CN111992728A - Preparation method of spherical metal powder for additive manufacturing - Google Patents

Preparation method of spherical metal powder for additive manufacturing Download PDF

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Publication number
CN111992728A
CN111992728A CN202010853326.4A CN202010853326A CN111992728A CN 111992728 A CN111992728 A CN 111992728A CN 202010853326 A CN202010853326 A CN 202010853326A CN 111992728 A CN111992728 A CN 111992728A
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China
Prior art keywords
smelting
powder
alloy
gas
inert gas
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CN202010853326.4A
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Chinese (zh)
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曹珺
赵栋
程乐心
张养德
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Suzhou Chaoxian New Material Co ltd
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Suzhou Chaoxian New Material Co ltd
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Priority to CN202010853326.4A priority Critical patent/CN111992728A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00Materials specially adapted for additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848Melting process before atomisation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention relates to the technical field of alloy powder manufacturing, in particular to a preparation method of spherical metal powder for additive manufacturing, which comprises the following steps: s1, putting the raw master alloy into a smelting furnace, vacuumizing, closing a vacuumizing system when the alloy in the induction smelting furnace is molten, introducing inert gas, smelting the alloy, introducing inert protective gas in the smelting process, and smelting for the second time after the first smelting; s2, putting the molten metal into a tundish, starting an inert gas heating device, and heating atomized gas; s3, introducing the molten metal into the improved tightly-coupled vacuum gas atomization equipment through a flow guide pipe, and solidifying the molten metal into spherical powder particles in the liquid flying process; and S4, performing water-powder separation through filtering and pressing, drying, and performing air flow classification to obtain the 3D printing metal powder. The 3D printing metal powder prepared by the VIGA method has the outstanding advantages of good sphericity, uniform particle size distribution, low oxygen content, good batch consistency and the like.

Description

Preparation method of spherical metal powder for additive manufacturing
Technical Field
The invention relates to the technical field of alloy powder manufacturing, in particular to a preparation method of spherical metal powder for additive manufacturing.
Background
The 3D printing is an emerging manufacturing technology for manufacturing solid objects by stacking materials layer by layer on the basis of a digital model, embodies the close combination of an information network technology, an advanced material technology and a digital manufacturing technology, and is an important component of the advanced manufacturing industry. Additive manufacturing has a profound effect on traditional process flow, production line, factory mode and industrial chain combination, and is a representative subversive technology of manufacturing industry. Because metal powder is expensive and related processes are immature, domestic 3D printing is still limited on plastic materials at present, the strength is low, and the characteristics of heat conduction and electric conduction are lacked, so that the application scene of the additive manufacturing technology is severely restricted, and particularly the direct manufacturing aspect of high-performance and difficult-to-process parts and dies in the fields of aerospace and the like is realized.
The patent with the publication number of CN109482862A discloses 3D printing metal powder and a preparation method thereof, and relates to the technical field of metal materials. Titanium alloy, nickel alloy and chromium alloy metal powder with larger apparent density is prepared. The preparation method of the metal powder specifically comprises the following steps: (1) pretreating, namely cleaning titanium alloy, nickel metal and chromium metal to remove impurities, then respectively smelting and purifying, and then carrying out ultrasonic treatment on each purified liquid for 40-80min to obtain each purified liquid; (2) ultrasonic water atomization, namely performing water atomization on each purified solution under the assistance of ultrasonic waves to prepare powder, and dehydrating, drying in vacuum and screening in grades the prepared powder; (3) and annealing, annealing the screened powder for 5-15 min, and stirring and mixing the annealed powder uniformly according to a ratio to obtain the 3D printing metal powder.
However, the patent of the invention has the following defects: 1. water vapor readily reacts with metals, resulting in water-atomized powders with a high oxygen content. 2. Only the apparent density of the product is considered, and the characteristics of the powder such as particle size distribution are not considered. 3. The yield is low (less than 20%), the nozzle is prone to failure and the cost is high.
Disclosure of Invention
The invention aims to solve the defects that the resistivity is reduced, a short-circuit gap exists and the heat conductivity and the magnetic conductivity cannot be simultaneously considered in the prior art, and provides a preparation method of spherical metal powder for additive manufacturing.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of spherical metal powder for additive manufacturing comprises the following steps:
s1, putting the raw master alloy into a smelting furnace, vacuumizing until the vacuum degree reaches 2x10-1Pa~10x10-1After Pa, when the alloy in the induction smelting furnace is melted and the air pressure reaches-0.05 Mpa to-0.03 Mpa, closing the vacuum-pumping system, introducing inert gas, smelting the alloy, introducing inert protective gas in the smelting process, standing for 20-25 min after the first smelting, and performing second smelting to ensure that the mother alloy phase is uniform;
s2, putting the molten metal into a tundish, presetting the outflow aperture at the bottom of the tundish to be 3-7 mm, effectively controlling the flow of the metal liquid, ensuring the particle size distribution of powder particles, starting an inert gas heating device, and heating atomized gas;
s3, introducing the molten metal into improved tightly-coupled vacuum gas atomization equipment through a flow guide pipe, atomizing and crushing the molten metal into a large number of fine liquid drops by high-pressure inert gas through a nozzle under the condition that the air pressure is 1-4 MPa, and solidifying the liquid into spherical powder particles in the flying process;
and S4, performing water-powder separation through filtering and pressing, drying, and performing air flow classification to obtain the 3D printing metal powder.
Preferably, in the step S3, the high-pressure inert gas may be one or a mixture of helium and argon.
The invention has the beneficial effects that:
1. the 3D printing metal powder prepared by the water atomization method has the prominent advantages of good sphericity, uniform particle size distribution, low oxygen content, good batch consistency and the like.
2. The invention adopts the improved vacuum atomization equipment, and has the advantages of low oxygen content of powder, good sphericity, fine granularity and high gas kinetic energy conversion rate. Is suitable for industrial production.
3. The atomizer provided by the invention adopts special materials and a reasonable structure (injection angle, air port and leakage nozzle width ratio, air inlet and outlet section ratio and air port shape), ensures the atomization efficiency, and solves the problem that the leakage nozzle is easy to block and the production is discontinuous.
In conclusion, the metal powder with smaller grain diameter can be obtained by impacting the molten metal flow with high-pressure water and high-pressure inert gas; the contact between water and metal powder is reduced, the oxygen content of the metal powder is effectively reduced, the improved tightly-coupled vacuum gas atomization equipment is utilized, the yield is improved, the preparation of the fine metal powder is very effective, the gas consumption is reduced, and the production cost is reduced.
Drawings
FIG. 1 is a microstructure of a metal powder according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1, a method of preparing a spherical metal powder for additive manufacturing, comprising the steps of:
s1, putting the raw master alloy into a smelting furnace, vacuumizing until the vacuum degree reaches 2x10-1After Pa, when the alloy in the induction smelting furnace is melted and the air pressure reaches-0.05 Mpa, closing the vacuum-pumping system, introducing inert gas, smelting the alloy, introducing inert protective gas in the smelting process, standing for 20min after the first smelting, and carrying out second smelting to ensure that the phase of the master alloy is uniform;
s2, putting the molten metal into a tundish, presetting the outflow aperture at the bottom of the tundish to be 3mm, effectively controlling the flow of the metal liquid, ensuring the particle size distribution of powder particles, starting an inert gas heating device, and heating atomized gas;
s3, introducing the molten metal into improved tightly-coupled vacuum gas atomization equipment through a guide pipe, atomizing and crushing the molten metal into a large number of fine liquid drops by a high-pressure inert gas (helium is selected as the high-pressure inert gas) through a nozzle under the condition that the air pressure is 1MPa, and solidifying the liquid into spherical powder particles in the flying process;
and S4, performing water-powder separation through filtering and pressing, drying, and performing air flow classification to obtain a 3D printing metal powder finished product I.
Embodiment 2, a method of preparing a spherical metal powder for additive manufacturing, comprising the steps of:
s1, putting the raw master alloy into a smelting furnace, vacuumizing until the vacuum degree reaches 6x10-1After Pa, when the alloy in the induction smelting furnace is melted and the air pressure reaches-0.04 Mpa, closing the vacuum-pumping system, introducing inert gas, smelting the alloy, introducing inert protective gas in the smelting process, standing for 23min after the first smelting, and carrying out second smelting to ensure that the phase of the master alloy is uniform;
s2, putting the molten metal into a tundish, presetting the outflow aperture at the bottom of the tundish to be 5mm, effectively controlling the flow of the metal liquid, ensuring the particle size distribution of powder particles, starting an inert gas heating device, and heating atomized gas;
s3, introducing the molten metal into improved tightly-coupled vacuum gas atomization equipment through a guide pipe, atomizing and crushing the molten metal into a large number of fine liquid drops by high-pressure inert gas (argon is selected as the high-pressure inert gas) through a nozzle under the condition that the air pressure is 2MPa, and solidifying the liquid into spherical powder particles in the flying process;
and S4, performing water-powder separation through filtering and pressing, drying, and performing air flow classification to obtain a 3D printing metal powder finished product II.
Embodiment 3, a method of preparing a spherical metal powder for additive manufacturing, comprising the steps of:
s1, putting the raw master alloy into a smelting furnace, vacuumizing until the vacuum degree reaches 10x10-1After Pa, when the alloy in the induction smelting furnace is melted and the air pressure reaches-0.03 Mpa, closing the vacuum-pumping system, introducing inert gas, smelting the alloy, introducing inert protective gas in the smelting process, standing for 25min after the first smelting, and carrying out second smelting to ensure that the phase of the master alloy is uniform;
s2, putting the molten metal into a tundish, presetting the outflow aperture at the bottom of the tundish to be 7mm, effectively controlling the flow of the metal liquid, ensuring the particle size distribution of powder particles, starting an inert gas heating device, and heating atomized gas;
s3, introducing the molten metal into improved tightly-coupled vacuum gas atomization equipment through a guide pipe, atomizing and crushing the molten metal into a large number of fine liquid drops through a nozzle by high-pressure inert gas (the high-pressure inert gas is selected to be mixed with helium and argon) under the condition that the air pressure is 4MPa, and solidifying the liquid into spherical powder particles in the flying process;
and S4, performing water-powder separation through filtering and pressing, drying, and performing air flow classification to obtain a 3D printing metal powder finished product III.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (2)

1. A preparation method of spherical metal powder for additive manufacturing is characterized by comprising the following steps:
s1, putting the raw master alloy into a smelting furnace, vacuumizing until the vacuum degree reaches 2x10-1Pa~10x10-1After Pa, when the alloy in the induction smelting furnace is melted and the air pressure reaches-0.05 Mpa to-0.03 Mpa, closing the vacuum-pumping system, introducing inert gas, smelting the alloy, introducing inert protective gas in the smelting process, standing for 20-25 min after the first smelting, and performing second smelting to ensure that the mother alloy phase is uniform;
s2, putting the molten metal into a tundish, presetting the outflow aperture at the bottom of the tundish to be 3-7 mm, effectively controlling the flow of the metal liquid, ensuring the particle size distribution of powder particles, starting an inert gas heating device, and heating atomized gas;
s3, introducing the molten metal into improved tightly-coupled vacuum gas atomization equipment through a flow guide pipe, atomizing and crushing the molten metal into a large number of fine liquid drops by high-pressure inert gas through a nozzle under the condition that the air pressure is 1-4 MPa, and solidifying the liquid into spherical powder particles in the flying process;
and S4, performing water-powder separation through filtering and pressing, drying, and performing air flow classification to obtain the 3D printing metal powder.
2. The method as claimed in claim 1, wherein in the step S3, the high-pressure inert gas is selected from helium, argon, or a mixture thereof.
CN202010853326.4A 2020-08-23 2020-08-23 Preparation method of spherical metal powder for additive manufacturing Pending CN111992728A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112517918A (en) * 2020-12-02 2021-03-19 青岛云路先进材料技术股份有限公司 Preparation method and production equipment of high-sphericity gas atomized powder
CN112828296A (en) * 2020-12-30 2021-05-25 中航迈特粉冶科技(固安)有限公司 Preparation method of chromium powder
CN113275577A (en) * 2021-04-20 2021-08-20 广州湘龙高新材料科技股份有限公司 Preparation method of zinc alloy additive
CN113369485A (en) * 2021-06-10 2021-09-10 盘星新型合金材料(常州)有限公司 Pilot-scale atomization furnace, Fe-based amorphous alloy powder and preparation method thereof
CN113414397A (en) * 2021-05-25 2021-09-21 鞍钢股份有限公司 Vacuum gas atomization continuous preparation method of iron-based metal powder
CN113547126A (en) * 2021-06-29 2021-10-26 鞍钢股份有限公司 Method for preparing fine powder by tight coupling gas atomization for preventing guide pipe from being blocked
CN114951667A (en) * 2022-05-27 2022-08-30 鞍钢股份有限公司 Method for preventing nozzle from being blocked in preparation of metal powder through gas atomization

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CN207806632U (en) * 2017-12-12 2018-09-04 广州纳联材料科技有限公司 Apparatus for preparing metal powder
CN109570519A (en) * 2019-01-31 2019-04-05 上海材料研究所 A kind of preparation method of the CoCrMo alloy powder for 3D printing
CN109750320A (en) * 2019-03-04 2019-05-14 张华宇 The method for preparing metal alloy powders is combined in atomization electrolysis
CN110480024A (en) * 2019-09-12 2019-11-22 陕西斯瑞新材料股份有限公司 A method of CuCrZr spherical powder is prepared based on VIGA technique
CN110666180A (en) * 2019-09-26 2020-01-10 安徽中体新材料科技有限公司 Preparation method of metal powder for 3D printing
US20200122237A1 (en) * 2018-08-23 2020-04-23 Beemetal Corp. Systems and methods for continuous production of gas atomized metal powders

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CN106166617A (en) * 2016-09-27 2016-11-30 中航迈特粉冶科技(北京)有限公司 A kind of preparation method of 3D printing titanium alloy powder
CN107876786A (en) * 2017-10-27 2018-04-06 湖南博锋新材料有限公司 A kind of method of oxidization of metal powder in reduction water atomization pulverization
CN207806632U (en) * 2017-12-12 2018-09-04 广州纳联材料科技有限公司 Apparatus for preparing metal powder
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CN109570519A (en) * 2019-01-31 2019-04-05 上海材料研究所 A kind of preparation method of the CoCrMo alloy powder for 3D printing
CN109750320A (en) * 2019-03-04 2019-05-14 张华宇 The method for preparing metal alloy powders is combined in atomization electrolysis
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112517918A (en) * 2020-12-02 2021-03-19 青岛云路先进材料技术股份有限公司 Preparation method and production equipment of high-sphericity gas atomized powder
CN112828296A (en) * 2020-12-30 2021-05-25 中航迈特粉冶科技(固安)有限公司 Preparation method of chromium powder
CN113275577A (en) * 2021-04-20 2021-08-20 广州湘龙高新材料科技股份有限公司 Preparation method of zinc alloy additive
CN113414397A (en) * 2021-05-25 2021-09-21 鞍钢股份有限公司 Vacuum gas atomization continuous preparation method of iron-based metal powder
CN113414397B (en) * 2021-05-25 2023-01-17 鞍钢股份有限公司 Vacuum gas atomization continuous preparation method of iron-based metal powder
CN113369485A (en) * 2021-06-10 2021-09-10 盘星新型合金材料(常州)有限公司 Pilot-scale atomization furnace, Fe-based amorphous alloy powder and preparation method thereof
CN113547126A (en) * 2021-06-29 2021-10-26 鞍钢股份有限公司 Method for preparing fine powder by tight coupling gas atomization for preventing guide pipe from being blocked
CN114951667A (en) * 2022-05-27 2022-08-30 鞍钢股份有限公司 Method for preventing nozzle from being blocked in preparation of metal powder through gas atomization

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Application publication date: 20201127