AU2020101398A4 - Process for ultrasonically exciting aluminum/salt mixed melt to prepare aluminum or aluminum alloy powder - Google Patents
Process for ultrasonically exciting aluminum/salt mixed melt to prepare aluminum or aluminum alloy powder Download PDFInfo
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- AU2020101398A4 AU2020101398A4 AU2020101398A AU2020101398A AU2020101398A4 AU 2020101398 A4 AU2020101398 A4 AU 2020101398A4 AU 2020101398 A AU2020101398 A AU 2020101398A AU 2020101398 A AU2020101398 A AU 2020101398A AU 2020101398 A4 AU2020101398 A4 AU 2020101398A4
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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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
- B22F2009/065—Melting inside a liquid, e.g. making spherical balls
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Abstract
The present invention discloses a process for ultrasonically exciting aluminum (Al)/salt
mixed melt to prepare Al or Al alloy powder, and belongs to the field of metal powder
preparation. The method uses water-soluble salts and Al alloy as raw materials. Salt
mixture and Al alloy are molten; immiscible salt and Al alloy are sonicated and excited;
ultrasonically, Al alloy melt is dispersed into fine spherical Al alloy droplets and
distributed in the molten salt; then, the molten salt is cooled and solidified rapidly to
obtain solidified molten salt distributing fine spherical Al alloy (Al) powders; the salt
mixture is dissolved in pure water and dried to obtain spherical Al alloy powders. The
method uses the effect of ultrasound to disperse liquid Al alloy as fine spherical droplets
into the molten salt, and then cools the molten salt containing Al alloy droplets to obtain
spherical Al alloy powders. Intense ultrasonication ensures the preparation of
micron-sized fine spherical Al alloy powders.
1/2
1
FIG1
Regulus 10O.0kV 8.7mm x50 LM(L) 06/01/2018 14:37 1.00mm
FIG 2
Description
1/2
1
FIG1
Regulus 10O.0kV 8.7mm x50 LM(L) 06/01/2018 14:37 1.00mm FIG 2
[0001] The present invention relates to the field of metal powder preparation, and in particular to a process for ultrasonically exciting mixed melt to prepare spherical aluminum (Al) or Al alloy powder using molten salt and Al or Al alloy as materials.
[0002] Al and Al alloy powders are widely used in powder metallurgy, injection molding, metal 3D printing, combustion improvers, dyes, etc. In fields of powder metallurgy and 3D printing, powders are required to be of high sphericity and extremely low oxygen content. Higher sphericity and lower oxygen content of powders lead to higher densification and performance of final powder metallurgy products and 3D printed parts. So far, processes for preparing metal powders principally cover mechanical crushing and ball milling process, electrolytic reduction process, atomization process, rotating electrode process, plasma atomization process, and ultrasonic atomization process.
[0003] Among the existing processes, gas atomization process is the most commonly used process for preparing metal powders, including gas atomization and water atomization processes, but the water atomization process cannot be used in preparing such active metal powders as Al alloy and magnesium alloy. In the field of atomization, metal powders prepared by the gas atomization process have excellent sphericity; however, atomization process fails to avoid satellite formation, leading to a phenomenon that a plurality of small pellets agglomerated around a spherical powder. Because the Al alloy is active, it is necessary to use highly pure inert argon or nitrogen as atomization gas in the process of atomization in order to avoid oxidation, greatly increasing preparation costs; moreover, the problem of oxidation of metal powders has not been well addressed yet.
[0004] In general, ultrasonic atomization can improve the sphericity of powder. So far, ultrasonic methods can usually be classified into two classes: one is ultrasound-assisted atomization, and the other is ultrasonic vibration-assisted atomization. Class I includes ultrasound-assisted gas atomization process and ultrasonic plasma atomization process. Class II, i.e., ultrasonic vibration-assisted atomization, usually spreads a molten metal on the surface of an ultrasonic vibration tool, and breaks the molten metal into droplets for atomization by means of interfacial waves generated by ultrasonic vibration; in addition, there is a ultrasonic standing wave atomization process. Relative to conventional gas atomization process, metal powders prepared by the above ultrasonic atomization processes have shown an improvement in sphericity. However, all the above ultrasonic atomization processes require high vacuum and inert gas consumption to avoid metal oxidation; particularly, preparation of powders of such active metal as Al alloy needs more costs to ensure low oxygen content of powders.
[0005] In view of this, the present invention provides a process for ultrasonically exciting Al/salt mixed melt to prepare spherical Al alloy powder. The method uses the effect of ultrasound to disperse molten Al alloy as fine spherical droplets into molten salt, and subsequently cools the molten salt containing Al alloy droplets to obtain spherical Al alloy powders. Intense ultrasonication ensures the preparation of micron-sized fine spherical Al alloy powders.
[0006] The technical solution adopted by the invention to solve the technical problem is as follows:
A process for ultrasonically exciting Al/salt mixed melt to prepare Al or Al alloy powder is provided, including the following steps:
1) blending: separately weighing desired water-soluble salts in mass percentage, mixing the weighed water-soluble salts well, drying to obtain a salt mixture, and weighing a material to be prepared in mass percentage, wherein the material to be prepared is Al or Al alloy;
2) smelting: first, placing the salt mixture obtained in step 1) in a crucible and heating until molten; then, adding the Al or Al alloy weighed in step 1) into the crucible and heating until molten completely; next, holding a temperature to obtain Al/salt mixed melt with the molten salt on the top and the molten Al or Al alloy at the bottom;
3) sonicating: inserting a tool head of an ultrasonic unit into the Al/salt mixed melt obtained in step 2), and holding the end surface of the tool head at a distance from the interface of the Al/salt melt; turn on the ultrasonic unit to sonicate the Al/salt mixed melt;
4) cooling and solidifying: after sonication, removing the molten salt on the top, cooling, and solidifying to obtain solidified molten salt; and
5) dissolving and separating: washing the solidified molten salt obtained in step 4) with pure water repeatedly, dissolving the salt mixture therein completely, filtering, and drying to obtain Al or Al alloy powders.
[0007] Further, the water-soluble salts used in step 1) include one or more of sodium nitrate, potassium nitrate, sodium carbonate, sodium bicarbonate, sodium chloride, potassium chloride, calcium chloride, sodium sulfate, and potassium sulfate.
[0008] Further, the Al alloy is anAl alloy with a melting point of <1,000°C. Further, the salt mixture prepared in step 1) has a lower melting point than the material to be prepared.
[0009] Further, a mass ratio of the salt mixture to the material to be prepared is 1:5.
[0010] Further, holding temperature instep 2) is 50-200°C higher than the melting point of the material to be prepared.
[0011] Further, in step 4), after sonication, the molten salt on the top is pouring onto a rotating cooling disk for cooling and solidification, to obtain the solidified molten salt.
[0012] The present invention has the following beneficial effects:
1. Inert molten salt is immiscible with and does not mutually react with molten Al or Al alloy, and the molten salt has a lower density than Al and Al alloy. Therefore, when melting, the molten salt will be separate from the molten Al or Al alloy, where the molten salt is on the top and the Al or Al alloy melt is at the bottom; the molten salt protects and refines the Al or Al alloy, avoiding the oxidation of the Al or Al alloy melt and playing a refining role in Al or Al alloy. In addition, Al or Al alloy micro-droplets generated by ultrasonic excitation are distributed into the molten salt, which are protected and refined by the molten salt. Therefore, throughout the preparation process of the present invention, the Al or Al alloy is always protected by the molten salt and does not come into contact with the air, avoiding oxidation; meanwhile, role of the salt in refining the Al or Al alloy further reduces the oxygen content of Al or Al alloy powders prepared. Compared with current preparation methods of Al or Al alloy powders, high-vacuum apparatus and a large amount of inert gas are not needed through this process. This not only ensures the oxygen content of powders, but also reduces preparation costs substantially.
2. The molten salt and the Al or Al alloy melt constitute an immiscible system; there is a large interfacial tension between two immiscible melts; to minimize the system energy, two immiscible melts tend to reduce the interface between two melts. Therefore, in the method of the present invention, the Al or Al alloy melt is sonicated into droplets and dispersed into the molten salt; in order to reduce the interface between droplets and molten salt, droplets will spontaneously exist in a spherical manner and thus solidify into microspheres to obtain powders with high sphericity.
3. In the method of the present invention, under continuous ultrasonic vibration, Al or Al alloy microspheres are well distributed in the salt without agglomeration in the presence of ultrasonic current, protecting the prepared Al or Al alloy powders from the satellite formation occurred in conventional atomization processes.
FIG. 1 is a schematic diagram of a preparation process of the present invention; FIG. 2 is the morphology of pure Al powders prepared in Example 1; FIG. 3 is the morphology of Al-7Si alloy powders prepared in Example 2; FIG. 4 is the morphology of Al-8Bi alloy powders prepared in Example 3;
In the figure: 1 represents an ultrasonic unit, 2 represents a salt/Al melt interface, and 3 represents a crucible.
[0013] The present invention is further described below with reference to the examples, but is not limited to the scope of the present invention.
[0014] Example 1: Preparation of pure spherical Al powders
[0015] The method included the following steps:
1) blending: separately weighing 20 parts by weight of NaCl, 40 parts by weight of CaC2, and 40 parts by weight of KCl in mass percentage to constitute a salt mixture, mixing the salts well in a blender mixer, and then drying the salt mixture in a drying oven for 3 h at 105°C; weighing 100 parts by weight of pure Al with a purity of 99.99% for use;
2) smelting: first, placing the salt mixture obtained in step 1) in alumina crucible 3, and heating the salt mixture to 850°C on a crucible melting resistance furnace until the salt mixture melt was in a molten state; then, adding the pure Al obtained in step 1) into the crucible 3 and heating until the pure Al was molten completely; next, holding the molten mixture at 800°C for 30 min to obtain Al/salt mixed melt with the molten salt on the top and the molten pure Al at the bottom;
3) sonicating: setting an output power of ultrasonic unit 1 as 300 W, and inserting a tool head of the ultrasonic unit 1 into the Al/salt mixed melt obtained in step 2), as shown in FIG. 1; holding the end surface of the tool head at a distance (M) of 30 mm from the interface 2 of the Al/salt melt; turn on the ultrasonic unit to sonicate the Al/salt mixed melt for 5 min;
4) cooling and solidifying: pouring the molten salt on the top onto a pure copper cooling disk rotating at 300 rpm for cooling and solidification, and collecting cooled and solidified molten salt; and
5) dissolving and separating: washing the solidified molten salt obtained in step 4) with pure water repeatedly, dissolving the salt completely, filtering Al powders through a 1,000 mesh sieve, and then drying naturally at room temperature to obtain pure Al powders.
[0016] As shown in FIG. 2, pure spherical Al powders obtained by the method have an average particle size of 52.6 m and an active Al content of >99.5%.
[0017] Example 2: Preparation of spherical Al-7Si alloy powders
[0018] The method included the following steps:
1) blending: separately weighing 30 parts by weight of NaCl and 70 parts by weight of KCl in mass percentage to constitute a salt mixture, mixing the salts well in a blender mixer, and then drying the salt mixture in a drying oven for 3 h at 105°C; weighing 20 parts by weight of Al-7Si alloy with 7 wt.% silicon (Si);
2) smelting: first, placing the salt mixture obtained in step 1) in alumina crucible 3, and heating the salt mixture to 850°C on a crucible melting resistance furnace until the salt mixture melt was in a molten state; then, adding the Al-7Si alloy obtained in step 1) into the crucible 3 and heating until the alloy was molten completely; next, holding the mixture at 780°C for 30 min to obtain Al/salt mixed melt with the molten salt on the top and the molten Al-7Si alloy at the bottom;
3) sonicating: setting an output power of ultrasonic unit 1 as 500 W, and inserting a tool head of the ultrasonic unit 1 into the Al/salt mixed melt obtained in step 2), as shown in FIG. 1; holding the end surface of the tool head at a distance (M) of 30 mm from the interface 2 of the Al/salt melt; turn on the ultrasonic unit to sonicate the Al/salt mixed melt for 5 min;
4) cooling and solidifying: pouring the molten salt on the top onto a pure copper cooling disk rotating at 300 rpm for cooling and solidification, and collecting cooled and solidified molten salt; and
5) dissolving and separating: washing the solidified molten salt obtained in step 4) with pure water repeatedly, dissolving the salt completely, filtering Al-7Si powders through a 1,000 mesh sieve, and then drying naturally at room temperature to obtain Al-7Si powders.
[0019] As shown in FIG. 3, spherical Al-7Si alloy powders obtained by the method have an average particle size of 41.5 m and an oxygen content of <0.5%.
[0020] Example 3: Preparation of spherical Al-8Bi alloy powders
[0021] The method included the following steps:
1) blending: separately weighing 40 parts by weight of NaCl, 40 parts by weight of KCl, and 20 parts by weight of CaCl2 in mass percentage to constitute a salt mixture, mixing the salts well in a blender mixer, and then drying the salt mixture in a drying oven for 3 h at 105°C; weighing 50 parts by weight of Al-8Bi alloy with 8 wt.% bismuth (Bi);
2) smelting: first, placing the salt mixture obtained in step 1) in alumina crucible 3, and heating the salt mixture to 850°C on a crucible melting resistance furnace until the salt mixture melt was in a molten state; then, adding the Al-8Bi alloy obtained in step 1) into the crucible 3 and heating until the Al-8Bi alloy was molten completely; next, holding the mixture at 850°C for 30 min to obtain Al/salt mixed melt with the molten salt on the top and the molten Al-8Bi alloy at the bottom;
3) sonicating: setting an output power of ultrasonic unit 1 as 250 W, and inserting a tool head of the ultrasonic unit 1 into the Al-8Bi alloy/salt mixed melt obtained in step 2), as shown in FIG. 1; holding the end surface of the tool head at a distance (M) of 40 mm from the interface 2 of the Al/salt melt; turn on the ultrasonic unit to sonicate the Al/salt mixed melt for 5 min;
4) cooling and solidifying: pouring the molten salt on the top onto a pure copper cooling disk rotating at 300 rpm for cooling and solidification, and collecting cooled and solidified molten salt; and
5) dissolving and separating: washing the solidified molten salt obtained in step 4) with pure water repeatedly, dissolving the salt completely, filtering Al-8Bi alloy powders through a 1,000 mesh sieve, and then drying naturally at room temperature to obtain Al-8Bi powders.
[0022] As shown in FIG. 3, spherical Al-8Bi alloy powders obtained by the method have an average particle size of 75 m and an oxygen content of <0.5%.
[0023] Herein, the ultrasonic unit 1 refers to an ultrasonic unit used in the field of metal fabrication, including, from top to bottom, a transducer, a horn, and a tool head; because the ultrasonic unit is known in the prior art, and specific structure thereof is will be omitted herein.
[0024] The horn and tool head of the ultrasonic unit 1 are made of any one of titanium alloy, niobium, tungsten, molybdenum, stainless steel, or ceramic material; the end surface of the tool head has a cross-sectional area of 0.5-10,000 mm2 , and preferably 200-1,500 mm22
[0025] As a specific embodiment, Examples 1, 2, and 3 select the horn and tool head made of Ti6 Al4V, and the end surface of the tool head has a cross-sectional area of 300 mm.2
[0026] The method of the present invention is suitable for the preparation of spherical Al and Al alloy powders. Different mixed salt systems should be selected when preparing Al powders or Al alloy powders with different components; a selection principle is that a salt mixture has a lower melting point than a material to be prepared, where the material to be prepared is Al or Al alloy. That is, when preparing spherical Al powders, the salt mixture should have a lower melting point than Al; when preparing an alloy with a component, the salt mixture should have a lower melting point than the Al alloy with the component. The melting point of the salt mixture can be realized by adjusting the types and ratios of water soluble salts in the salt mixture.
[0027] Herein, adjusting the types and ratios of water soluble salts in the salt mixture to realize the adjustment of the melting point is well-known to a person of ordinary skill in the art, and will not be repeated herein.
[0028] In view of Al and Al alloy with different component(s), the present invention can obtain spherical Al or Al alloy powders by adjusting an input power of the ultrasonic unit 1 and changing the distance between the tool head of the ultrasonic unit 1 and the interface 2 of the Al/salt melt.
Claims (5)
1. A process for ultrasonically exciting aluminum (Al)/salt mixed melt to prepare Al or Al alloy powder, comprising the following steps:
1) blending: separately weighing desired water-soluble salts in mass percentage, mixing the weighed water-soluble salts well, drying to obtain a salt mixture, and weighing a material to be prepared in mass percentage, wherein the material to be prepared is Al or Al alloy;
2) smelting: first, placing the salt mixture obtained in step 1) in a crucible and heating until molten; then, adding the Al or Al alloy weighed in step 1) into the crucible and heating until molten completely; next, holding a temperature to obtain Al/salt mixed melt with the molten salt on the top and the molten Al or Al alloy at the bottom;
3) sonicating: inserting a tool head of an ultrasonic unit into the Al/salt mixed melt obtained in step 2), and holding the end surface of the tool head at a distance from the interface of the Al/salt melt; turn on the ultrasonic unit to sonicate the Al/salt mixed melt;
4) cooling and solidifying: after sonication, removing the molten salt on the top, cooling, and solidifying to obtain solidified molten salt; and
5) dissolving and separating: washing the solidified molten salt obtained in step 4) with pure water repeatedly, dissolving the salt mixture therein completely, filtering, and drying to obtain Al or Al alloy powders.
2. The process for ultrasonically exciting Al/salt mixed melt to prepare Al or Al alloy powder according to claim 1, wherein the water-soluble salts used in step 1) comprise one or more of sodium nitrate, potassium nitrate, sodium carbonate, sodium bicarbonate, sodium chloride, potassium chloride, calcium chloride, sodium sulfate, and potassium sulfate.
3. The process for ultrasonically exciting Al/salt mixed melt to prepare Al or Al alloy powder according to claim 1, wherein the Al alloy is an Al alloy with a melting point of <1,000 0 C.
4. The process for ultrasonically exciting Al/salt mixed melt to prepare Al or Al alloy powder according to claim 1, wherein a mass ratio of the salt mixture to the material to be prepared is 1:5.
5. The process for ultrasonically exciting Al/salt mixed melt to prepare Al or Al alloy powder according to claim 1, wherein holding temperature in step 2) is 50-200°C higher than the melting point of the material to be prepared.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910739986.7A CN110355376B (en) | 2019-08-12 | 2019-08-12 | Method for preparing aluminum or aluminum alloy powder by exciting aluminum-salt mixed melt through ultrasonic waves |
| CN201910739986.7 | 2019-08-12 |
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| JPS61221310A (en) * | 1985-03-26 | 1986-10-01 | Agency Of Ind Science & Technol | Method and apparatus for producing pulverous powder of metal or alloy or the like |
| CN1253280C (en) * | 2004-04-08 | 2006-04-26 | 桂林市华纳光电材料有限责任公司 | Method for preparing nano metal powder |
| CN102773493B (en) * | 2012-08-24 | 2014-02-26 | 哈尔滨工业大学 | Device and method for preparing metal microballoons by using ultrasonic surface standing waves |
| CN104585238B (en) * | 2014-12-29 | 2017-11-21 | 华北理工大学 | Supersonic and co-deposition and ultrasonic molten-salt growth method prepare Ag2MoO4‑CuMoO4Compound antibacterial powder |
| CN106825593A (en) * | 2016-12-23 | 2017-06-13 | 南通金源智能技术有限公司 | The Al alloy powder preparation method of 3D printing material flowability can be improved |
| CN109576496B (en) * | 2018-12-29 | 2020-07-31 | 中北大学 | Method for preparing powder for selective laser melting by recycling waste aluminum, product and equipment |
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