CN111360245B - Preparation method of high-impedance iron-silicon-chromium material - Google Patents

Preparation method of high-impedance iron-silicon-chromium material Download PDF

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CN111360245B
CN111360245B CN201911292456.9A CN201911292456A CN111360245B CN 111360245 B CN111360245 B CN 111360245B CN 201911292456 A CN201911292456 A CN 201911292456A CN 111360245 B CN111360245 B CN 111360245B
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powder
silicon
iron
baking
chromium
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CN111360245A (en
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丁卫坡
王媛珍
王林科
方萌
郭宾
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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    • 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
    • B22F1/16—Metallic particles coated with a non-metal
    • 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
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
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    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus 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
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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus 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
    • H01F41/02—Apparatus 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
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    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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    • 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
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Abstract

The invention relates to the technical field of inductance materials, and discloses a preparation method of a high-impedance iron-silicon-chromium material aiming at the problems of poor powder coating performance and low performance index of an integrated inductor in the prior art, which comprises the following preparation steps: 1) selecting powder; 2) insulating and coating; 3) secondary coating; 4) granulating; 5) mixing powder; 6) pressing and forming; 7) baking the product and the like to finally obtain a finished product. According to the invention, the iron-silicon-chromium powder with a proper particle size is selected, and the insulating material is uniformly coated on the surface of the particles, so that the insulativity and the insulation resistance of the powder are greatly improved, and the integrated inductor with good insulation performance is prepared; under the heating condition, a material with good insulation effect is selected for coating, and then the material is dried to form a uniform, high-adhesion and high-temperature-resistant insulating film; the cost of each material is low, the composition of each material, the process steps and the use parameter range are clear, the preparation process is simple, and the high-quality yield is high.

Description

Preparation method of high-impedance iron-silicon-chromium material
Technical Field
The invention relates to the technical field of inductance materials, in particular to a preparation method of a high-impedance iron-silicon-chromium material.
Background
At present, many manufacturers can use alloy powder to manufacture an integrated inductor, the integrated inductor is the inductor formed by integrally molding powder and a coil, the coil is formed by winding enamelled copper wires, the problem of interlayer short circuit caused by damage of enamel skin of an enamelled wire during molding is an important link, the powder is a more critical factor, and poor insulativity among powder particles is an important factor for short circuit, so that the improvement of the insulativity of the powder particles has important significance for the integrated inductor.
Patent No. 201910265631.9 discloses a method for preparing a high-impedance iron-silicon material and an integrated inductor containing the iron-silicon material, and the method for preparing the high-impedance iron-silicon material comprises the following steps: selecting 400-500 meshes of water atomized iron-silicon powder for ball milling; adding the ball-milled powder into a coating liquid for insulating coating, wherein the coating liquid is prepared by dissolving two or more of phosphoric acid, aluminum dihydrogen phosphate, chromic acid and potash water glass in acetone; adding the powder subjected to insulation coating into secondary coating liquid for secondary coating, wherein the secondary coating liquid is prepared by dissolving one or more of silicone resin and liquid glue in acetone; sequentially granulating, airing and baking the secondarily coated powder; cooling to room temperature, adding auxiliary materials, stirring, and sieving.
The defects of the inductor are that acetone and phosphoric acid are adopted for coating at normal temperature, the coating property of powder is poor, the insulating property of the inductor needs to be improved, and the related performance index of the integrated inductor is low.
Disclosure of Invention
The invention aims to overcome the problems of poor coating property of powder and low performance index of an integrated inductor in the prior art, and provides a preparation method of a high-impedance iron-silicon-chromium material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-impedance iron-silicon-chromium material is characterized by comprising the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder;
2) insulating and coating: adding phosphoric acid, aluminum dihydrogen phosphate and nano silicon dioxide into deionized water, dissolving and primarily stirring to obtain a solution A, adding iron-silicon-chromium powder into the solution A, heating and stirring simultaneously, and baking for the first time;
3) secondary coating: uniformly mixing epoxy resin and a hardening agent, adding acetone for dilution, stirring and dissolving, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and uniformly stirring;
4) and (3) granulation: granulating the uniformly stirred powder to obtain granulated powder;
5) powder mixing: adding magnesium oxide and demolding powder, and stirring to obtain a blended powder;
6) and (3) pressing and forming: pressing and molding the blended powder obtained in the step 5) and the coil;
baking products: placing the formed product in an oven for secondary baking;
preferably, the raw materials in the step 2) comprise the following components in 100 parts by mass: 0.025-0.2 part of phosphoric acid, 0.075-0.6 part of aluminum dihydrogen phosphate, 0.01-0.08 part of nano silicon dioxide, and the balance of iron-silicon-chromium powder.
Preferably, the grain size of the ferrosilicon chromium powder selected in the step 1) is less than or equal to 325 meshes.
Preferably, the heating time in the heating and stirring in the step 2) is 80-98min, the heating temperature is 145-180 ℃, the first baking temperature is 141-162 ℃, and the baking time is 3.7-6.0 h.
The coating mechanism of the process is as follows: phosphoric acid reacts with iron to produce Fe2(PO4)3Coated involucra aluminium dihydrogen phosphate Al (H)2PO4)3Heating in water solution for polycondensation to form cross-linked structure Al2(H2P2O7)3And a coating film is generated on the surface of the iron, and the nano silicon dioxide reacts with water molecules in water to generate hydroxyl which can chemically react with the hydroxyl on the surface of Fe ions to form a chemical bond, so that a net structure is formed on the surface of the Fe, and the coating insulation property is improved. Through triple chemical coating of the three materials, the insulativity of the iron-silicon-chromium powder is greatly improved.
Preferably, the stirring and dissolving time in the step 3) is 30min, and the stirring and uniform stirring time is 45-80 min. The coating mechanism of the process is as follows: resin is diluted by acetone to form a glue solution, powder is mixed with the glue solution, and after acetone is volatilized, a resin film can be formed on the surface of powder particles. Therefore, under the dual coating action of primary coating and secondary coating, the impedance of the powder material can be continuously improved, and a better effect is achieved.
Preferably, the granulating in the step 4) is to granulate the uniformly stirred powder in the step 3) by using a 50-mesh net, air-dry the powder for 3-5h, sieve the powder by using a 40-mesh granulator, bake the powder for 81-102 min at 67-74 ℃, naturally cool the powder to room temperature, and sieve the powder by using a 40-mesh sieve again.
And (3) granulating to screen out powder with required particle size, improving the specific surface area of the powder, increasing the contact area between the powder, and preparing a product with strong binding capacity and high insulativity.
Preferably, the blended powder in the step 5) is calculated according to 100 mass parts: 0.15-0.5 part of magnesium oxide, 0.15-0.5 part of demoulding powder and the balance of granulation powder, and the powder mixing and stirring time is 10-20 min. .
Preferably, the demoulding powder consists of zinc stearate, magnesium stearate, polyethylene wax and pentaerythritol, and the composition ratio is that the zinc stearate: magnesium stearate: polyethylene wax: 48-52 parts of polypentaerythritol: 14-16 parts of: 8-12 parts of: 24-26 parts.
The four components have lubricating effect, the epoxy resin is used for secondary coating, the epoxy resin has excellent bonding force to other materials, no lubricating material is added, the friction force between the powder and the die is large after the powder is pressed, the die is easily damaged, the product is scraped, the lubricating material is added and still adheres to the surface of the powder, a layer of lubricating film can be formed between the surface of the product and the die in the pressing process, and the die and the product are not easily damaged in the product extruding process from the die.
Preferably, the molding pressure in the step 6) is 6-8T/cm2。
Preferably, the second baking in the step 7) is carried out at the temperature of 154-168 ℃, and the whole baking time is 3.5-7.0 h.
Therefore, the invention has the following beneficial effects: the second baking mechanism: the secondary coating is resin and a hardening agent, and does not react or reacts very weakly at low temperature; and the second baking temperature is high, the resin and the hardening agent are subjected to chemical reaction and are crosslinked to form a thermosetting structure, so that the overall strength of the product is improved.
(1) According to the invention, the iron-silicon-chromium powder with a proper particle size is selected, and the insulating material is uniformly coated on the surface of the particles, so that the insulativity and the insulation resistance of the powder are greatly improved, and the integrated inductor with good insulation performance is prepared;
(2) under the heating condition, a material with good insulation effect is selected for coating, and then a uniform, high-adhesion and high-temperature-resistant insulating film is formed through high-temperature drying;
(3) the cost of each material is low, the composition of each material, the process steps and the use parameter range are clear, the preparation process is simple, and the high-quality yield is high.
Detailed Description
The invention is further described with reference to specific embodiments.
Example 1
A preparation method of a high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: 0.25g of phosphoric acid, 0.75g of aluminum dihydrogen phosphate and 0.01g of nano silicon dioxide are added into 10 percent deionized water to be dissolved and stirred for 30min to obtain a solution A, 998.9g of iron-silicon-chromium powder is added into the solution A, the solution A is heated and stirred for 80min at 145 ℃, and then the first baking is carried out for 6h at 141 ℃.
3) Secondary coating: uniformly mixing 2.0% of epoxy resin and a hardening agent, adding 10% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 45 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3h, sieving the powder by using a 40-mesh granulator, baking the powder for 81min at 67 ℃, naturally cooling the powder to room temperature, and sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: adding 0.15g of magnesium oxide, 0.15g of demoulding powder and 99.7g of granulating powder, and stirring to obtain 100g of blended powder;
6) and (3) pressing and forming: pressing and molding the blended powder obtained in the step 5) and the coil together, wherein the molding pressure is 6T/cm2
7) Baking products: and placing the formed product in an oven for secondary baking, wherein the baking maximum temperature is 154 ℃, and the whole baking time is 210 min.
Example 2
The method is different from the embodiment 1 in that the preparation method of the high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: adding 0.5g of phosphoric acid, 1.5g of aluminum dihydrogen phosphate and 0.02g of nano silicon dioxide into 12% deionized water, dissolving and stirring for 30min to obtain a solution A, adding 997.8g of iron-silicon-chromium powder into the solution A, heating and stirring at 162 ℃ for 82min, and then carrying out primary baking at 148 ℃ for 5.2 h.
3) Secondary coating: uniformly mixing 2.5% of epoxy resin and a hardening agent, adding 12% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 50 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3h, sieving the powder by using a 40-mesh granulator, baking the powder for 84min at 68 ℃, naturally cooling the powder to room temperature, and sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: 0.2g of magnesium oxide, 0.2g of mold release powder, and 99.6g of granulation powder were added and stirred to obtain 100g of blended powder.
6) And (3) pressing and forming: pressing and molding the blend powder obtained in the step 5) and the coil together, wherein the molding pressure is 6.2T/cm2
7) Baking products: and placing the formed product in an oven for secondary baking, wherein the baking temperature is 156 ℃, and the whole baking time is 4.0 h.
Example 3
The method is different from the embodiment 1 in that the preparation method of the high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: 0.75g of phosphoric acid, 2.25g of aluminum dihydrogen phosphate and 0.3g of nano silicon dioxide are added into 14 percent deionized water to be dissolved and stirred for 30min initially to obtain a solution A, 996.7g of iron-silicon-chromium powder is added into the solution A, the solution A is heated and stirred for 88min at 155 ℃, and then primary baking is carried out for 5.3h at 147 ℃.
3) Secondary coating: uniformly mixing 3.0% of epoxy resin and a hardening agent, adding 14% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 55 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3h, sieving the powder by using a 40-mesh granulator, baking the powder for 87min at 69 ℃, naturally cooling the powder to room temperature, and sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: adding 0.25g of magnesium oxide, 0.25g of release powder and 99.5g of granulation powder, and stirring to obtain 100g of mixed powder
6) And (3) pressing and forming: pressing and molding the blend powder obtained in the step 5) and the coil together, wherein the molding pressure is 6.4T/cm2
7) Baking products: and placing the formed product in an oven for secondary baking, wherein the baking temperature is 158 ℃, and the whole baking time is 4.5 h.
Example 4
The method is different from the embodiment 1 in that the preparation method of the high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: 1.0g of phosphoric acid, 3.0g of aluminum dihydrogen phosphate and 0.4g of nano silicon dioxide are added into 16 percent deionized water to be dissolved and stirred for 34min initially to obtain a solution A, 995.6g of iron-silicon-chromium powder is added into the solution A, the solution A is heated and stirred for 90min at 160 ℃, and then primary baking is carried out for 5.0h at 150 ℃.
3) Secondary coating: uniformly mixing 3.5% of epoxy resin and a hardening agent, adding 16% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 60 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3h, sieving the powder by using a 40-mesh granulator, baking the powder for 90min at 70 ℃, naturally cooling the powder to room temperature, and sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: 0.3g of magnesium oxide, 0.3g of mold release powder, and 99.4g of granulation powder were added and stirred to obtain 100g of blended powder.
6) And (3) pressing and forming: pressing and molding the blend powder obtained in the step 5) and the coil together, wherein the molding pressure is 6.6T/cm2
7) Baking products: and placing the formed product in an oven for secondary baking, wherein the baking temperature is 160 ℃, and the whole baking time is 5.0 h.
Example 5
The method is different from the embodiment 1 in that the preparation method of the high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: adding 1.25g of phosphoric acid, 3.75g of aluminum dihydrogen phosphate and 0.5g of nano silicon dioxide into 18 percent deionized water to dissolve, stirring for 35min to obtain a solution A, adding 994.5g of iron-silicon-chromium powder into the solution A, heating and stirring for 92min at 165 ℃, and then baking for 4.7h at 150 ℃.
3) Secondary coating: uniformly mixing 4.0% of epoxy resin and a hardening agent, adding 18% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 65 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3h, sieving the powder by using a 40-mesh granulator, baking the powder for 93min at 71 ℃, naturally cooling the powder to room temperature, and sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: adding 0.35g of magnesium oxide, 0.35g of demoulding powder and 99.3g of granulating powder, and stirring to obtain 100g of blended powder;
6) and (3) pressing and forming: pressing the blended powder obtained in the step 5) and the coil togetherMolding under a molding pressure of 7T/cm2
7) Baking products: and placing the formed product in an oven for secondary baking, wherein the baking temperature is 162 ℃, and the whole baking time is 5.5 hours.
Example 6
The method is different from the embodiment 1 in that the preparation method of the high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: 1.5g of phosphoric acid, 4.5g of aluminum dihydrogen phosphate and 0.6g of nano silicon dioxide are added into 20 percent deionized water to be dissolved and stirred for 30min to obtain a solution A, 993.4g of iron-silicon-chromium powder is added into the solution A, the solution A is heated and stirred for 94min at the temperature of 170 ℃, and then primary baking is carried out for 4.3h at the temperature of 156 ℃.
3) Secondary coating: uniformly mixing 4.5% of epoxy resin and a hardening agent, adding 20% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 70 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3.0h, sieving the powder by using a 40-mesh granulator, baking the powder for 96min at 72 ℃, naturally cooling the powder to room temperature, and sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: 0.4g of magnesium oxide, 0.4g of mold release powder, and 99.2g of granulation powder were added and stirred to obtain 100g of blended powder.
6) And (3) pressing and forming: pressing and molding the blended powder obtained in the step 5) and the coil together, wherein the molding pressure is 7.4T/cm2
7) Baking products: and (3) placing the formed product in an oven for secondary baking, wherein the baking temperature is 164, and the whole baking time is 6.0 h.
Example 7
The method is different from the embodiment 1 in that the preparation method of the high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: 1.75g of phosphoric acid, 5.25g of aluminum dihydrogen phosphate and 0.7g of nano silicon dioxide are added into 22 percent deionized water to be dissolved and stirred for 30min to obtain a solution A, 992.3g of iron-silicon-chromium powder is added into the solution A, the solution A is heated and stirred for 96min at 175 ℃, and then primary baking is carried out for 4.0h at 159 ℃.
3) Secondary coating: uniformly mixing 5.0% of epoxy resin and a hardening agent, adding 22% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 75 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3.0h, sieving the powder by using a 40-mesh granulator, baking the powder at 73 ℃ for 99min, naturally cooling the powder to room temperature, and then sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: 0.45g of magnesium oxide, 0.45g of mold release powder, and 99.1g of granulation powder were added and stirred to obtain 100g of blended powder.
6) And (3) pressing and forming: pressing and molding the blended powder obtained in the step 5) and the coil together, wherein the molding pressure is 7.8T/cm2。
7) Baking products: and (3) placing the formed product in an oven for secondary baking, wherein the baking temperature is 166 ℃, and the whole baking time is 6.5 h.
Example 8
The method is different from the embodiment 1 in that the preparation method of the high-impedance iron-silicon-chromium material comprises the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder with the particle size of less than or equal to 325 meshes;
2) insulating and coating: adding 2g of phosphoric acid, 6g of aluminum dihydrogen phosphate and 0.8g of nano silicon dioxide into 24% deionized water to dissolve, primarily stirring for 30min to obtain a solution A, adding 991.2g of iron-silicon-chromium powder into the solution A, simultaneously heating and stirring at 180 ℃ for 98min, and then carrying out primary baking at 162 ℃ for 3.7 h.
3) Secondary coating: uniformly mixing 5.5% of epoxy resin and a hardening agent, adding 24% of acetone for dilution and stirring for 30min, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and stirring for 80 min;
4) and (3) granulation: granulating the uniformly stirred powder in the step 3) by using a 50-mesh net, airing the powder for 3h, sieving the powder by using a 40-mesh granulator, baking the powder for 102min at 74 ℃, naturally cooling the powder to room temperature, and sieving the powder by using a 40-mesh sieve again to obtain granulated powder;
5) powder mixing: 0.5g of magnesium oxide, 0.5g of mold release powder, and 99.0g of granulation powder were added and stirred to obtain 100g of blended powder.
6) And (3) pressing and forming: pressing and molding the blended powder obtained in the step 5) and the coil together, wherein the molding pressure is 8T/cm2。
7) Baking products: and placing the formed product in an oven for secondary baking, wherein the baking temperature is 168 ℃, and the whole baking time is 7.0 h.
Comparative example 1
The difference from example 1 is that: adjusting the insulating coating material in the step 2) to be coated by only one phosphoric acid material from three materials of phosphoric acid/aluminum dihydrogen phosphate/nano silicon dioxide.
Comparative example 2
The difference from example 2 is that: and (3) replacing the solvent water of the insulating coating material in the step 2) with acetone as a solvent.
Comparative example 3
The difference from example 3 is that: adjusting the heating coating in the step 2) to room temperature coating.
Comparative example 4
The difference from example 4 is that: the baking temperature in step 2) was reduced to 50 ℃.
Comparative example 5
The difference from example 5 is that: adjusting the baking time in the step 2) to 0.5 h.
Comparative example 6
The difference from example 6 is that: the proportion of solvent in step 3) is reduced to 5%.
Comparative example 7
The difference from example 7 is that: and (3) reducing the time for dissolving and stirring the resin in the step 3) to 1 min.
Comparative example 8
The difference from example 8 is that: raising the baking temperature in the step 4) to 100 ℃.
The results of the tests on the finished products obtained in examples 1 to 8 and comparative examples 1 to 8 are shown in Table 1.
TABLE 1 relevant Performance indices of the finished products in the examples and comparative examples
Figure GDA0002785894580000071
Figure GDA0002785894580000081
Conclusion analysis:
comparative example 1: aluminum dihydrogen phosphate/nano silicon dioxide/phosphoric acid triple coating is adopted, a cross-linked structure is formed on the surface of powder particles, the heat resistance of the aluminum dihydrogen phosphate/silicon dioxide is good, and the order of magnitude of the coating impedance is greatly improved by adopting phosphoric acid/aluminum dihydrogen phosphate/nano silicon dioxide coating; pure phosphoric acid is adopted for coating, so that the coating insulation property is poor.
Comparative example 2: water is used as a solvent to provide a large amount of hydroxyl, and the coating material is crosslinked under the condition and is easier to coat on the surface of the powder particles; acetone is used as a solvent, phosphoric acid reacts with the surfaces of the powder particles after the acetone is volatilized, the reaction speed is low, and agglomeration is easy to occur; the coating of water does not cause agglomeration of powder particles, so that the obtained coating material has better performance.
Comparative example 3: the heating coating can lead the coating material to be coated with the powder in a crosslinking way more quickly, and the coating property among the powder is good; the coating is carried out at normal temperature, the reaction between the coating material and the powder is slow, the drying period of the powder is long, and the coating effect is poor.
Comparative example 4: the baking temperature is increased, so that the powder solvent can be volatilized more quickly, and the coating material can be coated better; the baking temperature is low, the solvent and the steam of the powder are not completely volatilized, the moisture content of the powder is high, the proportion of the powder is reduced, the product characteristics are influenced, and the product characteristics are reduced.
Comparative example 5: the baking time is prolonged, the coating among powder particles is more compact, the solvent is volatilized more thoroughly, the baking time is short, the solvent and water vapor are not volatilized completely, the powder proportion is reduced, and the product characteristics are reduced.
Comparative example 6: the proportion of the solvent is low, the coating of the resin solution and the powder is incomplete, and the impedance of the product is reduced
Comparative example 7: the resin and the solvent belong to different materials, the shapes are different, the resin plays a role in coating in the process, and the solvent is only auxiliary; the resin and the solvent are mixed with each other for a long time, the mixing is relatively uniform, and the surface of powder particles can be uniformly coated in the powder coating process; and the mixing time of the resin and the solvent is short, the mixing is not uniform, the coating on the surface of the powder particles is not uniform, the insulation consistency of the product is influenced, and the impedance consistency of the product is poor.
Comparative example 8: the baking temperature is increased, and the solvent residue in the powder can be further volatilized; the cracking condition of the product caused by solvent volatilization in the baking process of the pressed product can be reduced.
It can be seen from the data of examples 1 to 8 and comparative examples 1 to 8 that only the solutions within the scope of the claims of the present invention can satisfy the above requirements in all aspects, and an optimized solution can be obtained, and a high-resistance fe-si-cr material with optimal performance can be obtained. The change of the mixture ratio, the replacement/addition/subtraction of raw materials or the change of the feeding sequence can bring corresponding negative effects.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.

Claims (10)

1. A preparation method of a high-impedance iron-silicon-chromium material is characterized by comprising the following preparation steps:
1) selecting powder: screening iron-silicon-chromium powder;
2) insulating and coating: adding phosphoric acid, aluminum dihydrogen phosphate and nano silicon dioxide into deionized water, dissolving and primarily stirring to obtain a solution A, adding iron-silicon-chromium powder into the solution A, heating and stirring simultaneously, and baking for the first time;
3) secondary coating: uniformly mixing epoxy resin and a hardening agent, adding acetone for dilution, stirring and dissolving, adding the solution into the iron-silicon-chromium powder coated in the insulation way in the step 2), and uniformly stirring;
4) and (3) granulation: granulating the uniformly stirred powder to obtain granulated powder;
5) powder mixing: adding magnesium oxide, demolding powder and granulating powder, and stirring to obtain blended powder;
6) and (3) pressing and forming: pressing and molding the blended powder obtained in the step 5) and the coil;
7) baking products: and placing the formed product in an oven for secondary baking.
2. The preparation method of the high-impedance iron-silicon-chromium material according to claim 1, wherein the raw materials in the step 2) comprise, by 100 parts by mass: 0.025-0.2 part of phosphoric acid, 0.075-0.6 part of aluminum dihydrogen phosphate, 0.01-0.08 part of nano silicon dioxide, and the balance of iron-silicon-chromium powder.
3. The method for preparing high-impedance Fe-Si-Cr material according to claim 1, wherein the grain size of the Fe-Si-Cr powder selected in step 1) is not more than 325 meshes.
4. The method for preparing a high-impedance Fe-Si-Cr material according to claim 1, wherein the initial stirring time in step 2) is 30-40min, the heating time in the heating and stirring process is 80-98min, the heating temperature is 145-180 ℃, the first baking temperature is 141-162 ℃, and the baking time is 3.7-6.0 h.
5. The method for preparing the high-impedance iron-silicon-chromium material according to claim 1 or 4, wherein the stirring and dissolving time in the step 3) is 30min, and the stirring and uniform time is 45-80 min.
6. The preparation method of the high-impedance iron-silicon-chromium material according to claim 1, wherein the granulation in the step 4) is that the powder uniformly stirred in the step 3) is granulated by a 50-mesh net, the powder is dried for 3-5h, sieved by a 40-mesh granulator, baked at 67-74 ℃ for 81-102 min, naturally cooled to room temperature, and then sieved by a 40-mesh sieve again.
7. The preparation method of the high-impedance iron-silicon-chromium material according to claim 1, wherein the blending powder in the step 5) comprises the following components in parts by mass (100 parts by mass): 0.15-0.5 part of magnesium oxide, 0.15-0.5 part of demoulding powder and the balance of granulation powder, and the powder mixing and stirring time is 10-20 min.
8. The method for preparing the high-impedance ferro-silicon-chromium material according to the claim 1 or 7, wherein the de-filming powder is composed of zinc stearate, magnesium stearate, polyethylene wax and polypentaerythritol, and the composition ratio is zinc stearate: magnesium stearate: polyethylene wax: polypentaerythritol =48-52 parts: 14-16 parts of: 8-12 parts of: 24-26 parts.
9. The method for preparing high-impedance Fe-Si-Cr material according to claim 1, wherein the forming pressure in step 6) is 6-8T/cm2。
10. The method for preparing the high-impedance Fe-Si-Cr material according to claim 1, wherein the second baking in step 7) is carried out at a temperature of 154-168 ℃ for a total baking time of 3.5-7.0 h.
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