CN111534765A - Spherical amorphous alloy powder preparation device and method - Google Patents
Spherical amorphous alloy powder preparation device and method Download PDFInfo
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- CN111534765A CN111534765A CN202010463311.7A CN202010463311A CN111534765A CN 111534765 A CN111534765 A CN 111534765A CN 202010463311 A CN202010463311 A CN 202010463311A CN 111534765 A CN111534765 A CN 111534765A
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- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 36
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 105
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
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- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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- 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
- B22F2009/0824—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 with a specific atomising fluid
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- 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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- 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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- 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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- 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
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- 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
- B22F2009/0888—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 casting construction of the melt process, apparatus, intermediate reservoir, e.g. tundish, devices for temperature control
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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Abstract
The invention discloses a spherical amorphous alloy powder preparation device, which comprises: the gas atomizer is used for crushing the alloy melt by adopting atomizing gas; and the liquid cooling device is positioned below the gas atomizer, arranged at the periphery of an airflow nozzle of the gas atomizer and used for cooling the crushed alloy powder intermediate of the gas atomizer to form spherical amorphous alloy powder. The invention also discloses a preparation method of the spherical amorphous alloy powder, which comprises the following steps: s1: melting the raw materials to obtain an alloy melt; s2: atomizing the alloy melt by adopting inert atomizing gas under vacuum or inert atmosphere to obtain an alloy powder intermediate; s3: and cooling the alloy powder intermediate in a cooling area to obtain the spherical amorphous alloy powder. The spherical amorphous alloy powder with more uniform granularity, more regular sphere and smaller oxygen content is prepared by the preparation device or the preparation method.
Description
Technical Field
The invention belongs to the technical field of atomization powder preparation, and particularly relates to a device and a method for preparing spherical amorphous alloy powder by adopting a gas atomization water cooling process.
Background
The atomized powder is a powder preparation method in which a rapidly moving atomizing medium (usually high-pressure water or gas) is struck and crushed to break metal or alloy liquid into fine liquid droplets, and then the fine liquid droplets are condensed into solid powder. The shape of the powders obtained varies greatly depending on the method of obtaining the powders.
The amorphous alloy product has high saturation magnetic induction intensity and high magnetic conductivity, solves the adverse effect of defects such as crystal grains, crystal boundaries, dislocation, interstitial atoms, magnetocrystalline anisotropy and the like on soft magnetic performance, is used for manufacturing transformers, mutual inductors, inductance elements and the like, has excellent magnetism, corrosion resistance, wear resistance, high strength, hardness, high resistivity and electric coupling performance, has a certain production scale in countries such as the United states, Japan, Germany and the like at present, and a large amount of amorphous alloys gradually replace permalloy and ferrite to flow to the market. With the development of high frequency and miniaturization of electronic devices, the market demands for high magnetic permeability and low loss soft magnetic powder at high frequency are becoming more and more severe. Therefore, the preparation of spherical, low-oxygen amorphous powder becomes the key to the problem.
At present, the methods for preparing amorphous soft magnetic powder mainly comprise two methods: (1) a strip crushing method; (2) and (4) atomizing. The amorphous powder prepared by the amorphous strip crushing method has many edges and corners, and is easy to pierce an insulating layer coated on the surface of the powder, so that the market expansion is limited. The photo of the amorphous powder prepared by the strip crushing method is shown in figure 1. The existing device for preparing amorphous powder by an atomization method is shown in figure 2 and comprises an atomizer 1, an air inlet pipe 2, an airflow nozzle 3, a liquid guide pipe 4 and a melt nozzle 5.
Disclosure of Invention
One of the purposes of the invention is to provide a spherical amorphous alloy powder preparation device, which has strong alloy amorphous forming capability and can ensure that the formed powder has good sphericity and low oxygen content.
The second purpose of the invention is to provide a preparation method of the spherical amorphous alloy powder, and the spherical amorphous alloy powder prepared by the method has good sphericity and low oxygen content. The prepared amorphous powder can meet the requirements of electronic devices on high magnetic conductivity and low loss amorphous powder under high frequency.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a spherical amorphous alloy powder preparation device in a first aspect, which comprises:
the gas atomizer is used for crushing the alloy melt by adopting atomizing gas;
and the liquid cooling device is positioned below the gas atomizer, arranged at the periphery of an airflow nozzle of the gas atomizer and used for cooling the alloy powder intermediate after the gas atomizer is crushed to form spherical amorphous alloy powder.
In some embodiments, the preparation apparatus further comprises a liquid guide pipe connecting the tundish containing the alloy melt and the gas atomizer.
In some embodiments, the catheter upper end communicates with the tundish.
In some embodiments, the lower end of the catheter is seated in a corresponding socket of the aerosolizer.
In some embodiments, the lumen of the catheter is reverse tapered from top to bottom with a taper angle of 0-15 °.
In some embodiments, the lumen of the catheter is inverted cone-shaped from top to bottom to be cylindrical, and the cone angle is 1-15 degrees.
In some embodiments, an air inlet pipe for introducing the atomizing gas into the atomizer is provided on a side wall of the atomizer.
In some embodiments, a gas flow nozzle for breaking up the alloy melt is provided around an alloy melt outlet in a lower portion of the gas atomizer.
In some embodiments, the gas flow nozzle is annularly disposed.
In some embodiments, the direction of the air flow from the air flow nozzle is 40-50 degrees from the vertical direction.
In some embodiments, the liquid cooling device is annularly arranged at the periphery of the airflow nozzle and used for forming an annular cooling area for cooling the alloy powder intermediate.
In some embodiments, the liquid cooling device is a cylindrical structure with double walls, and a cooling liquid outlet is arranged on the lower bottom surface of the liquid cooling device and used for allowing cooling liquid to flow downwards to form a cooling liquid curtain, and the cooling liquid curtain forms an annular cooling area for cooling the alloy powder intermediate.
In some embodiments, the cooling fluid is water.
In some embodiments, the liquid cooling device is a cylindrical structure with double walls, the space between the double walls is filled with cooling liquid, and the hollow area of the cylindrical structure is an annular cooling zone for cooling the alloy powder intermediate.
In some embodiments, the cooling fluid is liquid nitrogen.
In some embodiments, the liquid cooling device is secured to a lower bottom surface of the aerosolizer.
In some embodiments, a side wall of the liquid cooling device is provided with a liquid inlet pipe for injecting cooling liquid into the liquid cooling device.
In some embodiments, the amorphous alloy powder is a FeSiB-based amorphous alloy powder; preferably, the amorphous alloy powder comprises the following components in percentage by mass: si: 1-14%, B: 7-15%, C: less than or equal to 4 percent, Cu: less than or equal to 3 percent, Nb: less than or equal to 4 percent, P: less than or equal to 2 percent, and the balance of Fe and inevitable impurities.
In some embodiments, the FeSiB-based amorphous alloy powder is an AP01, AP02, or AP03 alloy powder;
the AP01 alloy powder comprises the following chemical components in percentage by mass: cu: 1%, Nb: 3%, Si: 13.5%, B: 9%, Fe: the balance and unavoidable impurities;
the AP02 alloy comprises the following chemical components in percentage by mass: cu: 1%, Nb: 1%, Si: 4%, B: 9%, C: 0.3%, Fe: the balance and unavoidable impurities;
the AP03 alloy comprises the following chemical components in percentage by mass: cu: 1.2%, Si: 2%, B: 12%, P: 2%, Fe: the balance and inevitable impurities.
The second aspect of the invention provides a preparation method of spherical amorphous alloy powder, which comprises the following steps:
s1: melting the raw materials to obtain an alloy melt;
s2: atomizing the alloy melt by adopting inert atomizing gas in vacuum or inert atmosphere to obtain an alloy powder intermediate;
s3: and cooling the alloy powder intermediate in a cooling area to obtain the spherical amorphous alloy powder.
In some embodiments, in step S1, the raw material is melted at a temperature 50 to 250 ℃ higher than the melting point of the raw material to obtain the alloy melt.
In some embodiments, in step S1, the raw material is melted at a temperature 150 to 200 ℃ higher than the melting point of the raw material to obtain the alloy melt.
In some embodiments, in step S2, the pressure of the atomizing gas during the atomizing treatment is 2 to 6 Mpa; the vacuum degree during the atomization treatment is controlled to be less than 10 Pa.
In some embodiments, in step S2, the inert atomizing gas is nitrogen or argon.
In some embodiments, in step S3, the cooling rate is 106K/s or more.
In some casesIn one embodiment, the cooling rate is 106-107K/s。
In some embodiments, the method for preparing spherical amorphous alloy powder is performed by using the apparatus for preparing spherical amorphous alloy powder according to the first aspect of the present invention.
The third aspect of the present invention provides a spherical amorphous alloy powder prepared by the apparatus for preparing a spherical amorphous alloy powder according to the first aspect of the present invention or the method for preparing a spherical amorphous alloy powder according to the second aspect of the present invention.
The technical features of the preparation device according to the invention can be used in any possible combination.
The method for preparing the spherical low-oxygen amorphous powder has the advantages that the method for preparing the spherical low-oxygen amorphous powder is found by improving the structure of the atomizer, is simple and feasible, can be used for carrying out structural modification on the basis of the original atomizer, and is low in cost and high in efficiency. The spherical and low-oxygen amorphous powder can be widely applied to the field of high-frequency and miniaturized electronic devices and has good market prospect. The particle size range D50 of the spherical amorphous powder prepared by the method is 5-30 mu m, and the oxygen content is less than 600 ppm.
Drawings
FIG. 1 is a photograph of amorphous powder prepared by a strip crushing method in the prior art.
FIG. 2 is a schematic structural diagram of a spherical amorphous alloy powder preparation device in the prior art.
FIG. 3 is a schematic structural diagram of an apparatus for preparing spherical amorphous alloy powder according to some embodiments of the present invention.
FIG. 4 is a schematic diagram of the structure and the operation state of the spherical amorphous alloy powder preparation device shown in FIG. 3.
FIG. 5 is a SEM scanning electron micrograph of the amorphous alloy powder prepared in example 1 of the present invention.
Fig. 6 is an XRD spectrum of the amorphous alloy powder prepared in example 1 of the present invention.
Fig. 7 is an SEM scanning electron micrograph of the alloy powder prepared in comparative example 1.
Fig. 8 is an XRD pattern of the alloy powder prepared in comparative example 1.
FIG. 9 is a SEM scanning electron micrograph of the amorphous alloy powder prepared in example 2 of the present invention.
Fig. 10 is an XRD spectrum of the amorphous alloy powder prepared in example 2 of the present invention.
Fig. 11 is an SEM scanning electron micrograph of the alloy powder prepared in comparative example 2.
Fig. 12 is an XRD pattern of the alloy powder prepared in comparative example 2.
FIG. 13 is a SEM scanning electron micrograph of the amorphous alloy powder prepared in example 3 of the present invention.
Fig. 14 is an XRD spectrum of the amorphous alloy powder prepared in example 3 of the present invention.
FIG. 15 is an SEM scanning electron micrograph of an alloy powder prepared according to comparative example 3 of the present invention.
Fig. 16 is an XRD pattern of the alloy powder prepared in comparative example 3 of the present invention.
The method comprises the following steps of 1-gas atomizer, 2-gas inlet pipe, 3-gas flow nozzle, 4-liquid guide pipe, 5-melt nozzle, 6-water cooling device, 7-water inlet pipe, 8-alloy melt liquid flow, 9-sprayed atomizing gas, 10-cooling water curtain and 11-amorphous alloy powder.
The XRD patterns of fig. 6, 8, 10, 12, 14, 16 have the abscissa of 2 θ (twice the incident angle of x-ray) and the ordinate of diffraction intensity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the apparatus and method of the present invention will be described in further detail with reference to the accompanying drawings.
The amorphous powder prepared by water atomization at present has poor sphericity and high oxygen content, and the oxygen content can reach about 2000ppm generally. The sphericity and oxygen content of the powder are improved by the gas atomization process, but the gas atomization process has the problem of difficult amorphous formation, especially for the powder particles with larger sizes. The invention provides an atomization powder preparation device and method, which can obtain spherical low-oxygen amorphous powder. The method combines the cooling after gas atomization and gas atomization to obtain amorphous powder with low oxygen and good sphericity, and the particle size range D50 of the prepared spherical amorphous powder is 5-30 mu m, and the oxygen content is less than 600 ppm.
The spherical amorphous alloy powder preparation device provided by the invention is characterized in that the existing gas atomization equipment is subjected to simple and easy-to-implement structural transformation, so that the alloy melt can be beaten and crushed by high-pressure gas, the metal liquid drops form spherical particles under the action of surface tension, and the particles are rapidly cooled by a cooling area formed by a cooling liquid (water) curtain, thereby obtaining spherical and low-oxygen amorphous powder. Referring to fig. 2-4, the preparation apparatus of the present invention includes an air atomizer 1 and a liquid cooling apparatus located below the air atomizer 1 and disposed at the periphery of an air flow nozzle of the air atomizer, and of course, the preparation apparatus of the present invention may further include a melting furnace for melting alloy, a tundish for containing alloy melt, a vacuum pump, a device for providing atomizing gas, a collecting device for collecting powder, and other devices for achieving atomized powder production.
The gas atomizer 1 crushes the alloy melt from the tundish with atomizing gas. The gas atomizer 1 used in the present invention may be a conventional apparatus used in the field of pulverization by atomization, and in the embodiment of the present invention, the gas atomizer 1 includes: the device comprises a body, a corresponding socket for inserting a liquid guide pipe 4, an air inlet pipe 2 for connecting atomizing gas, and an air flow nozzle 3 for spraying atomizing gas, wherein the liquid guide pipe 4 is used for connecting a tundish and an air atomizer 1 filled with alloy melt, the inner cavity of the liquid guide pipe 4 is inverted cone-shaped from top to bottom, the cone angle is 0-15 degrees, preferably, the inner cavity of the liquid guide pipe 4 is transited from the upside to the downside into a cylinder shape, and the cone angle of the inverted cone is 1-15 degrees (such as 2 degrees, 5 degrees, 7 degrees, 10 degrees, 12 degrees and 14 degrees). The direction of the air flow sprayed out from the air flow nozzle 3 forms an included angle of 40-50 degrees (such as 41 degrees, 43 degrees, 45 degrees, 47 degrees and 49 degrees) with the vertical direction (namely the axial direction of the liquid guide pipe) so as to ensure the atomization powder preparation effect and the particle size.
In the preferred embodiment of the invention, the upper end of the liquid guide tube 4 is communicated with the tundish, and the lower end seat of the liquid guide tube 4 is arranged on the corresponding socket of the gas atomizer 1, so that the alloy melt can be sprayed out from the bottom spray port of the liquid guide tube 4 to form a downward alloy melt flow 8, the inner cavity of the liquid guide tube 4 is changed into a cylinder shape from an upside to a downside, the cone angle of the upside is 10 degrees, and the cone structure can ensure that the alloy melt flow 8 has enough flow and pressure, thereby being beneficial to the gas atomization. Be provided with on the lateral wall of gas atomizer 1 and be used for letting in atomizing gas's intake pipe 2 in to gas atomizer 1, be provided with the air current nozzle 3 that is used for broken alloy melt liquid stream 8 around alloy melt outlet (being the bottom spout of catheter 4) in gas atomizer lower part, it can also be said, air current nozzle 3 is a plurality of, evenly set up in the lower bottom surface of gas atomizer 1 and around the bottom spout of catheter 4, a plurality of air current nozzles 3 are the annular setting, the direction of air current nozzle 3 blowout air current is 45 with vertical (being the axial of catheter), atomizing gas that gets into by intake pipe 2 reaches air current nozzle 3, it is broken with alloy melt liquid stream by this nozzle spun atomizing gas 9.
And the liquid cooling device is positioned below the gas atomizer 1 and arranged at the periphery of the airflow nozzle 3 of the gas atomizer 1 and used for cooling the crushed alloy powder intermediate of the gas atomizer 1 to form spherical amorphous alloy powder. The liquid cooling device of the present invention is any cooling device that can provide sufficient cooling rate for the crushed alloy powder intermediate, such as: the cooling device can be a double-wall cylindrical structure, the lower bottom surface of the cooling device is circumferentially provided with a cooling liquid outlet; or the cooling device is made of a material with good heat transfer, the cooling device can be a cylindrical structure such as a cylindrical, quadrangular or hexagonal cylinder, the cylinder wall is double-layer hollow, a space between double layers of walls is filled with cooling liquid such as liquid nitrogen, the lower bottom surface of the cooling device is not provided with a cooling liquid outlet, and the area in the middle of the cylinder of the cylindrical cooling device is a cooling area for cooling the alloy powder intermediate. The first cooling device forming the cooling water curtain has a vertical height smaller than that of the second cooling device. The liquid cooling device is arranged at the periphery of the airflow nozzle 3 in an annular shape, and the upper end of the liquid cooling device can be fixed on the lower bottom surface of the gas atomizer 1 and can also be arranged independently of the gas atomizer 1. Preferably, the surface of the cylinder wall is smooth or coated with a smooth coating so that the powder particles do not stick to the cylinder wall.
In a preferred embodiment of the present invention, the liquid cooling device is annularly disposed around the air flow nozzle 3, the upper end of the liquid cooling device is fixed on the lower bottom surface of the gas atomizer 1, the lower bottom surface of the liquid cooling device has a cooling liquid outlet, and the cooling liquid is water, so the cooling device is also called a water cooling device 6, the water cooling device 6 further includes a water inlet pipe 7 for water inlet, the water inlet pipe is disposed on the sidewall of the water cooling device 6 to supply cooling water to the inside of the water cooling device, the cooling water flows out from the cooling liquid outlet downwards to form an annular cooling water curtain 10, the inside of the cooling water curtain 10 is a cooling area for cooling the alloy powder intermediate to form the amorphous alloy powder 11. According to the invention, the annular water cooling device 6 is additionally arranged below the gas atomizer, the annular water cooling device 6 is positioned outside the gas flow nozzle 3, and the water cooling device 6 can flow out or spray cooling water downwards to ensure that a cooling area surrounded by the annular water curtain has proper temperature, so that alloy droplets passing through the cooling area are cooled to form amorphous powder. The alloy melt is sprayed out through the spraying port at the bottom of the liquid guide pipe 4, after the alloy melt is beaten by high-pressure gas and broken into small metal liquid drops, the cooling speed of the gas is far lower than that of water, so that the metal liquid drops form spherical powder particles under the action of surface tension, the powder particles are sprayed out through the annular water cooling device below the atomizer in the falling process to form a cooling water curtain 10, and the spherical particles are rapidly cooled to obtain amorphous alloy powder 11.
The preparation device is suitable for preparing various amorphous alloy powders, and is particularly suitable for preparing FeSiB amorphous alloy powders; preferably, the amorphous alloy powder comprises the following components in percentage by mass: si: 1-14%, B: 7-15%, C: less than or equal to 4 percent, Cu: less than or equal to 3 percent, Nb: less than or equal to 4 percent, P: less than or equal to 2 percent, and the balance of Fe and inevitable impurities; for example, the FeSiB amorphous alloy powder is AP01, AP02 or AP03 alloy powder; the AP01 alloy powder comprises the following chemical components in percentage by mass: cu: 1%, Nb: 3%, Si: 13.5%, B: 9%, Fe: the balance and unavoidable impurities; the AP02 alloy comprises the following chemical components in percentage by mass: cu: 1%, Nb: 1%, Si: 4%, B: 9%, C: 0.3%, Fe: the balance and unavoidable impurities; the AP03 alloy comprises the following chemical components in percentage by mass: cu: 1.2%, Si: 2%, B: 12%, P: 2%, Fe: the balance and inevitable impurities.
The invention also provides a preparation method of the spherical amorphous alloy powder, which comprises the following steps:
s1: putting metal raw materials into a vacuum medium-frequency induction furnace for heating and melting, wherein the temperature of molten steel is selected according to different materials; generally, the raw material is melted by heating to 1300 to 1600 ℃, preferably at a temperature higher than the melting point of the raw material by 50 to 250 ℃, more preferably 150 to 200 ℃, and the degree of vacuum is controlled to be less than 10Pa (for example, 9Pa, 7Pa, 6Pa, 1Pa, 0.1Pa) to obtain the alloy melt;
s2: atomizing the alloy melt by adopting inert atomizing gas in vacuum or inert atmosphere to obtain an alloy powder intermediate;
preferably, during the atomization treatment, an appropriate atomization pressure is selected according to the particle size requirement, and the atomization gas pressure (i.e. the ejection pressure of the gas for atomization) is 2-6 Mpa (such as 2.5Pa, 3Pa, 4Pa, 5Pa, 5.5 Pa); the vacuum degree during the atomization treatment is controlled to be less than or equal to 10Pa (such as 9Pa, 7Pa, 6Pa, 1Pa and 0.1 Pa); the inert atomizing gas is nitrogen or argon.
S3: the alloy powder intermediate enters a cooling area to be cooled, and the spherical amorphous alloy powder is obtained; preferably, the cooling rate is 106K/s or more (e.g. 2 x 10)6K/s、4*106K/s、6*106K/s、8*106K/s、9*106K/s、2*107K/s、4*107K/s、6*107K/s、8*107K/s、9*107K/s); more preferably, the cooling rate is 106-107K/s。
The preparation method of the present invention is further described by the following embodiments, and the following embodiments of the preparation method all adopt the preparation device of the present invention, wherein the direction of the air flow sprayed out from the air flow nozzle 3 forms 45 degrees with the vertical direction (i.e. the axial direction of the liquid guide tube), the inner cavity of the liquid guide tube 4 is changed into a cylinder shape from an inverted cone shape from top to bottom, the cone angle of the inverted cone shape is 10 degrees, the cooling liquid is water, and the liquid cooling device can form a cooling water curtain.
Example 1
This example produces an amorphous AP01 powder having the chemical composition (in mass percent) of: cu: 1%, Nb: 3%, Si: 13.5%, B: 9%, Fe: and (4) the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) heating the raw materials to 1325 ℃ to melt under the environment atmosphere of 5Pa of vacuum degree to obtain alloy melt;
(2) atomizing by using argon as atomizing gas under the environment of 5Pa of vacuum degree to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomizing temperature (namely the temperature of alloy melt in a tundish) is 1320 ℃, and the pressure of the atomizing gas is 2.2 Mpa;
(3) the alloy powder intermediate enters a cooling zone formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 106And K/s or above, and finally collecting the amorphous alloy powder.
When the alloy powder was observed by a Scanning Electron Microscope (SEM) and the photograph is shown in FIG. 5, it can be seen that the sphericity of the alloy powder prepared by the method of the present invention was very good, the particle size D50:28 μm. The oxygen content of the alloy powder was 319 ppm.
An XRD pattern is obtained by X-ray diffraction analysis, and referring to figure 6, the detected powder has no obvious diffraction peak and is amorphous alloy powder.
Comparative example 1
In the comparative example 1, the existing gas atomization equipment is adopted for preparing powder, the raw materials and the processes in the first two steps are the same as those in the example 1, and only the cooling step in the step (3) is omitted in the comparative example. The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), see fig. 7, and it can be seen from the figure that the sphericity of the powder was deteriorated due to the decrease in the cooling rate. The particle size D50 was 23 μm and the oxygen content was 613 ppm.
The XRD pattern was obtained by X-ray diffraction analysis, see fig. 8. As can be seen from the figure, the alloy powder prepared in this comparative example had a diffraction peak and the powder began to crystallize.
Example 2:
in this example, an AP02 amorphous alloy powder was prepared, which had the following chemical composition (by mass percent): cu: 1%, Nb: 1%, Si: 4%, B: 9%, C: 0.3%, Fe: and (4) the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) heating the raw materials to 1425 ℃ to melt under the environment atmosphere of 8Pa of vacuum degree, so as to obtain alloy melt;
(2) atomizing by using argon as atomizing gas under the environment of vacuum degree of 8Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomizing temperature (namely the temperature of alloy melt in a tundish) is 1420 ℃, and the pressure of the atomizing gas is 6 Mpa;
(3) the alloy powder intermediate enters a cooling zone formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 106And K/s or above, and finally collecting the amorphous alloy powder.
When the alloy powder was observed by a Scanning Electron Microscope (SEM) and the photograph is shown in FIG. 9, it can be seen that the sphericity of the alloy powder prepared by the method of the present invention was very good, and the particle size D50:10 μm. The oxygen content of the alloy powder was 503 ppm.
An XRD pattern is obtained by X-ray diffraction analysis, and referring to figure 10, the detected powder has no obvious diffraction peak and is amorphous alloy powder.
Comparative example 2
The comparative example 2 adopts the existing gas atomization equipment (namely, no liquid cooling device) to prepare powder, the raw materials and the processes in the first two steps are the same as those in the example 2, and the cooling step in the step (3) is omitted. The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), and as can be seen from fig. 11, irregular-shaped particles in the powder were significantly increased and the degree of sphericity was deteriorated due to the decrease in the cooling rate. The particle size D50 was 11 μm and the oxygen content was 762 ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and referring to FIG. 12, it can be seen that the alloy powder prepared by this comparative example had diffraction peaks and the powder began to crystallize.
Example 3:
in this example, an AP03 amorphous alloy powder was prepared, which had the following chemical composition (by mass percent): cu: 1.2%, Si: 2%, B: 12%, P: 2%, Fe: and (4) the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) heating the raw materials to 1385 ℃ under the environment atmosphere of 3Pa of vacuum degree to melt the raw materials to obtain alloy melt;
(2) atomizing by using argon as atomizing gas under the environment of vacuum degree of 3Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomizing temperature (namely the temperature of alloy melt in a tundish) is 1380 ℃, and the pressure of the atomizing gas is 3.6 Mpa;
(3) the alloy powder intermediate enters a cooling zone formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 106And K/s or above, and finally collecting the amorphous alloy powder.
When the alloy powder was observed by a Scanning Electron Microscope (SEM), referring to FIG. 13, it was found that the sphericity of the alloy powder prepared by the method of the present invention was very good, and the particle size D50:17 μm. The oxygen content of the alloy powder was 361 ppm.
An XRD pattern is obtained by X-ray diffraction analysis, and referring to figure 14, the detected powder has no obvious diffraction peak and is amorphous alloy powder.
Comparative example 3
The comparative example 3 adopts the existing gas atomization equipment to prepare powder, the raw materials and the processes in the first two steps are the same as those in the example 3, and only the cooling step in the step (3) is omitted. The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), and as can be seen from fig. 15, irregular-shaped particles in the powder were significantly increased and the degree of sphericity was deteriorated due to the decrease in the cooling rate. The particle size D50 was 18 μm and the oxygen content was 537 ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and it can be seen from FIG. 16 that the alloy powder prepared in this comparative example had diffraction peaks and the powder began to crystallize.
Small knot
The powder obtained in examples 1-3 has no obvious diffraction peak and is amorphous alloy powder, while the powder obtained in comparative examples 1-3 has obvious diffraction peak and is crystallized, so that the atomization powder preparation device can obtain amorphous powder with more uniform particle size, more regular sphere and less oxygen content. In addition, the method and the device can obtain the spherical amorphous powder with larger relative size, can improve the magnetic conductivity, and are particularly suitable for preparing the FeSiB amorphous alloy powder.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (10)
1. A spherical amorphous alloy powder preparation device, the preparation device includes:
the gas atomizer is used for crushing the alloy melt by adopting atomizing gas;
and the liquid cooling device is positioned below the gas atomizer, arranged at the periphery of an airflow nozzle of the gas atomizer and used for cooling the alloy powder intermediate after the gas atomizer is crushed to form spherical amorphous alloy powder.
2. The production apparatus according to claim 1, further comprising a liquid guiding pipe connecting a tundish containing the alloy melt and the gas atomizer;
preferably, the upper end of the liquid guide pipe is communicated with the tundish;
preferably, the lower end part of the liquid guide pipe is seated on a corresponding socket of the gas atomizer;
preferably, the inner cavity of the liquid guide pipe is in an inverted cone shape from top to bottom, and the cone angle is 0-15 degrees;
preferably, the cavity of the catheter is changed into a cylinder shape from an inverted cone from top to bottom, and the cone angle is 1-15 degrees.
3. The manufacturing apparatus according to claim 1,
the side wall of the gas atomizer is provided with a gas inlet pipe for introducing the atomizing gas into the gas atomizer;
preferably, a gas flow nozzle for crushing the alloy melt is arranged at the lower part of the gas atomizer around an alloy melt outlet;
preferably, the airflow nozzle is annularly arranged;
preferably, the direction of the airflow sprayed by the airflow nozzle forms an included angle of 40-50 degrees with the vertical direction.
4. The manufacturing apparatus according to claim 1,
the liquid cooling device is annularly arranged on the periphery of the airflow nozzle and is used for forming an annular cooling area for cooling the alloy powder intermediate;
preferably, the liquid cooling device is a cylindrical structure with double walls, and a cooling liquid outlet is arranged on the lower bottom surface of the liquid cooling device and used for allowing cooling liquid to flow downwards to form a cooling liquid curtain, wherein the cooling liquid curtain forms an annular cooling area for cooling the alloy powder intermediate, and more preferably, the cooling liquid is water; or the liquid cooling device is a cylindrical structure with double walls, the space between the double walls is filled with cooling liquid, the hollow area of the cylindrical structure is an annular cooling area for cooling the alloy powder intermediate, and more preferably, the cooling liquid is liquid nitrogen;
preferably, the liquid cooling device is fixed on the lower bottom surface of the gas atomizer;
preferably, a liquid inlet pipe for injecting cooling liquid into the liquid cooling device is arranged on the side wall of the liquid cooling device.
5. The manufacturing apparatus according to claim 1,
the amorphous alloy powder is FeSiB amorphous alloy powder; preferably, the amorphous alloy powder comprises the following components in percentage by mass: si: 1-14%, B: 7-15%, C: less than or equal to 4 percent, Cu: less than or equal to 3 percent, Nb: less than or equal to 4 percent, P: less than or equal to 2 percent, and the balance of Fe and inevitable impurities;
more preferably, the FeSiB amorphous alloy powder is AP01, AP02 or AP03 alloy powder;
the AP01 alloy powder comprises the following chemical components in percentage by mass: cu: 1%, Nb: 3%, Si: 13.5%, B: 9%, Fe: the balance and unavoidable impurities;
the AP02 alloy comprises the following chemical components in percentage by mass: cu: 1%, Nb: 1%, Si: 4%, B: 9%, C: 0.3%, Fe: the balance and unavoidable impurities;
the AP03 alloy comprises the following chemical components in percentage by mass: cu: 1.2%, Si: 2%, B: 12%, P: 2%, Fe: the balance and inevitable impurities.
6. A preparation method of spherical amorphous alloy powder comprises the following steps:
s1: melting the raw materials to obtain an alloy melt;
s2: atomizing the alloy melt by adopting inert atomizing gas in vacuum or inert atmosphere to obtain an alloy powder intermediate;
s3: and cooling the alloy powder intermediate in a cooling area to obtain the spherical amorphous alloy powder.
7. The method according to claim 6,
in step S1, melting the raw material at a temperature 50 to 250 ℃ higher than the melting point of the raw material to obtain the molten alloy;
preferably, in step S1, the raw material is melted at a temperature 150 to 200 ℃ higher than the melting point of the raw material to obtain the alloy melt.
8. The method according to claim 6,
in step S2, during the atomization process, the pressure of the atomization gas is 2 to 6 Mpa;
the vacuum degree during the atomization treatment is controlled to be below 10 Pa;
preferably, in step S2, the inert atomizing gas is nitrogen or argon;
preferably, in step S3, the cooling rate is 106K/s or more;
preferably, the cooling rate is 106-107K/s。
9. The method according to any one of claims 6 to 8,
the method for preparing spherical amorphous alloy powder is carried out by using the apparatus for preparing spherical amorphous alloy powder according to any one of claims 1 to 5.
10. A spherical amorphous alloy powder, which is prepared by the spherical amorphous alloy powder preparation device according to any one of claims 1 to 5 or the spherical amorphous alloy powder preparation method according to any one of claims 6 to 8.
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| CN112743094A (en) * | 2020-12-29 | 2021-05-04 | 南通金源智能技术有限公司 | Preparation method and device of novel superfine amorphous magnetic powder |
| WO2021139553A1 (en) * | 2020-05-27 | 2021-07-15 | 安泰（霸州）特种粉业有限公司 | Spherical amorphous alloy powder preparation apparatus and method |
| CN113369485A (en) * | 2021-06-10 | 2021-09-10 | 盘星新型合金材料(常州)有限公司 | Pilot-scale atomization furnace, Fe-based amorphous alloy powder and preparation method thereof |
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