CN115770880A - High-entropy alloy powder for additive manufacturing and preparation method thereof - Google Patents
High-entropy alloy powder for additive manufacturing and preparation method thereof Download PDFInfo
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- CN115770880A CN115770880A CN202211626877.2A CN202211626877A CN115770880A CN 115770880 A CN115770880 A CN 115770880A CN 202211626877 A CN202211626877 A CN 202211626877A CN 115770880 A CN115770880 A CN 115770880A
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- 239000000956 alloy Substances 0.000 title claims abstract description 61
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 60
- 239000000843 powder Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 239000000654 additive Substances 0.000 title claims abstract description 18
- 230000000996 additive effect Effects 0.000 title claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 100
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000005485 electric heating Methods 0.000 claims abstract description 8
- 230000005674 electromagnetic induction Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 8
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims 2
- 238000010146 3D printing Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910002555 FeNi Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000002932 luster Substances 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004372 laser cladding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- -1 at present Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention belongs to the technical field of additive manufacturing, and relates to high-entropy alloy powder for additive manufacturing and a preparation method thereof. The invention provides a preparation method of the high-entropy alloy powder, which comprises the following steps: uniformly mixing Nb, mn, ti and Cd, performing first ball milling, adding La and Si for second ball milling, adding Fe and Ni for third ball milling, and finally performing gradient heating by adopting an electromagnetic induction electric heating mode. The preparation method provided by the invention is simple and convenient to operate, easy to realize, good in denitrification effect, excellent in mechanical property and beneficial to improvement of the quality of a 3D printing product.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing, and relates to high-entropy alloy powder for additive manufacturing and a preparation method thereof.
Background
Additive Manufacturing (AM) is a technology for Manufacturing solid parts by using a layer-by-layer accumulation principle of discrete materials (liquid, powder, wire, sheet, plate, block, and the like) according to three-dimensional CAD design data. Additive manufacturing is a "bottom-up" material build-up manufacturing process relative to conventional material removal (e.g., cutting, etc.) techniques. The application of the additive manufacturing technology has more problems, one important technical bottleneck is the preparation of high-quality metal powder, at present, metal 3D printing powder at home and abroad is mostly prepared by adopting a traditional method, and the high-entropy alloy powder prepared by the methods has high impurity content and quality.
The high-entropy alloy is an alloy with a high entropy value, which is formed by five or more metals or non-metals with equal atomic ratio or near equal atomic ratio. Compared with the traditional alloy material, the high-entropy alloy has the advantages of high strength, high hardness, corrosion resistance, wear resistance and the like, and is applied to high-speed cutting tools, nuclear power station steam generator pipes, superconducting leads and the like. Among the methods for producing high-entropy alloys, the arc melting method is the most commonly used conventional production method. The arc melting method is easy to generate defects such as gaps, so that in recent years, novel preparation methods of high-entropy alloys are endless. The method for preparing the high-entropy alloy by using the ball milling mode is firstly appeared in 2007 and is successful. In recent years, great research progress is also made on the preparation of high-entropy alloy coatings by laser cladding, and the uniform-component coatings are difficult to obtain by using premixed simple substance powder in laser cladding, so that the quality and the surface continuity of the coatings are poor, and the preparation of the uniform-component high-entropy alloy powder has important research significance.
Disclosure of Invention
The invention aims at the problems and provides a high-entropy alloy powder for additive manufacturing. The high-entropy alloy powder prepared by the method has the advantages of low nitrogen content and high strength, and is particularly suitable for additive manufacturing.
In one aspect, the present invention relates to a method for preparing a high-entropy alloy powder, comprising: uniformly mixing Nb, mn, ti and Cd, performing first ball milling, adding La and Si, performing second ball milling, adding Fe and Ni, performing third ball milling, and performing gradient heating by adopting an electromagnetic induction electric heating mode.
Further, in the preparation method of the high-entropy alloy powder, the speed of the first ball milling is 200-400r/min, and the time of the first ball milling is 5-10h; the speed of the second ball milling is 250-350r/min, and the time of the second ball milling is 10-20h; the speed of the third ball milling is 500-600r/min, and the time of the third ball milling is 20-30h.
Further, in the preparation method of the high-entropy alloy powder provided by the invention, the gradient heating comprises the following steps: heating to 400 ℃ at 200 ℃ for 5-10min, keeping at 400 ℃ for 5min, heating to 800 ℃ at 400 ℃ for 10-15min, keeping at 800 ℃ for 5min, heating to 1200 ℃ for 5-10min, keeping at 1200 ℃ for 5min, heating to 1600 ℃ at 1200 ℃ for 5-10min, and keeping at 1600 ℃ for 10-15min.
Further, in the preparation method of the high-entropy alloy powder provided by the invention, the first ball milling, the second ball milling or the third ball milling is prepared in vacuum or inert atmosphere.
Further, in the preparation method of the high-entropy alloy powder, absolute ethyl alcohol is used as a ball milling medium for the first ball milling, distilled water and lauryl sodium sulfate are used as ball milling media for the second ball milling, and distilled water and lauryl phenol polyoxyethylene ether are used as ball milling media for the third ball milling.
Further, in the preparation method of the high-entropy alloy powder provided by the invention, the ratio of the distilled water to the sodium dodecyl sulfate is 1.
In another aspect, the invention relates to a high-entropy alloy powder, which is prepared by the preparation method of the high-entropy alloy powder; in particular, the application of the high-entropy alloy powder in additive manufacturing is included.
Compared with the prior art, the invention has the following beneficial effects or advantages:
the invention carries out 3 times of batch ball milling, and adopts different ball milling media to avoid the agglomeration phenomenon of powder particles, so that the prepared high-entropy alloy powder is uniformly dispersed and the particle size distribution is uniform; the invention designs a gradient temperature rise curve, so that each component is stably crystallized, and the hardness of the powder and the thermal stability of an amorphous phase are obviously improved.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the present invention will be further described with reference to the following specific examples, which are not intended to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the test articles and materials, unless otherwise specified, are commercially available.
Example 1
This example provides the preparation of a high entropy alloy powder for additive manufacturing.
The chemical formula of the high-entropy alloy powder is NbMnTiCdla 0.2 Si 0.8 FeNi。
And (4) polishing off oxides and attached impurities on the surface of the required alloy raw material until metallic luster appears. Then putting into alcohol or acetone solution and cleaning for 25min by ultrasonic wave, and after cleaning, putting into a 60 ℃ oven for drying for 10 h.
Uniformly mixing Nb, mn, ti and Cd, performing first ball milling, adding La and Si, performing second ball milling, adding Fe and Ni, performing third ball milling, and performing gradient heating by adopting an electromagnetic induction electric heating mode.
The speed of the first ball milling is 200r/min, and the time of the first ball milling is 5h; the speed of the second ball milling is 250r/min, and the time of the second ball milling is 10h; the speed of the third ball milling is 500r/min, and the time of the third ball milling is 20h.
The first ball milling takes absolute ethyl alcohol as a ball milling medium, the second ball milling takes distilled water and lauryl sodium sulfate as ball milling media, and the third ball milling takes distilled water and lauryl phenol polyoxyethylene ether as ball milling media. The volume ratio of the distilled water to the sodium dodecyl sulfate is 1, and the ratio of the distilled water to the dodecyl phenol polyoxyethylene ether is 2. The proportion of the ball milling medium to the material to be ball milled is 1.
The gradient heating is as follows: heating to 400 ℃ for 5min at 200 ℃, keeping the temperature for 5min at 400 ℃, heating to 800 ℃ for 10min at 400 ℃, keeping the temperature for 5min at 800 ℃, heating to 1200 ℃ for 5min at 800 ℃, keeping the temperature for 5min at 1200 ℃, heating to 1600 ℃ for 5min at 1200 ℃, and keeping the temperature for 10min at 1600 ℃.
And atomizing by using argon, and then screening the collected atomized powder by using cyclone separation equipment or a test sieve to obtain the high-entropy alloy powder.
Example 2
This example provides the preparation of a high entropy alloy powder for additive manufacturing.
The chemical formula of the high-entropy alloy powder is NbMnTiCdLa 0.2 Si 0.8 FeNi。
And (4) polishing off oxides and attached impurities on the surface of the required alloy raw material until metallic luster appears. Then putting into alcohol or acetone solution and cleaning for 25min by ultrasonic wave, and after cleaning, putting into a 60 ℃ oven for drying for 10 h.
Uniformly mixing Nb, mn, ti and Cd, performing first ball milling, adding La and Si for second ball milling, adding Fe and Ni for third ball milling, and finally performing gradient heating by adopting an electromagnetic induction electric heating mode.
The speed of the first ball milling is 400r/min, and the time of the first ball milling is 10h; the speed of the second ball milling is 350r/min, and the time of the second ball milling is 20h; the speed of the third ball milling is 600r/min, and the time of the third ball milling is 30h.
The first ball milling takes absolute ethyl alcohol as a ball milling medium, the second ball milling takes distilled water and lauryl sodium sulfate as ball milling media, and the third ball milling takes distilled water and lauryl phenol polyoxyethylene ether as ball milling media. The volume ratio of the distilled water to the sodium dodecyl sulfate is 1. The proportion of the ball milling medium to the material to be ball milled is 1.
The gradient heating is as follows: heating to 400 ℃ for 10min at 200 ℃, keeping the temperature for 5min at 400 ℃, heating to 800 ℃ for 15min at 400 ℃, keeping the temperature for 5min at 800 ℃, heating to 1200 ℃ for 10min at 800 ℃, keeping the temperature for 5min at 1200 ℃, heating to 1600 ℃ for 10min at 1200 ℃, and keeping the temperature for 15min at 1600 ℃.
And atomizing by using argon, and then screening the collected atomized powder by using cyclone separation equipment or a test sieve to obtain the high-entropy alloy powder.
Comparative example 1
This example provides the preparation of a high entropy alloy powder for additive manufacturing that was not ball milled three times.
The chemical formula of the high-entropy alloy powder is NbMnTiCdLa 0.2 Si 0.8 FeNi。
And (4) polishing off oxides and attached impurities on the surface of the required alloy raw material until metallic luster appears. Then putting into alcohol or acetone solution and cleaning for 25min by ultrasonic wave, and after cleaning, putting into a 60 ℃ oven for drying for 10 h.
Uniformly mixing Nb, mn, ti, cd, la, si, fe and Ni, then carrying out ball milling, and finally carrying out gradient heating by adopting an electromagnetic induction electric heating mode.
The ball milling speed is 500r/min, and the ball milling time is 35h. The method is characterized in that absolute ethyl alcohol is used as a ball milling medium, and the ratio of the ball milling medium to a material to be ball milled is 1.
The gradient heating is as follows: heating to 400 ℃ for 5min at 200 ℃, keeping the temperature for 5min at 400 ℃, heating to 800 ℃ for 10min at 400 ℃, keeping the temperature for 5min at 800 ℃, heating to 1200 ℃ for 5min at 800 ℃, keeping the temperature for 5min at 1200 ℃, heating to 1600 ℃ for 5min at 1200 ℃, and keeping the temperature for 10min at 1600 ℃.
And atomizing by using argon, and then screening the collected atomized powder by using cyclone separation equipment or a test sieve to obtain the high-entropy alloy powder.
Comparative example 2
This example provides the preparation of a high entropy alloy powder for additive manufacturing that is not gradient heated.
The chemical formula of the high-entropy alloy powder is NbMnTiCdLa 0.2 Si 0.8 FeNi。
And (4) polishing off oxides and attached impurities on the surface of the required alloy raw material until the metallic luster appears. Then putting into alcohol or acetone solution and cleaning for 25min by ultrasonic wave, and after cleaning, putting into a 60 ℃ oven for drying for 10 h.
Uniformly mixing Nb, mn, ti and Cd, performing first ball milling, adding La and Si, performing second ball milling, adding Fe and Ni, performing third ball milling, and heating by adopting an electromagnetic induction electric heating mode.
The speed of the first ball milling is 200r/min, and the time of the first ball milling is 5h; the speed of the second ball milling is 250r/min, and the time of the second ball milling is 10h; the speed of the third ball milling is 500r/min, and the time of the third ball milling is 20h.
The first ball milling takes absolute ethyl alcohol as a ball milling medium, the second ball milling takes distilled water and lauryl sodium sulfate as ball milling media, and the third ball milling takes distilled water and lauryl phenol polyoxyethylene ether as ball milling media. The volume ratio of the distilled water to the sodium dodecyl sulfate is 1, and the ratio of the distilled water to the dodecyl phenol polyoxyethylene ether is 2. The proportion of the ball milling medium to the material to be ball milled is 1.
The heating is as follows: heating to 1200 deg.C to 1600 deg.C for 35min, and maintaining at 1600 deg.C for 10min.
Atomizing by using argon, and then screening the collected atomized powder by using cyclone separation equipment or a test sieve to obtain the high-entropy alloy powder.
Comparative example 3
This example provides the preparation of a high entropy alloy powder for additive manufacturing.
The chemical formula of the high-entropy alloy powder is NbMnTiCdLa 0.2 Si 0.8 FeNi。
And (4) polishing off oxides and attached impurities on the surface of the required alloy raw material until metallic luster appears. Then putting into alcohol or acetone solution and cleaning for 25min by ultrasonic wave, and after cleaning, putting into a 60 ℃ oven for drying for 10 h.
Uniformly mixing Nb, mn, ti, cd, la, si, fe and Ni, then carrying out ball milling, and finally heating by adopting an electromagnetic induction electric heating mode.
The ball milling speed is 500r/min, and the ball milling time is 35h. The method is characterized in that absolute ethyl alcohol is used as a ball milling medium, and the ratio of the ball milling medium to a material to be ball milled is 1.
The heating is as follows: heating to 1600 deg.C for 35min at 1200 deg.C, and maintaining at 1600 deg.C for 10min.
And atomizing by using argon, and then screening the collected atomized powder by using cyclone separation equipment or a test sieve to obtain the high-entropy alloy powder.
The N content of the high-entropy alloy target-range powder obtained by melting and atomizing according to example 1, example 2 and comparative examples 1 to 3 was measured, and the measurement target was 3 furnaces, and the results are shown in Table 1 below.
TABLE 1N content in target stage powder of high entropy alloy
As can be seen from table 1, the content of N in the alloy smelted by the method is obviously lower than that obtained by the traditional method and is lower than 100ppm, which shows that the preparation method of the high-entropy alloy powder provided by the scheme has a good N removing effect and can greatly reduce the content of N in the alloy powder.
As described above, the present invention can be preferably implemented, and the above-mentioned embodiments are merely descriptions of preferred embodiments of the present invention, and do not limit the scope of the present invention, and various changes and modifications made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention shall fall within the protection scope defined by the present invention.
Claims (8)
1. A preparation method of high-entropy alloy powder is characterized by comprising the following steps: uniformly mixing Nb, mn, ti and Cd, performing first ball milling, adding La and Si, performing second ball milling, adding Fe and Ni, performing third ball milling, and performing gradient heating by adopting an electromagnetic induction electric heating mode.
2. A method for preparing high-entropy alloy powder according to claim 1, wherein the first ball milling speed is 200 to 400r/min, and the first ball milling time is 5 to 10 hours; the speed of the second ball milling is 250-350r/min, and the time of the second ball milling is 10-20h; the speed of the third ball milling is 500-600r/min, and the time of the third ball milling is 20-30h.
3. A method of producing a high-entropy alloy powder according to claim 1, wherein the gradient heating includes: heating to 400 ℃ at 200 ℃ for 5-10min, keeping at 400 ℃ for 5min, heating to 800 ℃ at 400 ℃ for 10-15min, keeping at 800 ℃ for 5min, heating to 1200 ℃ for 5-10min, keeping at 1200 ℃ for 5min, heating to 1600 ℃ at 1200 ℃ for 5-10min, and keeping at 1600 ℃ for 10-15min.
4. A method for preparing high entropy alloy powder according to claim 1, wherein the first ball milling, the second ball milling, or the third ball milling is performed in a vacuum or an inert atmosphere.
5. A method for preparing high-entropy alloy powder according to claim 1, wherein the first ball milling uses absolute ethyl alcohol as a ball milling medium, the second ball milling uses distilled water and sodium dodecyl sulfate as ball milling media, and the third ball milling uses distilled water and dodecylphenol polyoxyethylene ether as ball milling media.
6. A preparation method of high-entropy alloy powder according to claim 5, wherein the ratio of distilled water to sodium lauryl sulfate is 1.
7. A high-entropy alloy powder characterized by being produced by the production method for a high-entropy alloy powder according to any one of claims 1 to 6.
8. Use of the high entropy alloy powder of claim 7 in additive manufacturing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116254433A (en) * | 2023-03-17 | 2023-06-13 | 哈尔滨工业大学 | Preparation method of low-density high-strength high-toughness AlMoNbTaTiZr refractory high-entropy alloy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116254433A (en) * | 2023-03-17 | 2023-06-13 | 哈尔滨工业大学 | Preparation method of low-density high-strength high-toughness AlMoNbTaTiZr refractory high-entropy alloy |
| CN116254433B (en) * | 2023-03-17 | 2023-07-21 | 哈尔滨工业大学 | Preparation method of low-density high-strength high-toughness AlMoNbTaTiZr refractory high-entropy alloy |
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