CN116275066A - Water atomization iron silicon boron amorphous powder with excellent warm-pressing performance and application thereof - Google Patents
Water atomization iron silicon boron amorphous powder with excellent warm-pressing performance and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 119
- NFCWKPUNMWPHLM-UHFFFAOYSA-N [Si].[B].[Fe] Chemical compound [Si].[B].[Fe] NFCWKPUNMWPHLM-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000003825 pressing Methods 0.000 title claims abstract description 15
- 238000009692 water atomization Methods 0.000 title claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052742 iron Inorganic materials 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 229910008423 Si—B Inorganic materials 0.000 claims abstract description 19
- 229910052796 boron Inorganic materials 0.000 claims abstract description 19
- 239000010703 silicon Substances 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000292 calcium oxide Substances 0.000 claims abstract description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 7
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052918 calcium silicate Inorganic materials 0.000 claims description 4
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 4
- 238000010309 melting process Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
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- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
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- 230000005291 magnetic effect Effects 0.000 abstract description 29
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- 238000000889 atomisation Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 229910001004 magnetic alloy Inorganic materials 0.000 description 3
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- 238000000748 compression moulding Methods 0.000 description 2
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- 239000010949 copper Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
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- 241001391944 Commicarpus scandens Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- VAWNDNOTGRTLLU-UHFFFAOYSA-N iron molybdenum nickel Chemical compound [Fe].[Ni].[Mo] VAWNDNOTGRTLLU-UHFFFAOYSA-N 0.000 description 1
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 1
- -1 iron silicon aluminum Chemical compound 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
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- 229910000702 sendust Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- 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
-
- 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
- B22F1/08—Metallic powder characterised by particles having an amorphous microstructure
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
- B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
A water atomized Fe-Si-B amorphous powder with excellent warm-pressing performance and application thereof, wherein the preparation steps of the amorphous powder comprise: atomizing water to prepare powder; passivating; granulating; the raw materials used for water atomization powder preparation are as follows: pure boron, pure silicon, pure iron, silicon calcium powder, calcium oxide and AlN; phosphoric acid is used as a main agent of the passivating agent; adding resin for granulating; the invention also comprises application of the water atomized iron silicon boron amorphous powder with excellent temperature and pressure performance. The amorphous powder material has high magnetic permeability and high insulation resistance, and can be used for preparing products with magnetic permeability larger than 25 and insulation resistance larger than 40G omega; the difference of inductance values at 10kHz and 2000kHz is small, so that the output stability of the inductor is improved; the temperature and pressure process pressure can be lower than 600MPa, and the production problem of high amorphous powder forming pressure is solved.
Description
Technical Field
The invention relates to iron silicon boron powder with excellent warm-pressing performance and application thereof, in particular to iron silicon boron amorphous powder with excellent warm-pressing performance and application thereof.
Background
The metal soft magnetic powder core is a magnetic core material produced by processing metal and alloy soft magnetic powder through a special process, and is called as the metal soft magnetic powder core. As an important soft magnetic material, the metal soft magnetic powder core has the advantages of high saturation magnetic flux density, good DC bias performance, high Curie temperature, low magnetostriction coefficient, low loss, strong controllability and the like, and meets the development requirements of miniaturization, high frequency, high power, high efficiency and low noise of power electronic devices. The metal soft magnetic powder core is a composite soft magnetic material prepared from ferromagnetic particles with the surface insulated and coated by a powder metallurgy method, and can be divided into an iron powder core, a iron silicon powder core, an iron silicon aluminum powder core, an iron nickel molybdenum powder core, an amorphous powder core and the like. In practical production design application, the metal powder core is mainly manufactured into magnetic cores with various specifications, is used for passive elements such as inductors, transformers and the like in electricians and electronic equipment, and has very important significance for improving the performance and quality of electronic products.
The existing Fe-Si-B amorphous powder has magnetic permeability of 20-120 and low insulation resistance, so that the product manufactured by using the iron powder core has the defects of low inductance, low energy conversion efficiency, poor superposition performance and the like in the use process.
CN 111640567A discloses a process for preparing soft magnetic alloy material, the alloy material is composed of iron, silicon, aluminum, chromium, phosphorus, molybdenum, copper and carbon, and the mass ratio of each is: 80 to 95 weight percent of iron, 2 to 5.5 weight percent of silicon, 1.5 to 4.5 weight percent of aluminum, 0.35 to 2 weight percent of chromium, 0.5 to 2 weight percent of phosphorus, 0.5 to 2 weight percent of molybdenum, 0.05 to 0.5 weight percent of copper and 0.05 to 0.5 weight percent of carbon. The material process comprises the steps of mixing, coating, crushing and sieving soft magnetic metal powder and resin after heat treatment, molding under 300MPa pressure, and finally performing heat treatment at 180 ℃; although the forming pressure of the granular material manufactured by the method is not large, the magnetic conductivity is also large, but the insulating resistance performance is low, and the saturation current is also low.
CN105895290a discloses a method for preparing high temperature resistant magnetic powder, which takes iron silicon boron amorphous as main material, and after adding epoxy resin and phenolic resin, the molded product is solidified through a reasonable baking and sintering process, the process steps are simple, the operability is strong, the production cost is low, and the obtained product has excellent electromagnetic characteristics and excellent high temperature resistance, and can be used in a high temperature environment of 190 ℃. But the coating insulation performance is poor.
CN1516204 discloses a method for manufacturing soft magnetic inductive cores from sendust powder. Comprising the following steps: smelting of Fe-Si-Al alloy, coarse crushing of Fe-Si-Al alloy cast ingot, heat treatment, fine crushing into alloy powder, annealing treatment, granularity proportioning, passivation treatment, adding of insulating agent, adhesive and release agent into the alloy powder, compression molding, heat treatment and surface coating, and is characterized in that: the adhesive added after passivation treatment is an epoxy adhesive; tempering treatment after compression molding is to keep the molded alloy powder core at 600-800 ℃ for at least 30 minutes in nitrogen, argon or vacuum environment. The method has small influence on magnetic performance, and the manufactured soft magnetic powder core is not pulverized, is not cracked, has high mechanical strength, has good drop performance of alternating current-direct current superposition, and has low insulation resistance.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects in the prior art, and provides water atomized iron silicon boron amorphous powder with high magnetic conductivity and high insulation resistance and excellent temperature and pressure performance and application thereof.
The technical scheme adopted for solving the technical problems is as follows: the preparation method of the water-atomized Fe-Si-B amorphous powder with excellent warm-pressing performance comprises the following steps: atomizing water to prepare powder; passivating; granulating;
the raw materials used for water atomization powder preparation are as follows: 2-5wt% of pure boron, 4.5-8wt% of pure silicon, 88-93 wt% of pure iron, 0.3-1.5 wt% of calcium silicate powder, 0.8-2.5wt% of calcium oxide and 0.05-0.1wt% of AlN; wherein the amounts of pure boron, pure silicon and technical pure iron add up to 100wt%;
phosphoric acid is used as a main agent of the passivating agent for passivation; mixing the passivated powder with resin and granulating.
By adopting the technical scheme, the obtained Fe-Si-B amorphous powder has high magnetic permeability and high insulation resistance.
Preferably, the preparation steps comprise:
(1) Smelting alloy liquid;
(2) Taking low-pressure vortex gas as an atomizing medium, atomizing water to prepare powder, and obtaining amorphous powder;
(3) Annealing the amorphous powder and cooling;
(4) Soaking the annealed and cooled amorphous powder in a passivating agent for passivation; the passivating agent consists of a passivating agent main agent and a passivating diluent;
(5) And (3) drying the powder, adding the resin solution for granulating, sieving out 50-200 meshes of powder, baking the powder to solidify the resin, cooling, adding a lubricant, and uniformly mixing to obtain the water-atomized Fe-Si-B amorphous powder with excellent temperature and pressure properties.
By adopting the technical scheme, the obtained Fe-Si-B amorphous powder has high magnetic permeability and high insulation resistance.
When the alloy liquid is fed into an atomization tower, the atomized medium, namely low-pressure vortex gas, acts on the alloy liquid to forcefully crush the alloy liquid into a large number of fine metal droplets, and then the fine metal droplets are solidified into Fe-Si-B amorphous soft magnetic alloy spherical or sub-spherical powder under the action of surface tension in the precipitation cooling process. The method can be used for producing the Fe-Si-B amorphous powder on a large scale, and a low-cost production mode is realized.
Preferably, in the step (2), the pressure of the low-pressure vortex gas is 1-4MPa.
Preferably, in the step (2), the water atomization pulverizing is performed under a nitrogen atmosphere.
By adopting the technical scheme of the water atomization powder preparation, the powder particle size distribution X50 can be as follows: 10-22 mu m X: 35-53 μm.
Preferably, in the step (3), the annealing temperature is 400-500 ℃, and the annealing time is 1-2 hours. The annealing temperature is required to be lower than the crystallization temperature, and the method has good treatment effect and efficiency.
Preferably, in the step (4), a mixed solution of ethyl acetate and acetone in a volume ratio of 1:1 is used as a passivation diluent.
Preferably, in the step (4), the soaking passivation treatment is performed for 20-60 min.
Preferably, in the step (4), the dosage of the main agent of the passivating agent is 0.15-0.5 wt% of the annealed and cooled amorphous powder.
By adopting the passivation technical scheme, a proper protective layer can be formed on the separation surface, the reactivity of the surface of the amorphous powder is reduced, and the rust resistance of the finished powder is improved.
Preferably, in the step (5), the resin solution is a solution obtained by mixing a silicone modified epoxy resin with a phenolic resin.
Preferably, in the step (5), the mass ratio of the organosilicon modified epoxy resin to the phenolic resin is more preferably 1:0.4-1.
By adopting the technical scheme, better coating and molding effects can be obtained.
Preferably, in the step (5), the resin solution is used in an amount of 2 to 4wt% of the powder.
Preferably, in the step (5), the baking temperature is 70-100 ℃, and the baking time is 80-100 min.
By adopting the technical scheme, the baking temperature and the baking time are controlled, so that the resin solution can be promoted to be molded; the corresponding time when the baking temperature is increased is also shortened, and other temperatures and times may be employed as long as the molding effect is ensured and other chemical reactions do not occur.
Preferably, in the step (1), during smelting, pure boron, pure silicon and industrial pure iron are divided into two parts, one part of pure boron, pure silicon and iron are added at the bottom of the furnace, the other part of pure boron, pure silicon and the rest iron are sequentially added in the melting process, and the addition is completed before melting, the temperature of molten steel is more than or equal to 1600 ℃, and the smelting power is 60-200kW; reducing the power to 10-30kW, adding silicon-calcium powder, calcium oxide and aluminum nitride to cover molten steel, slagging and deslagging, and purifying to obtain alloy liquid.
Preferably, in step (1), the smelting is performed under an argon atmosphere.
By adopting the technical scheme for smelting, uniform alloy liquid can be obtained; other smelting methods may be used in the present invention as long as a homogeneous alloy liquid of the same composition is obtained.
Preferably, in the step (5), the drying method is that the drying is carried out for 20-60 min at 100-150 ℃; the temperature and time treatment can promote the powder to be dried, reduce impurities and facilitate granulation to obtain powder with good consistency; other temperature and time parameters may be used as long as similar drying effects are obtained.
Preferably, in step (5), the lubricant is nano zinc stearate.
Preferably, in the step (5), the amount of the lubricant is 0.1-0.3 wt% of the mass of the powder.
By adopting the technical scheme, a proper amount of lubricant is used, so that the effects of preventing adhesion and reducing friction can be achieved.
The invention has excellent temperature and pressure performance, and can be used as the raw material of miniature inductor or integrally formed inductor.
Preferably, the green body is formed by warm pressing under the pressure of 300-600 MPa, the green body is baked for 160-200 min at the temperature of 150-180 ℃, and the green body is cooled to room temperature along with a furnace, so that the inductor is obtained. By adopting the technical scheme, the product with the magnetic permeability larger than 25 and the insulation resistance larger than 40GΩ can be obtained.
The Fe-Si-B amorphous powder material Fe-Si-B amorphous powder has excellent antirust performance, high saturation magnetic induction intensity, low loss and the like, and can be widely applied to integrally formed inductors. The water atomized Fe-Si-B amorphous powder has lower loss, better saturation characteristic and good sphericity so as to ensure that the integrated inductor has better insulation reliability. The water atomization pulverizing process has the performances of accurate component control, stable granularity distribution and the like. In order to obtain higher insulation resistance value and magnetic permeability value, the method is realized by increasing the content of Fe/B and the content of proper Si, and the contents of Fe, si and B are needed to be matched and adjusted because certain excellent temperature and pressure performance is needed to be maintained. When the content of Fe, si and B is within the range of the scheme of the invention, the requirements of high insulation resistance, broadband performance and the like can be simultaneously met, and when the content of Fe is lower than the range of the scheme of the invention, the magnetic permeability is lower than 18. When the content of Fe is higher than the range of the scheme of the invention, the insulation resistance is far lower than 10G omega, so that the magnetic conductivity and the high-impedance performance cannot be considered; the addition of Si, B to Fe can increase the resistivity of the material, thereby reducing the loss Pe caused by eddy currents. When the Si content is 4.5-8.5wt%, the resistivity of the material can reach 40G omega cm, and further increase of the Si content can further increase the resistivity, but also reduce Ms of the material, but make the material become extremely brittle. When the content of B is 3-5wt%, the resistivity of the material can reach 40G omega cm, and when the content of B is further increased, the resistivity can be further increased, but the Ms of the material can be greatly reduced.
The heat treatment of the Fe-Si-B alloy is performed entirely in the ferrite phase region to make the ferrite grain size large, which contributes to Hc reduction and μm improvement. The magnetic properties can be further improved (about 10%) by coating with a modified epoxy resin process. The coating compounds have higher resistivity and are tightly combined with the matrix metal, can be continuously used as an insulating coating layer, and the coated magnetic powder core has better high-frequency magnetic conductivity and high insulating property.
The soft magnet-based amorphous magnetic powder has stable magnetic permeability, and the magnetic powder core has the advantage of uniformly distributing air gaps, is suitable for low magnetic loss requirements in high-frequency application, and can be applied to the emerging fields of photovoltaic inverters, UPS, APF, new energy automobiles, variable frequency air conditioners, industrial power supplies, charging piles and the like.
The Fe-Si-B amorphous powder has the advantages of high compressive strength, high Bs, high insulation resistance and the like, can be better applied to the electronic product industry such as integrated inductors and the like, has higher resistivity, is not easy to break down, resists large current, does not rust, and has simple and convenient mass production, good anti-interference capability, lower energy consumption and lower manufacturing cost. The sample can be used in the electronic industries of energy storage, isolation, interference reduction and the like under the high-frequency high-current condition, and is widely used in the fields of computers, televisions, power supplies, digital cameras, automobile electronics and the like, and the inductance requirement under the high-current condition is greatly met: the Fe-Si-B amorphous alloy does not rust and does not need spraying; the superposition characteristic can be better; after surface treatment, the developed water atomized powder has higher compressibility, higher insulation resistance and lower nonmetallic content.
The invention has the beneficial effects that:
(1) The water atomized iron silicon boron amorphous powder with excellent temperature and pressure performance has high magnetic conductivity and high insulation resistance, and can be used for preparing products with magnetic conductivity more than 25 and insulation resistance more than 40GΩ;
(2) The difference of inductance values at 10kHz and 2000kHz is small, and the problem that the inductance fluctuation of the material at the frequencies of 10kHZ and 2000kHZ is relatively large is solved, so that the output stability of the inductor is improved;
(3) The temperature and pressure process pressure can be lower than 600MPa, and the production problem of high amorphous powder forming pressure is solved.
Drawings
FIG. 1 is an electron microscope image of the powder obtained by water atomization milling of example 1 of the present invention after annealing and cooling.
Detailed Description
The present invention is further illustrated below with reference to examples, but the present invention is not limited to these examples.
The starting materials used in the examples of the present invention were all obtained by conventional commercial means.
Example 1
The water atomization iron silicon boron amorphous powder with excellent temperature and pressure performance comprises the following preparation steps: atomizing water to prepare powder; passivating; granulating;
the mass ratio of the raw materials used for water atomization powder preparation is as follows: 4.5wt% of pure boron, 4.5wt% of pure silicon and 91% of industrial pure iron; 0.65wt% of calcium silicate powder, 1.5wt% of calcium oxide and 0.08wt% of AlN;
phosphoric acid is used as a main agent of the passivating agent for passivation; mixing the passivated powder with resin and granulating.
The water atomization iron silicon boron amorphous powder with excellent temperature and pressure performance comprises the following preparation steps:
(1) Smelting alloy liquid;
(2) Taking low-pressure vortex gas as an atomizing medium, atomizing water to prepare powder, and obtaining amorphous powder;
(3) Annealing the amorphous powder and cooling;
(4) Soaking the annealed and cooled amorphous powder in a passivating agent for passivation; the passivating agent consists of a passivating agent main agent and a passivating diluent;
(5) And (3) drying the powder, adding the resin solution for granulating, sieving out 50-200 meshes of powder, baking the powder to solidify the resin, cooling, adding a lubricant, and uniformly mixing to obtain the water-atomized Fe-Si-B amorphous powder with excellent temperature and pressure properties.
Firstly, adding weighed iron, silicon and boron raw powder into a smelting crucible in an intermediate frequency induction furnace, and smelting to obtain alloy liquid. Smelting is carried out under argon atmosphere. In the smelting process, controlling the smelting power to be 60-200KW; dividing pure boron, pure silicon and industrial pure iron into two parts, adding one part of pure boron, pure silicon and iron into the furnace bottom during smelting, sequentially adding the other part of pure boron, pure silicon and residual iron in the melting process, and finishing the addition before melting; controlling the temperature of molten steel between 1600 and 1700 ℃; reducing the power to 10-30kW, adding silicon-calcium powder, calcium oxide and aluminum nitride to cover molten steel, slagging and deslagging, and purifying to obtain alloy liquid.
Under the protection of nitrogen, the alloy liquid is sent into an atomization tower, and in the sending process, the alloy liquid is acted on by an atomization medium, namely low-pressure vortex gas, so that the alloy liquid is forcefully crushed into a large number of tiny metal molten drops, and then cooled and solidified into Fe-Si-B amorphous soft magnetic alloy powder; the pressure of the low-pressure vortex gas is 1-4MPa.
And (3) carrying out heat treatment on the amorphous powder after sieving, wherein the temperature of the heat treatment annealing treatment process is 450 ℃ multiplied by 1.5h. The morphology of the powder after annealing and cooling is shown in figure 1.
In the passivation step, the passivating agent consists of a passivating agent main agent and a passivating diluent; phosphoric acid is used as a main agent of a passivating agent, a mixed solution (1:1) of ethyl acetate and acetone is used as a diluent, and the dosage of the main agent of the passivating agent is 0.2 wt% of that of the annealed and cooled amorphous powder; soaking for passivation treatment for 30 min, and filtering to obtain powder.
Treating at 150 ℃ for 25min to dry the powder, mixing the organosilicon modified epoxy resin with the mass of 1.5 and wt percent of the powder and the phenolic resin with the mass of 1.2 and wt percent of the powder into a resin solution, mixing the powder and the resin solution, granulating, and sieving to obtain 50-200 mesh powder; baking the powder at 80 ℃ for 90 min, cooling to room temperature along with a furnace, adding 0.25-wt% of nano zinc stearate by mass of the powder as a lubricant, and uniformly mixing to obtain the finished product powder.
And (3) testing the performance of the finished powder: 24.5 turns of copper wire with the wire diameter of 0.5 and mm are wound, and an Agilent 4991A precise LCR tester is adopted to test the inductance value of the magnetic ring.
The mu i of the obtained finished powder is 30+/-25% (25-35) (the test condition frequency f=100 kHz and f=2000 kHz, the voltage u=0.5V and the power supply power is 50W), the apparent density 3.967g/cm3 of the Fe-Si-B amorphous powder is 4.62g/cm3, the oxygen content is lower than 1500ppm, and the toroidal inductance density is 5.15g/cm under 300-600 MPa 3 。
The invention has excellent temperature and pressure performance, and is applied to water atomization of Fe-Si-B amorphous powder, which is used as a raw material of a miniature inductor or an integrally formed inductor: 2.85g of powder is weighed, a green body sample with the outer diameter of 14 mm and the inner diameter of 8 mm is pressed under the pressure condition of 400MPa, and the sample is baked for 180 min at 160 ℃ and then cooled to room temperature along with a furnace.
And (3) magnetic ring performance test: the sample loop obtained in this example was tested for inductance and Q using Agilent E4991a LCR tester for Agilent. The test conditions are respectively as follows: inductance was tested at f=100 kHz, f=2000 kHz u=0.5 v (power supply 50W) and converted to permeability; the inductance and the Q value of the baked ring with the outer diameter 14 and the inner diameter 8 of the magnetic ring under each frequency are tested by Agilent E4991A, the magnetic permeability mu i of a sample is calculated, and the insulation resistance of a square sample DR 6X 2mm is detected by a Chroma19053 insulation tester: each set of results is the average after 5 replicates. The test results are shown in Table 2.
Examples 2 to 8
Based on example 1, the tests of examples 2 to 8 were performed by adjusting part of the parameters. The specific process parameters for examples 2-8 are shown in Table 1; the parameters not shown in Table 1 were the same as those in example 1.
The performance test was performed on examples 2 to 8 using the same test method as example 1, and the test results are summarized in table 2.
Comparative examples 1 to 14
Based on example 1, some parameters were adjusted to conduct the tests of comparative examples 1 to 14. The specific process parameters for comparative examples 1-14 are shown in Table 1; the parameters not shown in Table 1 were the same as those in example 1.
Comparative examples 1 to 14 were subjected to performance test by the same test method as in example 1, and the test results are summarized in table 2.
TABLE 1 different parameter conditions for the ingredients and process recipe for examples 1-8 and comparative examples 1-14
Table 2 performance test tables of examples 1 to 8 and comparative examples 1 to 14
The green body samples of each example after warm compaction had a toroidal inductor density of 5.15g/cm after baking 3 The magnetic permeability after baking is greater than 25, and the insulation resistance of the sample is greater than 40G omega. Because of its excellent performance, the device can be used at very wide higher frequencies for practical applications in the product.
Claims (10)
1. The water atomized iron silicon boron amorphous powder with excellent warm-pressing performance is characterized by comprising the following preparation steps: atomizing water to prepare powder; passivating; granulating;
the raw materials used for water atomization powder preparation are as follows: 2-5wt% of pure boron, 4.5-8wt% of pure silicon, 88-93 wt wt% of pure iron, 0.3-1.5 wt% of calcium silicate powder, 0.8-2.5wt% of calcium oxide and 0.05-0.1wt% of AlN; wherein the amounts of pure boron, pure silicon and technical pure iron add up to 100wt%;
phosphoric acid is used as a main agent of the passivating agent for passivation; mixing the passivated powder with resin and granulating.
2. The water atomized iron silicon boron amorphous powder excellent in warm-pressing performance according to claim 1, wherein the preparation step comprises:
(1) Smelting alloy liquid;
(2) Taking low-pressure vortex gas as an atomizing medium, atomizing water to prepare powder, and obtaining amorphous powder;
(3) Annealing the amorphous powder and cooling;
(4) Soaking the annealed and cooled amorphous powder in a passivating agent for passivation; the passivating agent consists of a passivating agent main agent and a passivating diluent;
(5) And (3) drying the powder, adding the resin solution for granulating, sieving out 50-200 meshes of powder, baking the powder to solidify the resin, cooling, adding a lubricant, and uniformly mixing to obtain the water-atomized Fe-Si-B amorphous powder with excellent temperature and pressure properties.
3. The water atomized iron silicon boron amorphous powder with excellent warm-pressing performance according to claim 1 or 2, wherein in the step (2), the pressure of the low-pressure vortex gas is 1-4MPa; the water atomization pulverization is carried out under nitrogen atmosphere.
4. The water atomized iron silicon boron amorphous powder with excellent warm-pressing performance according to any one of claims 1 to 3, wherein in the step (3), the annealing temperature is 400 to 500 ℃ and the annealing time is 1 to 2 hours.
5. The water atomized iron silicon boron amorphous powder with excellent temperature and pressure performance according to any one of claims 1 to 4, wherein in the step (4), a mixed solution of ethyl acetate and acetone in a volume ratio of 1:1 is used as a passivation diluent; the soaking passivation treatment time is 20-60 min; the dosage of the main agent of the passivating agent is 0.15-0.5 wt% of the amorphous powder after annealing and cooling.
6. The water-atomized iron silicon boron amorphous powder with excellent temperature and pressure performance according to any one of claims 1 to 5, wherein in the step (5), the resin solution is a solution obtained by mixing an organosilicon modified epoxy resin and a phenolic resin; the mass ratio of the organic silicon modified epoxy resin to the phenolic resin is preferably 1:0.4-1; the consumption of the resin solution is 2-4wt% of the powder; the baking temperature is 70-100 ℃, and the baking time is 80-100 min.
7. The water atomized iron silicon boron amorphous powder with excellent temperature and pressure performance according to any one of claims 1-6, wherein in the step (1), pure boron, pure silicon and industrial pure iron are divided into two parts during smelting, one part of pure boron, pure silicon and iron are added at the furnace bottom, the other part of pure boron, pure silicon and residual iron are sequentially added in the melting process, and the melting process is completed before melting, the molten steel temperature is more than or equal to 1600 ℃, and the smelting power is 60-200kW; reducing the power to 10-30kW, adding calcium silicate powder, calcium oxide and aluminum nitride to cover molten steel, slagging and deslagging, and purifying to obtain alloy liquid; smelting is carried out under argon atmosphere.
8. The water atomized iron silicon boron amorphous powder with excellent warm-pressing performance according to any one of claims 1 to 7, wherein in the step (5), the drying method is that the water atomized iron silicon boron amorphous powder is treated for 20 to 60 minutes at 100 to 150 ℃; the lubricant is nano zinc stearate; the using amount of the lubricant is 0.1-0.3wt% of the mass of the powder.
9. The use of a water atomized iron silicon boron amorphous powder with excellent warm-pressing performance according to any one of claims 1 to 8, characterized in that it is used as a raw material of a micro inductor or an integrally formed inductor.
10. The application of the water atomized iron silicon boron amorphous powder with excellent warm-pressing performance according to claim 9, which is characterized in that the green body is obtained by warm-pressing under the pressure condition of 300-600 MPa, the green body is baked for 160-200 min at the temperature of 150-180 ℃, and the green body is cooled to room temperature along with a furnace, so that the inductor is obtained.
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