CN113113224A - Novel insulation coating method of soft magnetic powder for die-pressed inductor - Google Patents
Novel insulation coating method of soft magnetic powder for die-pressed inductor Download PDFInfo
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- CN113113224A CN113113224A CN202110399862.6A CN202110399862A CN113113224A CN 113113224 A CN113113224 A CN 113113224A CN 202110399862 A CN202110399862 A CN 202110399862A CN 113113224 A CN113113224 A CN 113113224A
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- 238000009413 insulation Methods 0.000 title claims abstract description 28
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- 229910052742 iron Inorganic materials 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- -1 iron silicon aluminum Chemical compound 0.000 claims description 4
- XEVZIAVUCQDJFL-UHFFFAOYSA-N [Cr].[Fe].[Si] Chemical compound [Cr].[Fe].[Si] XEVZIAVUCQDJFL-UHFFFAOYSA-N 0.000 claims description 3
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- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 3
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- 239000002184 metal Substances 0.000 description 10
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
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- 238000011160 research Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 3
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- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- H—ELECTRICITY
- 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
- 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
-
- 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
- H01F1/34—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 non-metallic substances, e.g. ferrites
- H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
Abstract
The invention provides a novel insulation coating method of soft magnetic powder for a molded inductor, which comprises the following steps: mixing ethanol, water, nano inorganic salt and a coupling agent to obtain modified nano inorganic salt; mixing the modified nano inorganic salt, acetone, epoxy resin, a lubricant and soft magnetic powder and then drying to obtain magnetic powder to be molded; pressing and forming the magnetic powder to be formed to obtain a blank; and annealing the blank to obtain the soft magnetic composite material. According to the invention, a compact and uniform nano inorganic salt-epoxy resin insulating layer is coated on the surface of the soft magnetic powder by a surface modification method, so that the resistivity of the coating layer can be obviously improved, the obtained composite material has good bonding strength and good thermal stability, and can be thermally annealed at high temperature, and the loss of a magnetic core is further reduced.
Description
Technical Field
The invention belongs to the technical field of soft magnetic material insulation coating, and particularly relates to a novel insulation coating method of soft magnetic powder for a die pressing inductor.
Background
The soft magnetic composite material has a special magnetoelectric conversion function, so that the soft magnetic composite material is widely applied to various electronic products and devices. The iron-based soft magnetic composite magnetic powder cores (SMCs) are formed by mixing and pressing ferromagnetic powder particles and insulating media by adopting a powder metallurgy process, and have the characteristics of small power loss, good thermal stability, constant magnetic conductivity and the like. Soft magnetic materials are widely used in electromagnetic inverters, filters, transformers and molded inductors.
The die pressing inductor is a device formed by uniformly coating a layer of insulating medium on the surface of metal magnetic powder, embedding a coil into the magnetic powder by using a powder metallurgy process and then pressing and forming the coil and the magnetic powder together; the method mainly comprises two steps: a molded coil and an integrally formed inductor belong to a form of a magnetic powder core. In practical applications, high eddy current loss caused by low resistivity limits high-frequency applications, and an insulating layer with high resistivity and good thermal stability is usually required to cover the surface of the soft magnetic powder to block eddy current, so that the core loss is reduced.
The molded inductor has the following advantages: magnetic leakage can be reduced, and the conversion efficiency is high; the precision and the quality are good; oxidation resistance, rust prevention and long service life; the molded inductor is integrally formed and has small volume; the working frequency coverage range is wide and reaches 10 MHz; the method is suitable for large-current environments and the like. Therefore, the method has important significance for the research of the molded inductor.
The existing soft magnetic powder insulation coating process for the die pressing inductor is mainly divided into inorganic coating and organic coating. The organic coating agent mainly comprises epoxy resin, phenolic resin, silicon resin and the like, and most experimental researches show that the resistivity of the metal magnetic powder core can be obviously improved by adopting the organic coating agent, and the defects that the adopted organic coating agent is a non-magnetic substance and is easy to generate thermal decomposition at high temperature are overcome. The current inorganic coating agent is mainly phosphoric acid passivation, and the phosphoric acid passivation process is the most common coating method in industrial production due to the characteristics of simplicity and low cost, but researches show that a phosphate coating layer can be decomposed during high-temperature annealing to cause the rapid reduction of the resistivity, so that the magnetic core loss is increased. In order to find an insulating medium to replace phosphate, thermally stable oxides include SiO2、MgO、Al2O3And ferrite, etc. are developed and researched successively, but the oxide has high brittleness, poor binding property with the soft magnetic powder matrix, easy cracking and even falling of the coating layer, and unsatisfactory coating effect.
Disclosure of Invention
In view of the above, the present invention provides a novel insulation coating method for soft magnetic powder for die-pressing inductor, and the composite insulation coating layer provided by the present invention has good resistivity and thermal stability.
The invention provides a novel insulation coating method of soft magnetic powder for a molded inductor, which comprises the following steps:
the nano inorganic salt is applied to the soft magnetic powder insulation coating method to generate a novel nano inorganic salt-epoxy resin composite insulation coating layer.
Preferably, the novel insulation coating method of the soft magnetic powder for the molded inductor specifically comprises the following steps:
mixing ethanol, water, nano inorganic salt and a coupling agent to obtain modified nano inorganic salt;
mixing the modified nano inorganic salt, acetone, epoxy resin, a lubricant and soft magnetic powder and then drying to obtain magnetic powder to be molded;
pressing and forming the magnetic powder to be formed to obtain a blank;
and annealing the blank to obtain the soft magnetic composite material.
Preferably, the nano inorganic salt is one or more selected from nano calcium carbonate, nano magnesium carbonate, nano barium titanate and nano calcium silicate.
Preferably, the coupling agent is selected from a silane coupling agent or a titanate coupling agent.
Preferably, the soft magnetic powder is selected from one or more of iron powder, iron silicon aluminum powder, iron silicon chromium powder, iron cobalt powder, iron nickel powder, carbonyl iron powder, iron nickel molybdenum powder, iron-based amorphous powder and iron-based nanocrystalline powder.
Preferably, the soft magnetic powder has a particle size of 100 to 500 mesh.
Preferably, the drying temperature is 30-60 ℃.
Preferably, the pressure intensity of the compression molding is 600-2000 MPa.
Preferably, the temperature of the annealing treatment is 200-800 ℃.
Preferably, the particle size of the nano inorganic salt is 1-100 nm.
The novel insulating coating layer provided by the invention overcomes the defects that a phosphorization layer is easily decomposed by heating and the heat-resistant temperature of an organic resin insulating coating layer is not high in the existing phosphoric acid passivation process, and the nano-composite insulating layer of the metal soft magnetic composite material (mould pressing inductor) is prepared by the method, so that nano inorganic salts are successfully introduced into the insulating coating of soft magnetic powder. The nano inorganic salt has the advantages of high melting point, high heat-resistant temperature, high resistivity, low price and the like, and the nano inorganic salt is often used for enhancing the mechanical property of organic resin and has mature process. According to the invention, a compact and uniform nano inorganic salt-epoxy resin insulating layer is coated on the surface of the soft magnetic powder by a surface modification method, so that the resistivity of the coating layer can be obviously improved, the obtained composite material has good bonding strength and good thermal stability, and can be thermally annealed at high temperature, and the loss of a magnetic core is further reduced.
Drawings
FIG. 1 is an SEM image of the surface topography of the Fe-Si-Cr soft magnetic composite material prepared in example 1 of the present invention;
FIG. 2 is a graph showing the core loss of the magnetic powder core prepared in example 1 of the present invention and the magnetic powder core prepared in comparative example 1;
fig. 3 shows effective permeability of the magnetic powder core prepared in example 1 of the present invention and the magnetic powder core prepared in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a novel insulation coating method of soft magnetic powder for a molded inductor, which comprises the following steps:
the nano inorganic salt is applied to the soft magnetic powder insulation coating method to generate a novel nano inorganic salt-epoxy resin composite insulation coating layer.
In the present invention, the novel insulation coating method of the soft magnetic powder for the molded inductor preferably includes:
mixing ethanol, water, nano inorganic salt and a coupling agent to obtain modified nano inorganic salt;
mixing the modified nano inorganic salt, acetone, epoxy resin, a lubricant and soft magnetic powder and then drying to obtain magnetic powder to be molded;
pressing and forming the magnetic powder to be formed to obtain a blank;
and annealing the blank to obtain the soft magnetic composite material.
In the present invention, the ethanol is preferably anhydrous ethanol; the water is preferably deionized water; the coupling agent is preferably selected from a silane coupling agent or a titanate coupling agent, more preferably a silane coupling agent, and most preferably a silane coupling agent KH550 or KH 560.
In the invention, the amount of the coupling agent is preferably 0.01-0.1% of the modified nano inorganic salt, more preferably 0.02-0.08%, more preferably 0.03-0.06%, and most preferably 0.04-0.05%.
In the invention, ethanol is used as a modification solvent to carry out surface modification on the nano inorganic salt; the mass ratio of water to ethanol is preferably not more than 1: 19, more preferably 1: (7-15), more preferably 1: (8-12), most preferably 1: 10.
in the invention, the nano inorganic salt is preferably selected from one or more of nano calcium carbonate, nano magnesium carbonate, nano barium titanate and nano calcium silicate. In the invention, the particle size of the nano inorganic salt is preferably 1-100 nm, more preferably 5-80 nm, more preferably 10-60 nm, more preferably 20-50 nm, more preferably 30-40 nm, and most preferably 35 nm; in the embodiment of the invention, the particle size of the nano inorganic salt is preferably 40-80 nm.
In the invention, the mass ratio of the ethanol to the water to the nano inorganic salt to the coupling agent is preferably (5-15): (1-5): (0.01-0.5): (0.01-0.2), more preferably (8-12): (2-4): (0.1-0.4): (0.05 to 0.15), most preferably 10: 3: (0.2-0.3): (0.08-0.12).
In the present invention, the preparation method of the modified nano inorganic salt preferably comprises:
adding nano inorganic salt into ethanol and water, then adding a silane coupling agent for full stirring, then carrying out rapid mechanical stirring, then carrying out water bath heating and ultrasonic treatment simultaneously, and continuously carrying out surface modification so as to fully disperse and modify the nano inorganic salt.
In the invention, the rotation speed of the mechanical stirring is preferably not less than 400r/min, more preferably 400-700 r/min, more preferably 500-600 r/min, and most preferably 550 r/min.
In the invention, the temperature of the water bath heating is preferably 40-80 ℃, more preferably 50-70 ℃, more preferably 55-65 ℃ and most preferably 60 ℃; in the embodiment of the invention, the temperature of the water bath heating is preferably 40-70 ℃.
In the invention, the ultrasonic frequency of the ultrasonic treatment is preferably 30-80 Hz, more preferably 40-70 Hz, more preferably 50-60 Hz, and most preferably 55 Hz; the power of ultrasonic treatment is preferably 100-150W, more preferably 110-140W, and most preferably 120-130W.
In the present invention, the time for the surface modification is preferably 0.5 to 1.5 hours, more preferably 0.8 to 1.2 hours, and most preferably 1 hour.
In the present invention, the mass of the nano inorganic salt is preferably 0 to 4%, more preferably 0.5 to 3.5%, more preferably 1 to 3%, more preferably 1.5 to 2.5%, and most preferably 2% of the mass of the soft magnetic powder; in an embodiment of the present invention, the mass of the nano inorganic salt is preferably 0.5 to 1.5% of the mass of the soft magnetic powder.
In the present invention, the acetone is preferably anhydrous acetone; the amount of acetone is larger than the volume of the soft magnetic powder.
In the present invention, the mass of the epoxy resin is preferably 0 to 3% of the mass of the soft magnetic powder, more preferably 0.5 to 2.5%, more preferably 1 to 2%, and most preferably 1.5%; in an embodiment of the present invention, the mass of the epoxy resin is preferably 0.5 to 2% of the mass of the soft magnetic powder.
In the present invention, the lubricant is preferably one or both of zinc stearate and barium stearate.
In the present invention, the lubricant preferably has a mass of not more than 1% of the mass of the soft magnetic powder, more preferably 0.2 to 0.8%, more preferably 0.3 to 0.6%, and most preferably 0.4 to 0.5%.
In the present invention, the soft magnetic powder preferably has a particle size of 100 to 500 mesh, more preferably 200 to 400 mesh, more preferably 250 to 350 mesh, and most preferably 300 mesh. In the present invention, the soft magnetic powder preferably has a mass content of-300 to +500 in terms of particle size of 50 to 80%, more preferably 55 to 75%, more preferably 60 to 70%, and most preferably 75%; the mass content of-200 to +300 meshes is preferably 20 to 50 percent, more preferably 25 to 45 percent, more preferably 30 to 40 percent, and most preferably 35 percent; the particle size of the soft magnetic powder of the remaining mass content is-100 to +200 mesh.
In the invention, the soft magnetic powder is preferably selected from one or more of iron powder, iron silicon aluminum powder, iron silicon chromium powder, iron cobalt powder, iron nickel powder, carbonyl iron powder, iron nickel molybdenum powder, iron-based amorphous powder and iron-based nanocrystalline powder. In the present invention, the shape (morphology) of the soft magnetic powder is preferably a flake shape or a sphere shape.
In the present invention, the method for preparing the magnetic powder to be molded preferably includes:
adding acetone into the modified nano inorganic salt (suspension), then adding epoxy resin, simultaneously adding a lubricant for facilitating demoulding, and finally adding soft magnetic powder; and under the condition of water bath, carrying out high-speed mechanical stirring while carrying out ultrasonic dispersion until the mixed solution is completely volatilized, and drying in a vacuum oven to obtain the composite coated soft magnetic powder, namely the magnetic powder to be molded.
In the invention, the temperature of the water bath condition is preferably 40-80 ℃, more preferably 50-70 ℃, more preferably 55-65 ℃ and most preferably 60 ℃; in the embodiment of the invention, the temperature of the water bath condition is preferably 40-70 ℃.
In the invention, the frequency of the ultrasonic dispersion is preferably 30-80 Hz, more preferably 40-70 Hz, more preferably 50-60 Hz, and most preferably 55 Hz.
In the invention, the speed of the mechanical stirring is preferably 400-700 r/min, more preferably 500-600 r/min, and most preferably 550 r/min.
In the invention, the drying temperature is preferably 30-60 ℃, more preferably 35-55 ℃, more preferably 40-50 ℃ and most preferably 45 ℃.
In the present invention, the press molding is preferably performed in an annular mold; the outer diameter of the annular die is preferably 20.3 mm; the inner diameter is preferably 12.7 mm.
In the present invention, after the magnetic ring is obtained by the press molding, the method preferably further includes:
and uniformly winding a coil around the magnetic ring.
In the invention, the diameter of the coil is preferably 0.5-0.7 mm, and more preferably 0.6 mm; the coil is preferably an insulated copper enameled wire; the winding number of the coil is preferably 15-25 turns, more preferably 18-22 turns, and most preferably 20 turns.
In the invention, the pressure intensity in the compression molding process is preferably 600-2000 MPa, more preferably 1000-1500 MPa, and most preferably 1200-1300 MPa; the pressure maintaining time in the compression molding process is preferably 60-100 s, more preferably 70-90 s, more preferably 75-85 s, and most preferably 80 s.
In the present invention, the press forming is preferably performed in a ring press; the press-forming is preferably integrally press-forming.
In the present invention, after obtaining the blank, it is preferable to further include:
and carrying out spraying treatment on the blank.
In the present invention, the spraying treatment is preferably spraying of an insulating paint.
In the invention, the annealing treatment temperature is preferably 200-800 ℃, more preferably 300-700 ℃, more preferably 400-600 ℃, and most preferably 500 ℃; the time of the annealing treatment is preferably 1-2 h, more preferably 1.2-1.8 h, and most preferably 1.4-1.6 h; the heat preservation time in the annealing treatment process is preferably 60-180 min, more preferably 80-160 min, more preferably 100-140 min, and most preferably 120-130 min.
In the present invention, the annealing treatment is preferably a vacuum annealing treatment.
The invention applies nano inorganic salt to soft magnetic powder insulation coating material to prepare novel nano inorganic salt-epoxy resin composite insulation coating layer. The invention provides a novel insulation coating material and a method for soft magnetic powder for a molded inductor, wherein a layer of nano inorganic salt-epoxy resin with high bonding strength is compounded on the surface of the soft magnetic powder, and inorganic salts are introduced into the insulation coating layer of the soft magnetic powder, so that the resistivity of the coating layer is greatly improved, the obtained composite material has good bonding strength and good thermal stability, can be subjected to high-temperature thermal annealing, and the loss of a magnetic core is effectively reduced.
The invention provides a novel insulating coating material and a method for a die-pressing inductor, which aims to overcome the defects that a phosphate layer is easily decomposed by heating and an organic resin insulating coating layer has low heat-resistant temperature in the prior phosphoric acid passivation process, and provides an insulating coating method for a nano composite insulating layer of a metal soft magnetic composite material (the die-pressing inductor).
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The raw materials used in the following examples of the present invention are all commercially available products.
Example 1
Selecting FeSiCr alloy soft magnetic powder with the granularity of 100-500 meshes for carrying out granularity matching, wherein the mass percentage of the mixed powder is as follows: 70 percent of-300 to +500 meshes, 20 percent of-200 to +300 meshes and 16g of the rest, wherein the total mass is-100 to +200 meshes, and then 4g of carbonyl iron powder (-500 meshes) is compounded with the carbonyl iron powder to obtain 20g of compounded metal soft magnetic composite powder.
And selecting nano calcium carbonate accounting for 1% of the mass fraction of the soft magnetic composite powder, wherein the size of the nano calcium carbonate is 40-80 nm. Firstly, 50ml of absolute ethyl alcohol and a small amount of deionized water, namely 5ml, are added into a beaker, then nano calcium carbonate is added, and simultaneously 1ml of silane coupling agent (KH550) is added, and after the materials are fully stirred by glass, the materials are mechanically stirred at a higher rotating speed, wherein the rotating speed is 560 r/min; then wrapping the mouth of the beaker by using a preservative film and a rubber band, heating the beaker in water bath at 50 ℃, simultaneously carrying out 120W ultrasonic treatment on the beaker, and continuously carrying out surface modification for one hour so as to fully disperse and modify the surface of the nano calcium carbonate.
Adding 30ml of anhydrous acetone into the modified nano calcium carbonate suspension, then adding an epoxy resin binder accounting for 2% of the mass fraction of the composite soft magnetic composite powder, simultaneously adding zinc stearate accounting for 0.5% of the mass fraction of the soft magnetic composite powder so as to facilitate later demolding, finally adding the proportioned composite soft magnetic powder, and firstly mixing and stirring the suspension by using a glass rod; and similarly, continuously performing ultrasonic dispersion and high-speed mechanical stirring at the same time under the condition of 50 ℃ water bath until the solvent of the mixed solution is completely volatilized, and drying in a vacuum oven at 50 ℃ to obtain the composite coated soft magnetic powder, namely the magnetic powder to be molded.
Putting the magnetic powder to be molded into an annular mold with the outer diameter of 20.3mm and the inner diameter of 12.7mm, and then performing compression molding by using a ring press, wherein the compression pressure is 600MPa, and the pressure maintaining time is 60s, so as to obtain a magnetic ring blank; winding a 20-turn coil on the magnetic ring blank by using an insulated copper enameled wire with the diameter of 0.6 mm; and then, spraying insulating paint on the magnetic ring blank, and finally carrying out vacuum annealing heat treatment, wherein the vacuum annealing temperature is 200 ℃, the annealing time is 1h, and the heat preservation time is 60min, so as to obtain the soft magnetic composite material.
SEM test is carried out on the surface morphology of the soft magnetic composite material prepared in the embodiment 1 of the invention, the test result is shown in figure 1, and as can be seen from figure 1, the surfaces of the magnetic powder particles are uniformly coated with the nano inorganic salt particle/epoxy resin nano composite insulating coating layer.
The fesicro soft magnetic composite material (magnetic powder core) prepared in example 1 of the present invention was subjected to an electromagnetic performance test using a (MATS-2010SA Linkjoin) power loss tester produced by allied technologies ltd. The detection result is that the magnetic permeability of the soft magnetic composite material is 27; direct current superposition performance: 1kHz, when H is 100Oe, L/Lo is 90%; under the condition of 100kHz/1V, the quality factor Q is 107; soft magnetic composite material loss: at 100kHz/50mT, the Pcv is 453.5mW/cm3(ii) a As shown in fig. 2 and 3.
Example 2
Selecting FeSiAl alloy soft magnetic powder with the granularity of 100-500 meshes for carrying out granularity proportioning, wherein the mass percentage of the mixed powder is-300 to +500 meshes accounting for 60 percent, the mass percentage of the mixed powder is-200 to +300 meshes accounting for 20 percent, the mass percentage of the rest is-100 to +200 meshes, and the total mass is 16g, and then compounding 4g of carbonyl iron powder (-500 meshes) with the carbonyl iron powder to obtain 20g of compounded metal soft magnetic composite powder.
And selecting nano barium titanate accounting for 1.5% of the mass fraction of the soft magnetic composite powder, wherein the size of the nano barium titanate is 40-80 nm. Firstly, adding a proper amount of 40ml of anhydrous ethanol and 10ml of deionized water into a beaker, then adding nano barium titanate, simultaneously adding 0.7ml of titanate coupling agent, fully stirring with glass, then carrying out mechanical stirring at a higher rotating speed of 550r/min, then wrapping the mouth of the beaker with a preservative film and a rubber band, then heating the beaker in a water bath at 50 ℃, simultaneously carrying out 120W ultrasonic treatment on the beaker, and continuously carrying out surface modification for one hour to ensure that the nano barium titanate is fully dispersed and surface modified.
Adding 40ml of anhydrous acetone into the surface-modified nano barium titanate suspension, then adding an epoxy resin binder accounting for 2 mass percent of the soft magnetic composite powder, simultaneously adding barium stearate accounting for 0.5 mass percent of the soft magnetic composite powder so as to facilitate later demolding, finally adding the proportioned mixed metal soft magnetic powder, and firstly mixing and stirring the mixed metal soft magnetic powder for a while by using a glass rod; and similarly, continuously performing ultrasonic dispersion and high-speed mechanical stirring at the same time under the condition of 50 ℃ water bath until the solvent of the mixed solution is completely volatilized, and drying in a vacuum oven at 50 ℃ to obtain the composite coated soft magnetic powder, namely the magnetic powder to be molded.
Putting magnetic powder to be molded into an annular mold with the outer diameter of 20.3mm and the inner diameter of 12.7mm, then performing compression molding by using a ring press, wherein the compression pressure is 1800MPa, the pressure maintaining time is 150s, so as to obtain a magnetic ring blank, and winding 20 turns of coils on the magnetic ring blank by using an insulated copper enameled wire with the diameter of 0.6 mm; and then, spraying insulating paint on the magnetic ring blank, and finally carrying out vacuum annealing heat treatment, wherein the vacuum annealing temperature is 700 ℃, the annealing time is 1h, and the heat preservation time is 120min, so as to obtain the soft magnetic composite material.
The electromagnetic performance test of the FeSiAl soft magnetic composite material (magnetic powder core) prepared in the embodiment 2 of the invention is performed according to the method of the embodiment 1, and the detection result is that the magnetic permeability of the soft magnetic composite material is 70; direct current superposition performance: 1kHz, when H is 100Oe, L/Lo is 56%; under the condition of 100kHz/1V, the quality factor Q is 73; when the loss of the soft magnetic composite material is 100kHz/50mT, the Pcv is 180.5mW/cm3。
Comparative example 1
Selecting FeSiCr alloy soft magnetic powder with the granularity of 100-500 meshes for carrying out the granularity proportioning, wherein the mass percentage of the mixed powder is-300 to +500 meshes for 70 percent, -200 to +300 meshes for 20 percent, the rest is-100 to +200 meshes, and the total mass is 16g, and then compounding 4g of carbonyl iron powder (-500 meshes) with the mixed powder to obtain 20g of compounded metal soft magnetic composite powder.
Firstly, adding 40ml of anhydrous acetone into a beaker, then adding an epoxy resin adhesive accounting for 2 mass percent of the soft magnetic composite powder and zinc stearate accounting for 0.5 mass percent of the soft magnetic composite powder so as to facilitate later demolding, finally adding the proportioned composite soft magnetic powder, and firstly mixing and stirring the materials by using a glass rod for a while to obtain a suspension; and (3) carrying out high-speed mechanical stirring while carrying out ultrasonic dispersion by 120W ultrasonic power under the condition of a water bath at 50 ℃, wherein the rotating speed is 570r/min until the solvent of the mixed solution is completely volatilized, and drying in a vacuum oven at 50 ℃ to obtain soft magnetic powder coated by pure epoxy resin, namely the magnetic powder to be molded.
Putting magnetic powder to be molded into an annular mold with the outer diameter of 20.3mm and the inner diameter of 12.7mm, then performing compression molding by using a ring press, wherein the compression pressure is 600MPa, the pressure maintaining time is 60s, so as to obtain a magnetic ring blank, and winding 20 turns of coils on the magnetic ring blank by using an insulated copper enameled wire with the diameter of 0.6 mm; and then, spraying insulating paint on the magnetic ring blank, and finally, carrying out vacuum annealing heat treatment on the pressed magnetic ring, wherein the vacuum annealing temperature is 200 ℃, the annealing time is 1h, and the heat preservation time is 60min, so as to obtain the soft magnetic composite material.
According to the method of the embodiment 1, the fesicro soft magnetic composite material (magnetic powder core) prepared in the comparative example 1 of the invention is subjected to an electromagnetic performance test, and the detection result is as follows: soft magnetic composite permeability 34; the direct current superposition performance is 1kHz, and when H is 100Oe, L/Lo is 84%; under the condition of 100kHz/1V, the quality factor Q is 105; when the loss of the soft magnetic composite material is 100kHz/50mT, the Pcv is 615.5mW/cm3(ii) a As shown in fig. 2 and 3.
The invention provides a novel soft magnetic powder insulation coating material and a method thereof, which overcome the defects that a phosphorization layer is easily decomposed by heating and the heat-resistant temperature of an organic resin insulation coating layer is not high in the prior phosphoric acid passivation process, and provide a preparation method of a nano composite insulation layer of a metal soft magnetic composite material (a die pressing inductor), so that nano inorganic salts are successfully introduced into the insulation coating of soft magnetic powder. The nano inorganic salt has the advantages of high melting point, high heat-resistant temperature, high resistivity, low price and the like, and the nano inorganic salt is often used for enhancing the mechanical property of organic resin and has mature process. According to the invention, a compact and uniform nano inorganic salt-epoxy resin insulating layer is coated on the surface of the soft magnetic powder by a surface modification method, so that the resistivity of the coating layer can be obviously improved, the obtained composite material has good bonding strength and good thermal stability, and can be thermally annealed at high temperature, and the loss of a magnetic core is further reduced.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A novel insulation coating method of soft magnetic powder for a molded inductor comprises the following steps:
the nano inorganic salt is applied to the soft magnetic powder insulation coating method to generate a novel nano inorganic salt-epoxy resin composite insulation coating layer.
2. The method as claimed in claim 1, wherein the novel insulation coating method of soft magnetic powder for molded inductors specifically comprises:
mixing ethanol, water, nano inorganic salt and a coupling agent to obtain modified nano inorganic salt;
mixing the modified nano inorganic salt, acetone, epoxy resin, a lubricant and soft magnetic powder and then drying to obtain magnetic powder to be molded;
pressing and forming the magnetic powder to be formed to obtain a blank;
and annealing the blank to obtain the soft magnetic composite material.
3. The method according to claim 2, wherein the nano inorganic salt is selected from one or more of nano calcium carbonate, nano magnesium carbonate, nano barium titanate and nano calcium silicate.
4. A method according to claim 2, characterized in that the coupling agent is selected from silane coupling agents or titanate coupling agents.
5. The method according to claim 2, wherein the soft magnetic powder is selected from one or more of iron powder, iron silicon aluminum powder, iron silicon chromium powder, iron cobalt powder, iron nickel powder, carbonyl iron powder, iron nickel molybdenum powder, iron-based amorphous powder and iron-based nanocrystalline powder.
6. The method as claimed in claim 2, wherein the soft magnetic powder has a particle size of 100 to 500 mesh.
7. The method according to claim 2, wherein the drying temperature is 30 to 60 ℃.
8. The method according to claim 2, wherein the pressure of the press forming is 600 to 2000 MPa.
9. The method according to claim 2, wherein the temperature of the annealing treatment is 200 to 800 ℃.
10. The method according to claim 2, wherein the nano inorganic salt has a particle size of 1 to 100 nm.
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