Wherein the mass ratio purity of each metal powder in the mixture is more than 99.5 wt.%, the particle size of the powder is 100-300 meshes, the atom percentage ratio of each element is 5-35 at.%, the drying time is 1-12 hours, the temperature of a vacuum drying oven is 30-120 ℃, and the oxygen content in a glove box is less than 1000 ppm.
Example 1: preparing CoCrFeNi high-entropy alloy powder:
According to the implementation steps, cobalt powder, chromium powder, iron powder and nickel powder with equal atomic ratio are filled into a ball milling tank in a glove box filled with argon, argon is filled into the ball milling tank, and high-energy ball milling is carried out on a planetary ball mill according to the following ball milling parameters: stainless steel is selected for ball milling, the diameter of a grinding ball is 16mm, and the mass ratio of ball materials is 5: 1, mixing the metal powder for 6h at a low rotating speed of 200rpm to uniformly mix the metal powder, and then carrying out high-energy ball milling for 84h at a high speed of 300 rpm. And after the high-energy ball milling is finished, opening a ball milling tank in a glove box filled with argon, and taking out the prepared nanocrystalline CoCrFeNi high-entropy alloy powder after the transition bin is passivated.
SEM observation of CoCrFeNi powder revealed a large number of irregular polygonal particles (see FIG. 2) with particle sizes between 10 and 500 μm, and XRD revealed that the powder had a BCC + FCC crystal structure (see FIG. 3), and the grain size was calculated to be 74nm by analysis.
Example 2: al (Al)0.3CoCrFeNi high-entropy alloy
According to the implementation steps, in a glove box filled with argon, aluminum powder, cobalt powder, chromium powder, iron powder and nickel powder are filled into a ball milling tank together, wherein the aluminum powder accounts for 7 at%, and other metals account for 23.25 at%. Argon is filled into the ball milling tank, and high-energy ball milling is carried out on a planetary ball mill according to the following ball milling parameters: stainless steel is selected for ball milling, the diameter of a grinding ball is 16mm, and the mass ratio of ball materials is 5: 1, mixing the metal powder for 6 hours at a low rotating speed of 200rpmThe powder is mixed evenly and then high-energy ball milling is carried out for 60 hours at a high speed of 300 rpm. After the high-energy ball milling is finished, opening a ball milling tank in a glove box filled with argon, passivating a transition bin, and taking out the prepared nanocrystalline Al0.3CoCrFeNi high-entropy alloy powder.
SEM Observation of Al0.3The CoCrFeNi powder found a large number of irregular polygonal particles (see FIG. 4) with particle sizes between 10 and 500 μm, and the XRD results found the powder to have a BCC + FCC crystal structure (see FIG. 5), with a grain size of 72nm as calculated by analysis.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. A preparation method of nanocrystalline high-entropy alloy powder is characterized by comprising the following preparation steps:
placing and drying a mixture of cobalt powder, chromium powder, iron powder, nickel powder, manganese powder, aluminum powder and titanium powder in a vacuum drying oven;
Secondly, putting the dried mixture into a ball milling tank in a glove box filled with argon;
filling inert gas into the ball milling tank, mixing powder at a low rotating speed, and then performing high-energy ball milling at a high rotating speed;
And step four, after the high-energy ball milling is finished, opening the ball milling tank in the glove box, then transferring the alloy powder to a transition bin, vacuumizing, filling air, standing for many times, repeating the steps to slowly passivate the alloy powder in the air, and taking out the prepared nanocrystalline high-entropy alloy powder after passivation.
2. the method for preparing nanocrystalline high-entropy alloy powder as claimed in claim 1, wherein in the mixture, the mass ratio purity of each metal powder is more than 99.5 wt.%, the particle size of the powder is 100-300 meshes, and the atomic percentage of each element is 5-35 at.%.
3. The method for producing a nanocrystalline high-entropy alloy powder according to claim 1, wherein the drying time is 1 to 12 hours, and the temperature of the vacuum drying oven is 30 to 120 ℃.
4. The method for producing a nanocrystalline high-entropy alloy powder according to claim 1, wherein the oxygen content in the glove box is less than 1000 ppm.
5. the method for preparing nanocrystalline high-entropy alloy powder according to claim 1, wherein the parameters of the high-energy ball milling are as follows: the mass ratio of the ball material is 1:1-50: 1.
6. The method for preparing nanocrystalline high-entropy alloy powder according to claim 1, wherein the rotation speed of the mixed powder is 50-200rpm, and the duration is 0.5-6 h; the rotation speed of the high-energy ball mill is 200-500rpm, and the time duration is 6-84 h.
7. the method for preparing a nanocrystalline high-entropy alloy powder according to claim 1, wherein the mixed powder is one of a planetary ball mill, a stirred ball mill, and a vibratory ball mill.
8. The method for preparing nanocrystalline high-entropy alloy powder according to claim 1, wherein a planetary ball mill is used for the high-energy ball milling, and the milling balls are high-chromium steel balls or stainless steel balls with the diameter of 5-25 mm.
9. A nanocrystalline high-entropy alloy powder obtained according to the preparation method of the nanocrystalline high-entropy alloy powder according to any one of claims 1 to 8, wherein the nanocrystalline high-entropy alloy powder is one of CoCrFeNiMn, CoCrFeNi, AlCoCrFeNi, CoCrFeNiTi, CoCrFeNiMnTi and CoCrFeNiAlTi high-entropy alloy powder.
10. The nanocrystalline high-entropy alloy powder of claim 9, wherein the nanocrystalline high-entropy alloy powder has an irregular polygonal shape, a particle size distribution of 10-500 μm, and a grain size distribution of 10-200 nm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111533191A (en) * | 2020-05-12 | 2020-08-14 | 辽宁大学 | Method for degrading dye wastewater by using high-entropy alloy |
| CN113399670A (en) * | 2021-05-19 | 2021-09-17 | 西安理工大学 | Double-element equivalent transformation high-entropy alloy powder and preparation method thereof |
| CN113996966A (en) * | 2021-11-02 | 2022-02-01 | 上海龙烁焊材有限公司 | Preparation method and application of aluminum-based light high-entropy alloy metal powder-cored welding wire |
| CN114309627A (en) * | 2022-03-15 | 2022-04-12 | 中南大学 | Preparation method of low-oxygen-content refractory high-entropy alloy powder |
| CN114892058A (en) * | 2022-04-13 | 2022-08-12 | 哈尔滨工业大学 | Quaternary high-entropy alloy powder with body-centered cubic structure and preparation method thereof |
| CN115401195A (en) * | 2022-09-13 | 2022-11-29 | 中国化学工程第十一建设有限公司 | Particle-reinforced high-entropy alloy powder and preparation method and application thereof |
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| CN113399670A (en) * | 2021-05-19 | 2021-09-17 | 西安理工大学 | Double-element equivalent transformation high-entropy alloy powder and preparation method thereof |
| CN113996966A (en) * | 2021-11-02 | 2022-02-01 | 上海龙烁焊材有限公司 | Preparation method and application of aluminum-based light high-entropy alloy metal powder-cored welding wire |
| CN114309627A (en) * | 2022-03-15 | 2022-04-12 | 中南大学 | Preparation method of low-oxygen-content refractory high-entropy alloy powder |
| CN114309627B (en) * | 2022-03-15 | 2022-05-17 | 中南大学 | Preparation method of low-oxygen-content refractory high-entropy alloy powder |
| CN114892058A (en) * | 2022-04-13 | 2022-08-12 | 哈尔滨工业大学 | Quaternary high-entropy alloy powder with body-centered cubic structure and preparation method thereof |
| CN115401195A (en) * | 2022-09-13 | 2022-11-29 | 中国化学工程第十一建设有限公司 | Particle-reinforced high-entropy alloy powder and preparation method and application thereof |
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Application publication date: 20191217 |
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| RJ01 | Rejection of invention patent application after publication |