CN112743094A - Preparation method and device of novel superfine amorphous magnetic powder - Google Patents

Preparation method and device of novel superfine amorphous magnetic powder Download PDF

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Publication number
CN112743094A
CN112743094A CN202011594517.XA CN202011594517A CN112743094A CN 112743094 A CN112743094 A CN 112743094A CN 202011594517 A CN202011594517 A CN 202011594517A CN 112743094 A CN112743094 A CN 112743094A
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crucible
magnetic powder
amorphous magnetic
powder
liquid
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胡玉
姜勇
梅述文
顾建东
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Nantong Jinyuan Intelligent Technology Co ltd
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Nantong Jinyuan Intelligent Technology Co ltd
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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
    • 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
    • B22F9/10Making 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 using centrifugal force
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15341Preparation processes therefor
    • H01F1/1535Preparation processes therefor by powder metallurgy, e.g. spark erosion

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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides a method and a device for preparing novel superfine amorphous magnetic powder, which adopts three-stage atomization to prepare Fe-based superfine amorphous magnetic powder: the first step is as follows: carrying out vacuum gas atomization on the Fe-based alloy ingot to form micro-fine alloy metal droplets; the second step is that: the fine alloy liquid drops enter a rotating horizontal disc under the state of liquid drops which are not solidified or semi-solidified, and are centrifuged and solidified into metal powder; the third step: the high-temperature metal powder freely falls into the cooling liquid and is chilled into amorphous spherical powder; the three steps must be completed continuously in a short time, and cannot be separated. The device comprises a crucible, a smelting coil, an atomizer, a horizontal disc, a rotating rod, a vacuum furnace, a partition plate and a cooling tower; the crucible, the smelting coil, the atomizer, the horizontal disc, the rotary rod and the vacuum furnace are all arranged in the vacuum furnace, the cooling tower is connected below the vacuum furnace, the bottom of the cooling tower is transversely provided with the partition plate, the partition plate and the bottom of the cooling tower form a closed space, and cooling liquid is stored in the closed space.

Description

Preparation method and device of novel superfine amorphous magnetic powder
Technical Field
The invention relates to the technical field of alloy preparation, in particular to a method and a device for preparing novel superfine amorphous magnetic powder.
Background
The amorphous alloy powder refers to amorphous powder prepared by quickly and cold atomizing certain alloy liquid drops. The Fe-based amorphous magnetically soft alloy powder has the characteristics of low cost, high direct current magnetic bias and low loss, and can obviously reduce the loss, thereby achieving the purpose of saving energy. The amorphous magnetic powder has the characteristics of excellent soft magnetic property, good mechanical property, high reaction activity, high catalytic performance and the like, and is more and more widely applied to the fields of aerospace, ships, automobiles, metallurgy, chemical industry and the like. The main application fields of the amorphous alloy powder are as follows: PFC inductance, a high-current alternating-current output reactor, an output reactor for an industrial power supply, a high-frequency flyback transformer and the like. Compared with the traditional iron-based soft magnetic material, the iron-based soft magnetic material has the advantages that: ultra-low magnetic core loss, excellent direct current magnetic bias characteristics, excellent frequency characteristics, good stability and the like. The high-quality amorphous magnetic powder has the characteristics of fine fineness, high purity, sphericization and concentrated particle size distribution.
Chinese patent CN201510103186.8 discloses a method for preparing bulk amorphous alloy from amorphous alloy powder, belonging to the field of metallic glass and powder metallurgy materials. The method is that after ball milling modification treatment is carried out on atomized amorphous alloy powder, the powder is solidified and formed below the temperature of 0.5Tg, and then the complete amorphous alloy with the density of 95 percent is prepared, wherein the Tg is the glass transition temperature of the amorphous alloy.
For another example, chinese patent CN201710806696.0 discloses an iron-based amorphous alloy powder and a method for preparing the same, wherein the alloy powder comprises the following elements by weight percent: fe 40-65%, Cr 15-25%, Mo 10-20%, W2-8%, Mn 1-5%, B1-4%, Si 0-4%, C0-3%, Ce 0-2%, Y0-2%; wherein, the four elements of Si, C, Ce and Y must exist more than 2 at the same time, and the total mass fraction is more than or equal to 1 percent. The powder is used as a thermal spraying raw material to prepare the powder.
Conventional preparation methods and problems:
theoretically, it is proved that when metal powder such as FeCrBSi, FeNiPb and the like is prepared by the atomization method, amorphous powder can be prepared by controlling the cooling speed to be larger than or equal to 106 ℃/s. The commonly used methods for producing amorphous alloy powders include high-speed rotating wheel thin strip method and atomization method.
The high-speed rotating wheel thin strip method is generally adopted, because the strip is thin, the cooling speed can reach 106 ℃/s, and the thin strip is crushed to obtain amorphous powder. The amorphous strip crushing method has the advantages that the material can be basically ensured to be amorphous, and has the defects of irregular powder appearance, poor sphericity and wide particle size distribution range.
The atomization method has the advantages of fine powder, sphericization and controllable particle size distribution, and has the defects of difficult control of completely amorphous powder, high oxygen content and the like.
Disclosure of Invention
The invention provides a novel method and a device for preparing superfine amorphous magnetic powder, aiming at solving the problems of difficulty in controlling complete amorphous state of powder, high oxygen content, irregular powder shape, poor sphericity and wide particle size distribution range in the prior art.
The technical scheme adopted by the invention is as follows: the preparation method of the novel superfine amorphous magnetic powder has the innovation points that: the method adopts three-stage atomization to prepare Fe-based superfine amorphous magnetic powder, and comprises the following specific steps:
the first step is as follows: carrying out vacuum gas atomization on the Fe-based alloy ingot to form micro-fine alloy metal droplets;
the second step is that: the fine alloy liquid drops enter a rotating horizontal disc under the state of liquid drops which are not solidified or semi-solidified, and are centrifuged and solidified into metal powder;
the third step: the high-temperature metal powder freely falls into the cooling liquid and is chilled into amorphous spherical powder;
the three steps must be completed continuously in a short time, and cannot be separated.
In some embodiments, the specific steps of the first step include: the method comprises the steps of inductively heating a Fe-based alloy ingot in a crucible to form liquid, carrying out supersonic gas atomization by using high-purity argon through an atomizer after the temperature of the Fe-based alloy ingot exceeds the melting point of the alloy by 150 degrees, and atomizing the metal liquid into fine alloy metal droplets.
In some embodiments, the second step is to throw the metal droplets into finer droplets under the action of centrifugal force in a tangential direction, and the droplets are rapidly solidified into metal powder.
Another objective of the present invention is to provide a device used in the method for preparing a novel fine amorphous magnetic powder, which has the innovative points that: comprises a crucible, a smelting coil, an atomizer, a horizontal disc, a rotating rod, a vacuum furnace, a partition plate and a cooling tower; the crucible, the smelting coil, the atomizer, the horizontal disc, the rotary rod and the vacuum furnace are all arranged in the vacuum furnace, the cooling tower is connected below the vacuum furnace, the bottom of the cooling tower is transversely provided with the partition plate, the partition plate and the bottom of the cooling tower form a closed space, and cooling liquid is stored in the closed space.
In some embodiments, the crucible is U-shaped, the melting coil is disposed on each side of the U-shaped crucible, the atomizer is disposed on the bottom of the crucible, and the crucible and the atomizer are vertical.
In some embodiments, the horizontal disc is positioned directly below the crucible, 20-30cm from the crucible; and a rotating rod which is obliquely arranged is connected below the horizontal disc.
In some embodiments, the angle of inclination of the rotating rod is 25 to 45 degrees.
In some embodiments, an alloy solution is placed in the U-shaped cavity of the U-shaped crucible.
In some embodiments, a bulk powder may be placed above the horizontal disk.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method adopts three-stage atomization to prepare the Fe-based superfine amorphous magnetic powder, and the produced powder has high amorphous degree, low oxygen content (less than 1000 ppm), high sphericity (more than 90 percent), fine granularity (the yield of fine powder less than 30 mu m is more than 80 percent) and concentrated granularity distribution.
(2) The invention adopts supersonic gas atomization method to prepare powder, which can ensure fine particle size and centralized distribution of the powder.
(3) The whole process is completed in a vacuum and argon protection closed cavity, and the low oxygen content of the powder is ensured.
(4) The invention adopts the rotary horizontal disc to spin and throw the semi-molten metal liquid drops into powder, thereby ensuring the high sphericity of the powder.
(5) The ultrahigh-sound-velocity atomization and cooling liquid chilling dual means ensure that the metal has a sufficiently high cooling speed from liquid to powder, and ensure the amorphous degree of the powder.
(6) The invention integrates three short processes into one device, and has high automation degree, high productivity, and simple operation after the parameters are set.
Drawings
FIG. 1 is a schematic diagram of the structure of the apparatus of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention discloses a preparation method of novel superfine amorphous magnetic powder, which adopts three-stage atomization to prepare Fe-based superfine amorphous magnetic powder and comprises the following specific steps:
the first step is as follows: carrying out vacuum gas atomization on the Fe-based alloy ingot to form micro-fine alloy metal droplets;
the second step is that: the fine alloy liquid drops enter a rotating horizontal disc under the state of liquid drops which are not solidified or semi-solidified, and are centrifuged and solidified into metal powder;
the third step: the high-temperature metal powder freely falls into the cooling liquid and is chilled into amorphous spherical powder;
the three steps must be completed continuously in a short time, and cannot be separated.
In the invention, if the first step of vacuum gas atomization adopts water atomization or air environment atomization, the oxygen content of the powder is difficult to ensure; secondly, the second step of rotating the disc can be replaced by a rotating cylinder, but the mechanical and electrical structures are more complicated; and finally, the cooling liquid is chilled in the third step to ensure the cooling speed, and the large temperature gradient can be realized only when the metal material is changed into a semi-solid state or a high-temperature solid state from liquid.
Therefore, to ensure the final effect, the three steps of the apparatus of the present invention must be completed continuously in a short time, and cannot be separated.
The method adopts three-stage atomization to prepare the Fe-based superfine amorphous magnetic powder, and the produced powder has high amorphous degree, low oxygen content (less than 1000 ppm), high sphericity (more than 90 percent), fine granularity (the yield of fine powder less than 30 mu m is more than 80 percent) and concentrated granularity distribution.
Specifically, the first step comprises the following specific steps: the method comprises the steps of inductively heating a Fe-based alloy ingot in a crucible to form liquid, carrying out supersonic gas atomization by using high-purity argon through an atomizer after the temperature of the Fe-based alloy ingot exceeds the melting point of the alloy by 150 degrees, and atomizing the metal liquid into fine alloy metal droplets.
Specifically, the second step is specifically that under the centrifugal force effect, the metal liquid drop is thrown into finer liquid drop along the effect of tangential direction centrifugal force, and the liquid drop solidifies into metal powder fast.
Another objective of the present invention is to provide a device used in the method for preparing a novel fine amorphous magnetic powder, which has the innovative points that: as shown in fig. 1: comprises a crucible 1, a smelting coil 2, an atomizer 3, a horizontal disc 4, a rotating rod 5, a vacuum furnace 6, a partition plate 7 and a cooling tower 8; crucible 1, smelting coil 2, atomizer 3, horizontal disc 4, rotary rod 5, vacuum furnace 6 all set up in vacuum furnace 6, cooling tower 8 is connected to vacuum furnace 6 below, 8 bottoms of cooling tower transversely set up baffle 7, baffle 7 and 8 bottoms of cooling tower form airtight space, deposit 11 liquid coolings in the airtight space. As shown in fig. 1: crucible 1 is the U type, and 1 both sides of U type crucible all set up one smelt coil 2, the bottom of crucible 1 sets up atomizer 3, crucible 1 with atomizer 3 is perpendicularly form.
Referring to fig. 1: the horizontal disc 4 is arranged under the crucible 1, and the distance from the crucible 1 is 20-30 cm; a rotating rod 5 which is obliquely arranged is connected below the horizontal disc 4.
As a further preference, in this embodiment of the present invention, the inclination angle of the rotating rod 5 is 25 to 45 degrees. As further preferable, the inclination angle of the rotating rod 5 is 40 degrees.
In the invention, specifically, an alloy solution 9 is placed in the U-shaped cavity of the U-shaped crucible 1. In addition, a pile of powder 10 can be placed above the horizontal disc 4.
The invention adopts supersonic gas atomization method to prepare powder, which can ensure fine particle size and centralized distribution of the powder.
The whole process is completed in a vacuum and argon protection closed cavity, and the low oxygen content of the powder is ensured.
The invention adopts the rotary horizontal disc to spin and throw the semi-molten metal liquid drops into powder, thereby ensuring the high sphericity of the powder.
The ultrahigh-sound-velocity atomization and cooling liquid chilling dual means ensure that the metal has a sufficiently high cooling speed from liquid to powder, and ensure the amorphous degree of the powder.
The invention integrates three short processes into one device, and has high automation degree, high productivity, and simple operation after the parameters are set.
In the description of the present invention, it is to be understood that the terms "coaxial", "bottom", "one end", "top", "middle", "other end", "upper", "one side", "top", "inner", "front", "center", "both ends", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "disposed," "connected," "secured," "screwed" and the like are to be construed broadly, e.g., as meaning fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; the terms may be directly connected or indirectly connected through an intermediate, and may be communication between two elements or interaction relationship between two elements, unless otherwise specifically limited, and the specific meaning of the terms in the present invention will be understood by those skilled in the art according to specific situations.
While the foregoing description shows and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. A preparation method of novel superfine amorphous magnetic powder is characterized by comprising the following steps: the method adopts three-stage atomization to prepare Fe-based superfine amorphous magnetic powder, and comprises the following specific steps:
the first step is as follows: carrying out vacuum gas atomization on the Fe-based alloy ingot to form micro-fine alloy metal droplets;
the second step is that: the fine alloy liquid drops enter a rotating horizontal disc under the state of liquid drops which are not solidified or semi-solidified, and are centrifuged and solidified into metal powder;
the third step: the high-temperature metal powder freely falls into the cooling liquid and is chilled into amorphous spherical powder;
the three steps must be completed continuously in a short time, and cannot be separated.
2. The method for preparing the novel superfine amorphous magnetic powder according to claim 1 is characterized in that: the first step comprises the following specific steps: the method comprises the steps of inductively heating a Fe-based alloy ingot in a crucible to form liquid, carrying out supersonic gas atomization by using high-purity argon through an atomizer after the temperature of the Fe-based alloy ingot exceeds the melting point of the alloy by 150 degrees, and atomizing the metal liquid into fine alloy metal droplets.
3. The method for preparing the novel superfine amorphous magnetic powder according to claim 1 is characterized in that: the second step is specifically that under the centrifugal force effect, the metal liquid drop is thrown into finer liquid drop along the tangential direction under the action of the centrifugal force, and the liquid drop is rapidly solidified into metal powder.
4. A device used in the preparation method of the novel superfine amorphous magnetic powder according to claim 1 is characterized in that: comprises a crucible, a smelting coil, an atomizer, a horizontal disc, a rotating rod, a vacuum furnace, a partition plate and a cooling tower; the crucible, the smelting coil, the atomizer, the horizontal disc, the rotary rod and the vacuum furnace are all arranged in the vacuum furnace, the cooling tower is connected below the vacuum furnace, the bottom of the cooling tower is transversely provided with the partition plate, the partition plate and the bottom of the cooling tower form a closed space, and cooling liquid is stored in the closed space.
5. The apparatus used in the method for preparing the novel superfine amorphous magnetic powder according to claim 4 is characterized in that: the crucible is the U type, and U type crucible both sides all set up one smelt the coil, the bottom of crucible sets up the atomizer, the crucible with the atomizer is perpendicularly form.
6. The apparatus used in the method for preparing the novel superfine amorphous magnetic powder according to claim 4 is characterized in that: the horizontal disc is arranged under the crucible and is 20-30cm away from the crucible; and a rotating rod which is obliquely arranged is connected below the horizontal disc.
7. The apparatus used in the method for preparing the novel superfine amorphous magnetic powder according to claim 6 is characterized in that: the inclination angle of the rotating rod is 25-45 degrees.
8. The apparatus used in the method for preparing the novel superfine amorphous magnetic powder according to claim 5 is characterized in that: and an alloy solution is placed in the U-shaped cavity of the U-shaped crucible.
9. The apparatus used in the method for preparing the novel superfine amorphous magnetic powder according to claim 6 is characterized in that: the stacking powder can be placed above the horizontal disc.
CN202011594517.XA 2020-12-29 2020-12-29 Preparation method and device of novel superfine amorphous magnetic powder Pending CN112743094A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010209409A (en) * 2009-03-10 2010-09-24 Nec Tokin Corp Method for producing amorphous soft magnetic alloy powder, amorphous soft magnetic alloy powder, and formed body using the same
CN102925824A (en) * 2012-11-23 2013-02-13 北京科技大学 Preparation method for zirconium-based amorphous alloy as well as powder and large-sized block of zirconium-based amorphous alloy
CN104084596A (en) * 2014-07-15 2014-10-08 中国科学院宁波材料技术与工程研究所 Method and device for manufacturing amorphous powder
CN105397100A (en) * 2014-08-25 2016-03-16 中国科学院宁波材料技术与工程研究所 Preparation method for fine metal powder and equipment achieving method
CN107900364A (en) * 2017-11-07 2018-04-13 常州大学 Cooling method prepares the device of amorphous metal powder to a kind of ultrasonic atomizatio again
CN111534765A (en) * 2020-05-27 2020-08-14 安泰(霸州)特种粉业有限公司 Spherical amorphous alloy powder preparation device and method
CN111968821A (en) * 2020-07-24 2020-11-20 泉州天智合金材料科技有限公司 Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010209409A (en) * 2009-03-10 2010-09-24 Nec Tokin Corp Method for producing amorphous soft magnetic alloy powder, amorphous soft magnetic alloy powder, and formed body using the same
CN102925824A (en) * 2012-11-23 2013-02-13 北京科技大学 Preparation method for zirconium-based amorphous alloy as well as powder and large-sized block of zirconium-based amorphous alloy
CN104084596A (en) * 2014-07-15 2014-10-08 中国科学院宁波材料技术与工程研究所 Method and device for manufacturing amorphous powder
CN105397100A (en) * 2014-08-25 2016-03-16 中国科学院宁波材料技术与工程研究所 Preparation method for fine metal powder and equipment achieving method
CN107900364A (en) * 2017-11-07 2018-04-13 常州大学 Cooling method prepares the device of amorphous metal powder to a kind of ultrasonic atomizatio again
CN111534765A (en) * 2020-05-27 2020-08-14 安泰(霸州)特种粉业有限公司 Spherical amorphous alloy powder preparation device and method
CN111968821A (en) * 2020-07-24 2020-11-20 泉州天智合金材料科技有限公司 Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof

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