CN111020579A - Preparation of TiB on titanium alloy2Method for particle reinforced high-entropy alloy coating - Google Patents
Preparation of TiB on titanium alloy2Method for particle reinforced high-entropy alloy coating Download PDFInfo
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- CN111020579A CN111020579A CN201911320284.1A CN201911320284A CN111020579A CN 111020579 A CN111020579 A CN 111020579A CN 201911320284 A CN201911320284 A CN 201911320284A CN 111020579 A CN111020579 A CN 111020579A
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
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- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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Abstract
The invention discloses a method for preparing TiB on titanium alloy2The method for preparing particle reinforced high-entropy alloy coating is characterized by that on the surface of titanium alloy base body a Co film, a Ni film and a Cr film are prefabricated in turn, then the Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB are mixed2The mixed powder is cladded on a titanium alloy matrix containing a prefabricated film to obtain TiB2The particle reinforced CoCrCuFeNiMoMn high-entropy alloy coating. The coating prepared by the method has the advantages of wear resistance and oxidation resistanceGood chemical ability.
Description
Technical Field
The invention relates to a preparation method of a high-entropy alloy coating, in particular to a method for preparing TiB on a titanium alloy2A method for particle reinforced high-entropy alloy coating.
Background
The high-entropy alloy is a novel alloy system, changes the design concept that the traditional alloy material is mainly made of a certain alloy element in the aspect of alloy design, adopts four or more elements to be configured according to equal atoms, and finally forms a multi-principal-element alloy system. The multi-principal element alloy is characterized by high mixed entropy and shape entropy, and a full solid solution microstructure is formed under the drive of the high entropy, so the multi-principal element alloy is called as a high entropy alloy. The research on the high-entropy alloy initially started around 1995 and in 2004, and taiwan scholars named the high-entropy alloy for the first time. Because of the full solid solution structure of the high-entropy alloy, the formation of brittle metal piece compounds is inhibited, and the structure is mainly face-centered cubic or body-centered cubic or the mixture of the face-centered cubic and the body-centered cubic. Due to the special metallographic structure, the alloy has very considerable mechanical properties, such as over-strength and high plasticity of some series of high-entropy alloys, and simultaneously has higher hardness, wear resistance, corrosion resistance, thermal resistance, electric resistance, magnetic properties and the like. Such excellent properties have attracted a great deal of attention from materials researchers, and the number of research reports on high-entropy alloys has been exponentially increased.
Although much research work has been carried out on the development of a new system for high-entropy alloys, there are still few research works on the connection of high-entropy alloys and the compounding of high-entropy alloys with existing metal materials, so that certain technologies and methods are still in the blank state. As is well known, titanium alloy is an alloy with excellent high-temperature performance and chemical corrosion resistance, and is often used in aerospace and military industries, but has the disadvantages of poor oxidation resistance and poor wear resistance, so that much research work is carried out on the surface modification and surface coating preparation technology of titanium alloy. The high-entropy alloy with high wear resistance and good mechanical property is compounded with the titanium alloy, a high-entropy alloy coating with excellent performance is formed on the surface of the titanium alloy, the defects of the titanium alloy can be effectively improved, the use range of the material is enlarged, the service life of the material is prolonged, and related researches are few at present.
Disclosure of Invention
The invention aims to provide a method for preparing TiB on titanium alloy2A method for particle reinforced high-entropy alloy coating. The coating prepared by the method has the advantages of wear resistance and oxidation resistanceGood force.
The technical scheme of the invention is as follows: preparation of TiB on titanium alloy2The method for preparing particle reinforced high-entropy alloy coating is characterized by that on the surface of titanium alloy base body a Co film, a Ni film and a Cr film are prefabricated in turn, then the Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB are mixed2The mixed powder is cladded on a titanium alloy matrix containing a prefabricated film to obtain TiB2The particle reinforced CoCrCuFeNiMoMn high-entropy alloy coating.
Preparation of TiB on titanium alloy as described above2The method for particle-reinforced high-entropy alloy coating is characterized in that the titanium alloy matrix is industrial pure titanium or Ti-6Al-4V alloy.
Preparation of TiB on titanium alloy as described above2The method for particle reinforced high-entropy alloy coating is characterized in that a titanium alloy substrate is polished and cleaned before Co, Ni and Cr films are prefabricated.
Preparation of TiB on titanium alloy as described above2The method for the particle-reinforced high-entropy alloy coating comprises the steps of polishing by using 2000-3000-mesh sand paper, ultrasonically cleaning for 20-40min after polishing, and drying at 30-50 ℃.
Preparation of TiB on titanium alloy as described above2The method for preparing the particle-reinforced high-entropy alloy coating comprises the step of preparing the Co film, the Ni film and the Cr film by magnetron sputtering equipment.
Preparation of TiB on titanium alloy as described above2The thickness of the Co film, the thickness of the Ni film and the thickness of the Cr film are respectively 10-100 nm.
Preparation of TiB on titanium alloy as described above2Method for particle-reinforced high-entropy alloy coatings of said Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB2Mixed powder of Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB2In a molar ratio of 1:1:1:1:1:1:1: 0.3.
preparation of TiB on titanium alloy as described above2Method for particle-reinforced high-entropy alloy coatings of said Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB2The particle size of the mixed powder is 10-30 μm.
Preparation of TiB on titanium alloy as described above2Method for particle-reinforced high-entropy alloy coating, and mixed powder claddingPlasma cladding is adopted.
The invention has the advantages of
Preparing TiB on the surface of the titanium alloy by the method of the invention2The enhanced CoCrCuFeNiMoMn high-entropy alloy coating can effectively improve the wear resistance and oxidation resistance of the surface of the titanium alloy.
The method comprises the following specific steps:
1. the alloy coating belongs to a novel high-entropy alloy system, although the high-entropy alloy forms a full solid solution structure after a plurality of alloy elements are matched in an equal proportion, the atomic radii are matched with each other, the high-entropy alloy can be formed without random mixing, accurate calculation and experimental verification are needed, and only dozens of high-entropy alloy systems are found at present. On the basis of the existing CoCrCuFeNi high-entropy alloy system, on the premise that alloy elements except Al and Ti are added into the alloy system to be difficult to form a high-entropy alloy, the solid solution of the elements can be promoted under the synergistic action of Mn and Mo obtained through further theoretical calculation and experimental verification, so that a brand-new CoCrCuFeNiMoMn high-entropy alloy system is obtained, the coating forming capacity is achieved, and the hardness and the oxidation resistance are improved.
2. The invention solves the problem of TiB by adding the reinforcing phase2The problem of the interface compatibility of the particles in the high-entropy alloy is solved, and TiB with good interface compatibility is successfully obtained2The high-entropy alloy coating of the particle CoCrCuFeNiMoMn alloy further improves the wear resistance.
3. The invention uses Co film, Ni film and Cr film to plate the pre-made film in a specific order to make TiB2The granular CoCrCuFeNiMoMn high-entropy alloy coating can be perfectly combined with pure titanium or Ti-6Al-4V alloy. Without this pre-filming process, there is no way to achieve the preparation of cocrccufenimomn high entropy alloy coatings on these two titanium alloys. The principle is that the Co film has good compatibility with titanium, and Ni and Cr can not achieve the effect. So firstly plating Co film, secondly plating Ni film, because of Co film as substrate and base body, Ni can easily form good combination, Cr film can only be plated finally, because these three metals, Cr has highest melting point, after high-temp. Cr plating, Co, Ni and Cr are no longer three kindsThe independent film forms a CoNiCr whole body, and the whole body does not form a full solid solution structure with high entropy completely, but also exists in the form of a semi-solid solution structure. When TiB2After the + CoCrCuFeNiMoMn is sprayed to the CoNiCr semi-solid solution structure, the whole solid solution TiB is formed2The high-entropy alloy structure of the + CoCrCuFeNiMoMn alloy enables the coating to be perfectly transited to the titanium alloy without an intermediate band of metal compounds, so that the structure that the coating and the matrix alloy are integrated is obtained.
The applicant made comparative tests in which the coated alloys prepared in examples 1 and 2 and the Ti-6Al-4V alloy without coating were subjected to a pin disc wear test and an oxidation resistance test, respectively, 10 times for each group, and the results were averaged, and are shown in Table 1.
Table 1 results of performance testing
As can be seen from the table, the high-entropy alloy coatings prepared according to the examples 1 and 2 have the advantages that the abrasion weight loss is reduced by more than 50% compared with the Ti-6Al-4V alloy without the coating, the abrasion resistance is improved by 2 times, the oxidation weight gain is only about 1/8 without the coating, and the oxidation resistance is improved by at least 8 times. Therefore, the coating prepared by the invention improves the service performance of the titanium alloy.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Examples of the invention
Example 1
TiB of Ti-6Al-4V alloy with dimensions of 150X 100X 10 mm2Particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating
Polishing the surface of the base material with 2500-mesh sand paper, ultrasonically cleaning for 30 min, drying at 40 ℃ in a resistance furnace, plating a Co film with the thickness of 30nm on Ti-6Al-4V alloy by using a magnetron sputtering device, then plating a Co film on the basis of the Co film by using Ni as a target materialPlating a Ni film with the thickness of 35nm, and finally plating a Cr film with the thickness of 45nm on the basis of the Co film and the Ni film by taking Cr as a target material. Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB with the granularity of 25 microns2Uniformly mixing the powder by a ball mill, wherein the molar ratio of Co: cr: cu: fe: ni: mo: mn: TiB21:1:1:1:1:1: 0.3. Adding the mixed powder into a feeding system of plasma cladding equipment, introducing 99.9% argon, spraying the mixed powder onto the surface of Ti-6Al-4V alloy under the pressure of the argon, and forming TiB on the surface of the alloy by taking plasma as a heat source2Carrying out primary cladding on the particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating to obtain a coating with the thickness of 1.2 mm.
Example 2
TiB of an industrially pure titanium (purity 99.7%) alloy having dimensions of 180X 100X 15 mm2Particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating
The surface of the parent metal is polished by 3000-mesh sand paper, cleaned by ultrasonic for 30 minutes and dried in a resistance furnace at 30 ℃. By utilizing magnetron sputtering equipment, Co is firstly used as a target material, a Co film is plated on the alloy, the thickness is 70nm, then Ni is used as the target material, a Ni film is plated on the basis of the Co film, the thickness is 70nm, finally Cr is used as the target material, and a Cr film is plated on the basis of the Co film and the Ni film, and the thickness is 70 nm. Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB with the granularity of 10 microns2Uniformly mixing the powder by a ball mill, wherein the molar ratio of Co: cr: cu: fe: ni: mo: mn: TiB21:1:1:1:1:1: 0.3. Adding the mixed powder into a feeding system of plasma cladding equipment, introducing 99.9% argon, spraying the mixed powder onto the surface of the alloy under the pressure of the argon, and forming TiB on the surface of the alloy by taking plasma as a heat source2And carrying out cladding twice on the particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating to obtain a coating with the thickness of 3.1 mm.
Example 3
TiB of an industrially pure titanium (purity 99.9%) alloy having dimensions of 180X 100X 25 mm2Particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating
Polishing the surface of the parent metal with 2000-mesh abrasive paper, ultrasonically cleaning for 20 min, and placing in a vacuum resistance furnaceDrying at 50 ℃. By utilizing magnetron sputtering equipment, Co is firstly used as a target material, a Co film is plated on the alloy, the thickness is 10nm, then Ni is used as the target material, a Ni film is plated on the basis of the Co film, the thickness is 10nm, finally Cr is used as the target material, and a Cr film is plated on the basis of the Co film and the Ni film, and the thickness is 10 nm. Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB with the granularity of 30 microns2Uniformly mixing the powder by a ball mill, wherein the molar ratio of Co: cr: cu: fe: ni: mo: mn: TiB21:1:1:1:1:1: 0.3. Adding the mixed powder into a feeding system of plasma cladding equipment, introducing 99.9% argon, spraying the mixed powder onto the surface of the alloy under the pressure of the argon, and forming TiB on the surface of the alloy by taking plasma as a heat source2And carrying out three times of cladding on the particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating to obtain a coating with the thickness of 5.1 mm.
Example 4
TiB of Ti-6Al-4V alloy with dimensions of 180X 100X 35 mm2Particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating
The surface of the parent metal is polished by 2500-mesh abrasive paper, cleaned by ultrasonic for 40 minutes and dried in a vacuum resistance furnace at 45 ℃. By utilizing magnetron sputtering equipment, Co is firstly used as a target material, a Co film is plated on the alloy, the thickness is 100nm, then Ni is used as the target material, a Ni film is plated on the basis of the Co film, the thickness is 100nm, finally Cr is used as the target material, and a Cr film is plated on the basis of the Co film and the Ni film, and the thickness is 100 nm. Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB with the granularity of 20 microns2Uniformly mixing the powder by a ball mill, wherein the molar ratio of Co: cr: cu: fe: ni: mo: mn: TiB21:1:1:1:1:1: 0.3. Adding the mixed powder into a feeding system of plasma cladding equipment, introducing 99.9% argon, spraying the mixed powder onto the surface of Ti-6Al-4V alloy under the pressure of the argon, and forming TiB on the surface of the alloy by taking plasma as a heat source2And carrying out cladding twice on the particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating to obtain a coating with the thickness of 2.9 mm.
Example 5
TiB of Ti-6Al-4V alloy with dimensions of 180X 100X 35 mm2Particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating
The surface of the parent material is polished by 2000-mesh sand paper, cleaned by ultrasonic for 20 minutes and dried in a vacuum resistance furnace at 30 ℃. By utilizing magnetron sputtering equipment, Co is firstly used as a target material, a Co film is plated on the alloy, the thickness is 10nm, then Ni is used as the target material, a Ni film is plated on the basis of the Co film, the thickness is 10nm, finally Cr is used as the target material, and a Cr film is plated on the basis of the Co film and the Ni film, and the thickness is 10 nm. Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB with the granularity of 10 microns2Uniformly mixing the powder by a ball mill, wherein the molar ratio of Co: cr: cu: fe: ni: mo: mn: TiB21:1:1:1:1:1: 0.3. Adding the mixed powder into a feeding system of plasma cladding equipment, introducing 99.9% argon, spraying the mixed powder onto the surface of Ti-6Al-4V alloy under the pressure of the argon, and forming TiB on the surface of the alloy by taking plasma as a heat source2And carrying out cladding twice on the particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating to obtain a coating with the thickness of 2.9 mm.
Example 6
TiB of Ti-6Al-4V alloy with dimensions of 180X 100X 35 mm2Particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating
The surface of the parent material is polished by 3000-mesh abrasive paper, cleaned by ultrasonic for 40 minutes and dried in a vacuum resistance furnace at 50 ℃. By utilizing magnetron sputtering equipment, Co is firstly used as a target material, a Co film is plated on the alloy, the thickness is 100nm, then Ni is used as the target material, a Ni film is plated on the basis of the Co film, the thickness is 100nm, finally Cr is used as the target material, and a Cr film is plated on the basis of the Co film and the Ni film, and the thickness is 100 nm. Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB with the granularity of 30 microns2Uniformly mixing the powder by a ball mill, wherein the molar ratio of Co: cr: cu: fe: ni: mo: mn: TiB21:1:1:1:1:1: 0.3. Adding the mixed powder into a feeding system of plasma cladding equipment, introducing 99.9% argon, spraying the mixed powder onto the surface of Ti-6Al-4V alloy under the pressure of the argon, and forming TiB on the surface of the alloy by taking plasma as a heat source2And carrying out cladding twice on the particle-reinforced CoCrCuFeNiMoMn high-entropy alloy coating to obtain a coating with the thickness of 2.9 mm.
The above description is only for the purpose of illustrating the present invention and the appended claims, and the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (9)
1. Preparation of TiB on titanium alloy2The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: sequentially prefabricating a Co film, a Ni film and a Cr film on the surface of a titanium alloy substrate, and then mixing Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB2The mixed powder is cladded on a titanium alloy matrix containing a prefabricated film to obtain TiB2The particle reinforced CoCrCuFeNiMoMn high-entropy alloy coating.
2. Preparation of TiB on titanium alloys according to claim 12The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: the titanium alloy matrix is industrial pure titanium or Ti-6Al-4V alloy.
3. Preparation of TiB on titanium alloys according to claim 12The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: before prefabricating Co, Ni and Cr films, the titanium alloy substrate is polished and cleaned.
4. Preparation of TiB on titanium alloys according to claim 32The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: the polishing is carried out by 2000-3000-mesh sand paper, ultrasonic cleaning is carried out for 20-40min after polishing, and then drying is carried out at 30-50 ℃.
5. Preparation of TiB on titanium alloys according to claim 12The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: the Co film, the Ni film and the Cr film are prepared by magnetron sputtering equipment.
6. Made on a titanium alloy according to claim 1Preparation of TiB2The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: the thicknesses of the Co film, the Ni film and the Cr film are respectively 10-100 nm.
7. Preparation of TiB on titanium alloys according to claim 12The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: the Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB2Mixed powder of Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB2In a molar ratio of 1:1:1:1:1:1:1: 0.3.
8. preparation of TiB on titanium alloys according to claim 12The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: the Co, Cr, Cu, Fe, Ni, Mo, Mn and TiB2The particle size of the mixed powder is 10-30 μm.
9. Preparation of TiB on titanium alloys according to claim 12The method for particle reinforced high-entropy alloy coating is characterized by comprising the following steps: and plasma cladding is adopted for cladding the mixed powder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112626406A (en) * | 2020-12-15 | 2021-04-09 | 江西省科学院应用物理研究所 | Grain-refined chromium-cobalt-nickel multi-principal-element alloy and preparation process thereof |
| CN112662984A (en) * | 2020-12-08 | 2021-04-16 | 武汉理工大学 | High-entropy alloy coating material and preparation method and application thereof |
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| CN112662984B (en) * | 2020-12-08 | 2023-03-21 | 武汉理工大学 | High-entropy alloy coating material and preparation method and application thereof |
| CN112626406A (en) * | 2020-12-15 | 2021-04-09 | 江西省科学院应用物理研究所 | Grain-refined chromium-cobalt-nickel multi-principal-element alloy and preparation process thereof |
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