WO2011082595A1 - Procédé de préparation d'une poudre néodyme-fer-bore sphérique superfine - Google Patents

Procédé de préparation d'une poudre néodyme-fer-bore sphérique superfine Download PDF

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Publication number
WO2011082595A1
WO2011082595A1 PCT/CN2010/077380 CN2010077380W WO2011082595A1 WO 2011082595 A1 WO2011082595 A1 WO 2011082595A1 CN 2010077380 W CN2010077380 W CN 2010077380W WO 2011082595 A1 WO2011082595 A1 WO 2011082595A1
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Prior art keywords
powder
ndfeb
hydrogen
fine spherical
plasma
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PCT/CN2010/077380
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English (en)
Chinese (zh)
Inventor
郭志猛
盛艳伟
曲选辉
郝俊杰
林涛
邵慧萍
罗骥
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北京科技大学
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Publication of WO2011082595A1 publication Critical patent/WO2011082595A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • 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
    • 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
    • B22F9/023—Hydrogen absorption
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/025—Making ferrous alloys by powder metallurgy having an intermetallic of the REM-Fe type which is not magnetic
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the invention belongs to the technical field of powder preparation, and in particular provides a preparation method of a fine spherical NdFeB powder.
  • Nd-Fe-B Rare earth permanent magnet materials have excellent magnetic properties, while Nd-Fe-B is called "magnetic king". Since the advent of the third-generation permanent magnet Nd-Fe-B in the 1980s, it has developed rapidly due to its high cost performance and abundant resources. NdFeB Yongshu magnetic materials can be divided into sintered NdFeB and bonded NdFeB, both of which have advantages and disadvantages. The magnetic properties of sintered NdFeB are better, but the production process is more complicated and the cost is higher. Bonded NdFeB magnets have reduced magnetic properties due to the addition of binders, but they are easy to mass-produce, accurate in manufacturing size, large in shape freedom, low in density, stable in magnetic properties, etc., and are compatible with electronic components. The development direction of thin, short and small has been widely used in electrical engineering, instrumentation, microwave communication, magnetic machinery, transportation, magnetic therapy, magnetic separation and magnetization.
  • Bonded magnets currently have two forming processes: compression molding and injection molding: the molding process is to press a mixture of magnetic powder and binder into a cavity of a press and press it at a certain pressure. The pressed magnet is cured at a temperature of 150 to 175 °C. The injection molding process is such that the heated mixture enters the cavity through the flow path, is formed, cooled and hardened in the cavity, and the loading of the powder is generally 70%.
  • Magnetic powder is the core part of manufacturing high-performance bonded magnets, and the performance of magnetic powder has a great influence on the magnetic properties of the final product.
  • the performance of magnetic powder is closely related to its preparation method, particle shape, particle size and particle size distribution.
  • the average particle size of magnetic powder should generally be less than 20 ⁇ , with good sphericity and wide particle size distribution.
  • the general purpose powder for bonded magnets is mainly produced by rapid quenching (MQ) and hydrogen processing (HDDR). Melt quenching method is quenched by melting in a quenching furnace It solidifies and turns into an amorphous ribbon, which is then crystallized to increase the coercive force.
  • the prepared magnetic powder has a very small crystal grain diameter of several tens of nanometers.
  • Hydrogenation is the process of placing the alloy ingot in hydrogen (hydrogenation), raising the temperature to 750 to 850 ° C, holding it for 2 h (disproportionation), evacuating (dehydrogenation and recombination), and then cooling to room temperature.
  • the features are simple equipment and process, and low cost.
  • Hydrogen blasting (HD) process is an effective process in the production of rare earth permanent magnet materials. This process utilizes a rare earth permanent magnet alloy to describe the grain boundary fracture and the transgranular fracture property of the alloy itself during hydrogen absorption and hydrogen evolution, resulting in alloy pulverization, thereby obtaining an alloy powder of a certain particle size.
  • An object of the present invention is to provide a method for preparing a fine spherical NdFeB powder for bonding NdFeB, which saves energy, reduces pollution, shortens the process flow, improves production efficiency, and reduces production cost.
  • the object of the present invention is to realize a method for preparing a fine spherical NdFeB powder by using a hydrogen absorbing NdFeB powder as a raw material, and discharging the hydrogen absorbing NdFeB powder by radio frequency (RF) plasma treatment. Hydrogen, spheroidization to prepare spherical NdFeB powder is completed in one step.
  • a method for preparing fine spherical NdFeB powder comprising the following steps:
  • the alloy ingot is subjected to vacuum annealing treatment, and the annealing temperature is 950 to 1050 ° C, and the time is 5 to 24 h;
  • the main process parameters are: power 30 ⁇ 80KW, argon working gas flow 20 ⁇ 50 slpm, argon book gas shielding gas flow 20 ⁇ 200slpm, system negative pressure 200 ⁇ 300mm Hg .
  • the hydrogen-absorbing NdFeB powder is fed into the plasma high-temperature zone with argon (or hydrogen) as the carrier gas.
  • the carrier gas flow rate is 4 ⁇ 10 slpm, and the powder feeding rate is 50 ⁇ 100g/min.
  • the hydrogen-absorbing NdFeB particles rapidly absorb the fine NdFeB powder formed by the explosion of hydrogen, and the NdFeB powder absorbs the heat and spheroidizes and rapidly solidifies into a spherical powder; the fine spherical NdFeB powder is collected by cyclone separation.
  • the hydrogen absorbing NdFeB powder raw material has an average particle size of 100 to 350 ⁇ m, and the prepared fine spherical titanium powder has a particle size of 10 to 100 ⁇ m.
  • the invention combines hydrogen blasting (HD) technology with radio frequency (RF) plasma spheroidization technology, and uses hydrogen absorbing NdFeB powder as raw material to pulverize and dehydrogenate hydrogen absorbing NdFeB powder by plasma treatment.
  • RF radio frequency
  • the hydrogen absorbing NdFeB powder prepared by the hydrogen blasting (HD) process is used as a raw material.
  • the preparation of fine spherical NdFeB powder by radio frequency (RF) plasma spheroidization technology has the advantages of: fine particle size, uniform composition, low oxygen content, high spheroidization rate, good sphericity and fluidity, and high packing density.
  • the prepared fine spherical NdFeB powder has small grain size, uniform composition, good fluidity, high spheroidization rate and low oxygen content, and is suitable for preparing bonded NdFeB permanent magnet materials.
  • the prepared neodymium iron boron powder is a spherical powder in an amorphous or microcrystalline state, and has high magnetic properties after tempering treatment.
  • Example 1 Preparation of fine spherical NdFeB powder with an average particle size of ⁇
  • the NdFeB alloy is smelted by vacuum induction, and the smelted alloy ingot is vacuum annealed and then crushed into a powder by a hydrogen explosion HD process. After sieving, the yttrium-doped NdFeB powder with an average particle size of ⁇ is used as a raw material to stabilize.
  • the operating RF (F) plasma power is 30 KW
  • the argon working gas flow is 30 slpm
  • the argon shielding gas flow is 40 slpm
  • the system negative pressure is 200 mm Hg.
  • the hydrogen absorbing NdFeB powder was sent to a high temperature plasma at a flow rate of 4 slpm, and the powder rate was 50 g/min.
  • Example 2 Preparation of fine spherical NdFeB powder with an average particle size of 20 ⁇ m The NdFeB alloy is smelted by vacuum induction, and the smelted alloy ingot is vacuum annealed and then crushed into powder by hydrogen explosion HD process. After sieving, the yttria-absorbing NdFeB powder with an average particle size of 150 ⁇ m is used as a raw material to stabilize.
  • the operating radio frequency (RF) plasma power is 55 KW
  • the argon working gas flow rate is 35 slpm
  • the argon shielding gas flow rate is lOOslpm
  • the system negative pressure is 250 mm Hg.
  • the hydrogen-absorbing NdFeB powder was sent to a high-temperature plasma at a flow rate of 5 slpm, and the powder was transported at a rate of 55 g/min. After spheroidization, a fine spherical ruthenium with an average particle size of 20 ⁇ m was obtained by cyclone separation. Iron boron powder.
  • Example 3 Preparation of fine spherical neodymium iron boron powder having an average particle diameter of 60 ⁇ m
  • the NdFeB alloy is smelted by vacuum induction, and the smelted alloy ingot is subjected to vacuum annealing treatment, and then pulverized into a book powder by a hydrogen blasting HD process, and after sieving, a hydrogen absorbing NdFeB powder having an average particle size of 200 ⁇ m is used as a raw material.
  • the stable operation of the radio frequency (RF) plasma power is 60 KW, the argon working gas flow rate is 40 slpm, the argon shielding gas flow rate is 150 slpm, and the system negative pressure is 280 mm Hg.
  • the hydrogen absorbing NdFeB powder was sent to a high temperature plasma at a flow rate of 6 slpm, and the powder rate was 60 g/min.
  • the neodymium-iron-boron alloy is smelted by vacuum induction, and the smelted alloy ingot is vacuum-annealed and then crushed into powder by hydrogen explosion HD process.
  • the hydrogen absorbing NdFeB powder with an average particle size of 350 ⁇ m is used as a raw material to stabilize.
  • the operating radio frequency (RF) plasma power is 80 KW
  • the argon working gas flow rate is 50 slpm
  • the argon shielding gas flow rate is 200 slpm
  • the system negative pressure is 300 mm Hg.
  • the hydrogen absorbing NdFeB powder was sent to a high temperature plasma with an argon gas flow rate of 8 slpm, and the powder transfer rate was 85 g/min.
  • the fine spherical yttrium iron having an average particle size of ⁇ was obtained by cyclone separation. Boron powder.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne un procédé de préparation d'une poudre d'alliage Nd-Fe-B sphérique superfine qui consiste : à broyer un lingot de coulée d'un alliage Nd-Fe-B pour le réduire en différentes poudres grâce à un processus de décrépitation par l'hydrogène ; à réaliser une sphéroïdisation par plasma de la poudre d'alliage Nd-Fe-B à l'aide d'un plasma radiofréquence (RF) ; et à obtenir ainsi une poudre Nd-Fe-B sphérique superfine.
PCT/CN2010/077380 2010-01-05 2010-09-27 Procédé de préparation d'une poudre néodyme-fer-bore sphérique superfine WO2011082595A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2010100337322A CN101767200B (zh) 2010-01-05 2010-01-05 一种微细球形Nd-Fe-B粉的制备方法
CN201010033732.2 2010-01-05

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WO2011082595A1 true WO2011082595A1 (fr) 2011-07-14

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
TWI628016B (zh) * 2016-08-22 2018-07-01 中國鋼鐵股份有限公司 釹鐵硼合金的氫碎製程
CN114101693A (zh) * 2020-08-31 2022-03-01 厦门稀土材料研究所 一种用于3d打印的低氧铕镍粉体及其制备方法
CN115768909A (zh) * 2020-07-01 2023-03-07 耶达研究与发展有限公司 从铁磁性合金中回收稀土金属
CN115889794A (zh) * 2022-11-14 2023-04-04 北京兴荣源科技有限公司 一种低成本球形钴铬钼3d打印粉的制备方法

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CN101767200B (zh) * 2010-01-05 2012-05-09 北京科技大学 一种微细球形Nd-Fe-B粉的制备方法
CN104582877A (zh) * 2012-03-23 2015-04-29 苹果公司 无定形合金铸块的连续无模制造
CN102888498A (zh) * 2012-11-01 2013-01-23 山西京宇天成科技有限公司 一种钕铁硼双相脱氢工艺方法
CN105215372B (zh) * 2015-10-21 2017-08-29 龙岩紫荆创新研究院 一种3d打印用钕铁硼磁粉的制备
CN108213404B (zh) 2016-12-21 2022-01-28 三环瓦克华（北京）磁性器件有限公司 制备钕铁硼永磁材料的微粉、靶式气流磨制粉方法及出粉

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI628016B (zh) * 2016-08-22 2018-07-01 中國鋼鐵股份有限公司 釹鐵硼合金的氫碎製程
CN115768909A (zh) * 2020-07-01 2023-03-07 耶达研究与发展有限公司 从铁磁性合金中回收稀土金属
CN114101693A (zh) * 2020-08-31 2022-03-01 厦门稀土材料研究所 一种用于3d打印的低氧铕镍粉体及其制备方法
CN115889794A (zh) * 2022-11-14 2023-04-04 北京兴荣源科技有限公司 一种低成本球形钴铬钼3d打印粉的制备方法

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