CN110670037A - Preparation method for FeAlCoCuNiV high-entropy alloy target material through hot isostatic pressing - Google Patents
Preparation method for FeAlCoCuNiV high-entropy alloy target material through hot isostatic pressing Download PDFInfo
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- CN110670037A CN110670037A CN201911051519.1A CN201911051519A CN110670037A CN 110670037 A CN110670037 A CN 110670037A CN 201911051519 A CN201911051519 A CN 201911051519A CN 110670037 A CN110670037 A CN 110670037A
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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
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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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
- 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
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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
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a preparation method for forming a FeAlCoCuNiV high-entropy alloy target by hot isostatic pressing, which comprises the following steps: step 1, selecting and proportioning alloy raw materials; step 2, performing non-consumable vacuum melting on the proportioned alloy raw materials; step 3, powdering the alloy smelting cast ingot obtained in the step 2; step 4, packaging the alloy powder through a sheath; step 5, performing hot isostatic pressing on the sheath filled with the alloy powder to obtain a bar blank; and 6, removing the sheath of the rod blank through machining, and processing the rod blank to a specific size to obtain the high-entropy alloy target material. Before the powder of the target material is sintered, atoms in the target material can be fully fused through the smelting treatment of a non-consumable vacuum smelting furnace, so that the generation of composition and tissue segregation phenomena is avoided; in the manufacturing process, the processes from alloy smelting to powder hot isostatic pressing are carried out in the protection of vacuum mixed inert gas, so that the problem of oxidation in the preparation process of the target material can be avoided.
Description
Technical Field
The invention belongs to the technical field of metal powder processing, and relates to a preparation method for hot isostatic pressing forming of a FeAlCoCuNiV high-entropy alloy target.
Background
The high-entropy alloy is a multi-principal-element and high-mixed-entropy alloy prepared from five or more metal and nonmetal elements according to an equimolar or near-equimolar ratio, has the advantages of excellent mechanics, chemistry, electromagnetism, high-temperature oxidation resistance and the like, and particularly shows superiority when being applied to the field of magnetic recording media.
In the preparation process of the traditional target material, a process route of mixing elemental metal powder and a compression molding process is often directly adopted, and the process usually generates: the problems of inter-grain pores and the like caused by powder oxidation, segregation of various components and structures, poor infiltration of powder grain boundaries and the like finally cause the problems of more defects, low density, poor machining and forming performances and the like of the prepared target material.
Disclosure of Invention
The invention provides a preparation method of FeAlCoCuNiV high-entropy alloy target material hot isostatic pressing molding, which is characterized in that through a vacuum melting process after raw material proportioning, atoms in the target material are fully fused, and no component macrosegregation is generated; the vacuum canning powder filling technology is adopted, the near-net forming of the target material after hot pressing is realized by placing the preset shrinkage rate, and the powder can be further densified before the hot pressing forming; and hot isostatic pressing is adopted for high-temperature and high-pressure forming, so that the density of the target material is further improved.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the FeAlCoCuNiV high-entropy alloy target material hot isostatic pressing forming is implemented according to the following steps:
step 1, selecting and proportioning alloy raw materials;
step 2, performing non-consumable vacuum melting on the proportioned alloy raw materials;
step 3, powdering the alloy smelting cast ingot obtained in the step 2;
step 4, packaging the alloy powder through a sheath;
step 5, performing hot isostatic pressing on the sheath filled with the alloy powder to obtain a bar blank;
and 6, removing the sheath of the rod blank through machining, and processing the rod blank to a specific size to obtain the high-entropy alloy target material.
The step 1 specifically comprises the following steps: selecting Fe, Al, Co, Cu, Ni and V bulk metals with the purity of more than 99.9%, and mixing the bulk metals according to the atomic equimolar ratio to obtain an alloy raw material;
the step 2 specifically comprises the following steps: smelting the mixed alloy raw materials in a non-consumable vacuum smelting furnace to obtain an alloy ingot; the smelting is carried out under the argon atmosphere of 1Pa at the current of 250A for 5-8 times.
The step 3 specifically comprises the following steps: the powdering treatment is carried out by refining and ingot casting through a mechanical stamping method, ball milling and powder mixing are carried out through a mechanical vacuum ball milling method, a ball milling is GGr15, the ball-material ratio is 8:1, ball milling is carried out for 1-3 h in an argon atmosphere under 1Pa, and the grain size of the obtained alloy powder is 10-30 mu m.
The step 4 specifically comprises the following steps: 4.1, the sheath is made into a closed cylinder (a reserved powder filling hole) by adopting a No. 20 rigid plate with the thickness of 6 mm;
4.2 preheating the alloy powder to 450 ℃ and ensuring the vacuum degree to be less than 1 Pa;
4.3, filling the alloy powder into the sheath;
4.4 after the powder filling is finished, carrying out laser welding sealing treatment on the powder filling hole of the sheath.
In the step 5, the hot isostatic pressing temperature is 890-910 ℃, the heat preservation time is 2-2.5 h, the pressure is 120-140 Mpa, and the tapping temperature is lower than 300 ℃.
The invention has the beneficial effects that:
① before sintering the powder of the target material, the atoms in the target material can be fully fused by the smelting treatment of a non-consumable vacuum smelting furnace, thereby avoiding the generation of composition and tissue segregation phenomena;
② in the manufacturing process, the processes from alloy smelting to powder hot isostatic pressing are all carried out in vacuum or mixed inert gas protection, which can avoid the oxidation problem in the target material preparation process;
③ hot isostatic pressing, which is beneficial to improving the density of the target and reducing the formation probability of internal defects;
④ the method can be widely used for manufacturing the target material of the metal-oxide composite material and is suitable for continuous industrial production.
Drawings
FIG. 1 is a powder SEM image of an alloy ingot of the present invention after ball milling;
FIG. 2 is a film SEM image of the alloy target material prepared by the invention after magnetron sputtering.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1, as shown in fig. 1-2, a method for forming a FeAlCoCuNiV high-entropy alloy target by hot isostatic pressing is specifically performed according to the following steps:
step 1, selecting and proportioning alloy raw materials;
step 2, performing non-consumable vacuum melting on the proportioned alloy raw materials;
step 3, powdering the alloy smelting cast ingot obtained in the step 2;
step 4, packaging the alloy powder through a sheath;
step 5, performing hot isostatic pressing on the sheath filled with the alloy powder to obtain a bar blank;
and 6, removing the sheath of the rod blank through machining, and processing the rod blank to a specific size to obtain the high-entropy alloy target material.
The step 1 specifically comprises the following steps: selecting Fe, Al, Co, Cu, Ni and V bulk metals with the purity of more than 99.9%, and mixing the bulk metals according to the atomic equimolar ratio to obtain an alloy raw material;
and 2, specifically, smelting the mixed alloy raw materials in a non-consumable vacuum smelting furnace (WK- П type) to obtain an alloy ingot, wherein the smelting is carried out for 5 times under the argon atmosphere of 1Pa at the current of 250A, and the alloy ingot with uniformly distributed raw material components can be obtained.
The step 3 specifically comprises the following steps: the powdering treatment is carried out by refining by a mechanical stamping method, ingot casting is crushed, and ball milling and powder mixing are carried out by a mechanical vacuum ball milling method, wherein a ball is GGr15, the ball-material ratio is 8:1, and the ball milling is carried out for 3h in an argon atmosphere under 1Pa, so that the grain size of the obtained alloy powder is 10 mu m.
The step 4 specifically comprises the following steps: 4.1, the sheath is made into a closed cylinder (a reserved powder filling hole) by adopting a No. 20 rigid plate with the thickness of 6 mm;
4.2 preheating the alloy powder to 450 ℃ and ensuring the vacuum degree to be less than 1 Pa;
4.3, filling alloy powder into the sheath;
4.4 after the powder filling is finished, carrying out laser welding sealing treatment on the powder filling hole of the sheath.
In the step 5, the hot isostatic pressing temperature is 890 ℃, the heat preservation time is 2.5h, the pressure is 120Mpa, and the tapping temperature is lower than 300 ℃.
Example 2
This example differs from example 1 only in that:
and 2, specifically, smelting the mixed alloy raw materials in a non-consumable vacuum smelting furnace (WK- П type) to obtain an alloy ingot, wherein the smelting is carried out under the argon atmosphere of 1Pa for 8 times at a current of 250A, and the alloy ingot with uniformly distributed raw material components can be obtained.
The step 3 specifically comprises the following steps: the powdering treatment is carried out by refining by a mechanical stamping method, ingot casting is crushed, and ball milling and powder mixing are carried out by a mechanical vacuum ball milling method, wherein a ball is GGr15, the ball-material ratio is 8:1, and the ball milling is carried out for 1h in an argon atmosphere under 1Pa, so that the grain size of the obtained alloy powder is 30 mu m.
In the step 5, the hot isostatic pressing temperature is 910 ℃, the heat preservation time is 2 hours, the pressure is 140Mpa, and the tapping temperature is lower than 300 ℃.
Example 3
This example differs from example 1 only in that:
the step 2 specifically comprises the following steps: smelting the mixed alloy raw materials in a non-consumable vacuum smelting furnace to obtain an alloy ingot; the melting was carried out at a current of 250A under an argon atmosphere of 1Pa, and the number of times was 6.
The step 3 specifically comprises the following steps: the powdering treatment is carried out by refining by a mechanical stamping method, ingot casting is crushed, and ball milling and powder mixing are carried out by a mechanical vacuum ball milling method, wherein a ball is GGr15, the ball-material ratio is 8:1, and the ball milling is carried out for 2h in an argon atmosphere under 1Pa, so that the grain size of the obtained alloy powder is 20 mu m.
In the step 5, the hot isostatic pressing temperature is 900 ℃, the heat preservation time is 2.2h, the pressure is 130Mpa, and the tapping temperature is lower than 300 ℃.
In the preparation process of the alloy target material, the problems of powder oxidation, segregation of various tissue components and structures, poor infiltration of powder crystal boundary, generation of intercrystalline pores and the like in the alloy target material can be effectively solved through vacuum melting of Fe, Al, Co, Cu, Ni and V alloys, powdering of alloy ingots, sleeving, degassing and sealing treatment of alloy powder and hot isostatic pressing treatment, the uniformity of the components of the alloy target material, the flatness and the density of the structures are further improved, the physical and chemical properties of the material are effectively improved, the tissue uniformity of the target material is good, and no cracks are generated.
Claims (6)
1. A preparation method for forming a FeAlCoCuNiV high-entropy alloy target by hot isostatic pressing is characterized by comprising the following steps:
step 1, selecting and proportioning alloy raw materials;
step 2, performing non-consumable vacuum melting on the proportioned alloy raw materials;
step 3, powdering the alloy smelting cast ingot obtained in the step 2;
step 4, packaging the alloy powder through a sheath;
step 5, performing hot isostatic pressing on the sheath filled with the alloy powder to obtain a bar blank;
and 6, removing the sheath of the rod blank through machining, and processing the rod blank to a specific size to obtain the high-entropy alloy target material.
2. The method for preparing the FeAlCoCuNiV high-entropy alloy target material by hot isostatic pressing according to claim 1, wherein the step 1 is specifically as follows: fe, Al, Co, Cu, Ni and V bulk metals with the purity of more than 99.9 percent are selected and mixed according to the proportion of atom equal molar ratio to obtain the alloy raw material.
3. The method for preparing the FeAlCoCuNiV high-entropy alloy target material by hot isostatic pressing according to claim 1, wherein the step 2 is specifically as follows: smelting the mixed alloy raw materials in a non-consumable vacuum smelting furnace to obtain an alloy ingot; the smelting is carried out under the argon atmosphere of 1Pa at the current of 250A for 5-8 times.
4. The method for preparing the FeAlCoCuNiV high-entropy alloy target material by hot isostatic pressing according to claim 1, wherein the step 3 is specifically as follows: and the powdering treatment comprises the steps of refining by a mechanical stamping method, crushing cast ingots, and ball-milling and mixing powder by a mechanical vacuum ball-milling method, wherein a ball is GGr15, the ball-material ratio is 8:1, and the ball-milling is carried out for 3 hours in an argon atmosphere under 1Pa, so that the grain size of the obtained alloy powder is 10-30 mu m.
5. The method for preparing the FeAlCoCuNiV high-entropy alloy target material by hot isostatic pressing according to claim 1, wherein the step 4 is specifically as follows:
4.1, the sheath is made into a closed cylinder (a reserved powder filling hole) by adopting a No. 20 rigid plate with the thickness of 6 mm;
4.2 preheating the alloy powder to 450 ℃ and ensuring the vacuum degree to be less than 1 Pa;
4.3, filling alloy powder into the sheath;
4.4 after the powder filling is finished, carrying out laser welding sealing treatment on the powder filling hole of the sheath.
6. The preparation method for hot isostatic pressing forming of the FeAlCoCuNiV high-entropy alloy target material according to claim 1, wherein in the step 5, the hot isostatic pressing temperature is 890-910 ℃, the heat preservation time is 2-2.5 h, the pressure is 120-140 Mpa, and the tapping temperature is lower than 300 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111321335A (en) * | 2020-03-06 | 2020-06-23 | 中南大学 | High-corrosion-resistance high-toughness FeCrNi series multi-principal-element alloy and preparation method thereof |
| CN118417566A (en) * | 2024-07-01 | 2024-08-02 | 中国航发北京航空材料研究院 | Powder high Wen Gaoshang alloy blade size control method |
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| CN106475567A (en) * | 2015-08-27 | 2017-03-08 | 宁波江丰电子材料股份有限公司 | The manufacture method of chrome molybdenum target blankss |
| CN106881466A (en) * | 2017-03-23 | 2017-06-23 | 江西理工大学 | Rare earth modified grapheme strengthens the preparation method of metal-based compound bar |
| CN108103464A (en) * | 2017-11-21 | 2018-06-01 | 航天海鹰(哈尔滨)钛业有限公司 | A kind of preparation method of Fe, Al, Co, Cu, Cr, Mn alloy target material |
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- 2019-10-31 CN CN201911051519.1A patent/CN110670037A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102352483A (en) * | 2011-11-15 | 2012-02-15 | 江苏美特林科特殊合金有限公司 | Preparation method of silicon-aluminium alloy hollow rotary target for vacuum sputtering coating |
| CN106475567A (en) * | 2015-08-27 | 2017-03-08 | 宁波江丰电子材料股份有限公司 | The manufacture method of chrome molybdenum target blankss |
| CN106881466A (en) * | 2017-03-23 | 2017-06-23 | 江西理工大学 | Rare earth modified grapheme strengthens the preparation method of metal-based compound bar |
| CN108103464A (en) * | 2017-11-21 | 2018-06-01 | 航天海鹰(哈尔滨)钛业有限公司 | A kind of preparation method of Fe, Al, Co, Cu, Cr, Mn alloy target material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111321335A (en) * | 2020-03-06 | 2020-06-23 | 中南大学 | High-corrosion-resistance high-toughness FeCrNi series multi-principal-element alloy and preparation method thereof |
| CN118417566A (en) * | 2024-07-01 | 2024-08-02 | 中国航发北京航空材料研究院 | Powder high Wen Gaoshang alloy blade size control method |
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