CN109355546B - Multi-principal-element alloy for manufacturing target and preparation method thereof - Google Patents
Multi-principal-element alloy for manufacturing target and preparation method thereof Download PDFInfo
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- CN109355546B CN109355546B CN201811372673.4A CN201811372673A CN109355546B CN 109355546 B CN109355546 B CN 109355546B CN 201811372673 A CN201811372673 A CN 201811372673A CN 109355546 B CN109355546 B CN 109355546B
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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
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
The invention provides a multi-principal-element alloy for manufacturing a target material and a preparation method thereof, belonging to the field of metal materials and preparation thereof. The chemical formula of the multi-principal element alloy is AlxCoCuMnyNiTizWherein x is more than or equal to 0.1 and less than or equal to 1.2; y is more than or equal to 0.1 and less than or equal to 1.2; z is more than or equal to 0.1 and less than or equal to 1.2; 0.01<x/(x+y+z+3)<0.30；0.01<y/(x+y+z+3)<0.30；0.01<z/(x+y+z+3)<0.30. The components of the multi-principal-element alloy material prepared by the method are consistent with the proportioning components of the raw materials; certain pressure is kept in the sintering process, so that the expansion behavior in the sintering process is weakened to a great extent, the density of the alloy is improved to the maximum extent, and the gaps of the material are reduced; the method has the advantages of simple process, low equipment cost and controllable operation, and is suitable for industrial large-scale production.
Description
Technical Field
The invention relates to the field of metal materials and preparation thereof, in particular to a multi-principal-element alloy for preparing a target material and a preparation method thereof.
Background
The target material is used as a material source of the coating technology, and directly influences the type and performance of the coating. Combining target components with coating properties, it is of great importance to provide target component designs for coatings of specific applications. Common preparation methods of the target material mainly comprise a melting casting method and a powder metallurgy method. However, for targets composed of a plurality of metal elements having large differences in melting points or densities, it is difficult to obtain alloy targets having uniform components by the fusion casting method.
The method for preparing the target material by powder metallurgy mainly comprises a hot isostatic pressing method, a hot pressing method, a cold isostatic pressing-sintering method, a discharge plasma sintering method and the like. Different methods are different according to the component granularity and the heating mode of the raw material powder, and the tissue structures of the prepared target materials are different. In the preparation process of the target material, besides strict requirements on the purity, density, grain size and orientation of the material, certain requirements are also provided for alloy components, heat treatment process, forming processing and the like of the target material, so that the quality of the target material and a corresponding coating is ensured. In 2004, the multi-principal-element high-entropy alloy is reported for the first time, and has attracted extensive attention due to the design concept and the performances of high hardness, temper softening resistance, high temperature resistance, corrosion resistance, wear resistance and the like which are different from the traditional alloy, and the excellent performances determine that the multi-principal-element high-entropy alloy has huge application potential in the fields of coating materials and target materials. Therefore, the design of a novel multi-principal-element alloy material for manufacturing the target material has huge market demand and wide application prospect.
Disclosure of Invention
The invention provides a multi-principal-element alloy for preparing a target material and a preparation method thereof, and Al is prepared by adopting a vacuum hot-pressing sintering processxCoCuMnyNiTizThe multi-principal-element alloy keeps a certain pressure in the sintering process, so that the expansion behavior in the sintering process is weakened to a great extent, the density of the alloy is improved to the maximum extent, and the gaps of the material are reduced.
The technical scheme for realizing the invention is as follows: a multi-principal-element alloy for preparing target material, whose chemical formula is AlxCoCuMnyNiTizWherein x is more than or equal to 0.1 and less than or equal to 1.2; y is more than or equal to 0.1 and less than or equal to 1.2; z is more than or equal to 0.1 and less than or equal to 1.2; 0.01<x/(x+y+z+3)<0.30；0.01<y/(x+y+z+3)<0.30；0.01<z/(x+y+z+3)<0.30。
The preparation method of the multi-principal-element alloy for manufacturing the target comprises the following steps:
(1) according to AlxCoCuMnyNiTizWeighing various pure metal powders according to a stoichiometric ratio, placing the pure metal powders in a ball milling tank, adding stainless steel balls, and then sealing the ball milling tank containing the pure metal powders under a protective atmosphere environment;
(2) placing the sealed ball milling tank on a planetary ball mill for mixing;
(3) and (3) putting the uniformly mixed powder into a graphite die in a protective atmosphere environment, and then carrying out vacuum hot-pressing sintering to obtain the multi-principal-element alloy.
The protective atmosphere is argon or nitrogen.
The adding amount of the stainless steel balls in the step (1) is that the ball-material mass ratio (5-10) is 1.
And (3) in the step (2), the mixing speed is 50-250rpm, and the time is 0.5-6 h.
In the step (3), the vacuum hot-pressing sintering temperature is 1000-.
The invention has the beneficial effects that: the components of the multi-principal-element alloy material prepared by the method are consistent with the proportioning components of the raw materials; certain pressure is kept in the sintering process, so that the expansion behavior in the sintering process is weakened to a great extent, the density of the alloy is improved to the maximum extent, and the gaps of the material are reduced; the method has the advantages of simple process, low equipment cost and controllable operation, and is suitable for industrial large-scale production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an X-ray diffraction pattern of a multi-principal element alloy prepared in example 1 of the present invention;
FIG. 2 is a process flow diagram of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A preparation method of a multi-principal-element alloy for manufacturing a target material comprises the following steps:
according to the chemical formula AlCoCuMnNiTi0.1Respectively weighing 0.40mol of aluminum powder, cobalt powder, copper powder, manganese powder and nickel powder and 0.04mol of titanium powder, wherein the purity of each pure metal powder is higher than 99.5%; placing the weighed pure metal powder into a ball milling tank, adding stainless steel balls according to the ball-to-material ratio of 8:1, and then sealing the ball milling tank containing the pure metal powder in a nitrogen environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the mixing rotating speed is 150rpm, and the mixing time is 2 hours; and (3) loading the uniformly mixed powder into a graphite die in a nitrogen environment, and then carrying out vacuum hot-pressing sintering at the sintering temperature of 1200 ℃, the sintering time of 1.5h and the sintering pressure of 30MPa to obtain the required multi-principal-element alloy.
Example 2
A preparation method of a multi-principal-element alloy for manufacturing a target material comprises the following steps:
according to the chemical formula AlCoCuMn0.5Respectively weighing 0.40mol of aluminum powder, cobalt powder, copper powder, nickel powder and titanium powder and 0.20mol of manganese powder by using NiTi, wherein the purity of each pure metal powder is higher than 99.5%; placing the weighed pure metal powder into a ball milling tank, adding stainless steel balls according to the ball-to-material ratio of 5:1, and then sealing the ball milling tank containing the pure metal powder in a nitrogen environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the mixing rotation speed is 250rpm, and the mixing time is 0.5 h; and (3) loading the uniformly mixed powder into a graphite die in a nitrogen environment, and then carrying out vacuum hot-pressing sintering at the sintering temperature of 1400 ℃, the sintering time of 0.5h and the sintering pressure of 20MPa to obtain the required multi-principal-element alloy.
Example 3
A preparation method of a multi-principal-element alloy for manufacturing a target material comprises the following steps:
according to the chemical formula Al0.5Respectively weighing 0.20mol of aluminum powder and 0.40mol of cobalt powder, copper powder, manganese powder, nickel powder and titanium powder by using CoCuMnNiTi, wherein the purity of each pure metal powder is higher than 99.5%; placing the weighed pure metal powder into a ball milling tank, and adding stainless steel ballsThe ball-material ratio is 10:1, and then the ball-milling tank containing pure metal powder is sealed under the nitrogen environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the mixing rotating speed is 50rpm, and the mixing time is 6 hours; and (3) loading the uniformly mixed powder into a graphite die in a nitrogen environment, and then carrying out vacuum hot-pressing sintering at the sintering temperature of 1000 ℃, the sintering time of 3h and the sintering pressure of 35MPa to obtain the required multi-principal-element alloy.
Example 4
A preparation method of a multi-principal-element alloy for manufacturing a target material comprises the following steps:
according to the chemical formula Al1.2CoCuMn0.1NiTi0.5Respectively weighing 0.48mol of aluminum powder, 0.40mol of cobalt powder, copper powder and nickel powder, 0.04mol of manganese powder and 0.20mol of titanium powder, wherein the purity of each pure metal powder is higher than 99.5%; placing the weighed pure metal powder into a ball milling tank, adding stainless steel balls at a ball-to-material ratio of 10:1, and sealing the ball milling tank containing the pure metal powder in an argon environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the mixing rotating speed is 50rpm, and the mixing time is 6 hours; and (3) loading the uniformly mixed powder into a graphite die in an argon environment, and then carrying out vacuum hot-pressing sintering at the sintering temperature of 1000 ℃, the sintering time of 3h and the sintering pressure of 35MPa to obtain the required multi-principal-element alloy.
Example 5
A preparation method of a multi-principal-element alloy for manufacturing a target material comprises the following steps:
according to the chemical formula Al0.1CoCuMn1.2NiTi0.5Respectively weighing 0.04mol of aluminum powder, 0.40mol of cobalt powder, copper powder and nickel powder, 0.48mol of manganese powder and 0.20mol of titanium powder, wherein the purity of each pure metal powder is higher than 99.5%; placing the weighed pure metal powder into a ball milling tank, adding stainless steel balls according to the ball-to-material ratio of 5:1, and then sealing the ball milling tank containing the pure metal powder in an argon environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the mixing rotation speed is 250rpm, and the mixing time is 0.5 h; loading the uniformly mixed powder into a graphite die in an argon environment, and then sintering by vacuum hot pressingThe sintering temperature is 1400 ℃, the time is 0.5h, and the pressure is 20MPa, so that the required multi-principal-element alloy is obtained.
Example 6
A preparation method of a multi-principal-element alloy for manufacturing a target material comprises the following steps:
according to the chemical formula Al0.1CoCuMn0.1NiTi1.2Respectively weighing 0.04mol of aluminum powder and manganese powder, 0.40mol of cobalt powder, copper powder and nickel powder and 0.48mol of titanium powder, wherein the purity of each pure metal powder is higher than 99.5%; placing the weighed pure metal powder into a ball milling tank, adding stainless steel balls according to the ball-to-material ratio of 8:1, and then sealing the ball milling tank containing the pure metal powder in a nitrogen environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the mixing rotating speed is 150rpm, and the mixing time is 2 hours; and (3) loading the uniformly mixed powder into a graphite die in a nitrogen environment, and then carrying out vacuum hot-pressing sintering at the sintering temperature of 1200 ℃, the sintering time of 1.5h and the sintering pressure of 30MPa to obtain the required multi-principal-element alloy.
Example 7
A preparation method of a multi-principal-element alloy for manufacturing a target material comprises the following steps:
respectively weighing 0.40mol of aluminum powder, cobalt powder, copper powder, manganese powder, nickel powder and titanium powder according to a chemical formula of AlCoCuMnNiTi, wherein the purity of each pure metal powder is higher than 99.5%; placing the weighed pure metal powder into a ball milling tank, adding stainless steel balls according to the ball-to-material ratio of 8:1, and then sealing the ball milling tank containing the pure metal powder in a nitrogen environment; placing the sealed ball milling tank on a planetary ball mill for mixing materials, wherein the mixing rotating speed is 150rpm, and the mixing time is 2 hours; and (3) loading the uniformly mixed powder into a graphite die in a nitrogen environment, and then carrying out vacuum hot-pressing sintering at the sintering temperature of 1200 ℃, the sintering time of 1.5h and the sintering pressure of 30MPa to obtain the required multi-principal-element alloy.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A multi-principal-element alloy for manufacturing a target material is characterized in that: the chemical formula of the multi-principal element alloy is AlxCoCuMnyNiTizWherein x is more than or equal to 0.1 and less than or equal to 1.2; y is more than or equal to 0.1 and less than or equal to 1.2; z is more than or equal to 0.1 and less than or equal to 1.2; 0.01<x/(x+y+z+3)<0.30；0.01<y/(x+y+z+3)<0.30；0.01<z/(x+y+z+3)<0.30；
The preparation method of the multi-principal-element alloy for manufacturing the target comprises the following steps:
(1) according to AlxCoCuMnyNiTizWeighing various pure metal powders according to a stoichiometric ratio, placing the pure metal powders in a ball milling tank, adding stainless steel balls, and then sealing the ball milling tank containing the pure metal powders under a protective atmosphere environment;
(2) placing the sealed ball milling tank on a planetary ball mill for mixing;
(3) and (3) putting the uniformly mixed powder into a graphite die in a protective atmosphere environment, and then carrying out vacuum hot-pressing sintering to obtain the multi-principal-element alloy.
2. The multi-element alloy for manufacturing a target according to claim 1, wherein: the purities of the pure metal powders are all higher than 99.5%.
3. The multi-element alloy for manufacturing a target according to claim 1, wherein: the protective atmosphere is argon or nitrogen.
4. The multi-element alloy for manufacturing a target according to claim 1, wherein: the adding amount of the stainless steel balls in the step (1) is that the ball-material mass ratio (5-10) is 1.
5. The multi-element alloy for manufacturing a target according to claim 1, wherein: and (3) in the step (2), the mixing speed is 50-250rpm, and the time is 0.5-6 h.
6. The multi-element alloy for manufacturing a target according to claim 1, wherein: in the step (3), the vacuum hot-pressing sintering temperature is 1000-.
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| JPH05186841A (en) * | 1991-11-15 | 1993-07-27 | Furukawa Electric Co Ltd:The | Electromagnetic wave shielding material |
| US20170314097A1 (en) * | 2016-05-02 | 2017-11-02 | Korea Advanced Institute Of Science And Technology | High-strength and ultra heat-resistant high entropy alloy (hea) matrix composites and method of preparing the same |
| TWI595098B (en) * | 2016-06-22 | 2017-08-11 | 國立清華大學 | High-entropy superalloy |
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| CN106041031A (en) * | 2016-07-29 | 2016-10-26 | 河海大学常州校区 | Preparation method of high-entropy alloy coating layer on surface of casting |
| CN106868381A (en) * | 2017-03-02 | 2017-06-20 | 中原工学院 | A kind of coating multi-principal elements alloy powder and preparation method thereof |
| CN106893923A (en) * | 2017-03-02 | 2017-06-27 | 中原工学院 | A kind of cutter multi-principal elements alloy and preparation method thereof |
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