CN111304479A - Preparation method of VCrNbMoW refractory high-entropy alloy - Google Patents
Preparation method of VCrNbMoW refractory high-entropy alloy Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 47
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 35
- 238000000498 ball milling Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 7
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000009768 microwave sintering Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 239000011812 mixed powder Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 12
- 238000011065 in-situ storage Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 238000003825 pressing Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
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- 239000004576 sand Substances 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
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- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 1
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- 238000010952 in-situ formation Methods 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
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- 230000001681 protective effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/10—Sintering only
- B22F3/1039—Sintering only by reaction
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- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B22F9/00—Making metallic powder or suspensions thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
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Abstract
The invention relates to a preparation method of a VCrNbMoW refractory high-entropy alloy, which comprises the following steps of mixing elementary substance powder of V, Cr, Nb, Mo and W according to a molar ratio of 1.1-1.3: 1: 1: 1: 1, weighing and mixing powder, uniformly mixing the weighed and mixed metal element powder in a ball milling tank, taking out the powder after ball milling for a certain time by using a ball milling medium which is water or alcohol, drying, sieving and granulating the powder, and then carrying out cold press molding and cold isostatic pressing with a certain pressure to obtain a pressed blankSintering in a microwave oven, keeping the temperature of the blank after reaching a certain temperature by adopting a certain heating rate, and cooling along with the oven after sintering2O3The particles are uniformly distributed in the VCrNbMoW refractory high-entropy alloy matrix, and the aim is to refine the VCrNbMoW refractory high-entropy alloy grains so as to improve the mechanical property of the composite material.
Description
Technical Field
The invention belongs to the technical field of preparation of refractory high-entropy alloy composite materials, and provides a preparation method of a VCrNbMoW refractory high-entropy alloy.
Technical Field
In order to improve the high strength and toughness performance of the metal material, in 1995, professor Leyu Yi proposes a multi-principal-element high-entropy alloy concept. High Entropy Alloys (HEAs) have excellent properties such as high strength, high hardness, high work hardening, high wear resistance, high temperature stability, and corrosion resistance compared to other alloys. As a potential functional material and engineering material, HEAs have wide application prospect in the aspects of high-speed cutting tools, dies, nuclear power engineering, ship materials, battery materials and the like.
The high-entropy alloy generally comprises more than 5 elements, and the content (atomic fraction, the same applies below) of the high-entropy alloy can be adjusted within the range of 5-35%, so that the high-entropy alloy has a plurality of systems. High entropy alloys can be classified by crystal structure into Body Centered Cubic (BCC), Face Centered Cubic (FCC), and Hexagonal Close Packing (HCP).
The invention adopts the powder metallurgy-microwave sintering method to prepare the second phase V in situ2O3The VCrNbMoW doped refractory high-entropy alloy. Because the pure VCrNbMoW refractory high-entropy alloy belongs to a body-centered cubic (BCC) structure, the toughness is insufficient, the brittleness is large, and the requirement of the mechanical property of a structural material cannot be met。
Disclosure of Invention
The technical problem to be solved by the invention is as follows: by in situ formation of V2O3The nano particles are uniformly distributed in the VCrNbMoW refractory high-entropy alloy matrix, and the aim is to refine the VCrNbMoW refractory high-entropy alloy grains so as to improve the mechanical property of the composite material. The high-entropy alloy structure is a single body-centered cubic structure and has the characteristics of high melting point, high strength, high hardness and the like.
The technical scheme of the invention is as follows:
the invention relates to a preparation method of a VCrNbMoW refractory high-entropy alloy. The powder metallurgy-microwave sintering method is adopted to prepare V in situ2O3The doped VCrNbMoW refractory high-entropy alloy powder has a single-body-centered cubic structure, and specifically comprises the following steps:
(1) the method comprises the following steps of mixing elementary substance powder of V, Cr, Nb, Mo and W according to a molar ratio of 1.1-1.3: 1: 1: 1: 1, weighing and mixing powder, namely uniformly mixing the weighed and mixed metal element powder in a ball milling tank, wherein a ball milling medium is water or alcohol, and ball milling and mixing are adopted;
(2) drying, sieving and granulating the uniformly mixed powder, and pressing the powder into a green body;
(3) heating to a certain temperature by adopting a microwave sintering furnace under a protective atmosphere, and preserving heat for a certain time to sinter the blank;
when the VCrNbMoW refractory high-entropy alloy is prepared in situ, the ball milling time is 12-24 h, and the cold isostatic pressure is 100-300 MPa.
When the VCrNbMoW refractory high-entropy alloy is prepared in situ, the heating rate is 5-20 ℃/min, the sintering temperature is 1400-1700 ℃, the heat preservation time is 30-120 min, and the sintering atmosphere is vacuum or argon atmosphere.
When the VCrNbMoW refractory high-entropy alloy is prepared in situ, the high-entropy alloy composite material with a single body-centered cubic structure is prepared by adopting a powder metallurgy-microwave sintering method.
The invention adopts a powder metallurgy-microwave sintering method to prepare the VCrNbMoW refractory high-entropy alloy composite material in situ, and the pure VCrNbMoW refractory high-entropy alloy composite materialOn the basis of alloy preparation, 10-30% of V powder is added, and V is formed in situ after ball milling2O3Nanoparticles, in situ formed V2O3The nano particles can be uniformly distributed in the VCrNbMoW refractory high-entropy alloy matrix and play a role in refining the VCrNbMoW refractory high-entropy alloy grains, so that the toughness of the VCrNbMoW refractory high-entropy alloy material can be effectively improved.
Compared with other technologies, the invention has the outstanding advantages that:
(1) the powder metallurgy-microwave sintering technology is adopted, so that the cost is reduced, and no pollution is caused.
(2) A single body-centered cubic structure is formed.
(3) Prepared in situ and comprising V2O3The refractory high-entropy alloy composite material of the nano particles can ensure that the composite material has higher toughness.
Drawings
FIG. 1 is an XRD pattern of a pure VCrNbMoW refractory high-entropy alloy sample prepared by microwave sintering.
FIG. 2 is a microwave sintering in situ prepared V2O3XRD pattern of the VCrNbMoW doped refractory high-entropy alloy composite material.
FIG. 3 is the in situ prepared V of microwave sintering in example 12O3Fracture SEM image of the doped VCrNbMoW refractory high-entropy alloy composite material.
Detailed Description
The invention is explained in more detail below by means of specific embodiments and figures, but the following detailed description is only exemplary and not restrictive, and the technical features or combinations of technical features described in the embodiments should not be considered in isolation, but they can be combined with one another to achieve better technical features.
Example 1
A preparation method of VCrNbMoW refractory high-entropy alloy comprises the following steps of mixing raw material powder according to the molar ratio of V, Cr, Nb, Mo and W being 1.2: 1: 1: 1: 1, weighing and mixing powder, wherein the excessive amount of the powder V is 20%, the total amount of the mixed powder is 20g, adding all the weighed powder into a ball milling tank, and then adding 20ml of alcohol as a ball milling medium for ball milling; ball milling is carried out for 12h at 150r/min by using a high-energy ball mill. Then drying the mixture by using a drying oven at 100 ℃, sieving the mixture by using a 200-mesh sieve, adding 9 drops of 5% PVA, grinding and granulating, pressing and molding the material by using a stainless steel grinding tool with the diameter of 10mm and the pressure of 20MPa, and then maintaining the pressure for 3min by using cold isostatic pressing and the pressure of 200 MPa. And then placing the blank body in a microwave sintering furnace for sintering, introducing Ar gas for protection in the sintering process, heating at the heating rate of 10 ℃/min, keeping the temperature at 1550 ℃ for 30min, then cooling the furnace and taking out, and grinding a surface burning loss layer and an oxidation layer by using a diamond sand table.
Example 2
A preparation method of VCrNbMoW refractory high-entropy alloy comprises the following steps of mixing raw material powder according to the molar ratio of V, Cr, Nb, Mo and W being 1.1: 1: 1: 1: 1, weighing and mixing powder, wherein the excessive amount of the powder V is 10 percent, the total amount of the mixed powder is 20g, all the weighed powder is added into a ball milling tank, and then 20ml of alcohol is added as a ball milling medium for ball milling; ball milling is carried out for 12h at 150r/min by using a high-energy ball mill. Then drying the mixture by using a drying oven at 100 ℃, sieving the mixture by using a 200-mesh sieve, adding 9 drops of 5% PVA, grinding and granulating, pressing and molding the material by using a stainless steel grinding tool with the diameter of 10mm and the pressure of 20MPa, and then maintaining the pressure for 3min by using cold isostatic pressing and the pressure of 200 MPa. And then placing the blank body in a microwave sintering furnace for sintering, introducing Ar gas for protection in the sintering process, heating at the heating rate of 10 ℃/min, keeping the temperature at 1550 ℃ for 30min, then cooling the furnace and taking out, and grinding a surface burning loss layer and an oxidation layer by using a diamond sand table.
Example 3
A preparation method of VCrNbMoW refractory high-entropy alloy comprises the following steps of mixing raw material powder according to the molar ratio of V, Cr, Nb, Mo and W being 1.3: 1: 1: 1: 1, weighing and mixing powder, wherein the excessive amount of the powder V is 30 percent, the total amount of the mixed powder is 20g, all the weighed powder is added into a ball milling tank, and then 20ml of alcohol is added as a ball milling medium for ball milling; ball milling is carried out for 12h at 150r/min by using a high-energy ball mill. Then drying the mixture by using a drying oven at 100 ℃, sieving the mixture by using a 200-mesh sieve, adding 9 drops of 5% PVA, grinding and granulating, pressing and molding the material by using a stainless steel grinding tool with the diameter of 10mm and the pressure of 20MPa, and then maintaining the pressure for 3min by using cold isostatic pressing and the pressure of 200 MPa. And then placing the blank body in a microwave sintering furnace for sintering, introducing Ar gas for protection in the sintering process, heating at the heating rate of 10 ℃/min, keeping the temperature at 1550 ℃ for 30min, then cooling the furnace and taking out, and grinding a surface burning loss layer and an oxidation layer by using a diamond sand table.
Reference 1
Referring to fig. 1, the preparation of the pure VCrNbMoW refractory high-entropy alloy comprises the following steps of mixing raw material powder according to the molar ratio of V, Cr, Nb, Mo and W, wherein the raw material powder comprises the following components in a proportion of 1: 1: 1: 1: 1, weighing and mixing powder, setting the total amount of the mixed powder to be 20g, adding all the weighed powder into a ball milling tank, and then adding 20ml of alcohol as a ball milling medium for ball milling; ball milling is carried out for 12h at 150r/min by using a high-energy ball mill. Then drying the mixture by using a drying oven at 100 ℃, sieving the mixture by using a 200-mesh sieve, adding 9 drops of 5% PVA, grinding and granulating, pressing and molding the material by using a stainless steel grinding tool with the diameter of 10mm and the pressure of 20MPa, and then maintaining the pressure for 3min by using cold isostatic pressing and the pressure of 200 MPa. And then placing the blank body in a microwave sintering furnace for sintering, introducing Ar gas for protection in the sintering process, heating at the heating rate of 10 ℃/min, keeping the temperature at 1550 ℃ for 30min, then cooling the furnace and taking out, and grinding a surface burning loss layer and an oxidation layer by using a diamond sand table.
1. For the VCrNbMoW refractory high-entropy alloy composite materials produced in example 1, example 2, example 3 and comparative example 1, respectively, the hardness of a sample is measured by using a vickers hardness tester MH5L type, the experimental load is 1000g, the sample is kept for 10s, the sample is randomly tested for 9 points, the maximum value and the minimum value are removed, the average value of the remaining 7 points is taken as the final hardness value, and the final alloy hardness test result is as follows:
| loaded load | Retention time | Hardness of | |
| Example 1V | |||
| 20% | 1000g | 10s | 3916.3 |
| Example 2V | |||
| 30% | 1000g | 10s | 3745.8Hv |
| Example 3V 10% | 1000g | 10s | 3616.5Hv |
| Comparative example 1 No | 1000g | 10s | 3536.7Hv |
It can be seen that the alloy hardness of examples 1, 2 and 3 is stronger than that of comparative example 1 (the comparative example does not add a large amount of V), wherein the strength of V added by 20% in the case of example 1 is stronger than that added by 30% in the case of example 1, and the optimum ratio is that of example 1.
While embodiments of the present invention have been described herein, it will be understood by those skilled in the art that changes may be made to the embodiments herein without departing from the spirit of the invention. The above examples are merely illustrative and should not be taken as limiting the scope of the invention.
Claims (3)
1. A preparation method of VCrNbMoW refractory high-entropy alloy is characterized by comprising the following specific steps:
1) the method comprises the following steps of mixing elementary substance powder of V, Cr, Nb, Mo and W according to a molar ratio of 1.1-1.3: 1: 1: 1: 1, weighing and mixing powder, namely uniformly mixing the weighed and mixed metal element powder in a ball milling tank, wherein a ball milling medium is water or alcohol, and ball milling and mixing are adopted;
2) drying, sieving and granulating the mixed powder obtained in the step 1), and then using cold press molding and cold isostatic pressing with certain pressure.
3) And (3) placing the pressed blank in a microwave sintering furnace, and keeping the blank at a certain temperature through a certain heating rate.
4) The refractory high-entropy alloy-based composite material with the body-centered cubic structure can be obtained through the steps.
2. The preparation method of the VCrNbMoW refractory high-entropy alloy as claimed in claim 1, wherein the ball milling time is 12-24 h, and the cold isostatic pressure is 100-300 MPa.
3. The method for preparing the VCrNbMoW refractory high-entropy alloy as claimed in claim 1, wherein the heating rate is 5-20 ℃/min, the sintering temperature is 1400-1700 ℃, the heat preservation time is 30-120 min, and the sintering atmosphere is vacuum or argon atmosphere.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939575A (en) * | 2021-01-29 | 2021-06-11 | 哈尔滨工业大学 | Method for rapidly preparing manganese-cobalt spinel coating by microwave mixing and heating |
| CN113234983A (en) * | 2021-04-13 | 2021-08-10 | 哈尔滨工业大学（深圳） | NbTaTiZr double-equal atomic ratio high-entropy alloy and preparation method thereof |
| CN113549780A (en) * | 2021-07-12 | 2021-10-26 | 中国工程物理研究院材料研究所 | Powder metallurgy refractory multi-principal-element high-entropy alloy and preparation method thereof |
| CN114734041A (en) * | 2022-04-29 | 2022-07-12 | 上海交通大学 | Light refractory high-entropy alloy powder material, preparation method and application thereof in additive manufacturing |
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| CN106834878A (en) * | 2017-04-01 | 2017-06-13 | 南京理工大学 | A kind of method that microwave sintering prepares endogenous high-entropy alloy-base composite material |
| CN109628818A (en) * | 2018-12-27 | 2019-04-16 | 南昌航空大学 | A kind of VCrNbMoW infusibility high entropy alloy material and preparation method thereof |
| KR20190108413A (en) * | 2018-03-14 | 2019-09-24 | 한국생산기술연구원 | Preparation method of body-centered cubic high-entropy alloy powder and the powder thereof |
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- 2020-03-18 CN CN202010192512.8A patent/CN111304479A/en active Pending
Patent Citations (3)
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| CN106834878A (en) * | 2017-04-01 | 2017-06-13 | 南京理工大学 | A kind of method that microwave sintering prepares endogenous high-entropy alloy-base composite material |
| KR20190108413A (en) * | 2018-03-14 | 2019-09-24 | 한국생산기술연구원 | Preparation method of body-centered cubic high-entropy alloy powder and the powder thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939575A (en) * | 2021-01-29 | 2021-06-11 | 哈尔滨工业大学 | Method for rapidly preparing manganese-cobalt spinel coating by microwave mixing and heating |
| CN113234983A (en) * | 2021-04-13 | 2021-08-10 | 哈尔滨工业大学（深圳） | NbTaTiZr double-equal atomic ratio high-entropy alloy and preparation method thereof |
| CN113549780A (en) * | 2021-07-12 | 2021-10-26 | 中国工程物理研究院材料研究所 | Powder metallurgy refractory multi-principal-element high-entropy alloy and preparation method thereof |
| CN113549780B (en) * | 2021-07-12 | 2022-05-27 | 中国工程物理研究院材料研究所 | Powder metallurgy refractory multi-principal-element high-entropy alloy and preparation method thereof |
| CN114734041A (en) * | 2022-04-29 | 2022-07-12 | 上海交通大学 | Light refractory high-entropy alloy powder material, preparation method and application thereof in additive manufacturing |
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