CN111192735A - Insulation coated metal soft magnetic powder and preparation method and application thereof - Google Patents
Insulation coated metal soft magnetic powder and preparation method and application thereof Download PDFInfo
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- CN111192735A CN111192735A CN202010051762.XA CN202010051762A CN111192735A CN 111192735 A CN111192735 A CN 111192735A CN 202010051762 A CN202010051762 A CN 202010051762A CN 111192735 A CN111192735 A CN 111192735A
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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
- H01F1/147—Alloys characterised by their composition
- H01F1/14708—Fe-Ni based alloys
- H01F1/14733—Fe-Ni based alloys in the form of particles
- H01F1/14741—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together
- H01F1/1475—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together the particles being insulated
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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
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
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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
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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
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The invention relates to an insulation coated metal soft magnetic powder and a preparation method and application thereof. The method comprises the following steps: (1) mixing the metal soft magnetic powder with an insulating agent and a solvent, and removing the solvent to obtain pre-coated powder; (2) and (2) carrying out high-temperature heat treatment on the pre-coated powder obtained in the step (1) to obtain the insulated and coated metal soft magnetic powder. According to the preparation method provided by the invention, the surface of the metal soft magnetic powder is coated with the uniform and compact organic insulating layer, so that the flowability of the metal soft magnetic powder is effectively improved; the fluidity of the metal soft magnetic powder coated in an insulating way can reach below 35s/50g, the density and the internal uniformity of the metal soft magnetic powder core are improved, the magnetic properties such as magnetic conductivity, loss and the like are improved, the problems of long pressing period, low production efficiency, high production cost and the like are solved, and the metal soft magnetic powder coated in an insulating way has high application value.
Description
Technical Field
The invention relates to the technical field of soft magnetic materials, in particular to metal soft magnetic powder coated in an insulating way, a preparation method and application thereof.
Background
The metal soft magnetic powder core is a common soft magnetic material and is widely applied to the fields of electronic communication, switching power supplies and the like. The metal soft magnetic powder core is prepared by adopting a powder metallurgy method to prepare metal powder, and is prepared by insulating coating, press forming, high-temperature heat treatment and other processes, and has the characteristics of small high-frequency eddy current loss, high magnetic conductivity, high temperature stability and the like.
The insulation manner of the metal powder includes organic insulation and inorganic insulation. Common organic insulating agents include epoxy resins, phenolic resins, and the like, but organic materials generally have poor heat resistance. Inorganic insulation is generally passivated by phosphoric acid, and the insulation layer is decomposed and cracked during high-temperature heat treatment. In order to improve the heat resistance of the insulating layer, different solutions are proposed at home and abroad, and the high-temperature resistance of the insulating layer is improved to a great extent. CN106229104A discloses a soft magnetic composite powder and a preparation method of a magnetic powder core thereof, belonging to the technical field of powder metallurgy and magnetic materials. According to the different magnetic properties of the metal soft magnetic powder, the amorphous powder, the nanocrystalline powder and the ferrite powder, the requirements of different magnetic properties are met through linear calculation and optimized design of the magnetic properties; meanwhile, the particle size of the powder is calculated and matched; shaping powder and screening; annealing the powder; insulating coating and mixing of the powder: and respectively carrying out passivation and insulation treatment on the powder with different components, weighing according to the weight ratio, and uniformly mixing to obtain the composite powder. The soft magnetic composite powder prepared by the invention has regular shape, good dispersibility and good apparent density.
CN100500783A discloses an inorganic insulating adhesive for a metal soft magnetic powder core, which is made of SiO2、AlO2、ZrO2The method for preparing the metal soft magnetic powder core by using the inorganic insulating adhesive has the advantages that on one hand, other insulating agents can not be added, the addition of nonmagnetic substances is reduced, and the magnetic performance of the powder core is favorably improved.
CN1167990A discloses an iron powder core, an iron powder for the iron powder core and a method for preparing the iron powder core, wherein the method adopts an organic-inorganic composite insulation mode to obtain a high temperature resistant insulation coating film, and specifically, the method adopts an iron powder with a particle size of 75-200 μm to prepare the iron powder core, and 0.015-0.15 wt% of silica sol, 0.05-0.5 wt% of siloxane resin and 10-50 wt% of organic titanium compound (based on the siloxane resin) are added into the iron powder. The iron powder is subjected to curing treatment at 50-250 ℃, powder briquetting and annealing at 550-650 ℃ in an inert atmosphere to obtain an iron powder core.
In the above documents, the flowability of the coated metal soft magnetic powder is poor, which results in the problems of low density of the metal soft magnetic powder core, large high frequency loss, long pressing period, low production efficiency, and the like.
Therefore, it is an urgent need to develop an insulation-coated metal soft magnetic powder with high fluidity to improve the density and internal uniformity of the metal soft magnetic powder core, reduce the loss of the magnetic core, shorten the pressing period, and improve the production efficiency.
Disclosure of Invention
In order to solve the technical problems, the invention provides an insulation coated metal soft magnetic powder and a preparation method and application thereof. According to the method, the surface of the metal soft magnetic powder is coated with the uniform and compact insulating layer, so that the flowability of the powder is effectively improved, the forming period is shortened, the production efficiency is improved, and the production cost is reduced. In addition, due to good powder fluidity, the density of the metal soft magnetic powder core can be improved, the density uniformity can be improved, and the performance of the metal soft magnetic powder core can be optimized.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an insulation-coated metallic soft magnetic powder, the method comprising the steps of:
(1) mixing the metal soft magnetic powder with an insulating agent and a solvent, and removing the solvent to obtain pre-coated powder;
(2) and (2) carrying out high-temperature heat treatment on the pre-coated powder obtained in the step (1) to obtain the insulated and coated metal soft magnetic powder.
According to the preparation method of the metal soft magnetic powder coated in the insulating manner, provided by the invention, the pre-coated powder is subjected to heat treatment, so that the interaction of O atoms, N atoms and the like in the resin and Fe atoms on the surface of the metal soft magnetic powder can be effectively promoted, the surface of the powder is coated with the uniform and compact insulating layer, the fluidity of the metal soft magnetic powder is effectively improved, and the problems of long pressing period, low production efficiency, high production cost and the like are solved; the method has simple process, mild condition and easy industrialization. In addition, the fluidity of the metal soft magnetic powder is improved, the density and the uniformity of the metal soft magnetic powder core are improved, the magnetic permeability, the high-frequency loss and other properties of the metal soft magnetic powder core are optimized, and the application value is high.
Preferably, the metal soft magnetic powder in step (1) comprises any one or a combination of at least two of iron powder, iron silicon aluminum powder, iron nickel powder or iron nickel molybdenum powder, wherein the combination is typically but not limited to: iron powder and iron silicon powder, iron powder and iron nickel powder, iron silicon aluminum powder and iron nickel molybdenum powder and the like.
Preferably, the average particle size of the metallic soft magnetic powder of step (1) is 20 to 200 μm, for example, 20 μm, 25 μm, 30 μm, 50 μm, 70 μm, 100 μm, 120 μm, 150 μm, 180 μm, 190 μm, or 200 μm, etc., preferably 30 to 150 μm; if the particle size is less than 20 μm, the powder has poor flowability, the coating difficulty is high, and the density of a pressed green body is low; the grain diameter is larger than 200 mu m, and the eddy current loss of the finished product is large under high frequency.
Preferably, the insulating agent of step (1) comprises any one of epoxy resin, phenolic resin, silicone resin, polyamide resin or polyimide resin or a combination of at least two thereof, wherein the combination is typically but not limited to: epoxy resins and silicone resins, silicone resins and phenolic resins, polyamide resins and polyimide resins, and the like, preferably polyamide resins and/or polyimide resins. The polyamide resin and the polyimide resin contain amino groups, can be spontaneously adsorbed on the surface of the metal soft magnetic powder, are beneficial to uniform coating of the resin and the powder, and improve the powder flowability.
Preferably, the solvent of step (1) comprises any one or a combination of at least two of acetone, ethanol or toluene, wherein the typical but non-limiting combination: acetone and ethanol, acetone and toluene, ethanol and toluene, and the like.
Preferably, the mixing in step (1) comprises: adding the insulating agent into the solvent, stirring, then adding the metal soft magnetic powder, and stirring.
Preferably, the mass ratio of the metal soft magnetic powder to the insulating agent in the step (1) is 100 (0.5-7), and may be, for example, 100:0.5, 100:0.8, 100:1, 100:2, 100:4, 100:5, 100:6 or 100:7, and the like, and is preferably 100 (0.5-4).
Preferably, the mass ratio of the solvent to the insulating agent in the step (1) is (1-10):1, for example, 1:1, 3:1, 5:1, 8:1 or 10:1, and the like, preferably (2-5): 1.
In the present invention, the specific method for removing the solvent is not limited, and any method commonly used by those skilled in the art can be applied to the present invention. Illustratively, the metallic soft magnetic powder is mixed with an insulating agent and a solvent, and the solvent is removed by heating to 80-100 ℃.
Preferably, the temperature of the high temperature heat treatment in step (2) is 250-500 ℃, such as 250 ℃, 280 ℃, 300 ℃, 350 ℃, 400 ℃, 450 ℃, 480 ℃ or 500 ℃, preferably 300-450 ℃; if the temperature is below 250 ℃, O, N is not favorable for the interaction with Fe; the temperature is higher than 500 ℃, the resin curing and compression molding difficulty is improved, and the production cost is increased.
Preferably, the high temperature heat treatment in step (2) is carried out for 3-6h, such as 3h, 3.5h, 4h, 5h, 5.5h or 6h, etc., preferably 4-5 h; if the time is less than 3h, O, N interaction with Fe is not favored; the time is longer than 6h, the production period is long, and the cost is increased.
According to the invention, the high-temperature heat treatment promotes the interaction between O atoms and N atoms in the resin and Fe atoms on the surface of the powder, so that the resin can be uniformly coated on the surface of the powder, the resin is prevented from being agglomerated and accumulated on the surface of the powder, and the sphericity of the insulating powder is improved.
As a further preferred embodiment of the present invention, the method comprises the steps of:
(1) mixing a solvent and an insulating agent according to the mass ratio of (1-10) to 1, stirring until the insulating agent is completely dissolved, adding metal soft magnetic powder with the average particle size of 20-200 mu m, controlling the mass ratio of the metal soft magnetic powder to the insulating agent to be 100 (0.5-10), heating to 80-100 ℃, and continuously stirring until the solvent is completely volatilized to obtain pre-coated powder;
(2) and (3) heating the pre-coated powder obtained in the step (1) to 250-500 ℃ in the air atmosphere, preserving the heat for 3-6h, and then cooling to obtain the metal soft magnetic powder coated with the insulation.
In a second aspect, the present invention provides the insulation-coated metallic soft magnetic powder prepared by the method according to the first aspect.
The metal soft magnetic powder coated in an insulating way has good fluidity, the density of the metal soft magnetic powder core is improved, the uniformity of the density is improved, and the performances of the metal soft magnetic powder core such as magnetic conductivity, high-frequency loss and the like are improved.
Preferably, the insulation-coated metal soft magnetic powder comprises metal soft magnetic powder and an organic insulation coating layer coated on the surface of the metal soft magnetic powder;
the thickness of the organic insulating coating layer is preferably 1 to 200nm, and may be, for example, 1nm, 5nm, 10nm, 20nm, 50nm, 100nm, 120nm, 150nm, 180nm, 190nm, or 200nm, and preferably 20 to 150 nm.
In a third aspect, the present invention provides a method for preparing a metallic soft magnetic powder core, comprising the steps of:
the metal soft magnetic powder coated with insulation according to the first aspect is subjected to compression molding and then heat treatment in an inert atmosphere to obtain a metal soft magnetic powder core.
According to the preparation method of the metal soft magnetic powder core, the soft magnetic metal powder coated in an insulating mode and good in flowability is adopted, so that the compression molding period is shortened, the production efficiency is improved, the production cost is reduced, and the preparation method has high application value.
Preferably, the pressure of the press forming process is 1200-2000MPa, such as 1200MPa, 1500MPa, 1700MPa, 1900MPa or 2000 MPa.
Preferably, the inert atmosphere comprises any one of nitrogen, argon or helium or a combination of at least two of them, with typical but non-limiting combinations: nitrogen and argon, nitrogen and helium.
Preferably, the temperature of the heat treatment is 650-.
Preferably, the time of the heat treatment is 0.5 to 8 hours, for example, 0.5 hour, 1 hour, 2 hours, 5 hours, 7 hours, 8 hours or the like, preferably 1 to 5 hours.
In the invention, heat treatment is carried out in an inert atmosphere after the press forming to eliminate internal stress.
In a fourth aspect, the present invention further provides a metal soft magnetic powder core prepared by the method of the third aspect.
The metal soft magnetic powder core provided by the invention has the advantages of high density, good density uniformity, high magnetic conductivity, low high-frequency loss and excellent performance.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) according to the preparation method of the metal soft magnetic powder coated in the insulating manner, the pre-coated powder is subjected to heat treatment, and the surface of the metal soft magnetic powder is coated with the uniform and compact organic insulating layer, so that the flowability of the metal soft magnetic powder is effectively improved, and the method is simple in process, mild in condition and easy to industrialize;
(2) the metal soft magnetic powder coated in an insulating way has good fluidity which can reach below 35s/50g, the density of the metal soft magnetic powder core is improved, the uniformity of the density is improved, the magnetic conductivity, the loss and other properties of the metal soft magnetic powder core are improved, the problems of long pressing period, low production efficiency, high production cost and the like are solved, and the metal soft magnetic powder coated in an insulating way has wide application prospect.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a metal soft magnetic powder core, which comprises the following steps:
(1) dissolving 10g of silicon resin KR311 in 30g of acetone, uniformly stirring to completely dissolve the silicon resin, adding 1kg of ferrum-silicon-aluminum powder with the average particle size of 28 micrometers, heating to 80 ℃, and continuously stirring to remove the acetone to obtain pre-coated ferrum-silicon-aluminum powder;
(2) placing the pre-coated ferrosilicon aluminum powder in a drying furnace, heating to 400 ℃ in air, and preserving heat for 3 hours to obtain ferrosilicon aluminum powder coated by silicon resin;
(3) and (3) pressing and molding the silicon resin coated ferrosilicon aluminum powder under the condition of 1800MPa, then heating to 780 ℃, and preserving heat for 2h to obtain the ferrosilicon aluminum powder core.
Example 2
The embodiment provides a preparation method of a metal soft magnetic powder core, which comprises the following steps:
(1) dissolving 10g of polyamide resin in 30g of acetone, uniformly stirring to completely dissolve the polyamide resin, adding 1kg of ferrosilicon powder with the average particle size of 28 microns, heating to 90 ℃, and continuously stirring to remove the acetone to obtain pre-coated ferrosilicon powder;
(2) placing the pre-coated iron silicon powder in a drying furnace, heating to 450 ℃ in the air, and preserving heat for 4 hours to obtain polyurethane resin coated iron silicon powder;
(3) and (3) pressing and molding the iron-silicon powder coated by the polyurethane resin under the condition of 2000MPa, then heating to 700 ℃, and preserving heat for 5 hours to obtain the iron-silicon powder core.
Example 3
The embodiment provides a preparation method of a metal soft magnetic powder core, which comprises the following steps:
(1) dissolving 10g of polyimide resin in 30g of acetone, uniformly stirring to completely dissolve the polyimide resin, adding 1kg of iron-nickel powder with the average particle size of 28 microns, heating to 90 ℃, and continuously stirring to remove the acetone to obtain pre-coated iron-nickel powder;
(2) putting the pre-coated iron nickel powder into a drying furnace, heating to 450 ℃ in the air, and preserving heat for 4 hours to obtain polyurethane resin coated iron nickel powder;
(3) and (3) pressing and molding the polyurethane resin-coated iron-nickel powder under the condition of 1500MPa, heating to 650 ℃, and preserving heat for 1h to obtain the iron-nickel powder core.
Example 4
The embodiment provides a preparation method of a metal soft magnetic powder core, which comprises the following steps:
(1) dissolving 10g of phenolic resin in 100g of ethanol, uniformly stirring to completely dissolve the phenolic resin, adding 1kg of iron-nickel-molybdenum powder with the average particle size of 100 micrometers, heating to 100 ℃, and continuously stirring to remove acetone to obtain pre-coated iron-nickel-molybdenum powder;
(2) placing the pre-coated iron-nickel-molybdenum powder in a drying furnace, heating to 500 ℃ in the air, and preserving heat for 5 hours to obtain iron-nickel-molybdenum powder coated with phenolic resin;
(3) and pressing and molding the iron-nickel-molybdenum powder coated with the phenolic resin under the condition of 1500MPa, heating to 670 ℃, and preserving heat for 6 hours to obtain the iron-nickel-molybdenum powder core.
Example 5
The embodiment provides a preparation method of a metal soft magnetic powder core, which comprises the following steps:
(1) dissolving 10g of epoxy resin in 12g of toluene, uniformly stirring to completely dissolve the epoxy resin, adding 1kg of ferrosilicon aluminum powder with the average particle size of 150 mu m, heating to 100 ℃, and continuously stirring to remove the toluene to obtain pre-coated ferrosilicon aluminum powder;
(2) placing the pre-coated iron-silicon-aluminum powder in a drying furnace, heating to 300 ℃ in the air, and preserving heat for 5 hours to obtain epoxy resin coated iron-silicon-aluminum powder;
(3) and (3) pressing and molding the epoxy resin coated ferrosilicon aluminum powder under the condition of 1200MPa, then heating to 700 ℃, and preserving heat for 3h to obtain the ferrosilicon aluminum powder core.
Example 6
The embodiment provides a preparation method of a metal soft magnetic powder core, which comprises the following steps:
(1) dissolving 10g of silicon resin KR311 in 60g of ethanol, uniformly stirring to completely dissolve the silicon resin, adding 1kg of ferrum-silicon-aluminum powder with the average particle size of 200 mu m, heating to 90 ℃, and continuously stirring to remove acetone to obtain pre-coated ferrum-silicon-aluminum powder;
(2) placing the pre-coated ferrosilicon aluminum powder in a drying furnace, heating to 450 ℃ in the air, and preserving heat for 3 hours to obtain ferrosilicon aluminum powder coated by silicon resin;
(3) and (3) pressing and molding the silicon resin coated iron-silicon-aluminum powder under the condition of 1500MPa, then heating to 750 ℃, and preserving heat for 2 hours to obtain the iron-silicon powder core.
Example 7
The only difference compared to example 1 is that the high temperature heat treatment temperature in step (2) was replaced with 200 ℃.
Example 8
The difference compared to example 1 is only that the high temperature heat treatment temperature in step (2) is replaced with 550 ℃.
Example 9
The embodiment provides a preparation method of a metal soft magnetic powder core, which comprises the following steps:
(1) dissolving 70g of epoxy resin in 100g of toluene, uniformly stirring to completely dissolve the epoxy resin, adding 1kg of iron powder with the average particle size of 20 mu m, heating to 100 ℃, and continuously stirring to remove acetone to obtain pre-coated iron powder;
(2) placing the pre-coated iron powder in a drying furnace, heating to 250 ℃ in the air, and preserving heat for 5 hours to obtain epoxy resin coated iron powder;
(3) and (3) pressing and molding the epoxy resin coated iron powder under the condition of 1200MPa, then heating to 680 ℃, and preserving heat for 7 hours to obtain the iron powder core.
Comparative example 1
The iron-silicon-aluminum powder core is prepared by adopting the preparation method provided by CN 100500783A.
Performance evaluation of the metal soft magnetic powder and the metal soft magnetic powder core:
the metal soft magnetic powder and the metal soft magnetic powder core coated with insulation prepared in each of the above examples and comparative examples were respectively subjected to fluidity test, density test, and magnetic property test, and the fluidity test method was as follows: using a hall rheometer, the time to flow 50g of powder out of the leak was tested.
The density test method is as follows: and actually testing the mass and the size of the metal powder core, and calculating and solving.
The magnetic properties were tested as follows: core loss was tested using a B-H analyzer SY-8219 manufactured by Kawasaki communications. The test conditions were 50kHz, 100 mT.
The test results are shown in table 1.
TABLE 1
The following points can be seen from table 1;
(1) as can be seen from the combination of examples 1 to 9, examples 1 to 9 in which the metal soft magnetic powder was coated with the insulating agent, the obtained insulation-coated metal soft magnetic powder had a flowability of 35s/50g or less, and the metal soft magnetic powder cores prepared therefrom had a density of 5.9 to 7.54g/cm3The magnetic permeability is 19-65, the loss is 203-457mW/cm under the conditions of 50kHz and 100mT3Thus, it is demonstrated that the metal soft magnetic powder of the insulation coating of examples 1 to 9 has good fluidity, and the metal soft magnetic powder core prepared therefrom has large density and permeability, small loss, and good magnetic properties;
(2) it can be seen from the combination of example 1 with examples 7 and 8 that the metal soft magnetic powder and the metal soft magnetic powder core of example 1 both have better performance than examples 7 and 8 because the temperature of the high temperature heat treatment in example 7 is low, so that the insulating powder has poor fluidity, resulting in lower product density and high loss; in example 8, the temperature of the high-temperature heat treatment is high, and after the insulating powder is subjected to compression molding, the density is low and the loss is high;
(3) as can be seen from a combination of example 1 and comparative example 1, the flowability of the silicon-aldehyde resin-coated ferrosilicon powder obtained in example 1 was 31s/50g, and the density of the ferrosilicon powder core prepared therefrom was 6.22g/cm3Magnetic permeability of 61 and loss of 203mW/cm3As compared with the inorganic insulation-coated iron silicon powder provided in comparative example 1, the flowability was 36s/50g, and the density of the iron silicon powder core prepared therefrom was 5.95g/cm3Magnetic permeability of 57 and loss of 258mW/cm3It is thus demonstrated that the method of example 1 is more advantageous for obtaining an insulating coated ferrosilicon powder with better flowability, and the ferrosilicon powder core prepared therefrom has better properties.
In conclusion, the preparation method of the metal soft magnetic powder coated in the insulating mode, provided by the invention, has the advantages that the pre-coated powder is subjected to heat treatment in the air, the uniform and compact organic insulating layer is coated on the surface of the metal soft magnetic powder, the flowability of the metal soft magnetic powder is effectively improved, the process is simple, the condition is mild, and the industrialization is easy to realize; the metal soft magnetic powder coated in an insulating way has good fluidity which can reach below 35s/50g, the density and the uniformity of the metal soft magnetic powder core prepared from the metal soft magnetic powder are improved, the performances of the metal soft magnetic powder core such as magnetic conductivity, loss and the like are improved, the problems of long pressing period, low production efficiency, high production cost and the like are solved, and the metal soft magnetic powder coated in an insulating way has wide application prospect.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A method for preparing insulation coated metal soft magnetic powder, characterized in that the method comprises the following steps:
(1) mixing the metal soft magnetic powder with an insulating agent and a solvent, and removing the solvent to obtain pre-coated powder;
(2) and (2) carrying out high-temperature heat treatment on the pre-coated powder obtained in the step (1) to obtain the insulated and coated metal soft magnetic powder.
2. The method according to claim 1, wherein the metal soft magnetic powder in step (1) comprises any one or a combination of at least two of iron powder, iron silicon aluminum powder, iron nickel powder or iron nickel molybdenum powder;
preferably, the average particle diameter of the metallic soft magnetic powder of step (1) is 20 to 200 μm, preferably 30 to 150 μm;
preferably, the insulating agent in step (1) comprises any one or a combination of at least two of epoxy resin, phenolic resin, silicone resin, polyamide resin or polyimide resin, preferably polyamide resin and/or polyimide resin;
preferably, the solvent in step (1) comprises any one or a combination of at least two of acetone, ethanol or toluene.
3. The method of claim 1 or 2, wherein the mixing of step (1) comprises: adding the insulating agent into the solvent, stirring, then adding the metal soft magnetic powder, and stirring;
preferably, the mass ratio of the metal soft magnetic powder to the insulating agent in the step (1) is 100 (0.5-7), preferably 100 (0.5-4);
preferably, the mass ratio of the solvent to the insulating agent in the step (1) is (1-10):1, preferably (2-5): 1.
4. The method according to any one of claims 1 to 3, wherein the temperature of the high temperature heat treatment in step (2) is 250-500 ℃, preferably 300-450 ℃;
preferably, the high-temperature heat treatment in the step (2) is carried out for 3 to 6 hours, preferably 4 to 5 hours.
5. Method according to any of claims 1-4, characterized in that the method comprises the steps of:
(1) mixing a solvent and an insulating agent according to the mass ratio of (1-10) to 1, stirring until the insulating agent is completely dissolved, adding metal soft magnetic powder with the average particle size of 20-200 mu m, controlling the mass ratio of the metal soft magnetic powder to the insulating agent to be 100 (0.5-7), heating to 80-100 ℃, and continuously stirring until the solvent is completely volatilized to obtain pre-coated powder;
(2) and (2) heating the pre-coated powder obtained in the step (1) to 250-500 ℃ in the air atmosphere, preserving the heat for 3-6h, and then cooling to obtain the metal soft magnetic powder coated in an insulating way.
6. An insulation-coated metallic soft magnetic powder prepared by the method according to any one of claims 1 to 5.
7. The insulation-coated metal soft magnetic powder as claimed in claim 6, wherein the insulation-coated metal soft magnetic powder comprises a metal soft magnetic powder and an organic insulation coating layer coated on the surface thereof;
preferably, the thickness of the organic insulating coating layer is 1 to 200nm, preferably 20 to 150 nm.
8. The preparation method of the metal soft magnetic powder core is characterized by comprising the following steps:
the insulation-coated metallic soft magnetic powder according to claim 6 or 7, which is press-formed and then heat-treated in an inert atmosphere, to obtain a metallic soft magnetic powder core.
9. The method as claimed in claim 8, wherein the pressure forming process is a pressure of 1200-2000 MPa;
preferably, the inert atmosphere comprises any one of nitrogen, argon or helium or a combination of at least two thereof;
preferably, the temperature of the heat treatment is 650-800 ℃, preferably 670-740 ℃;
preferably, the heat treatment time is 0.5 to 8 hours, preferably 1 to 5 hours.
10. A metallic soft magnetic powder core prepared by the method according to claim 8 or 9.
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| CN202010051762.XA CN111192735A (en) | 2020-01-17 | 2020-01-17 | Insulation coated metal soft magnetic powder and preparation method and application thereof |
| PCT/CN2020/087676 WO2021142974A1 (en) | 2020-01-17 | 2020-04-29 | Metal soft magnetic powder coated with insulation and preparation method therefor and use thereof |
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