CN116352094A - Preparation method of superfine alloy powder - Google Patents

Preparation method of superfine alloy powder Download PDF

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Publication number
CN116352094A
CN116352094A CN202310574073.0A CN202310574073A CN116352094A CN 116352094 A CN116352094 A CN 116352094A CN 202310574073 A CN202310574073 A CN 202310574073A CN 116352094 A CN116352094 A CN 116352094A
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Prior art keywords
alloy
inert gas
powder
alloy powder
gas
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CN202310574073.0A
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Inventor
钱铸
闫祖鹏
高莹
王高红
王师会
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Tianjin Zhujin Technology Development Corp
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Tianjin Zhujin Technology Development Corp
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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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making 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
    • B22F9/082—Making 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
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making 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
    • B22F9/082—Making 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
    • B22F2009/0844—Making 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 in controlled atmosphere
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making 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
    • B22F9/082—Making 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
    • B22F2009/0848—Melting process before atomisation
    • 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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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention provides a preparation method of superfine alloy powder, which belongs to the technical field of alloy powder preparation, and in a high-purity inert gas environment, alloy coarse powder is heated by laser and then melted to form alloy liquid drops; alloy liquid drops fall into an air flow impact area under the action of gravity and are impacted by high-purity inert gas air flow to form atomized liquid drops; the atomized droplets cool to form ultrafine alloy powder. The invention uses laser as heating source, primary gas atomization coarse powder is used as raw material, the laser heating and re-atomization process can rapidly heat coarse powder generated in the common inert gas atomization process, and the high-purity inert gas is blown for further atomization to form finer atomized molten drops, so as to prepare the ultrafine powder material with low oxygen content and high fluidity.

Description

Preparation method of superfine alloy powder
Technical Field
The invention belongs to the technical field of alloy powder preparation, and particularly relates to a preparation method of superfine alloy powder.
Background
The preparation of the alloy powder is mainly divided into a mechanical method and a chemical method, wherein the mechanical method is divided into a ball milling method and an atomization method, and the chemical method is divided into a carbonyl method and a chemical deposition method. The powder prepared by the atomization method in the methods has high production efficiency and less environmental pollution, and is the main production process of the alloy powder at present. The traditional water (gas) atomization technology mainly comprises a smelting part and an atomization nozzle part, wherein the smelting part is responsible for smelting metal and pouring the metal through a runner to form molten metal liquid flow, the atomization part sprays water (water atomization) and gas (gas atomization) to crush the molten metal liquid flow to form fine molten drops, and the fine molten drops are cooled to form atomized powder. As shown in fig. 1. As the powder granularity produced by the atomization method is linearly distributed, for the water atomization process, the atomization water pressure can be increased, and the high-pressure crushing and atomization are carried out to obtain the water atomization powder with finer whole, but the water atomization powder has different morphologies and poor fluidity, and is generally difficult to be applied to the process fields of laser cladding, remanufacturing, 3D printing and the like. The inert gas atomization powder making technology has the advantages that the cooling speed is low, the molten liquid is easy to ball in the atomization and crushing process, so that the prepared powder has good fluidity, but the difficulty of increasing the gas pressure is high, so that the powder prepared by the gas atomization powder making technology is generally coarser.
Along with the development of 3d printing technology, MIM technology and other technologies, the application of fine powder is increasing, and the fine powder is prepared by an atomization method, particularly an aerosol method, and can only be finished by adopting a plurality of repeated processes of smelting and atomizing and sieving. The times of melting in the furnace are very large, the problems of burning loss, oxidation and the like are caused during the process, the quality of the atomized fine powder is reduced for many times, and meanwhile, energy is wasted greatly due to the fact that the fine powder is melted for many times. The phase change promotes the cost of fine powder and creates a bottleneck for the development of 3d printing technology, MIM technology and the like.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a preparation method of superfine alloy powder, which uses laser as a heating source, primary gas atomization coarse powder is used as a raw material, the laser heating and re-atomization process can rapidly heat coarse powder generated in the common inert gas atomization process again, and fine atomized molten drops are formed by measuring and blowing high-purity inert gas for further atomization, so that the superfine powder material with low oxygen content and high fluidity is prepared.
The technical scheme adopted by the invention is as follows: in the high-purity inert gas environment, the coarse alloy powder is heated by laser and then melted to form alloy liquid drops; alloy liquid drops fall into an air flow impact area under the action of gravity and are impacted by high-purity inert gas air flow to form atomized liquid drops; the atomized droplets cool to form ultrafine alloy powder.
Further, the laser beam emitted by the semiconductor laser is focused through the lens, the alloy coarse powder is sprayed to the laser beam focus by the coarse powder spray nozzle, and the alloy liquid drops are formed by melting at the laser beam focus.
Further, the semiconductor laser emits laser beams vertically downwards, and the included angle between the center line of the coarse powder nozzle and the vertical direction is 30-60 degrees.
Further, the laser power is 1000-4000W, the wavelength of the semiconductor laser is 900-1000nm, the powder feeding speed of the alloy coarse powder is 2.5-20kg/h, and the particle size D50 of the coarse powder is more than 100 meshes.
Further, the focal length of the lens is 150-300mm.
Further, the high-purity inert gas sprayed from the gas nozzle forms high-purity inert gas flow, and the gas pressure of the gas nozzle is 0.1-0.8Mpa.
Further, the included angle between the central line of the gas nozzle and the horizontal plane is 30-60 degrees.
Further, the intersection of the center line of the gas jet and the liquid drop is 5-6mm below the laser beam focus.
Further, the high purity inert gas environment is provided by a high purity inert gas cartridge.
Further, the high-purity inert gas is high-purity nitrogen or high-purity argon with the gas purity not less than 99.999%.
Further, the equipment can achieve a theoretical working time of 7 x 24 h.
Compared with the prior art, the invention has the following beneficial effects:
1. compared with the traditional atomization, the molten metal in the invention is obtained by directly placing the process coarse powder into a laser area and instantly heating and liquefying the process coarse powder, and no special part of the molten metal exists. The traditional atomization technology needs a molten metal container which needs to resist the high temperature of about 1700 ℃, special refractory materials are needed, and 7 x 24h continuous operation cannot be achieved due to the limited service life of the refractory materials. The invention adopts laser instant heating and then atomizing by airflow, and does not use a container for holding molten metal, so that theoretical working time of 7 x 24h can be easily achieved.
2. The gas pressure used by the invention is 0.1-0.8Mpa, which is far less than the powder making pressure above 10Mpa in the traditional gas atomization, so that the whole powder making process is safer. Meanwhile, under the condition of low nozzle pressure, the coarse powder material with the granularity distribution D50 being more than 150 microns is atomized into the superfine powder material with the granularity being less than 45 microns, and the powder with the granularity being less than 45 microns obtained by one-time pulverization exceeds 90 percent, so that the subdivision yield is high. The flowability index of the obtained powder material is less than 25s/50g.
3. The whole melting and atomizing processes of the invention are all carried out in high-purity inert gas, so that the oxygenation of powder is extremely low in the whole pulverizing process, the content of iron-based materials is generally not more than 500ppm, and the content of nickel-based materials and cobalt-based materials is less than 300ppm.
4. The invention adopts atomized coarse powder as raw material, omits the coarse powder furnace returning process, saves the consumption of secondary furnace returning, and reduces smelting times on the basis of obtaining the same powder material.
Drawings
FIG. 1 is a schematic illustration of an implementation of a prior art water (gas) atomization technique;
FIG. 2 is a schematic illustration of an embodiment of the present invention;
FIG. 3 is a graph showing the results of the analysis of the fine powder particle size of the coarse powder of the 316L alloy of example 1 of the present invention;
FIG. 4 is a graph showing the result of analysis of the fine powder particle size of the ultra-fine alloy powder produced in example 1 of the present invention;
FIG. 5 is a graph showing the results of the analysis of the fine powder particle size of FeSi6.5 alloy coarse powder of example 2 of the present invention;
FIG. 6 is a graph showing the result of analysis of the fine powder particle size of the ultrafine alloy powder obtained in example 2 of the present invention.
In the figure: 1-laser beam, 2-lens, 3-coarse powder nozzle, 4-alloy liquid drop, 5-gas nozzle and 6-atomized liquid drop.
Detailed Description
The present invention will be described in detail below with reference to the drawings and the specific embodiments, so that those skilled in the art can better understand the technical solutions of the present invention.
Example 1
The embodiment of the invention provides a preparation method of superfine alloy powder, which is carried out in a high-purity inert gas environment in the whole process as shown in fig. 2, wherein the high-purity inert gas environment is provided by a high-purity inert gas bin. The high-purity inert gas is high-purity nitrogen with the gas purity not less than 99.999 percent. The semiconductor laser, the lens 2, the coarse powder nozzle 3 and the gas nozzle 5 are arranged in the high-purity inert gas bin. The semiconductor laser is adjusted to emit a laser beam 1 vertically downwards with a laser power of 4000W. The lens 2 is located directly below the semiconductor laser, and the focal length b of the lens 2 is 300mm. The coarse powder nozzle 3 is arranged on the side surface below the lens 2, the included angle alpha between the central line of the coarse powder nozzle 3 and the vertical direction is 60 degrees, and the powder feeding speed of the alloy coarse powder is 10kg/h. The gas jet 5 is arranged below the coarse powder jet 3, the included angle beta between the central line of the gas jet 5 and the horizontal plane is 30 degrees, the distance a between the intersection of the central line of the gas jet 5 and the alloy liquid drop 4 and lower than the focal point of the laser beam is 5mm, and the air pressure of the gas jet 5 is 0.5Mpa.
The semiconductor laser emits a laser beam 1 vertically downwards, the laser beam 1 emitted by the semiconductor laser is focused through a lens 2, the alloy coarse powder is sprayed to a laser beam focus through a coarse powder spray orifice 3, and after being heated by the laser beam 1, the alloy coarse powder is melted to form alloy liquid drops 4. The high purity inert gas is ejected from the gas nozzle 5, and a gas flow impact area is formed in front of the gas nozzle 5. Alloy liquid drops 4 fall into an air flow impact area under the action of gravity and are impacted by high-purity inert gas air flow to form atomized liquid drops 6; the atomized liquid drops 6 continue to fall, and cool during the falling process to form ultrafine alloy powder.
The alloy meal in this example was 316L alloy meal, the meal size is shown in fig. 3, and the alloy meal D50 is 280 microns. The particle size analysis is carried out on the prepared superfine alloy powder by adopting a Markov 3000 laser particle sizer, the particle size distribution is shown in figure 4, the volume median D (50) of the superfine alloy powder is 33.7 microns, and the particle size is finer.
Oxygen content analysis was performed ON the alloy Jin Cufen and the ultrafine alloy powder by LECO company ON736 oxygen nitrogen analyzer, and 3 groups of alloy coarse powder and ultrafine alloy powder were measured respectively. As shown in Table 1, the average oxygenation in the pulverizing process was 90ppm.
TABLE 1 test table of oxygen content of 316L before and after pulverizing
Oxygen content PPM Group 1 Group 2 Group 3 Average value of
Coarse powder of alloy 300 340 350 330
Superfine alloy powder 400 420 440 420
The fluidity of the prepared superfine alloy powder is tested by adopting a standard funnel method for measuring the fluidity of GB 1482-2010-T metal powder, and the fluidity is 19.2s/50g after 3 times of testing and taking an average value.
Example 2
The embodiment of the invention provides a preparation method of superfine alloy powder, which is carried out in a high-purity inert gas environment in the whole process as shown in fig. 2, wherein the high-purity inert gas environment is provided by a high-purity inert gas bin. The high-purity inert gas is high-purity argon with the gas purity not less than 99.999 percent. The semiconductor laser, the lens 2, the coarse powder nozzle 3 and the gas nozzle 5 are arranged in the high-purity inert gas bin. The semiconductor laser is adjusted to emit a laser beam 1 vertically downwards with a laser power of 4000W. The lens 2 is located directly below the semiconductor laser, and the focal length b of the lens 2 is 300mm. The coarse powder nozzle 3 is arranged on the side surface below the lens 2, the included angle alpha between the central line of the coarse powder nozzle 3 and the vertical direction is 30 degrees, and the powder feeding speed of the alloy coarse powder is 8kg/h. The gas jet 5 is arranged below the coarse powder jet 3, the included angle beta between the central line of the gas jet 5 and the horizontal plane is 60 degrees, the distance a between the intersection of the central line of the gas jet 5 and the alloy liquid drop 4 and lower than the focal point of the laser beam is 6mm, and the air pressure of the gas jet 5 is 0.3Mpa.
The semiconductor laser emits a laser beam 1 vertically downwards, the laser beam 1 emitted by the semiconductor laser is focused through a lens 2, the alloy coarse powder is sprayed to a laser beam focus through a coarse powder spray orifice 3, and after being heated by the laser beam 1, the alloy coarse powder is melted to form alloy liquid drops 4. The high purity inert gas is ejected from the gas nozzle 5, and a gas flow impact area is formed in front of the gas nozzle 5. Alloy liquid drops 4 fall into an air flow impact area under the action of gravity and are impacted by high-purity inert gas air flow to form atomized liquid drops 6; the atomized liquid drops 6 continue to fall, and cool during the falling process to form ultrafine alloy powder.
The alloy coarse powder in this example was FeSi6.5 alloy coarse powder, the coarse powder particle size is shown in FIG. 5, and the alloy coarse powder D50 is 252 microns. The particle size analysis is carried out on the prepared superfine alloy powder by adopting a Markov 3000 laser particle sizer, the particle size distribution is shown in figure 6, the volume median D (50) of the superfine alloy powder is 35.5 microns, and the particle size is finer.
Oxygen content analysis was performed ON the alloy Jin Cufen and the ultrafine alloy powder by LECO company ON736 oxygen nitrogen analyzer, and 3 groups of alloy coarse powder and ultrafine alloy powder were measured respectively. As shown in Table 2, the average aeration rate in the pulverizing process was 3.3ppm.
TABLE 2 test table of oxygen content of 316L before and after pulverizing
Oxygen content PPM Group 1 Group 2 Group 3 Average value of
Coarse powder of alloy 300 350 360 336.7
Superfine alloy powder 290 360 370 340
The fluidity of the prepared superfine alloy powder is tested by adopting a standard funnel method for measuring the fluidity of GB 1482-2010-T metal powder, and the fluidity of the superfine alloy powder is 20s/50g after 3 times of testing and averaging.
The present invention has been described in detail by way of examples, but the description is merely exemplary of the invention and should not be construed as limiting the scope of the invention. The scope of the invention is defined by the claims. In the technical scheme of the invention, or under the inspired by the technical scheme of the invention, similar technical schemes are designed to achieve the technical effects, or equivalent changes and improvements to the application scope are still included in the protection scope of the patent coverage of the invention.

Claims (10)

1. A preparation method of superfine alloy powder is characterized in that in a high-purity inert gas environment, alloy coarse powder is heated by laser and then melted to form alloy liquid drops; alloy liquid drops fall into an air flow impact area under the action of gravity and are impacted by high-purity inert gas air flow to form atomized liquid drops; the atomized droplets cool to form ultrafine alloy powder.
2. The method for preparing ultrafine alloy powder according to claim 1, wherein the laser beam emitted from the semiconductor laser is focused by a lens, and the coarse powder of the alloy is sprayed from a coarse powder nozzle toward a laser beam focus, and melted at the laser beam focus to form the alloy droplet.
3. The method for preparing ultrafine alloy powder according to claim 2, wherein the semiconductor laser emits a laser beam vertically downward, and the angle between the center line of the coarse powder nozzle and the vertical direction is 30-60 °.
4. The method for preparing ultrafine alloy powder according to claim 3, wherein the semiconductor laser has a wavelength of 900-1000nm, a laser power of 1000-4000W, a powder feeding speed of 2.5-20kg/h, and a coarse powder particle diameter D50 of more than 100 meshes.
5. The method for preparing ultrafine alloy powder according to claim 2, wherein the focal length of the lens is 150-300mm.
6. The method for preparing ultrafine alloy powder according to claim 1, wherein the high-purity inert gas ejected from the gas nozzle forms a high-purity inert gas flow, and the gas nozzle has a gas pressure of 0.1 to 0.8Mpa.
7. The method of producing ultrafine alloy powder according to claim 6, wherein the angle between the center line of the gas jet and the horizontal plane is 30 ° to 60 °.
8. The method of producing ultrafine alloy powder according to claim 6, wherein the intersection of the center line of the gas jet and the droplet is 5-6mm below the focal point of the laser beam.
9. The method of producing ultra-fine alloy powder according to claim 1, wherein the high purity inert gas atmosphere is provided by a high purity inert gas silo.
10. The method for producing an ultrafine alloy powder according to claim 1, wherein the high-purity inert gas is high-purity nitrogen or high-purity argon having a gas purity of not less than 99.999%.
CN202310574073.0A 2023-05-22 2023-05-22 Preparation method of superfine alloy powder Pending CN116352094A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117753979A (en) * 2024-02-22 2024-03-26 西安赛隆增材技术股份有限公司 Device for preparing metal powder with fine particle size by using coarse powder and application method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117753979A (en) * 2024-02-22 2024-03-26 西安赛隆增材技术股份有限公司 Device for preparing metal powder with fine particle size by using coarse powder and application method thereof
CN117753979B (en) * 2024-02-22 2024-05-10 西安赛隆增材技术股份有限公司 Device for preparing metal powder with fine particle size by using coarse powder and application method thereof

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