CN109285685B - Preparation method of high-permeability gas-atomized Fe-Si-Al magnetic powder core - Google Patents

Preparation method of high-permeability gas-atomized Fe-Si-Al magnetic powder core Download PDF

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CN109285685B
CN109285685B CN201810726383.9A CN201810726383A CN109285685B CN 109285685 B CN109285685 B CN 109285685B CN 201810726383 A CN201810726383 A CN 201810726383A CN 109285685 B CN109285685 B CN 109285685B
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CN109285685A (en
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郭宾
吕世雅
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206Manufacturing of magnetic cores by mechanical means
    • H01F41/0246Manufacturing of magnetic circuits by moulding or by pressing powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/052Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102Metallic powder coated with organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/142Thermal or thermo-mechanical treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C23C22/36Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
    • C23C22/368Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing magnesium cations
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2222/00Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/20Use of solutions containing silanes

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Abstract

The invention relates to the technical field of metal soft magnetic materials, and discloses a preparation method of a high-permeability gas-atomized Fe-Si-Al magnetic powder core. The preparation method comprises the following steps: 1) atomizing to prepare powder; 2) combining the particle sizes; 3) carrying out heat treatment on the powder; 4) insulating and coating; 5) secondary coating; 6) pressing and forming; 7) annealing the magnetic core; 8) and (4) dipping and spraying. The gas atomized sendust magnetic powder core prepared by the invention has the advantages of good formability and high magnetic conductivity.

Description

Preparation method of high-permeability gas-atomized Fe-Si-Al magnetic powder core
Technical Field
The invention relates to the technical field of metal soft magnetic materials, in particular to a preparation method of a high-permeability gas-atomized Fe-Si-Al magnetic powder core.
Background
The sendust is an important one of metal magnetic powder cores, plays an important role in soft magnetic materials in the electronic industry due to low loss and low cost, and the application range and the use amount of the sendust are rapidly increased along with the development of new energy industries; since sendust is brittle and is easily made into powder, american companies have invented sendust by crushing, then through insulation cladding, forming and annealing, a powder core is made. At present, the preparation method of the gas atomization sendust magnetic powder core mainly adopts a crushing method in China, for example, Chinese patent publication No. CN101226804 discloses a method for manufacturing the sendust magnetic powder core with the magnetic conductivity mu of 125, the selected powder has the granularity of-150 meshes, the formability is better, the coarse powder magnetic conductivity is easy to be high, but the superposition and the loss are poor, and the process is complicated; chinese patent publication No. CN101599334 discloses a preparation method of a high-resistivity and high-permeability Fe-Si soft magnetic material, wherein 1-10 wt% of Ni powder which is expensive is added into traditional crushed Fe-Si-Al powder, ethyl orthosilicate is adjusted by ammonia water to coat a layer of SiO2 insulating film on the outer layer of the Fe-Si-Al powder, and the method is high in cost and harsh in conditions. Along with the development of powder metallurgy technology, the air atomization method for preparing the sendust spherical powder appears in the market before and after 2015, and the sendust powder prepared by the new process has lower loss, higher superposition saturation characteristic and good frequency characteristic. However, since spherical ferrosilicoaluminophosphate powder has a problem of poor moldability, the moldability of the powder is improved by increasing the amount of the insulating agent and the amount of the binder in the insulating coating, and the decrease in sensitivity is caused by the increase in the amount of the coating; therefore, the air supply atomization sendust products in the market are mainly products with magnetic permeability of mu 26 and 60 and a small amount of products with magnetic permeability of mu 90, and the air supply atomization sendust products with magnetic permeability of more than mu 90 are rarely seen in the market. The current electronic technology is developed rapidly, terminal products are continuously developed towards miniaturization and high power, and the requirements for the characteristics of magnetic powder core powder are more and more diversified, so that the gas atomization sendust core with high magnetic conductivity is necessarily developed.
Disclosure of Invention
The invention provides a preparation method of a gas atomization sendust magnetic powder core with good formability and high magnetic conductivity, aiming at solving the problem that the formability and the magnetic conductivity of the sendust magnetic powder core prepared by an aerosol method in the prior art can not be simultaneously optimized.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a high-permeability gas-atomized Fe-Si-Al magnetic powder core comprises the following steps:
1) gas atomization powder preparation: smelting raw materials of aluminum ingots, ferrosilicon and iron in a vacuum high-frequency induction furnace, and then atomizing to prepare powder under the pressure of nitrogen through a tundish of atomizing equipment;
2) and (3) granularity combination: sieving the powder prepared in the step 1) according to the granularity, and then combining the granularity;
3) powder heat treatment: mixing the powder obtained in step 2) with H2Carrying out heat treatment for 1-6 h in the atmosphere, and controlling the temperature of the heat treatment at 750-850 ℃ to obtain Fe-Si-Al powder;
4) insulating and coating: putting the prepared ferrum-silicon-aluminum powder into an aluminum alloy chromium-free passivator solution, mixing and stirring for 10-30 min, taking out, airing at room temperature for 4-8 h, putting into a high-temperature oven for drying, and opening the oven to cool the powder along with the oven;
5) secondary coating: diluting 0.3-0.5 wt% of organic silicon resin with ultrahigh bonding property by using 8-10 wt% of acetone to obtain a mixed solution, adding the mixed solution into the iron-silicon-aluminum powder coated in the step 4), stirring for 30-40 min, taking out the powder, airing for more than 6h at room temperature, and sieving by using a 60-80-mesh sieve;
6) and (3) pressing and forming: adding 0.3-0.5 wt% of high-temperature release agent into the powder, uniformly stirring, and forming to obtain a magnetic core, wherein the forming pressure is 1600-1800 MPa;
7) annealing the magnetic core: placing the formed magnetic core in an inert gas atmosphere for annealing treatment, wherein the annealing temperature is 750-800 ℃, and the annealing time is 120-150 min;
8) impregnation and spraying: and adding the prepared magnetic powder core into an impregnation solution of epoxy resin and phenolic resin, soaking for 5-15 min, removing and cleaning, then baking at 120-160 ℃, and finally performing paint spraying or powder spraying.
The coating process for preparing the alloy powder is simple, the raw powder of Fe-Si-Al with the particle size of-200 meshes is selected, and the types of the used reagents are only four: 1 insulating agent (aluminum alloy chromium-free passivator), 1 adhesive (silicone resin), 1 demolding agent (high-temperature resistant type) and 1 diluent (acetone). In the industry, water glass, tetraethoxysilane and phosphating solution which are commonly used are taken as insulating agents, and inorganic insulating powder such as kaolin, mica powder, zirconia or silicon dioxide is added; because the inorganic powder is difficult to be mixed with the alloy powder uniformly, the ultrafine inorganic powder with more than 1000 meshes is often selected (the cost is higher); the method comprises the steps of firstly introducing an aluminum alloy chromium-free passivator to replace an insulating agent and inorganic powder on the aluminum alloy chromium-free passivator, wherein the passivator has good wettability, so that the aluminum alloy chromium-free passivator can be uniformly and rapidly coated on the surface of gas atomized ferrum-silicon-aluminum powder after being mixed and stirred, and then is dried at low temperature to form a uniform, high-adhesive-force and high-temperature-resistant insulating film, so that a non-magnetic material inorganic insulating agent can not be added, the smell of a magnetic core is reduced, and the magnetic conductivity of the magnetic; the modified organic silicon resin with ultrahigh bonding property is matched to replace epoxy resin and phenolic resin in the industry, so that the formability and the flowability of powder are improved, the forming pressure is reduced, and the obtained sendust core has good formability; according to the scheme, the release agent with the temperature resistance of more than 800 ℃ is adopted to replace stearic acid release agent commonly used in the industry, and the high-temperature release agent can improve the heat treatment temperature of the magnetic core.
Preferably, the raw materials in the step 1) comprise the following components in percentage by weight: 5.2-5.8 wt% of aluminum ingot, 10.7-12.8 wt% of ferrosilicon and the balance of iron.
Preferably, the nitrogen pressure in the step 1) is 1.8-3.6 MPa.
Preferably, the combination of the particle sizes of the powders in the step 2) is as follows: the mass ratio of the powder with the particle sizes of 200 to 300 meshes, 300 to 400 meshes and below 400 meshes, 200 to 300 meshes, 300 to 400 meshes and below 400 meshes is as follows: 1-5: 10-18.
Preferably, in the step 5), the weight of the organic silicon resin is 0.4-0.6% of the weight of the insulation-coated sendust powder, and the weight of the mixed liquid is 8-10% of the weight of the insulation-coated sendust powder.
Preferably, the silicone resin is one or more of polyalkyl silicone resin, polyaryl silicone resin, polyalkyl aryl silicone resin, silicone acrylic resin, silicone alkyd resin and silicone polyester resin.
Preferably, the high-temperature release agent is a mixture of one or two of a silicon release agent, a fluorine release agent, a wax release agent, and a surfactant release agent as a main component.
Therefore, the invention has the following beneficial effects: (1) the aluminum alloy chromium-free passivator is introduced to replace the insulating agent and the inorganic powder, and the passivator has good wettability, so that the aluminum alloy chromium-free passivator can be uniformly and rapidly coated on the surface of the gas atomized ferrum-silicon-aluminum powder after being mixed and stirred and then is dried at low temperature to form a uniform, high-adhesion and high-temperature-resistant insulating film, so that the non-magnetic material inorganic insulating agent can not be added any more, the magnetic core odor is reduced, and the magnetic conductivity is improved; (2) the ultrahigh-bonding-property organic silicon resin is used for replacing epoxy resin and phenolic resin in the industry, so that the formability and the flowability of powder are improved, the forming pressure is reduced, and the obtained sendust core has good formability.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
Weighing raw materials with the total weight of 200kg, wherein 10.8kg of aluminum ingot, 25.6kg of silicon iron ingot and the balance of iron are arranged, the silicon content in the silicon iron ingot is 75 wt%, putting the silicon iron ingot into a vacuum high-frequency induction furnace for smelting, and removing scum after the silicon iron ingot is molten; selecting nitrogen with the pressure of 2.5MPa for atomizing and pulverizing the tundish of the atomizing equipment; sieving the powder, and combining the powder with particle size distribution of-200- +300 meshes, -300- +400 meshes and-400 meshes or less in weight ratio of 2:3: 15; placing the mixed powder in H2Carrying out heat treatment for 1.5 hours under the protection of atmosphere, wherein the heat treatment temperature is 800 ℃; mixing and stirring 20kg of the heat-treated powder with 1kg of aluminum alloy chromium-free passivator solution for 25 minutes, taking out, airing at room temperature for 4 hours, then placing in an oven, flattening to 2 square meters, firstly heating to 95 ℃, preserving heat for 1 hour, then heating to 160 ℃, baking for 2 hours, and opening the oven to cool the powder along with the oven; cooling, performing secondary insulation coating treatment, namely diluting 0.6kg of polyalkyl organic silicon resin by using 1.6kg of acetone, stirring for 10 minutes, standing for 30 minutes to obtain a mixed solution, adding the mixed solution into the cooled iron-silicon-aluminum powder, stirring for 30 minutes, taking out, flattening for 2 square meters, airing for 6 hours, and screening by using a 60-mesh screen; adding 0.08kg of high-temperature silicon release agent into the secondarily coated powder, stirring for 10 minutes, uniformly mixing, taking the powder, performing compression molding under the molding pressure of 1800MPa, and pressing into a magnetic core with the thickness of 26.9mm multiplied by 14.6mm multiplied by 11.2 mm; placing the prepared blank magnetic core in N2Annealing in a medium annealing furnace, wherein the annealing temperature is 760 ℃, the annealing time is 150 minutes, and cooling along with the furnace is carried out; and finally, chamfering, impregnating and powder painting the blank magnetic core to obtain a finished product magnetic core.
The aluminum alloy chromium-free passivator comprises the following raw materials in parts by weight:
4 parts of magnesium fluoride, 1.5 parts of sodium tripolyphosphate, 1.5 parts of fluotitanic acid, 3 parts of sodium fluosilicate, 1 part of hydrochloric acid, 1 part of vinyl triacetoxysilane, 4 parts of calcium nitrate, 1 part of corrosion inhibitor and 2 parts of chelating agent.
Example 2
Weighing 200kg of raw materials with the total weight of 10.4kg of aluminum ingot, 20.5kg of silicon iron ingot and the balance of iron,wherein the silicon content in the ferrosilicon ingot is 90 wt%, the ferrosilicon ingot is placed in a vacuum high-frequency induction furnace for smelting, and scum is removed after the ferrosilicon ingot is smelted; selecting nitrogen with the pressure of 3MPa for atomizing and pulverizing the tundish pressure of atomizing equipment; sieving the powder, and combining the powder particle size distribution of-200- +300 meshes, -300- +400 meshes and-400 meshes or less, wherein the weight ratio of the powder particle size distribution to the powder particle size distribution is 1:1: 10; placing the mixed powder in H2Carrying out heat treatment for 3 hours under the protection of atmosphere, wherein the heat treatment temperature is 760 ℃; mixing and stirring 20kg of the heat-treated powder and 1.2kg of aluminum alloy chromium-free passivator solution for 20 minutes, taking out, airing at room temperature for 6 hours, then placing in an oven, flattening the mixture to 2 square meters, firstly heating to 95 ℃, preserving heat for 1 hour, then heating to 180 ℃, baking for 1.5 hours, and opening the oven to cool the powder along with the oven; cooling, performing secondary insulation coating treatment, namely diluting 0.6kg of polyaryl organic silicon resin by using 1.6kg of acetone, stirring for 10 minutes, standing for 30 minutes to obtain a mixed solution, adding the mixed solution into the cooled iron-silicon-aluminum powder, stirring for 30 minutes, taking out, flattening for 2 square meters, airing for 6 hours, and screening by using a 60-mesh screen; adding 0.08kg of high-temperature fluorine-based release agent into the secondarily coated powder, stirring for 10 minutes, uniformly mixing, taking the powder, performing compression molding under the molding pressure of 1600MPa, and pressing into a magnetic core with the thickness of 26.9mm multiplied by 14.6mm multiplied by 11.2 mm; placing the obtained blank magnetic core in H2Annealing in a medium annealing furnace at 780 ℃ for 120 minutes, and cooling along with the furnace; and finally, chamfering, impregnating and powder painting the blank magnetic core to obtain a finished product magnetic core.
The aluminum alloy chromium-free passivator comprises the following raw materials in parts by weight:
3 parts of magnesium fluoride, 2 parts of sodium tripolyphosphate, 1 part of fluotitanic acid, 5 parts of sodium fluosilicate, 2 parts of hydrochloric acid, 1 part of vinyl triacetoxysilane, 4 parts of calcium nitrate, 2 parts of corrosion inhibitor and 1 part of chelating agent.
Example 3
Weighing raw materials with the total weight of 200kg, wherein 11.6kg of aluminum ingot, 21.6kg of silicon iron ingot and the balance of iron are arranged, the silicon content in the silicon iron ingot is 95 wt%, putting the silicon iron ingot into a vacuum high-frequency induction furnace for smelting, and removing scum after the silicon iron ingot is molten; in the atomizing apparatusThe pressure of the tundish is 3MPa, and nitrogen is selected for atomization powder preparation; sieving the powder, and combining the powder with particle size distribution of-200- +300 meshes, -300- +400 meshes and-400 meshes or less in weight ratio of 3:4: 13; placing the mixed powder in H2Carrying out heat treatment for 3 hours under the protection of atmosphere, wherein the heat treatment temperature is 760 ℃; mixing and stirring 20kg of the heat-treated powder and 1.2kg of aluminum alloy chromium-free passivator solution for 20 minutes, taking out, airing at room temperature for 6 hours, then placing in an oven, flattening the mixture to 2 square meters, firstly heating to 95 ℃, preserving heat for 1 hour, then heating to 180 ℃, baking for 1.5 hours, and opening the oven to cool the powder along with the oven; cooling, performing secondary insulation coating treatment, namely diluting 0.6kg of polyalkylaryl organic silicon resin by using 1.6kg of acetone, stirring for 10 minutes, standing for 30 minutes to obtain a mixed solution, adding the mixed solution into the cooled sendust powder, stirring for 30 minutes, taking out, flattening for 2 square meters, airing for 6 hours, and screening by using a 60-mesh screen; adding 0.08kg of high-temperature wax mold release agent into the secondarily coated powder, stirring for 10 minutes, uniformly mixing, taking the powder, performing compression molding under the molding pressure of 1700MPa, and pressing into a magnetic core with the thickness of 26.9mm multiplied by 14.6mm multiplied by 11.2 mm; placing the prepared blank magnetic core in N2Annealing in a medium annealing furnace at 770 ℃ for 120 minutes, and cooling along with the furnace; and finally, chamfering, impregnating and powder painting the blank magnetic core to obtain a finished product magnetic core.
The aluminum alloy chromium-free passivator comprises the following raw materials in parts by weight:
5 parts of magnesium fluoride, 1 part of sodium tripolyphosphate, 1 part of fluotitanic acid, 4 parts of sodium fluosilicate, 3 parts of hydrochloric acid, 3 parts of vinyl triacetoxysilane, 4 parts of calcium nitrate, 2 parts of corrosion inhibitor and 2 parts of chelating agent.
Example 4
Weighing raw materials with the total weight of 200kg, wherein 10.4kg of aluminum ingot, 20.4kg of silicon iron ingot and the balance of iron are arranged, the silicon content in the silicon iron ingot is 75 wt%, putting the silicon iron ingot into a vacuum high-frequency induction furnace for smelting, and removing scum after the silicon iron ingot is molten; selecting nitrogen with the pressure of 1.8MPa for atomizing and pulverizing the tundish of the atomizing equipment; sieving the powder, and combining the powder with the particle size distribution of200 to 300 meshes, 300 to 400 meshes and less than 400 meshes, wherein the weight ratio of the three is 1:1: 10; placing the mixed powder in H2Carrying out heat treatment for 1 hour under the protection of atmosphere, wherein the heat treatment temperature is 750 ℃; mixing and stirring 20kg of the heat-treated powder and 1.2kg of aluminum alloy chromium-free passivator solution for 10 minutes, taking out, airing for 4 hours at room temperature, then placing in an oven, flattening to 2 square meters, firstly heating to 95 ℃, keeping the temperature for 1 hour, then heating to 180 ℃, baking for 1.5 hours, and opening the oven to cool the powder along with the oven; cooling, performing secondary insulation coating treatment, namely diluting 0.6kg of organic silicon acrylic resin by 1.6kg of acetone, stirring for 10 minutes, standing for 30 minutes to obtain a mixed solution, adding the mixed solution into the cooled sendust powder, stirring for 30 minutes, taking out, flattening for 2 square meters, airing for 7 hours, and screening by a 60-mesh screen; adding 0.08kg of high-temperature surfactant release agent into the secondarily coated powder, stirring for 10 minutes, uniformly mixing, taking the powder, performing compression molding under the molding pressure of 1600MPa, and pressing into a magnetic core with the thickness of 26.9mm multiplied by 14.6mm multiplied by 11.2 mm; placing the prepared blank magnetic core in N2Annealing in a medium annealing furnace at 750 ℃ for 120 minutes, and cooling along with the furnace; and finally, chamfering, impregnating and powder painting the blank magnetic core to obtain a finished product magnetic core.
The aluminum alloy chromium-free passivator comprises the following raw materials in parts by weight:
3 parts of magnesium fluoride, 1 part of sodium tripolyphosphate, 1 part of fluotitanic acid, 2 parts of sodium fluosilicate, 1 part of hydrochloric acid, 1 part of vinyl triacetoxysilane, 3 parts of calcium nitrate, 1 part of corrosion inhibitor and 1 part of chelating agent.
Example 5
Weighing raw materials with the total weight of 200kg, wherein 11.6kg of aluminum ingot, 25.6kg of silicon iron ingot and the balance of iron are arranged, the silicon content in the silicon iron ingot is 95 wt%, putting the silicon iron ingot into a vacuum high-frequency induction furnace for smelting, and removing scum after the silicon iron ingot is molten; selecting nitrogen with the pressure of 3.6MPa for atomizing and pulverizing the tundish of the atomizing device; sieving the powder, and combining the powder with particle size distribution of-200- +300 meshes, -300- +400 meshes and-400 meshes or less in weight ratio of 5:5: 18; placing the mixed powder in H2Carrying out heat treatment for 6 hours under the protection of atmosphere, wherein the heat treatment temperature is 850 ℃; mixing and stirring 20kg of the heat-treated powder and 1.2kg of aluminum alloy chromium-free passivator solution for 30 minutes, taking out, airing for 8 hours at room temperature, then placing in an oven, flattening to 2 square meters, firstly heating to 95 ℃, preserving heat for 1 hour, then heating to 180 ℃, baking for 1.5 hours, and opening the oven to cool the powder along with the oven; cooling, performing secondary insulation coating treatment, namely diluting 0.6kg of organic silicon alkyd resin by 1.6kg of acetone, stirring for 10 minutes, standing for 30 minutes to obtain a mixed solution, adding the mixed solution into the cooled sendust powder, stirring for 40 minutes, taking out, flattening for 2 square meters, airing for 8 hours, and sieving by a 80-mesh sieve; adding 0.08kg of high-temperature silicon release agent into the secondarily coated powder, stirring for 10 minutes, uniformly mixing, taking the powder, performing compression molding under the molding pressure of 1800MPa, and pressing into a magnetic core with the thickness of 26.9mm multiplied by 14.6mm multiplied by 11.2 mm; placing the obtained blank magnetic core in H2Annealing in a medium annealing furnace at 800 ℃ for 150 minutes, and cooling along with the furnace; and finally, chamfering, impregnating and powder painting the blank magnetic core to obtain a finished product magnetic core.
The aluminum alloy chromium-free passivator comprises the following raw materials in parts by weight:
8 parts of magnesium fluoride, 2 parts of sodium tripolyphosphate, 2 parts of fluotitanic acid, 7 parts of sodium fluosilicate, 3 parts of hydrochloric acid, 3 parts of vinyl triacetoxysilane, 5 parts of calcium nitrate, 2 parts of corrosion inhibitor and 2 parts of chelating agent.
The silicon-aluminum magnetic powder cores prepared in the examples 1 to 3 were subjected to performance tests, and the results are shown in the following table:
Figure BDA0001719837260000061
note: the loss test instrument adopts the rock distortion 8218, 30:5Ts and 25 DEG C
The result proves that the silicon-aluminum magnetic powder core prepared by the aerosol method has higher magnetic conductivity and better superposition performance.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (3)

1. A preparation method of a high-permeability gas-atomized Fe-Si-Al magnetic powder core is characterized by comprising the following steps:
1) gas atomization powder preparation: smelting raw materials of aluminum ingots, silicon iron ingots and iron in a vacuum high-frequency induction furnace, and then atomizing to prepare powder under the pressure of nitrogen through a tundish of atomizing equipment; the raw materials comprise the following components in percentage by weight: 5.2-5.8 wt% of aluminum ingot, 10.2-12.8 wt% of ferrosilicon ingot and the balance of iron;
2) and (3) granularity combination: sieving the powder prepared in the step 1) according to the granularity, and then carrying out granularity combination, wherein the granularity combination of the powder is as follows: the mass ratio of the powder with the granularity of-200 to +300 meshes to-300 to +400 meshes to-400 meshes below, the granularity of-200 to +300 meshes to-300 to +400 meshes to-400 meshes below is as follows: 1-5: 10-18;
3) powder heat treatment: mixing the powder obtained in step 2) with H2Carrying out heat treatment for 1-6 h in the atmosphere, and controlling the temperature of the heat treatment at 750-850 ℃ to obtain Fe-Si-Al powder;
4) insulating and coating: adding the prepared ferrum-silicon-aluminum powder into an aluminum alloy chromium-free passivator, mixing and stirring for 10-30 min, taking out, airing at room temperature for 4-8 h, putting into a high-temperature oven for drying, and opening the oven to cool the powder along with the oven; the aluminum alloy chromium-free passivator comprises the following raw materials in parts by weight:
3-8 parts of magnesium fluoride, 1-2 parts of sodium tripolyphosphate, 1-2 parts of fluotitanic acid, 2-7 parts of sodium fluosilicate, 1-3 parts of hydrochloric acid, 1-3 parts of vinyl triacetoxysilane, 3-5 parts of calcium nitrate, 1-2 parts of a corrosion inhibitor and 1-2 parts of a chelating agent;
5) secondary coating: diluting organic silicon resin with ultrahigh adhesion by using acetone to obtain a mixed solution, adding the mixed solution into the iron-silicon-aluminum powder coated in the insulation manner in the step 4), stirring for 30-40 min to obtain powder, taking out the powder, airing for more than 6h at room temperature, and sieving by using a 60-80-mesh sieve; the organic silicon resin is one or more of polyalkyl organic silicon resin, polyaryl organic silicon resin, polyalkylaryl organic silicon resin, organic silicon acrylic resin and organic silicon alkyd resin;
6) and (3) pressing and forming: adding a high-temperature release agent into the powder, uniformly stirring, and performing compression molding to obtain a blank magnetic core, wherein the molding pressure is 1600-1800 MPa, and the main component of the high-temperature release agent is one or two of a silicon release agent, a fluorine release agent, a wax release agent and a surfactant release agent;
7) annealing the magnetic core: placing the formed blank magnetic core in N2Or H2Annealing treatment is carried out in the atmosphere, the annealing temperature is 750-800 ℃, and the annealing time is 120-150 min;
8) impregnation and spraying: and chamfering, impregnating and powder spraying the prepared magnetic core to obtain a finished magnetic core.
2. The method for preparing the high-permeability gas-atomized sendust magnetic powder core according to claim 1, wherein the silicon content in the silicon iron ingot is 75-95 wt%.
3. The method for preparing the high-permeability gas-atomized sendust magnetic powder core according to claim 1, wherein the nitrogen pressure in the step 1) is 1.8-3.6 MPa.
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