CN114974873A - Soft magnetic composite material, preparation method thereof and molded inductor - Google Patents

Soft magnetic composite material, preparation method thereof and molded inductor Download PDF

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Publication number
CN114974873A
CN114974873A CN202210703275.6A CN202210703275A CN114974873A CN 114974873 A CN114974873 A CN 114974873A CN 202210703275 A CN202210703275 A CN 202210703275A CN 114974873 A CN114974873 A CN 114974873A
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soft magnetic
powder
composite material
magnetic composite
thermosetting resin
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苗弘
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Suzhou Jinlin Electronic Technology Co ltd
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Suzhou Jinlin Electronic Technology Co ltd
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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
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00—Details of transformers or inductances, in general
    • H01F27/24—Magnetic cores
    • H01F27/255—Magnetic cores made from particles

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention discloses a preparation method of a soft magnetic composite material, which comprises the following steps: mixing the soft magnetic metal powder and the thermosetting resin system for granulation treatment to obtain granulated powder; pretreating the granulated powder to enable the state of a thermosetting resin system in the pre-gel state granulated powder to be between an initial state and a gel state, so as to obtain pre-gel state granulated powder; and carrying out warm-pressing treatment on the pre-gel state granulation powder to obtain the soft magnetic composite material. The viscosity of the granulation powder under the condition of warm-pressing treatment is increased, and the coating effect of the thermosetting resin system on the soft magnetic metal powder is improved, so that the soft magnetic composite material with higher insulation resistance is prepared. Correspondingly, the invention also discloses a soft magnetic composite material prepared by the preparation method of the soft magnetic composite material, and a die-pressed inductor prepared from the soft magnetic composite material, which have higher pressing density and insulation resistance.

Description

Soft magnetic composite material, preparation method thereof and molded inductor
Technical Field
The invention relates to the technical field of electrical elements, in particular to a soft magnetic composite material, a preparation method thereof and a die-pressed inductor.
Background
The molded inductor is widely applied to various power electronic devices as one of key devices in the field of modern power electronics, and along with popularization and application of electric vehicles, internet of things, cloud servers, intelligent technologies and new-generation semiconductor materials, the molded inductor has higher and higher stability requirements, the use working condition of the molded inductor is more and more rigorous, and the thermal stability of the related molded inductor is required to be higher and higher, so that the improvement of the insulation resistance of the molded inductor is a core problem in the technical development of the products.
The soft magnetic composite material takes soft magnetic metal powder as a matrix and is coated with the composite material of at least one dielectric phase, the soft magnetic composite material has the advantages of low eddy current loss, high magnetic conductivity, low coercive force and high insulation resistance, and in addition, the soft magnetic composite material also has the advantages of three-dimensional anisotropy and easy machining, and is widely applied to the preparation of molded inductors.
However, in the actual production of soft magnetic composite materials using a thermosetting resin system as a dielectric phase, the insulation resistance may be reduced due to uneven dispersion of the resin and poor coating of the soft magnetic metal powder.
Disclosure of Invention
The invention aims to solve the technical problem of how to simultaneously enable the soft magnetic composite material and the molded inductor to have higher insulation resistance and pressing density.
In order to solve the technical problem, the invention provides a preparation method of a soft magnetic composite material, which comprises the following steps:
and mixing the soft magnetic metal powder and the thermosetting resin system, and then granulating to obtain granulated powder.
And (3) pretreating the granulated powder to enable the state of the thermosetting resin system to be between an initial state and a gel state, so as to obtain the pregel-state granulated powder. And
and carrying out warm-pressing treatment on the pre-gel granulation powder to obtain the soft magnetic composite material.
In a possible implementation, the pre-gelled granulated powder has a significantly increased viscosity compared to the initial state and is capable of being transformed into a gelled state within 5s to 60s at the temperature of the warm compaction process.
In one possible implementation, the temperature of the pretreatment is 30 ℃ to 80 ℃ lower than the temperature of the warm-pressing treatment.
In one possible implementation, the thermosetting resin system is bisphenol A cyanate ester and bisphenol A epoxy resin, the pretreatment temperature is 100-140 ℃, and the pretreatment time is 30-120 min.
In one possible implementation mode, the temperature of the warm-pressing treatment is 150-200 ℃, and the time of the warm-pressing treatment is 15-180 s.
In one possible implementation, the thermosetting resin system includes a thermosetting resin and a curing agent, wherein the thermosetting resin is selected from at least one of an epoxy resin, a cyanate ester resin, and a novolac resin.
In a possible implementation, the soft magnetic metal powder is selected from carbonyl iron powder, reduced iron powder, atomized Fe (100-x-y) Si x Cr y At least one of powder (x ═ 3.5-6.5, y ═ 0.0-6.5), iron-based amorphous soft magnetic powder, iron-based amorphous nanocrystalline powder, Sandust powder, and HighFlux powder.
In one possible implementation, the metallic soft magnetic powder is subjected to a surface insulation treatment before the step of mixing the metallic soft magnetic powder and the thermosetting resin system for granulation treatment.
The implementation of the invention has the following beneficial effects:
according to the invention, the pre-gel state granulated powder is obtained through pretreatment before the granulated powder is subjected to warm-pressing treatment, so that the viscosity of the granulated powder under the warm-pressing treatment condition is increased, the coating effect of a thermosetting resin system on the soft magnetic metal powder is improved, and the soft magnetic composite material with higher insulation resistance is prepared. In the method, the thermosetting resin system is in a pre-gel state after being pretreated, so that the condition that the pressing density of the prepared soft magnetic composite material is too low due to overheating and crosslinking of the thermosetting resin system is avoided, and the soft magnetic composite material can have higher insulation resistance and pressing density at the same time.
The soft magnetic composite material prepared by the method has the pressing density of 5.60g/cm 3 ～6.20g/cm 3 And the insulation resistance is more than or equal to 100M omega @ 100V.
Correspondingly, the invention also provides a soft magnetic composite material which is prepared by any one of the preparation methods of the soft magnetic composite material and has higher insulation resistance and pressing density.
Correspondingly, the invention also provides a molded inductor which is prepared from the soft magnetic composite material and has higher insulation resistance and higher molding density.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanied with the present invention are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
A method for preparing a soft magnetic composite material comprises the following steps:
and mixing the soft magnetic metal powder and the thermosetting resin system for granulation treatment to obtain granulated powder.
And (3) pretreating the granulated powder to enable the state of the thermosetting resin system to be between an initial state and a gel state, so as to obtain the pregel-state granulated powder. And
and carrying out warm-pressing treatment on the pre-gel granulation powder to obtain the soft magnetic composite material.
According to the invention, by adding the step of pretreatment before the warm-pressing treatment of the granulated powder, the thermosetting resin system in the granulated powder is softened and flows under the action of the pretreatment and generates a certain degree of crosslinking reaction, so that the viscosity of the granulated powder under the warm-pressing treatment condition is increased, the coating effect of the thermosetting resin system on the soft magnetic metal powder is improved, and the soft magnetic composite material with higher insulation resistance is prepared. In the method, the thermosetting resin system is in a pre-gel state after being pretreated, so that the condition that the pressing density of the prepared soft magnetic composite material is too low due to overheating and crosslinking of the thermosetting resin system is avoided, and the soft magnetic composite material can have higher insulation resistance and pressing density at the same time.
The pre-gel state referred to in the present invention means that the degree of reaction of the thermosetting resin system in the granulated powder is less than the critical gel point. At this time, the viscosity of the pre-gel state granulated powder is obviously increased compared with granulation and/or the pre-gel state granulated powder can be converted into a gel state within 5s to 60s at the temperature of warm-pressing treatment.
In one possible implementation, the temperature of the pre-treatment is 30-80 ℃ lower than the temperature of the warm-pressing treatment.
Wherein, different thermosetting resin systems correspond to different temperature and pressure treatment temperatures, and the temperature of the temperature and pressure treatment is generally 30-50 ℃ higher than the reaction peak temperature measured by a DSC curve of the thermosetting resin system.
When the temperature difference between the pretreatment temperature and the warm-pressing temperature is too small, the pre-gel state granulated powder is converted into a gel state, the crosslinking degree between thermosetting resin systems is high, cavities are formed between crosslinking networks, and the pressing density of the prepared soft magnetic composite material is low.
In a feasible implementation mode, the thermosetting resin system is bisphenol A cyanate ester and bisphenol A epoxy resin, the pretreatment temperature is 100-140 ℃, and the pretreatment time is 30-120 min.
When the pretreatment temperature is too low, the viscosity of the pre-gel granulation powder is too low, and the insulation resistance of the prepared soft magnetic composite material is low; when the temperature of the pretreatment is too high, the pre-gel state granulated powder is converted into a gel state, and the prepared soft magnetic composite material has lower compression density.
As the time of pretreatment increases, the degree of crosslinking of the thermosetting resin system increases, so that the viscosity of the pregel-state granulated powder increases and the pressed density of the soft magnetic composite material decreases. If the pretreatment time is too short, the viscosity of the pre-gel granulation powder is too low, and the insulation resistance of the prepared soft magnetic composite material is low; if the pretreatment time is too long, the crosslinking degree of the pre-gel granulation powder is too high, and the prepared soft magnetic composite material has lower pressing density.
In one possible implementation, the temperature of the warm-pressing treatment is 150-200 ℃, and the time of the warm-pressing treatment is 15-180 s.
In one possible implementation, the thermosetting resin system includes a thermosetting resin and a curing agent, wherein the thermosetting resin is selected from at least one of an epoxy resin, a cyanate ester resin, and a novolac resin.
In a possible implementation, the soft magnetic metal powder is selected from carbonyl iron powder, reduced iron powder, atomized Fe (100-x-y) Si x Cr y At least one of powder (x ═ 3.5-6.5, y ═ 0.0-6.5), iron-based amorphous soft magnetic powder, iron-based amorphous nanocrystalline powder, Sandust powder, and HighFlux powder.
In one possible implementation, the soft magnetic metal powder is a mixture of carbonyl iron powder and iron-based amorphous powder. The carbonyl iron powder with small particle size and the iron-based amorphous powder with large particle size are mixed, so that the effect of three-dimensional coating after warm pressing treatment is realized, and the insulation resistance of the soft magnetic composite material is improved.
In one possible implementation, the soft magnetic metal powder is subjected to a surface insulation treatment before the step of mixing the soft magnetic metal powder and the thermosetting resin system for granulation treatment. The current path can be further blocked through surface insulation treatment, and the eddy current loss of the soft magnetic composite material is effectively reduced.
The invention also provides a soft magnetic composite material, which is prepared by any one of the preparation methods of the soft magnetic composite material, and has high insulation resistance and pressing density, wherein the pressing density is 5.60g/cm 3 -6.20g/cm 3 And the insulation resistance is more than or equal to 100M omega @ 100V.
The invention also provides a die-pressed inductor which is obtained by firstly placing the winding in a die and then adding the soft magnetic composite material for pressing, and has higher insulation resistance and pressing density.
With reference to the above implementation contents, in order to make the technical solution of the present invention more specific and clear and easy to understand, the technical solution of the present invention is exemplified, but it should be noted that the contents to be protected by the present invention are not limited to the following embodiments 1 to 10.
Example 1
1000g of carbonyl iron powder having an average particle size of 5 μm was subjected to surface insulation treatment using 2g of phosphoric acid and 50g of acetone to obtain passivated carbonyl iron powder.
1000g of iron-based amorphous powder having an average particle size of 15 μm was subjected to surface insulation treatment using 2g of phosphoric acid and 50g of acetone to obtain passivated iron-based amorphous powder.
700g of passivated carbonyl iron powder, 300g of passivated iron-based amorphous powder, 24g of bisphenol A cyanate ester, 6g of bisphenol A epoxy resin and 100g of acetone are mixed and granulated to obtain granulated powder.
Drying the granulated powder, and then pretreating at 100 ℃ for 30min to obtain pre-gel granulated powder.
And (3) carrying out warm-pressing treatment on the pre-gel granulation powder at 180 ℃ and under the pressure of 200MPa for 120s to prepare a soft magnetic composite material sample with the size of 10mm x 3 mm.
Example 2
Example 2 differs from example 1 in that the temperature of the pretreatment was 110 ℃.
Example 3
Example 3 differs from example 1 in that the temperature of the pretreatment was 120 ℃.
Example 4
Example 4 differs from example 1 in that the temperature of the pretreatment was 130 ℃.
Example 5
Example 5 differs from example 1 in that the temperature of the pretreatment was 140 ℃.
Example 6
Example 6 differs from example 1 in that the pretreatment time was 60 min.
Example 7
Example 7 differs from example 1 in that the pretreatment time was 120 min.
Example 8
Example 8 is different from example 1 in that the temperature of the pretreatment is 130 ℃ and the time of the pretreatment is 10 min.
Example 9
Example 9 differs from example 9 in that the temperature of the pretreatment was 140 ℃.
Example 10
Example 10 differs from example 9 in that the temperature of the pretreatment was 150 ℃.
Comparative example 1
Comparative example 1 differs from example 1 in that the temperature of the pretreatment was 70 ℃.
Comparative example 2
Comparative example 2 differs from example 1 in that the temperature of the pretreatment was 80 ℃.
Comparative example 3
Comparative example 3 differs from example 1 in that the temperature of the pretreatment was 90 ℃.
Comparative example 4
Comparative example 4 differs from example 1 in that the temperature of the pretreatment was 150 ℃.
Comparative example 5
Comparative example 5 differs from example 1 in that the temperature of the pretreatment was 160 ℃.
Comparative example 6
Comparative example 6 differs from example 1 in that the pretreatment time was 15 min.
Comparative example 7
Comparative example 7 differs from example 1 in that the pretreatment time was 240 min.
Comparative example 8
Comparative example 8 differs from example 8 in that the temperature of the pretreatment was 120 ℃.
Comparative example 9
Comparative example 9 differs from example 8 in that the temperature of the pretreatment was 160 ℃.
Comparative example 10
Comparative example 10 differs from example 8 in that the temperature of the pretreatment was 170 ℃.
And (3) performance testing:
the viscosity and gel time of the pre-gel state granulated powder after the pre-treatment in comparative examples 1 to 10 and examples 1 to 10 were tested, and the compression density and insulation resistance of the soft magnetic composite material:
the viscosity test in the invention is to use a viscometer to test the pretreated pre-gel granulation powder after heat preservation for 2min at 120 ℃;
gel time in the present invention was measured using a Brookfield gel time tester: 100ml of the granulated powder in the pre-gel state was placed in a sample cup, and a glass rod was immersed in the granulated powder in the pre-gel state, with the end of the glass rod being spaced 0.5 inches from the bottom of the sample cup. Setting the rotating speed to be 1RPM, setting the testing temperature to be 180 ℃, starting a viscometer motor, starting testing, observing the change conditions of viscosity and torque, and recording the time when the viscosity and the torque are rapidly increased, namely the gelling time;
the pressed density in the invention is tested by using a ZMD electronic densitometer;
the insulation resistance in the invention is tested by using a chroma19053 withstand voltage tester, the voltage is set as 100V, and the test time is 3 s;
the test results are shown in tables 1 to 3.
TABLE 1 Performance test of comparative examples 1 to 5 and examples 1 to 5
Figure BDA0003705180010000081
TABLE 2 Performance test of comparative examples 6 to 7 and example 1 and 6 to 7
Figure BDA0003705180010000082
Figure BDA0003705180010000091
TABLE 3 Performance test of comparative examples 8 to 10 and examples 8 to 10 (temperature of warm-pressing treatment: 180 ℃ C.)
Figure BDA0003705180010000092
As can be seen from Table 1, the pressed densities of examples 1 to 5 were all 5.60g/cm 3 The insulation resistance is more than or equal to 100 MOmega @ 100V; compared with the comparative examples 1 to 3, the viscosity of the pre-gel granulation powder is too low due to too low pretreatment temperature, and the insulation resistance of the soft magnetic composite material is further low; comparative examples 4 and 5 since the sample has reached the gel state due to the excessively high temperature of the pretreatment, resulting in a low compression density of the soft magnetic composite material, the temperature of the pretreatment should be set between 100 c and 140 c.
As can be seen from table 2, the soft magnetic composite materials obtained in examples 1, 6 and 7 can achieve higher compression density and insulation resistance; the pretreatment time of the comparative example 6 is shorter, and the insulation resistance of the soft magnetic composite material is lower; comparative example 7 the time for the pretreatment was too long, and the press density of the soft magnetic composite material was low, so the time for the pretreatment should be set between 30min and 120 min.
As can be seen from table 3, the soft magnetic composite materials prepared in examples 8 to 10 can achieve higher compression density and insulation resistance; in comparative example 8, the insulation resistance was low because the difference between the pressing temperature and the pretreatment temperature was large; comparative examples 9 to 10 have a reduced pressing density because the difference between the pressing temperature and the pretreatment temperature is small.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all feasible combinations of the technical features in the embodiments described above are not described, but should be considered as the scope of the description of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.

Claims (10)

1. A preparation method of a soft magnetic composite material is characterized by comprising the following steps:
mixing the soft magnetic metal powder and the thermosetting resin system, and then carrying out granulation treatment to obtain granulated powder;
pretreating the granulated powder to enable the state of the thermosetting resin system to be between an initial state and a gel state, so as to obtain pre-gel state granulated powder; and
and carrying out warm-pressing treatment on the pre-gel state granulation powder to obtain the soft magnetic composite material.
2. A method for the preparation of a soft magnetic composite material according to claim 1, characterized in that the pre-gel granulated powder has a significantly increased viscosity compared to the initial state;
the pre-gel state granulation powder can be converted into a gel state within 5s-60s at the temperature of the warm-pressing treatment.
3. The method for preparing a soft magnetic composite material according to claim 1, wherein the temperature of the pre-treatment is 30 ℃ to 80 ℃ lower than the temperature of the warm-pressing treatment.
4. The method for preparing the soft magnetic composite material according to claim 1, wherein the thermosetting resin system is bisphenol A cyanate ester and bisphenol A epoxy resin, the temperature of the pretreatment is 100 ℃ to 140 ℃, and the time of the pretreatment is 30min to 120 min.
5. The process for preparing soft magnetic composite material according to claim 4, wherein the temperature of warm pressing treatment is 150-200 ℃ and the time of warm pressing treatment is 15-180 s.
6. A method for the preparation of a soft magnetic composite material according to claim 1, characterized in that the thermosetting resin system comprises a thermosetting resin and a curing agent;
the thermosetting resin is at least one selected from epoxy resin, cyanate ester resin and linear phenolic resin.
7. Process for the preparation of soft magnetic composite material according to claim 1, characterized in that the soft magnetic metal powder is selected from carbonyl iron powder, reduced iron powder, atomized Fe (100-x-y) Si x Cr y At least one of powder (x ═ 3.5-6.5, y ═ 0.0-6.5), iron-based amorphous soft magnetic powder, iron-based amorphous nanocrystalline powder, Sandust powder, and HighFlux powder.
8. A method for preparing a soft magnetic composite material according to claim 1, wherein the metallic soft magnetic powder is subjected to surface insulation treatment before the step of mixing the metallic soft magnetic powder and the thermosetting resin system for granulation treatment.
9. A soft magnetic composite material, characterized by being produced by the method for producing a soft magnetic composite material according to any one of claims 1 to 8.
10. An embossed inductor, characterized in that the material from which the embossed inductor is made comprises the soft magnetic composite material according to claim 9.
CN202210703275.6A 2022-06-21 2022-06-21 Soft magnetic composite material, preparation method thereof and molded inductor Pending CN114974873A (en)

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Application Number Priority Date Filing Date Title
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