CN111014701B - Method for preparing high-conductivity metal powder by electrode induction melting gas atomization method - Google Patents
Method for preparing high-conductivity metal powder by electrode induction melting gas atomization method Download PDFInfo
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- CN111014701B CN111014701B CN201911304508.XA CN201911304508A CN111014701B CN 111014701 B CN111014701 B CN 111014701B CN 201911304508 A CN201911304508 A CN 201911304508A CN 111014701 B CN111014701 B CN 111014701B
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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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- B22F2009/0848—Melting process before atomisation
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Abstract
The invention discloses a method for preparing high-conductivity metal powder by an electrode induction melting gas atomization method, which comprises the following steps: (1) putting a prepared alumina funnel into an induction coil in atomization equipment; (2) then placing the graphite funnel in the alumina funnel; (3) loading a high-conductivity metal bar with a specific size into atomizing equipment; (4) vacuumizing the equipment, and then filling high-purity argon as protective gas; (5) heating and melting a high-conductivity metal bar through an induction coil, and then atomizing to prepare powder; (6) and after the powder is cooled, taking the powder out of the powder collecting tank. The invention improves the electrode induction smelting gas atomization device, adds the graphite funnel which can be inductively heated and can be used as an auxiliary reinforcing heat source, thereby realizing the preparation of the electrode induction smelting gas atomization method of high-conductivity metal powder, and the powder has no pollution and high purity.
Description
Technical Field
The invention belongs to the field of metal powder preparation, and particularly relates to a method for preparing high-conductivity metal powder by an electrode induction melting gas atomization method.
Background
The 3D printing technology, also known as additive manufacturing, is a new technology that is completely different from traditional "subtractive manufacturing" technologies such as machining. The manufacturing technology can realize the manufacturing of complex structural parts without traditional tools or dies, can effectively simplify the production process, shortens the manufacturing period, and particularly can be combined with personalized design to manufacture the structural parts with complex shapes. Therefore, the 3D printing technology has become a hot research problem in the aerospace and medical fields. In order to meet the process requirements of metal 3D printing, the metal powder has the characteristics of low nitrogen and oxygen content, high purity, narrow particle size distribution interval, good sphericity and the like. Wherein, the purity of the metal powder has certain influence on the performance research of the 3D printed metal implant.
At present, metal powder for 3D printing is generally prepared by an air atomization method. The gas atomization method mainly comprises vacuum induction melting gas atomization (VIGA) with a crucible and electrode induction melting gas atomization (EIGA) without a crucible. Metal powder with low melting point and low superheat degree is usually prepared by a VIGA method, however, the method cannot avoid the contact of liquid metal and a crucible in the smelting process, and atomized powder contains nonmetallic inclusions, so that the purity of the powder is reduced, and the requirements of aerospace and medical 3D printing cannot be met.
Because the electrode induction melting gas atomization (EIGA) method does not need a crucible in the melting process, the pollution of molten metal can be effectively avoided, and the quality of metal powder is further improved. However, compared with the smelting of titanium alloy, the EIGA method has slow heat generation for metals with high conductivity due to small resistivity, strong conductivity and small eddy current loss, and the smelting of pure copper bars and silver bars with the same specification requires higher power and longer heating time, even cannot be melted, thus causing resource loss and waste.
Disclosure of Invention
The invention aims to provide a method for preparing high-conductivity metal powder by an electrode induction melting gas atomization method, which solves the problem that EIGA equipment cannot normally melt high-conductivity metal materials, and obtains high-purity metal powder required by aerospace and medical 3D printing industries.
The technical solution for realizing the purpose of the invention is as follows: a method for preparing high-conductivity metal powder by an electrode induction smelting gas atomization method is characterized in that an electrode induction smelting gas atomization device is improved, an aluminum oxide funnel and a graphite funnel are added, the aluminum oxide funnel serves as an insulation protection device, the graphite funnel serves as an auxiliary reinforcing heat source, the aluminum oxide funnel is arranged in the graphite funnel, heating and melting of a high-conductivity metal bar are achieved, the bar is not contacted with any medium in the melting and liquid flow dropping processes, atomization equipment is vacuumized firstly and then filled with argon, and 3-5 MPa argon gas flow is used for impacting metal liquid to form fine powder particles in the atomization process.
Furthermore, the high-conductivity metal bar is made of bars of pure copper, silver, gold and the like.
Furthermore, the inner diameter of a large opening of the alumina funnel is 64-68 mm, the inner diameter of a small opening of the alumina funnel is 18-22 mm, and the thickness of the alumina funnel is 3-4 mm.
Furthermore, the inner diameter of a large opening of the graphite funnel is 56-60 mm, the inner diameter of a small opening of the graphite funnel is 10-14 mm, and the thickness of the graphite funnel is 3-4 mm.
Further, the degree of vacuum was 7.6X 10-3Pa or less.
Compared with the prior art, the invention has the remarkable advantages that:
(1) the electrode induction smelting gas atomization device is improved, an aluminum oxide funnel and a graphite funnel are added, the aluminum oxide funnel is used as an insulation protection device, and the graphite funnel is used as an auxiliary reinforcing heat source, so that the electrode induction smelting gas atomization method preparation of high-conductivity metal powder such as pure copper, silver, gold and the like is realized.
(2) The prepared powder has the advantages of no pollution, high purity and the like.
(3) Can meet the requirements of 3D printing of medical metal implants, aerospace components and the like on high-purity metal powder.
Drawings
Fig. 1 is a structural schematic diagram of an electrode induction melting gas atomization device after improvement.
FIG. 2 is a macro topography of the silver powder prepared by the present invention.
In the figure, 1 is an induction coil, 2 is an alumina funnel, 3 is a graphite funnel, and 4 is a metal bar.
Detailed Description
Referring to fig. 1, a method for preparing high-conductivity metal powder by an electrode induction melting gas atomization method comprises the following steps:
step one, the manufactured alumina funnel 2 is placed into an induction coil 1, the inner diameter of a large opening of the alumina funnel 2 is 64-68 mm, the inner diameter of a small opening of the alumina funnel 2 is 18-22 mm, and the thickness of the alumina funnel is 3-4 mm.
And step two, placing the manufactured graphite funnel 3 in the alumina funnel 2, so that the graphite funnel 3 can be prevented from being in direct contact with the induction coil 1, and the induction coil 1 can be prevented from being damaged during heating. The graphite funnel 3 has a large opening with an inner diameter of 56-60 mm, a small opening with an inner diameter of 10-14 mm and a thickness of 3-4 mm.
And step three, filling high-conductivity metal bars 4 of pure copper, silver, gold and the like with specific dimensions into the atomization equipment.
Step four, vacuumizing the equipment until the vacuum degree reaches 7.6 multiplied by 10-3Pa or lessAnd introducing high-purity argon as a protective gas to prevent the powder from being oxidized.
And fifthly, heating and melting the high-conductivity metal bar 4 through the induction coil 1, enabling molten liquid flow to freely drop, and then atomizing to prepare powder, wherein argon is used as atomizing gas, and the air pressure is controlled to be 3-5 MPa.
And step six, after the powder is cooled, taking the powder out of the powder collecting tank, screening according to the particle size range, and packaging.
The present invention is further illustrated by the following examples.
Example 1
The method for preparing the high-conductivity metal powder by adopting the electrode induction melting gas atomization method provided by the invention is used for preparing the pure copper powder, and the method comprises the following specific steps:
step one, placing the manufactured alumina funnel 2 into an induction coil 1, wherein the inner diameter of a large opening of the alumina funnel is 66mm, the inner diameter of a small opening of the alumina funnel is 20mm, and the thickness of the alumina funnel is 4 mm.
And step two, placing the manufactured graphite funnel 3 into an alumina funnel 2, wherein the inner diameter of a large opening of the graphite funnel is 60mm, the inner diameter of a small opening of the graphite funnel is 14mm, and the graphite funnel is 3mm thick.
And step three, filling pure copper bars 4 with specific sizes into the atomization equipment.
Step four, vacuumizing the equipment until the vacuum degree reaches 7.6 multiplied by 10-3And (4) delivering argon below Pa to ensure that the air pressure in the smelting chamber and the atomizing chamber is equal to the standard atmospheric pressure, and filling the argon as a protective gas to prevent the powder from being oxidized.
And fifthly, heating and melting the pure copper bar 4 through the induction coil 1, enabling molten liquid flow to freely drop, and then atomizing to prepare powder, wherein argon is selected as atomizing gas, and the air pressure is controlled to be 3-5 MPa.
Step six, after the atomization is finished and the powder is cooled, collecting 3130g of powder from the powder collecting tank, sieving the powder in sieves of minus 80M, plus 80M minus 250M and plus 250M minus M, respectively, weighing 215g, 1206g and 1709g after sieving, filling the powder into different containing bottles and storing the powder in vacuum. The fine powder rate of the pure copper powder prepared by the invention is 54.60% below 250M.
Example 2
The method for preparing the silver powder by adopting the electrode induction melting gas atomization method comprises the following specific steps:
step one, the manufactured alumina funnel 2 is placed in an induction coil 1, the inner diameter of a large opening of the alumina funnel is 64mm, the inner diameter of a small opening of the alumina funnel is 18mm, and the thickness of the alumina funnel is 4 mm.
And step two, placing the manufactured graphite funnel 3 into an alumina funnel 2, wherein the inner diameter of a large opening of the graphite funnel is 58mm, the inner diameter of a small opening of the graphite funnel is 12mm, and the graphite funnel is 3mm thick.
And step three, filling silver rods 4 with specific sizes into the atomization equipment.
Step four, vacuumizing the equipment until the vacuum degree reaches 7.6 multiplied by 10-3And (4) delivering argon below Pa to ensure that the air pressure in the smelting chamber and the atomizing chamber is equal to the standard atmospheric pressure, and filling the argon as a protective gas to prevent the powder from being oxidized.
And fifthly, heating and melting the silver bar 4 through the induction coil 1, enabling the molten liquid flow to freely drop, and then atomizing to prepare powder, wherein argon is selected as atomizing gas, and the air pressure is controlled to be 3-5 MPa.
Step six, after the atomization is finished and the powder is cooled, 4603g of powder is collected from the powder collecting tank, sieved in screens of +/-80M, +80M/-250M and + 250M/-M, weighed after sieving are 361g, 1883g and 2359g, and filled into different containing bottles and stored in vacuum. The fine powder rate of the silver powder prepared by the invention is 51.25% below 250M.
FIG. 2 is a macro-morphology diagram of silver powder prepared by electrode induction melting gas atomization method. Therefore, the silver powder prepared by the method has the advantages of high sphericity, good fluidity, narrow particle size range and the like.
Claims (1)
1. A method for preparing high-conductivity metal powder by an electrode induction melting gas atomization method is characterized by comprising the following steps: electrode induction melting gas atomization device has improved, alumina funnel and graphite funnel have been increased, alumina funnel is as insulation protection device, the graphite funnel is as supplementary reinforcing heat source, the graphite funnel is arranged in the alumina funnel, thereby realized the heating and the melting of high conductivity metal rod, the rod melts, the in-process that the liquid stream drips does not contact with any medium, atomization plant evacuation earlier, the back argon gas that fills, utilize 3~5MPa argon gas air current impact metal liquid to become tiny powder granule in the atomizing process, specifically as follows:
the method comprises the following steps that firstly, a manufactured alumina funnel (2) is placed into an induction coil (1), the inner diameter of a large opening of the alumina funnel (2) is 64-68 mm, the inner diameter of a small opening of the alumina funnel is 18-22 mm, and the thickness of the alumina funnel is 3-4 mm;
secondly, placing the manufactured graphite funnel (3) in an alumina funnel (2) to prevent the graphite funnel (3) from directly contacting with an induction coil (1) to damage the induction coil (1) during heating; the inner diameter of a large opening of the graphite funnel (3) is 56-60 mm, the inner diameter of a small opening is 10-14 mm, and the thickness is 3-4 mm;
step three, loading a high-conductivity metal bar (4) with a specific size into atomization equipment;
step four, vacuumizing the equipment until the vacuum degree reaches 7.6 multiplied by 10-3Introducing high-purity argon as a protective gas below Pa to prevent the powder from being oxidized;
fifthly, heating and melting the high-conductivity metal bar (4) through the induction coil (1), enabling molten liquid flow to freely drop, and then atomizing to prepare powder, wherein argon is used as atomizing gas, and the air pressure is controlled to be 3-5 MPa;
and step six, after the powder is cooled, taking the powder out of the powder collecting tank, screening according to the particle size range, and packaging.
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| JPH09302403A (en) * | 1996-05-13 | 1997-11-25 | Asahi Chem Ind Co Ltd | Novel fine powder of copper alloy, and its manufacture |
| US20080277265A1 (en) * | 2007-05-11 | 2008-11-13 | Plasco Energy Group, Inc. | Gas reformulation system comprising means to optimize the effectiveness of gas conversion |
| CN101328072A (en) * | 2008-08-04 | 2008-12-24 | 西峡龙成特种材料有限公司 | Furnace brick lining of large-sized vacuum intermediate frequency induction smelting furnance and making method thereof |
| CN103359768B (en) * | 2012-04-06 | 2016-08-10 | 周俊和 | A kind of Electric furnace for production of fluoride salt induction coil mounting structure |
| CN104501580A (en) * | 2014-12-01 | 2015-04-08 | 咸阳华光窑炉设备有限公司 | Electric-heating ultrahigh-temperature internal heating type rotary kiln |
| CN104588671B (en) * | 2015-01-09 | 2017-04-05 | 中国久远高新技术装备公司 | The metal powder preparation method and device of contactless melting are heated based on straight resistance |
| CN206106337U (en) * | 2016-11-01 | 2017-04-19 | 郭锦宏 | Induction heating's quick shaping consumptive material regeneration machine |
| CN209598210U (en) * | 2019-02-27 | 2019-11-08 | 马鞍山新康达磁业有限公司 | A kind of atomization of close coupling is let slip a remark system |
| CN110480024B (en) * | 2019-09-12 | 2022-05-17 | 陕西斯瑞新材料股份有限公司 | Method for preparing CuCrZr spherical powder based on VIGA process |
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