CN111534765B - Spherical amorphous alloy powder preparation device and method - Google Patents
Spherical amorphous alloy powder preparation device and method Download PDFInfo
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- CN111534765B CN111534765B CN202010463311.7A CN202010463311A CN111534765B CN 111534765 B CN111534765 B CN 111534765B CN 202010463311 A CN202010463311 A CN 202010463311A CN 111534765 B CN111534765 B CN 111534765B
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- 239000000843 powder Substances 0.000 title claims abstract description 172
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims description 28
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 105
- 239000000956 alloy Substances 0.000 claims abstract description 105
- 238000001816 cooling Methods 0.000 claims abstract description 105
- 239000007789 gas Substances 0.000 claims abstract description 72
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 238000000889 atomisation Methods 0.000 claims description 29
- 239000000110 cooling liquid Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000012809 cooling fluid Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 16
- 230000000052 comparative effect Effects 0.000 description 20
- 238000002441 X-ray diffraction Methods 0.000 description 19
- 239000000498 cooling water Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- 238000009689 gas atomisation Methods 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000012387 aerosolization Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910000889 permalloy Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/086—Cooling after atomisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/086—Cooling after atomisation
- B22F2009/0872—Cooling after atomisation by water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/088—Fluid nozzles, e.g. angle, distance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0888—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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/02—Amorphous
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Disintegrating Or Milling (AREA)
- Powder Metallurgy (AREA)
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; the liquid cooling device is positioned below the gas atomizer and arranged on the periphery of the gas flow nozzle of the gas atomizer and is used for cooling the alloy powder intermediate after the gas atomizer is broken 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 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 (5) cooling the alloy powder intermediate in a cooling area to obtain spherical amorphous alloy powder. The spherical amorphous alloy powder with more uniform granularity, more regular spheres 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 an air atomization water cooling process.
Background
Atomization milling is a powder preparation process in which a rapidly moving atomizing medium (typically high pressure water or gas) is used to break up a metal or alloy liquid into fine droplets, followed by condensation into a solid powder. The shape of the powder obtained varies greatly, due to the method by which the powder is produced.
The amorphous alloy product has high saturation magnetic induction intensity and high magnetic permeability, solves the adverse effect of defects such as crystal grains, crystal boundaries, dislocation, interstitial atoms, magnetocrystalline anisotropy and the like on soft magnetic performance, has excellent magnetic property, corrosion resistance, wear resistance, high intensity, hardness, high resistivity and electric coupling performance when being used for manufacturing transformers, mutual inductors, inductance elements and the like, has a certain production scale in the countries such as the United states, japan, germany and the like at present, and a large amount of amorphous alloy gradually replaces permalloy and ferrite to be rushed into markets. With the development of high frequency and miniaturization of electronic devices, the market demands for soft magnetic powder with high magnetic permeability and low loss at high frequency are also becoming more and more demanding. Therefore, the preparation of spherical, low-oxygen amorphous powders is critical to the solution of the problem.
At present, two main ways of preparing amorphous soft magnetic powder are: (1) a belt crushing method; (2) atomization method. The amorphous powder prepared by adopting the amorphous strip crushing method is easy to puncture an insulating layer coated on the surface of the powder due to a large number of powder edges, so that the market expansion of the amorphous powder is limited. The amorphous powder photograph produced by the ribbon crushing process is shown in FIG. 1. The prior device for preparing amorphous powder by an atomization method is shown in fig. 2, and comprises an atomizer 1, an air inlet pipe 2, an air flow nozzle 3, a liquid guide pipe 4 and a melt nozzle 5.
Disclosure of Invention
An object of the present invention is to provide an apparatus for producing spherical amorphous alloy powder which is strong in the amorphous forming ability of the alloy and can ensure that the powder formed has good sphericity and low oxygen content.
The second purpose of the invention is to provide a preparation method of 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 high magnetic permeability and low loss of the amorphous powder under high frequency of electronic devices.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the first aspect of the present invention provides a spherical amorphous alloy powder production apparatus, comprising:
the gas atomizer is used for crushing the alloy melt by adopting atomizing gas;
the liquid cooling device is positioned below the gas atomizer and arranged at the periphery of the gas flow nozzle of the gas atomizer, and is used for cooling the alloy powder intermediate after the gas atomizer is broken to form spherical amorphous alloy powder.
In some embodiments, the preparation device further comprises a catheter connecting the tundish containing the alloy melt and the aerosolizer.
In some embodiments, the catheter upper end communicates with the tundish.
In some embodiments, the catheter lower end seats against a corresponding socket of the aerosolizer.
In some embodiments, the lumen of the catheter is inverted tapered from top to bottom with a taper angle of 0-15 °.
In some embodiments, the lumen of the catheter transitions from a reverse taper to a cylindrical shape with a taper angle of 1-15 °.
In some embodiments, an air inlet pipe for introducing the atomizing gas into the gas atomizer is arranged on the side wall of the gas atomizer.
In some embodiments, an air flow nozzle for breaking up the alloy melt is provided around the alloy melt outlet in a lower portion of the air atomizer.
In some embodiments, the air flow nozzles are arranged in a ring.
In some embodiments, the direction of the air flow ejected by the air flow nozzle forms an included angle of 40-50 degrees with the vertical direction.
In some embodiments, the liquid cooling device is annularly arranged at the periphery of the airflow nozzle and is 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 is used for enabling cooling liquid to flow downwards to form a cooling liquid curtain, and the cooling liquid curtain forms an annular cooling zone 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 having double walls, the space between the double walls being filled with a cooling liquid, and the hollow region of the cylindrical structure is an annular cooling region for cooling the alloy powder intermediate.
In some embodiments, the cooling liquid is liquid nitrogen.
In some embodiments, the liquid cooling device is secured to a lower bottom surface of the aerosolizer.
In some embodiments, a liquid inlet pipe for injecting cooling liquid into the liquid cooling device is arranged on the side wall of 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 unavoidable 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 unavoidable impurities.
The second aspect of the present invention provides a method for producing spherical amorphous alloy powder, the method comprising the steps of:
s1: melting the raw materials to obtain 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 the alloy powder intermediate enters a cooling zone for cooling 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 150 to 200 ℃ above the melting point of the raw material to obtain the alloy melt.
In some embodiments, in the step S2, the pressure of the atomizing gas is 2 to 6Mpa during the atomizing treatment; 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 rate of cooling is 10 6 K/s or more.
In some embodiments, the cooling rate is 10 6 -10 7 K/s。
In some embodiments, the spherical amorphous alloy powder production method is performed using the spherical amorphous alloy powder production apparatus of the first aspect of the invention.
According to a third aspect of the present invention, there is provided a spherical amorphous alloy powder produced by the spherical amorphous alloy powder production apparatus according to the first aspect of the present invention or the spherical amorphous alloy powder production method 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 invention has the advantages that the method for preparing spherical low-oxygen amorphous powder is found by improving the structure of the atomizer, the method is simple and easy to implement, and the structure can be improved on the basis of the original atomizer, so that the cost is low and the efficiency is high. The spherical low-oxygen amorphous powder can be widely applied to the field of high-frequency and miniaturized electronic devices, and has good market prospect. The granularity range D50 of the spherical amorphous powder prepared by the method is 5-30 mu m, and the oxygen content is below 600 ppm.
Drawings
FIG. 1 is a photograph of amorphous powder prepared by a prior art tape crushing method.
Fig. 2 is a schematic structural diagram of a prior art spherical amorphous alloy powder preparation apparatus.
Fig. 3 is a schematic structural view of a spherical amorphous alloy powder preparation apparatus according to some embodiments of the present invention.
FIG. 4 is a schematic diagram showing the structure and the use state of the apparatus for preparing spherical amorphous alloy powder shown in FIG. 3.
Fig. 5 is an SEM scanning electron micrograph of the amorphous alloy powder prepared in example 1 of the present invention.
Fig. 6 is an XRD pattern of 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 an SEM scanning electron micrograph of the amorphous alloy powder prepared in example 2 of the present invention.
Fig. 10 is an XRD pattern of 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 an SEM scanning electron micrograph of the amorphous alloy powder prepared in example 3 of the present invention.
Fig. 14 is an XRD pattern of amorphous alloy powder prepared in example 3 of the present invention.
FIG. 15 is an SEM photograph of the alloy powder prepared in comparative example 3 of the present invention.
FIG. 16 is an XRD pattern of alloy powder prepared in comparative example 3 of the present invention.
The device comprises a 1-gas atomizer, a 2-gas inlet pipe, a 3-gas flow nozzle, a 4-liquid guide pipe, a 5-melt nozzle, a 6-water cooling device, a 7-water inlet pipe, an 8-alloy melt liquid flow, 9-sprayed atomized gas, a 10-cooling water curtain and 11-amorphous alloy powder.
The XRD patterns of fig. 6, 8, 10, 12, 14, 16 have an abscissa of 2θ (twice the incident angle of x-rays) and an ordinate of diffraction intensity.
Detailed Description
For the purpose of making 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 existing amorphous powder prepared by water atomization has poor sphericity and high oxygen content, and the oxygen content can reach about 2000 ppm. With the gas atomization process, the sphericity and oxygen content of the powder are improved, but with the gas atomization process, the amorphous formation is difficult, especially with some larger size powder particles, which is more difficult. The invention provides an atomization powder preparation device and an atomization powder preparation method, which can obtain spherical low-oxygen amorphous powder. The invention combines the gas atomization and the cooling after the gas atomization, can obtain the amorphous powder with low oxygen and good sphericity, and the granularity range D50 of the prepared spherical amorphous powder is 5-30 mu m, and the oxygen content is below 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, alloy melt can be subjected to high-pressure gas striking and crushing, 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, so that spherical and low-oxygen amorphous powder is obtained. Referring to fig. 2 to 4, the preparation apparatus of the present invention includes an air atomizer 1 and a liquid cooling apparatus disposed 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 holding alloy melt, a vacuum pump, an apparatus for supplying atomized gas, an apparatus for collecting powder, and the like for realizing atomized pulverization, and since these apparatuses are all conventional apparatuses for atomized pulverization, they will not be described in detail herein, and only the portions closely related to the realization of the object of the present invention will be described in detail below.
The gas atomizer 1 breaks up the alloy melt from the tundish using atomizing gas. The gas atomizer 1 used in the present invention may be a conventional apparatus used in the field of atomizing pulverization, and in the embodiment of the present invention, the gas atomizer 1 includes: the body is used for being inserted into a corresponding socket of the liquid guide pipe 4, is used for being connected with the air inlet pipe 2 of atomizing air, is used for spraying out the air flow nozzle 3 of atomizing air, the liquid guide pipe 4 is used for connecting a tundish filled with alloy melt and the air atomizer 1, the inner cavity of the liquid guide pipe 4 is in an inverted cone shape from top to bottom, the cone angle is 0-15 degrees, preferably, the inner cavity of the liquid guide pipe 4 is in a cylindrical shape in a transition mode from top to bottom from the inverted cone shape, 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), and the cone structure can ensure that the alloy melt flow 8 has enough flow and pressure, so that the air atomization is facilitated. The direction of the air flow sprayed by 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 tube) so as to ensure the atomizing powder making effect and granularity.
In the preferred embodiment of the invention, the upper end of the liquid guide pipe 4 is communicated with the tundish, the lower end part of the liquid guide pipe 4 is arranged at the corresponding socket of the gas atomizer 1, therefore, alloy melt can be sprayed out from the bottom spraying outlet of the liquid guide pipe 4 to form a downward alloy melt flow 8, the inner cavity of the liquid guide pipe 4 is transited from the reverse taper shape to the cylindrical shape from top to bottom, the taper angle of the reverse taper shape is 10 degrees, and the taper structure can ensure that the alloy melt flow 8 has enough flow and pressure, thereby being beneficial to gas atomization. The side wall of the gas atomizer 1 is provided with an air inlet pipe 2 for introducing atomizing gas into the gas atomizer 1, the lower part of the gas atomizer is provided with a plurality of gas flow nozzles 3 for crushing the alloy melt liquid flow 8 around an alloy melt outlet (namely, a bottom ejection port of the liquid guide pipe 4), the plurality of gas flow nozzles 3 are uniformly arranged on the lower bottom surface of the gas atomizer 1 and around the bottom ejection port of the liquid guide pipe 4, the plurality of gas flow nozzles 3 are annularly arranged, the direction of the gas flow ejected by the gas flow nozzles 3 is 45 degrees with the vertical direction (namely, the axial direction of the liquid guide pipe), the atomizing gas entering from the air inlet pipe 2 reaches the gas flow nozzles 3, and the alloy melt liquid flow is crushed by the atomizing gas 9 ejected by the nozzles.
The liquid cooling device is positioned below the gas atomizer 1 and arranged at the periphery of the gas flow nozzle 3 of the gas atomizer 1, and is used for cooling the alloy powder intermediate after the gas atomizer 1 is broken to form spherical amorphous alloy powder. The liquid cooling device of the present invention is any cooling device that can provide a sufficient cooling rate for the crushed alloy powder intermediate, such as: the cooling device can form a cooling area surrounded by cooling liquid sprayed from a cooling liquid outlet, the alloy powder intermediate just passes through the cooling area, the cooling liquid can be water, and the cooling device can be of a double-wall cylindrical structure with the lower bottom surface provided with the cooling liquid outlet in the circumferential direction; or the cooling device is made of good heat transfer material, the cooling device can be a cylindrical or quadrangular cylinder or a hexagonal cylinder and the like, the cylinder wall is double-layer hollow, the space between the double-layer walls is filled with cooling liquid such as liquid nitrogen and the like, 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 a cooling water curtain has a vertical height that is smaller than that of the second cooling device. The liquid cooling device is annularly arranged on the periphery of the air flow nozzle 3, and the upper end of the liquid cooling device can be fixed on the lower bottom surface of the air atomizer 1 or can be arranged independently of the air atomizer 1. Preferably, the wall surface is smooth or coated with a lubricious coating so that the powder particles do not adhere to the wall.
In a preferred embodiment of the present invention, the liquid cooling device is annularly disposed on the periphery of the air flow nozzle 3, the upper end of the liquid cooling device is fixed on the lower bottom surface of the air atomizer 1, the lower bottom surface of the liquid cooling device is provided with a cooling liquid outlet, and the cooling liquid adopts water, so the cooling device is also called a water cooling device 6, the water cooling device 6 further comprises a water inlet pipe 7 for water inlet, which is disposed on the side wall of the water cooling device 6, so as to supply cooling water to the inside of the water cooling device, the cooling water flows downwards from the cooling liquid outlet to form an annular cooling water curtain 10, and the inside of the cooling water curtain 10 is a cooling area for cooling the alloy powder intermediate to form amorphous alloy powder 11. According to the invention, an annular water cooling device 6 is added below the air atomizer, the annular water cooling device 6 is positioned at the outer side of the air flow nozzle 3, and cooling water can flow downwards or be sprayed out from the water cooling device 6, so that a cooling area surrounded by an annular water curtain is ensured to have proper temperature, and alloy small liquid drops passing through the cooling area are cooled to form amorphous powder. When the alloy melt is sprayed out through the spraying port at the bottom of the liquid guide pipe 4 and is beaten and broken into small metal liquid drops by high-pressure gas, the gas cooling speed 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 pass through the cooling water curtain 10 sprayed out by the annular water cooling device below the atomizer in the falling process, and the spherical particles are rapidly cooled to obtain amorphous alloy powder 11.
The preparation device is suitable for preparing various amorphous alloy powder, in particular for preparing 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 unavoidable 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 unavoidable impurities.
The invention also provides a preparation method of the spherical amorphous alloy powder, which comprises the following steps:
s1: heating and melting metal raw materials in a vacuum intermediate frequency induction furnace, wherein the temperature of molten steel is selected according to different materials; heating to 1300-1600 deg.c, preferably to 50-250 deg.c, and more preferably 150-200 deg.c higher than the melting point of the material, and vacuum degree below 10Pa (9 Pa, 7Pa, 6Pa, 1Pa, 0.1 Pa) to obtain molten alloy;
s2: atomizing the alloy melt by adopting inert atomizing gas under vacuum or inert atmosphere to obtain an alloy powder intermediate;
preferably, during the atomization treatment, an appropriate atomization pressure is selected according to the granularity requirement, and the pressure of an atomization gas (namely, the spraying pressure of the gas for atomization) is 2-6 Mpa (such as 2.5Pa, 3Pa, 4Pa, 5Pa and 5.5 Pa); the vacuum degree during the atomization treatment is controlled to be less than 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 zone for cooling to obtain the spherical amorphous alloy powder; preferably the cooling rate is 10 6 K/s or more (e.g. 2 x 10 6 K/s、4*10 6 K/s、6*10 6 K/s、8*10 6 K/s、9*10 6 K/s、2*10 7 K/s、4*10 7 K/s、6*10 7 K/s、8*10 7 K/s、9*10 7 K/s); more preferably the cooling rate is 10 6 -10 7 K/s。
The preparation method of the present invention is further described by the following examples, which all use the preparation apparatus of the present invention, wherein the direction of the air flow ejected from the air flow nozzle 3 forms 45 ° with the vertical direction (i.e. the axial direction of the catheter), the inner cavity of the catheter 4 transitions from the inverted cone shape to the cylindrical shape from top to bottom, the cone angle of the inverted cone shape is 10 °, the cooling liquid is water, and the liquid cooling apparatus can form a cooling water curtain.
Example 1
The AP01 amorphous powder is prepared in this example, and its chemical components (in mass percent) are: cu:1%, nb:3%, si:13.5%, B:9%, fe: the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) Heating the raw materials to 1325 ℃ under the atmosphere of 5Pa of vacuum degree to melt to obtain alloy melt;
(2) Carrying out atomization treatment by adopting argon as atomization gas in an ambient atmosphere with the vacuum degree of 5Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomization temperature (i.e. the temperature of alloy melt in a tundish) is 1320 ℃, and the pressure of the atomization gas is 2.2MPa;
(3) The alloy powder intermediate enters a cooling area formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 10 6 And collecting amorphous alloy powder at last, wherein K/s is more than K.
When the alloy powder is observed by a Scanning Electron Microscope (SEM), and a photograph is shown in FIG. 5, the sphericity of the alloy powder prepared by the method of the invention is very good, and the granularity D50 is 28 mu m. The oxygen content of the alloy powder was 319ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and as seen in FIG. 6, the powder was an amorphous alloy powder without significant diffraction peaks.
Comparative example 1
This comparative example 1, in which the existing aerosolization apparatus was used for pulverizing, was identical to example 1 in both the raw material and the first two steps, and omitted only the cooling step of step (3). The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), and as can be seen from fig. 7, the sphericity of the powder was deteriorated due to the decrease in cooling rate. The particle size D50 was 23. Mu.m, and the oxygen content was 613ppm.
XRD patterns were obtained by X-ray diffraction analysis, see figure 8. As can be seen from the figure, the alloy powder prepared in this comparative example has already exhibited diffraction peaks and crystallization of the powder is started.
Example 2:
the chemical components (in mass percent) of the AP02 amorphous alloy powder are as follows: cu:1%, nb:1%, si:4%, B:9%, C:0.3%, fe: the balance. The elements not mentioned are unavoidable impurities.
The preparation method comprises the following steps:
(1) Heating the raw materials to 1425 ℃ under the ambient atmosphere with the vacuum degree of 8Pa, and melting to obtain alloy melt;
(2) Carrying out atomization treatment by adopting argon as atomization gas in an ambient atmosphere with the vacuum degree of 8Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomization temperature (namely the temperature of alloy melt in a tundish) is 1420 ℃, and the pressure of the atomization gas is 6MPa;
(3) The alloy powder intermediate enters a cooling area formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 10 6 And collecting amorphous alloy powder at last, wherein K/s is more than K.
When the alloy powder is observed by a Scanning Electron Microscope (SEM), the picture is shown in FIG. 9, and the sphericity of the alloy powder prepared by the method of the invention is very good, and the granularity D50 is 10 mu m. The oxygen content of the alloy powder was 503ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and as seen in FIG. 10, the powder was an amorphous alloy powder without significant diffraction peaks.
Comparative example 2
In this comparative example 2, the existing gas atomization apparatus (i.e., without a liquid cooling device) was used for pulverizing, and the raw materials and the former two steps were the same as those in example 2, and only the cooling step in step (3) was omitted in this comparative example. The alloy powder obtained in this comparative example was observed by a Scanning Electron Microscope (SEM), and as can be seen from fig. 11, irregularly shaped particles in the powder significantly increased and sphericity deteriorated due to a decrease in cooling rate. The particle size D50 was 11. Mu.m, and the oxygen content was 762ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and as can be seen from fig. 12, the alloy powder prepared in this comparative example had developed diffraction peaks and the powder started to crystallize.
Example 3:
the chemical components (according to mass percent) of the AP03 amorphous alloy powder are as follows: cu:1.2%, si:2%, B:12%, P:2%, fe: 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 atmosphere of 3Pa of vacuum degree to melt to obtain alloy melt;
(2) Carrying out atomization treatment by adopting argon as atomization gas in an ambient atmosphere with the vacuum degree of 3Pa to obtain a crushed and spheroidized alloy powder intermediate, wherein the atomization temperature (namely the temperature of alloy melt in a tundish) is 1380 ℃, and the pressure of the atomization gas is 3.6MPa;
(3) The alloy powder intermediate enters a cooling area formed by a cooling water curtain downwards for cooling, and the cooling speed is 2 x 10 6 And collecting amorphous alloy powder at last, wherein K/s is more than K.
As can be seen from a Scanning Electron Microscope (SEM) observation of the alloy powder, referring to FIG. 13, the alloy powder prepared by the method of the present invention has very good sphericity and a particle size D50: 17. Mu.m. The oxygen content of the alloy powder was 361ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and as seen in FIG. 14, the powder was an amorphous alloy powder without significant diffraction peaks.
Comparative example 3
This comparative example 3, in which the existing aerosolization apparatus was used for pulverizing, was identical to example 3 in both the raw material and the first two steps, and only the cooling step of step (3) was 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, irregularly shaped particles in the powder significantly increased and sphericity deteriorated due to a decrease in cooling rate. The particle size D50 was 18. Mu.m, and the oxygen content was 537ppm.
The XRD pattern was obtained by X-ray diffraction analysis, and as can be seen from fig. 16, the alloy powder prepared in this comparative example had developed diffraction peaks and the powder started to crystallize.
Knot (S)
The powder obtained in examples 1 to 3 had no obvious diffraction peak, and the powder obtained in comparative examples 1 to 3 had obvious diffraction peak, and the powder was crystallized, so that it was found that the atomized powder preparation apparatus of the present invention could obtain amorphous powder having more uniform particle size, more regular spherical shape and less oxygen content. In addition, the method and the device can obtain spherical amorphous powder with larger relative size, can improve magnetic permeability, and are particularly suitable for preparing FeSiB amorphous alloy powder.
It will be appreciated by those skilled in the art that the present invention can be carried out in other embodiments without departing from the spirit or essential characteristics thereof. Accordingly, the above disclosed embodiments are illustrative in all respects, and not exclusive. All changes that come within the scope of the invention or equivalents thereto are intended to be embraced therein.
Claims (17)
1. A spherical amorphous alloy powder preparation device, characterized in that the preparation device comprises:
the gas atomizer is used for crushing the alloy melt by adopting atomizing gas;
an air flow nozzle for crushing the alloy melt is arranged around the alloy melt outlet at the lower part of the air atomizer; the direction of the airflow sprayed by the airflow nozzle forms an included angle of 40-50 degrees with the vertical direction;
the liquid cooling device is positioned below the gas atomizer and arranged at the periphery of the gas flow nozzle of the gas atomizer, and is used for cooling the alloy powder intermediate crushed by the gas atomizer to form spherical amorphous alloy powder;
the liquid cooling device is annularly arranged at the periphery of the airflow nozzle and is used for forming an annular cooling area for cooling the alloy powder intermediate; the cooling rate is 10 6 K/s or more;
the liquid cooling device is of a cylindrical structure with double walls, a cooling liquid outlet is formed in the lower bottom surface of the liquid cooling device and used for enabling 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; or the liquid cooling device is of a cylindrical structure with double walls, the space between the double walls is filled with cooling liquid, and a hollow area of the cylindrical structure is an annular cooling area for cooling the alloy powder intermediate;
the preparation device also comprises a liquid guide tube, and is connected with the tundish filled with the alloy melt and the gas atomizer; the inner cavity of the catheter is transited from an inverted cone shape to a cylindrical shape from top to bottom, and the cone angle is 1-15 degrees;
the amorphous alloy powder is FeSiB amorphous alloy powder;
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 unavoidable impurities;
the granularity range D50 of the prepared spherical amorphous powder is 17-28 mu m.
2. The preparation device according to claim 1, wherein the upper end of the catheter is in communication with the tundish.
3. The preparation device according to claim 1, wherein the lower end of the catheter is seated in a corresponding socket of the aerosolizer.
4. The apparatus according to claim 1, wherein an air inlet pipe for introducing the atomizing gas into the atomizer is provided on a side wall of the atomizer.
5. The preparation device according to claim 1, wherein the gas flow nozzles are arranged in a ring shape.
6. The manufacturing apparatus of claim 1, wherein the cooling fluid is water.
7. The manufacturing apparatus of claim 1, wherein the cooling liquid is liquid nitrogen.
8. The apparatus according to claim 1, wherein the liquid cooling device is fixed to a lower bottom surface of the atomizer.
9. The apparatus according to claim 1, wherein a liquid inlet pipe for injecting a cooling liquid into the liquid cooling apparatus is provided on a side wall of the liquid cooling apparatus.
10. A method for preparing spherical amorphous alloy powder, which is characterized by comprising the following steps:
s1: melting the raw materials to obtain alloy melt;
s2: atomizing the alloy melt by adopting inert atomizing gas under vacuum or inert atmosphere to obtain an alloy powder intermediate;
s3: the alloy powder intermediate enters a cooling zone for cooling to obtain the spherical amorphous alloy powder;
in step S3, the cooling rate is 10 6 K/s or more;
the granularity range D50 of the prepared spherical amorphous powder is 17-28 mu m.
11. The method according to claim 10, wherein 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.
12. The production method according to claim 11, wherein in step S1, the raw material is melted at 150 to 200 ℃ higher than the melting point of the raw material to obtain the alloy melt.
13. The method of claim 10, wherein,
in the step S2, during the atomization treatment, the pressure of the atomization gas is 2-6 mpa;
the vacuum degree during the atomization treatment is controlled to be less than 10 Pa.
14. The method of claim 10, wherein in step S2, the inert atomizing gas is nitrogen or argon.
15. The method of claim 10, wherein the cooling is at a rate of 10 6 -10 7 K/s。
16. The method according to any one of claim 10 to 15,
the spherical amorphous alloy powder production method is carried out using the spherical amorphous alloy powder production apparatus according to any one of claims 1 to 9.
17. Spherical amorphous alloy powder, characterized in that it is produced according to the spherical amorphous alloy powder production apparatus according to any one of claims 1 to 9 or the spherical amorphous alloy powder production method according to any one of claims 10 to 16.
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| CN112170857B (en) * | 2020-09-30 | 2023-07-07 | 宁波中科毕普拉斯新材料科技有限公司 | Preparation method of fine alloy powder |
| 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 |
| 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 |
| CN113649581B (en) * | 2021-07-29 | 2023-05-12 | 南方科技大学 | Atomization system and solid powder preparation method |
| CN113652625B (en) * | 2021-08-17 | 2023-05-05 | 上海浦海求实电力新技术股份有限公司 | Electric power grid inner surface spraying material for diamond-type power distribution network and preparation method thereof |
| CN114589310A (en) * | 2022-03-11 | 2022-06-07 | 晶高优材(北京)科技有限公司 | Preparation method of micron spherical silver powder |
| CN116103577A (en) * | 2022-12-19 | 2023-05-12 | 中材人工晶体研究院(山东)有限公司 | Preparation method and device of diamond catalyst powder |
| CN116043138B (en) * | 2023-01-03 | 2024-09-13 | 深圳市铂科新材料股份有限公司 | Iron-based amorphous soft magnetic material and preparation method thereof |
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