CN109273235B - Double-shell insulation coating method for metal soft magnetic composite material - Google Patents
Double-shell insulation coating method for metal soft magnetic composite material Download PDFInfo
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- CN109273235B CN109273235B CN201811125037.1A CN201811125037A CN109273235B CN 109273235 B CN109273235 B CN 109273235B CN 201811125037 A CN201811125037 A CN 201811125037A CN 109273235 B CN109273235 B CN 109273235B
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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
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- 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
Abstract
The invention discloses a double-shell insulation coating method of a metal soft magnetic composite material, which coats a layer of inorganic salt/oxide composite insulation layer on the surface of metal magnetic powder by a sol-gel process. The inner inorganic salt is used as a buffer layer, so that the bonding strength of the insulating layer and the compact density are improved; the outer oxide can effectively prevent the decomposition of the inner inorganic salt during high-temperature annealing, and the thermal stability of the insulating layer is improved. The soft magnetic composite material is obtained through compression molding, high-temperature heat treatment and spraying process. According to the invention, the metal magnetic powder is subjected to insulation coating by adopting a sol-gel method, the obtained composite coating layer has good binding property with the magnetic powder and high thermal stability, no adhesive is required to be added, the production cost is reduced, meanwhile, the composite coating layer is an inorganic coating material, the resistivity is higher, and the magnetic core loss of the soft magnetic composite material is effectively reduced.
Description
Technical Field
The invention relates to the technical field of preparation of magnetic materials, in particular to a double-shell insulation coating treatment method of a metal soft magnetic composite material.
Background
The soft magnetic composite material (also called magnetic powder core) is formed by uniformly coating a layer of insulating medium on the surface of metal magnetic powder and pressing the metal magnetic powder into various shapes by using a powder metallurgy process. Because of its high magnetic permeability, high saturation magnetic flux density and low core loss, it has been widely used in the electronic and electric fields such as transformers, sensors and choke coils. However, in practical applications, the high eddy current loss caused by low resistivity limits the high frequency applications, and usually an insulating layer with high resistivity and good thermal stability is required to be coated on the surface of the magnetic powder to block eddy current, so that the magnetic core loss is reduced.
The current insulation coating process is mainly based on inorganic matter coating. The phosphoric acid passivation process is the most commonly used 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 and increase the loss of a magnetic core. 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 magnetic powder matrix, easy cracking and even falling of a coating film, and unsatisfactory coating effect.
The invention of chinese patent No. 201510524515.6 is to passivate magnetic powder by mixing phosphoric acid solution with high molecular surfactant, which improves the compact density of powder, but the heat-resistant temperature of the passivation layer is not high, and high-temperature annealing heat treatment cannot be performed to sufficiently eliminate the internal stress generated in the pressing process, so the magnetic core loss is high.
The invention of chinese patent No. 201710593950.3 utilizes aqueous solution of phosphoric acid to passivate magnetic powder, and mixed oxide is insulated to coat for improving thermal stability, and the insulating coating layer prepared by the method has poor bonding strength and uneven coating.
Disclosure of Invention
The invention aims to overcome the defect of low heat-resistant temperature of an insulating film in the prior passivation process and provides a double-shell insulating coating method of a metal soft magnetic composite material. A compact oxide insulating layer is uniformly coated by using a sol-gel process, so that the magnetic core has good bonding strength and good thermal stability, can be thermally annealed at high temperature, further reduces the loss of the magnetic core, and simultaneously keeps better magnetic performance.
The double-shell layer insulation coating method of the metal soft magnetic composite material comprises the following steps:
1) selecting 200-mesh 400-mesh metal magnetic powder for particle size matching, wherein the mass percentage of the mixed powder is as follows: 50-80% of-200- +300 meshes, 20-50% of-300- +400 meshes and the balance of-400 meshes; the metal magnetic powder is one or more of iron powder, iron silicon aluminum powder, iron silicon chromium powder, iron cobalt powder, iron nickel molybdenum powder and iron-based amorphous powder;
2) insulating the proportioned metal magnetic powder by using a passivating agent, and stirring and drying under the water bath condition of 50-90 ℃; then carrying out insulation coating on the magnetic powder by using a sol-gel method, dissolving aluminum isopropoxide which accounts for 5-15% of the weight of ethanol in absolute ethanol, dripping nitric acid to adjust the pH value of the solution to 4-6, uniformly stirring for 30-60 min to obtain sol, adding 10-30 mL of sol into the passivated magnetic powder, and mixing and stirring for 10-30 min to obtain suspension; dropwise adding 2-5 mL of deionized water, and stirring in a water bath at 50-70 ℃ until the mixture is completely dried to obtain composite coated magnetic powder; adding a lubricant into the coated magnetic powder to obtain magnetic powder to be molded;
3) pressing and molding the magnetic powder to be molded, wherein the pressing pressure is 500-2000 MPa, and the pressure maintaining time is 10-20 s, so as to obtain a magnetic ring;
4) carrying out annealing heat treatment on the magnetic ring by adopting nitrogen or argon as protective atmosphere, wherein the heat treatment temperature is 400-750 ℃, and the heat preservation time is 30-120 min;
5) and 4) spraying a layer of epoxy resin insulating paint on the surface of the magnetic ring treated in the step 4) to obtain a finished product of the metal soft magnetic composite material.
Preferably, the weight of the metal magnetic powder is 10-30 g, and the mass of the absolute ethyl alcohol in the sol is 20-50 g.
Preferably, the passivating agent is one or more of phosphoric acid and chromic acid, and the adding amount of the passivating agent accounts for 0.4-2.0% of the total weight of the magnetic powder.
Preferably, the lubricant is one or more of zinc stearate, barium stearate, calcium stearate or molybdenum disulfide.
According to the soft magnetic composite material prepared by the invention, the magnetic powder is subjected to in-situ passivation to form an inorganic salt layer with high bonding strength, and then a compact oxide film is uniformly grown on the outer layer by using a sol-gel method, so that no adhesive is required to be added, the industrial production cost is reduced, the green compact density is improved, the thermal stability is improved, and the magnetic core loss is effectively reduced.
Drawings
Fig. 1 shows the magnetic loss (test condition 100mT) of the sendust soft magnetic composite material prepared by the double-shell insulation coating method and the sample prepared by the traditional phosphoric acid passivation and the single-layer alumina.
Fig. 2 shows the effective permeability (test condition 100mT) of the sendust soft magnetic composite material prepared by the double-shell insulation coating method and the sample prepared by the traditional phosphoric acid passivation and single-layer alumina.
Detailed Description
The soft magnetic composite material is prepared by passivating magnetic powder in situ, coating a layer of oxide on the outer layer by using a sol-gel process, adding a lubricant, performing compression molding, annealing heat treatment and spraying. The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention.
Example 1
Taking 15g of iron powder (namely metal magnetic powder), wherein the iron powder with the granularity of-200 to +300 meshes accounts for 60 percent of the total mass, the iron powder with the granularity of-300 to +400 meshes accounts for 30 percent of the total mass, and the iron powder with the granularity of more than 400 meshes accounts for 10 percent of the total mass. And passivating the proportioned iron powder by using phosphoric acid, and stirring and drying under the condition of water bath at 60 ℃ to obtain passivated magnetic powder, wherein the mass of the phosphoric acid accounts for 0.5 percent of the total weight of the iron powder. And (3) insulating and coating the passivated magnetic powder by using a sol-gel method, dissolving 6g of aluminum isopropoxide in 40g of absolute ethyl alcohol, dripping nitric acid to adjust the pH value of the solution to 6, uniformly stirring for 50min to obtain sol, adding 10mL of sol into the passivated magnetic powder, and mixing and stirring for 10min to obtain suspension. Dropwise adding 2mL of deionized water, and stirring at 50 ℃ in a water bath until the mixture is completely dried to obtain the composite coated magnetic powder. And adding zinc stearate accounting for 0.5 percent of the total weight of the coated magnetic powder into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded. Pressing the magnetic powder to be molded into a magnetic ring with the outer diameter of 23.4mm, the inner diameter of 14.4mm and the height of 8.8mm under the pressure of 700MPa, and keeping the pressure for 15 s. And (3) adopting nitrogen as a protective atmosphere, placing the magnetic ring in an environment with the temperature of 550 ℃ for heat preservation for 60min, and spraying a layer of epoxy resin insulating paint on the surface of the magnetic ring to obtain the iron-based soft magnetic composite material.
The electromagnetic performance of the prepared soft magnetic composite material is tested, and the electromagnetic performance is as follows:
(1) magnetic permeability of the soft magnetic composite material: 87;
(2) direct current superposition performance: 1kHz, H100 Oe, LH/LO＝57.2％；
(3) Under the condition of 100kHz/1V, the quality factor Q is 62;
(4) soft magnetic composite material loss: at 50kHz/100mT, PCV＝810.3mW/cm3。
Example 2
20g of ferro-silicon-aluminum powder is taken, wherein the magnetic powder with the particle size of-200 to +300 meshes accounts for 50 percent of the total mass, the magnetic powder with the particle size of-300 to +400 meshes accounts for 40 percent of the total mass, and the magnetic powder with the particle size of more than 400 meshes accounts for 10 percent of the total mass. And passivating the proportioned iron-silicon-aluminum powder by using chromic acid, and stirring and drying under the condition of a water bath at 50 ℃ to obtain passivated magnetic powder, wherein the mass of the chromic acid accounts for 0.8 percent of the total weight of the magnetic powder. And (2) insulating and coating the passivated magnetic powder by using a sol-gel method, dissolving 4g of aluminum isopropoxide in 30g of absolute ethyl alcohol, dripping nitric acid to adjust the pH value of the solution to 4, uniformly stirring for 30min to obtain sol, adding 25mL of sol into the passivated magnetic powder, mixing and stirring for 20min to obtain suspension, dripping 4mL of deionized water dropwise, and stirring under the water bath condition of 70 ℃ until the mixture is completely dried to obtain the composite coated magnetic powder. And adding barium stearate accounting for 1.2 percent of the total weight of the coated magnetic powder into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded. Pressing the magnetic powder to be molded into a magnetic ring with the outer diameter of 23.4mm, the inner diameter of 14.4mm and the height of 8.8mm under the pressure of 1800MPa, and keeping the pressure for 20 s. And (3) adopting nitrogen as a protective atmosphere, placing the magnetic ring in an environment at 750 ℃ for heat preservation for 50min, and spraying a layer of epoxy resin insulating paint on the surface of the magnetic ring to obtain the Fe-Si-Al soft magnetic composite material.
As can be seen from fig. 1, the magnetic loss of the sendust soft magnetic composite material prepared by the double-shell insulation coating method is obviously lower than that of the samples prepared by phosphoric acid passivation and single-layer alumina, and the magnetic core loss is effectively reduced; from fig. 2, it can be seen that the effective permeability of the sendust soft magnetic composite material prepared by the double-shell insulation coating method is higher than that of the sample prepared by single-layer alumina, but lower than that of the phosphate-passivated sample, because the bond strength of the phosphate-passivated and magnetic powder is high, and the bond strength is reduced after the oxide is composited, but still kept at a higher level.
The electromagnetic performance of the prepared soft magnetic composite material is tested, and the electromagnetic performance is as follows:
(1) magnetic permeability of the soft magnetic composite material: 124;
(2) direct current superposition performance: 1kHz, H100 Oe, LH/LO＝38.2％；
(3) Under the condition of 100kHz/1V, the quality factor Q is 72;
(4) soft magnetic composite material loss: at 50kHz/100mT, PCV＝250.4mW/cm3。
Example 3
10g of iron-nickel powder is taken, wherein the magnetic powder with the granularity of-200 to +300 meshes accounts for 70 percent of the total mass, the magnetic powder with the granularity of-300 to +400 meshes accounts for 25 percent of the total mass, and the magnetic powder with the granularity of more than 400 meshes accounts for 5 percent of the total mass. And passivating the proportioned iron-nickel powder by using phosphoric acid, and stirring and drying the iron-nickel powder under the condition of 80 ℃ water bath to obtain passivated magnetic powder, wherein the mass of the phosphoric acid accounts for 1.0 percent of the total weight of the magnetic powder. And (3) insulating and coating the passivated magnetic powder by using a sol-gel method, dissolving 3g of aluminum isopropoxide in 25g of absolute ethyl alcohol, dripping nitric acid to adjust the pH value of the solution to 5, uniformly stirring for 20min to obtain sol, adding 15mL of sol into the passivated magnetic powder, and mixing and stirring for 15min to obtain suspension. Dropwise adding 3mL of deionized water, and stirring at 60 ℃ in a water bath until the mixture is completely dried to obtain the composite coated magnetic powder. And adding calcium stearate accounting for 0.8 percent of the total weight of the coated magnetic powder into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded. Pressing the magnetic powder to be molded into a magnetic ring with the outer diameter of 23.4mm, the inner diameter of 14.4mm and the height of 8.8mm under the pressure of 1300MPa, and keeping the pressure for 10 s. And (3) adopting argon as a protective atmosphere, placing the magnetic ring in an environment of 670 ℃ for heat preservation for 70min, and spraying a layer of epoxy resin insulating paint on the surface of the magnetic ring to obtain the iron-nickel-based soft magnetic composite material.
The electromagnetic performance of the prepared soft magnetic composite material is tested, and the electromagnetic performance is as follows:
(1) magnetic permeability of the soft magnetic composite material: 128;
(2) direct current superposition performance: 1kHz, H100 Oe, LH/LO＝59.3％；
(3) Under the condition of 100kHz/1V, the quality factor Q is 67;
(4) soft magnetic composite material loss: at 50kHz/100mT, PCV＝280.6mW/cm3。
Claims (4)
1. A double-shell insulation coating method of a metal soft magnetic composite material is characterized by comprising the following steps:
1) selecting 200-mesh 400-mesh metal magnetic powder for particle size matching, wherein the mass percentage of the mixed powder is as follows: 50-80% of-200 to +300 meshes, 20-50% of-300 to +400 meshes and the balance of-400 meshes; the metal magnetic powder is one or more of iron powder, iron silicon aluminum powder, iron silicon chromium powder, iron cobalt powder, iron nickel molybdenum powder and iron-based amorphous powder;
2) insulating the proportioned metal magnetic powder by using a passivating agent, and stirring and drying under the water bath condition of 50-90 ℃; then carrying out insulation coating on the magnetic powder by using a sol-gel method, dissolving aluminum isopropoxide accounting for 5-15% of the weight of ethanol in absolute ethanol, dripping nitric acid to adjust the pH value of the solution to 4-6, uniformly stirring for 30-60 min to obtain sol, adding 10-30 mL of sol into the passivated magnetic powder, and mixing and stirring for 10-30 min to obtain suspension; dropwise adding 2-5 mL of deionized water, and stirring in a water bath at 50-70 ℃ until the mixture is completely dried to obtain composite coated magnetic powder; adding a lubricant into the coated magnetic powder to obtain magnetic powder to be molded;
3) pressing and molding the magnetic powder to be molded, wherein the pressing pressure is 500-2000 MPa, and the pressure maintaining time is 10-20 s, so as to obtain a magnetic ring;
4) carrying out annealing heat treatment on the magnetic ring by adopting nitrogen or argon as a protective atmosphere, wherein the heat treatment temperature is 400-750 ℃, and the heat preservation time is 30-120 min;
5) and 4) spraying a layer of epoxy resin insulating paint on the surface of the magnetic ring treated in the step 4) to obtain a finished product of the metal soft magnetic composite material.
2. The double-shell insulation coating method of the metal soft magnetic composite material according to claim 1, wherein the weight of the metal magnetic powder is 10-30 g, and the mass of the absolute ethyl alcohol in the sol is 20-50 g.
3. The double-shell insulation coating method of the metal soft magnetic composite material according to claim 1, wherein the passivating agent is one or more of phosphoric acid and chromic acid, and the adding amount of the passivating agent is 0.4-2.0% of the total weight of the magnetic powder.
4. The method for double-shell insulation cladding of metallic soft magnetic composite material according to claim 1, characterized in that said lubricant is one or more of zinc stearate, barium stearate, calcium stearate or molybdenum disulfide.
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| CN111370214A (en) * | 2019-11-20 | 2020-07-03 | 横店集团东磁股份有限公司 | Method for preparing magnetic powder core from alloy composite powder |
| CN111029126B (en) * | 2019-12-12 | 2022-09-23 | 安徽工业大学 | All-inorganic high-temperature-resistant insulating bonding method for iron-based metal soft magnetic composite material |
| CN112908677B (en) * | 2021-02-08 | 2022-09-27 | 浙江工业大学 | Preparation method of high-permeability low-loss integrated inductance material |
| CN113113224A (en) * | 2021-04-14 | 2021-07-13 | 中国科学院宁波材料技术与工程研究所 | Novel insulation coating method of soft magnetic powder for die-pressed inductor |
| CN113451039B (en) * | 2021-07-01 | 2023-03-14 | 中钢天源股份有限公司 | FeSi-based water atomized Fe-Si-Cr soft magnetic powder core and preparation method thereof |
| CN113674984B (en) * | 2021-08-26 | 2023-03-21 | 合肥工业大学 | Preparation method of FeSiAlZrScSr magnetic powder core |
| CN113744989A (en) * | 2021-09-02 | 2021-12-03 | 横店集团东磁股份有限公司 | Metal magnetic powder core and preparation method and application thereof |
| CN113996781B (en) * | 2021-10-12 | 2023-10-13 | 内蒙金属材料研究所 | Soft magnetic composite material and preparation method thereof |
| CN114068167A (en) * | 2021-11-15 | 2022-02-18 | 横店集团东磁股份有限公司 | Soft magnetic composite material and preparation method and application thereof |
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