CN113410021A - Coated magnetic powder core of thermoplastic resin and epoxy resin composite adhesive and preparation method thereof - Google Patents

Coated magnetic powder core of thermoplastic resin and epoxy resin composite adhesive and preparation method thereof Download PDF

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CN113410021A
CN113410021A CN202110552565.0A CN202110552565A CN113410021A CN 113410021 A CN113410021 A CN 113410021A CN 202110552565 A CN202110552565 A CN 202110552565A CN 113410021 A CN113410021 A CN 113410021A
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magnetic powder
epoxy resin
powder core
thermoplastic resin
composite adhesive
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任碧野
罗盘
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/20Magnets 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
    • H01F1/22Magnets 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
    • H01F1/24Magnets 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
    • H01F1/26Magnets 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/147Alloys characterised by their composition
    • H01F1/14766Fe-Si based alloys
    • H01F1/14791Fe-Si-Al based alloys, e.g. Sendust
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0206Manufacturing of magnetic cores by mechanical means
    • H01F41/0246Manufacturing of magnetic circuits by moulding or by pressing powder

Abstract

The invention discloses a coated magnetic powder core of a thermoplastic resin and epoxy resin composite adhesive and a preparation method thereof, wherein a powder core blank is obtained by curing at the temperature of 150-180 ℃, the powder core blank is obtained by cold press molding of coated magnetic powder, and the coated magnetic powder is obtained by processing passivated magnetic powder with a coupling agent, drying, and coating with the thermoplastic resin, epoxy resin composite adhesive and a lubricant; the thermoplastic resin and epoxy resin composite adhesive is formed by compounding thermoplastic resin, epoxy resin and an epoxy resin curing agent. The invention improves the compounding effect of the thermoplastic resin adhesive and the epoxy resin adhesive, and integrates the advantages of the thermoplastic resin and the epoxy resin.

Description

Coated magnetic powder core of thermoplastic resin and epoxy resin composite adhesive and preparation method thereof
Technical Field
The invention relates to an insulating magnetic powder core, in particular to a coated magnetic powder core of a thermoplastic resin and epoxy resin composite adhesive and a preparation method thereof, belonging to the field of manufacturing of magnetic material insulating magnetic powder.
Background
The magnetic powder core is a composite soft magnetic material formed by mixing and pressing magnetic metal particles and an insulating medium. The magnetic powder core has higher saturation magnetic induction intensity, better direct current superposition characteristic, good frequency and temperature stability and lower cost, and is widely applied, but in practical application, the electrical resistivity of the metal magnetic powder core is too low, so that the eddy current loss is larger, the loss at high frequency is very large, and the coating of an insulating film on the surface of the magnetic powder particles is an effective way for improving the electrical resistivity of the magnetic powder core and reducing the eddy current loss. Therefore, the insulation coating is a key process in the preparation process of the magnetic powder core, and the adhesive is a main factor influencing the insulation coating. The adhesive is added to coat the magnetic powder core, so that the flowability of magnetic powder particles is improved, the formability of the powder during pressing is improved, the insulation effect is enhanced, the eddy current loss among the particles is reduced, and the mechanical property of the magnetic powder core is improved.
At present, the commonly used magnetic powder core adhesive mainly comprises an inorganic adhesive and an organic adhesive. Inorganic binders such as SiO2、Fe3O4、TiO2And the water glass and the like have good thermal stability, are not easy to decompose at high temperature, can ensure that the magnetic powder core is subjected to heat treatment at higher temperature, fully eliminate internal stress and improve the mechanical property of the magnetic powder core, but have poor bonding effect with magnetic powder, are far less than organic bonding agents, cannot well promote the compression molding of the magnetic powder, and further influence the magnetic property of the magnetic powder core. Organic adhesives such as epoxy resin and thermoplastic resin have good adhesion effect with magnetic powder, and can promote compression molding and improve the density of magnetic powder core, so most of the organic adhesives are organic adhesives, and the epoxy resin in the organic adhesives is most used at present.
The Chinese invention patent 201510961792.3 discloses a method for preparing an amorphous or nanocrystalline soft magnetic powder core, which comprises the following steps: passivating the amorphous or nanocrystalline soft magnetic powder; coating the passivated amorphous or nanocrystalline soft magnetic powder by using an organic binder; then adding a lubricant and an insulating agent into the magnetic powder to obtain magnetic powder to be compressed; pressing and forming the obtained magnetic powder to be compressed by adopting a mould at normal temperature, and demoulding to obtain a pressed blank; applying compressive stress to the obtained pressed compact for curing or plasticizing; impregnating the pressed compact with an inorganic binder solution and carrying out stabilization treatment; carrying out high-temperature annealing heat treatment on the obtained pressed blank; impregnating the obtained annealed pressed blank skeleton with a high-strength binder solution and carrying out curing or stabilizing treatment; and carrying out subsequent processing on the obtained blank with higher strength to obtain a finished product. The technology can obtain amorphous or nanocrystalline soft magnetic powder cores with higher density and higher soft magnetic performance at lower forming pressure. Although the inorganic adhesive improves the thermal stability of the adhesive and enables the magnetic powder core to have higher heat treatment temperature, the mechanical property of the magnetic powder core is reduced due to the poor adhesive property of the inorganic adhesive.
Chinese patent 201410230405.4 discloses an insulating adhesive for preparing metal soft magnetic composite material and its application method, the insulating adhesive is a nano modified organic silicon resin insulating adhesive, and its components are epoxy modified organic silicon resin and inorganic nano dispersion. The insulating binder greatly improves the heat-resistant temperature of the organic silicon resin, improves the mechanical strength of the magnetic powder core, has reasonable component selection and good use effect, and has good insulating and binding effect on iron-based, nickel-based and other components of metal soft magnetic powder. The magnetic powder core prepared by the insulating binder provided by the invention has comprehensive excellent magnetic property and mechanical property. The insulating adhesive used by the method has good heat resistance and good soft magnetic performance, but the radial tensile strength of the prepared magnetic powder core is 7.04MPa, and the prepared magnetic powder core has certain mechanical property but is slightly insufficient, and when the soft magnetic composite material is applied to an inductor, the prepared inductor is easy to crack, thereby affecting the performance of the inductor.
Chinese patent 201410230351.1 discloses a method for preparing an inorganic-organic composite binder coated soft magnetic composite material, which comprises the following steps of (1) mixing metal magnetic powder according to a particle size ratio; (2) passivating the magnetic powder proportioned in the step (1) by using a passivating agent; (3) coating the passivated magnetic powder particles in the step (2) with a binding agent compounded by an organic binding agent and an inorganic binding agent; (4) pressing and molding the bonded magnetic powder in the step (3) to obtain a magnetic powder core; (5) and (4) carrying out heat treatment on the magnetic powder core pressed in the step (4), and spraying to obtain a target product. The prepared magnetic powder core has excellent magnetic performance, the effective magnetic conductivity reaches 132.3 when f is 100KHz, but the prepared magnetic powder core has poor mechanical property, the tensile strength is only 5.81MPa, and the magnetic powder core is easy to crack when being transported or wound with a coil.
The Chinese invention patent application CN105225783A discloses a preparation method of an epoxy modified organic silicon resin coated magnetic powder core. According to the preparation method, the epoxy modified organic silicon resin obtained after the reaction of the epoxy resin, the organic silicon resin, the catalyst and the coupling agent is used for coating the magnetic powder core, so that the coating condition of the magnetic core powder particles can be effectively improved, the product performance is improved, and the magnetic loss is effectively reduced. The technology adopts epoxy modified organic silicon resin as an adhesive to coat the magnetic powder core, and the adhesive is still insufficient because the main body of the adhesive is still organic silicon resin although the high adhesiveness of the epoxy resin and the high thermal stability of the organic silicon resin are combined, so that the magnetic powder core is easy to crack when being transported or wound with a coil.
Disclosure of Invention
In view of the above situation, the invention provides a preparation method of a thermoplastic resin and epoxy resin composite adhesive coated magnetic powder core, which improves the composite effect of the thermoplastic resin adhesive and the epoxy resin adhesive, integrates the respective advantages of the thermoplastic resin and the epoxy resin, and has excellent mechanical properties of the prepared magnetic powder core without reducing the magnetic properties of the magnetic powder core.
The epoxy resin has excellent bonding performance and mechanical property, but the brittleness and the toughness of the epoxy resin are poor, so that the epoxy resin is not beneficial to coating the magnetic powder core, and the further improvement of the mechanical property and the magnetic property of the magnetic powder core is hindered. The thermoplastic resin has excellent bonding performance and mechanical property and high toughness, but the thermoplastic resin has larger molecular weight, correspondingly larger viscosity when dissolved in a solvent, and difficult effective coating of the magnetic powder core when the addition amount is excessive, so the addition amount cannot be excessive when the thermoplastic resin is used as the magnetic powder adhesive. Therefore, the thermoplastic resin needs to be added in a strictly controlled amount, and further improvement of the mechanical property and the magnetic property of the magnetic powder core is also hindered to a certain extent. However, the thermoplastic resin and epoxy resin composite adhesive of the invention is compounded by the thermoplastic resin, the epoxy resin and the epoxy resin curing agent to effectively solve the problems.
In order to realize the purpose of the invention, the invention provides the following technical scheme:
a thermoplastic resin and epoxy resin composite adhesive coated magnetic powder core is obtained by curing a powder core blank at the temperature of 150-180 ℃, wherein the powder core blank is obtained by cold press molding of coated magnetic powder, and the coated magnetic powder is obtained by treating passivated magnetic powder with a coupling agent, drying, and coating with a thermoplastic resin and epoxy resin composite adhesive and a lubricant; the thermoplastic resin and epoxy resin composite adhesive is formed by compounding thermoplastic resin, epoxy resin and an epoxy resin curing agent.
Preferably, the magnetic powder is sendust magnetic powder.
The preparation method of the thermoplastic resin and epoxy resin composite adhesive coated magnetic powder core comprises the following steps:
1) passivating the magnetic powder by using a passivating agent, drying, adding a coupling agent for coupling, drying, and adding a thermoplastic resin, an epoxy resin composite adhesive and a lubricant for coating; the thermoplastic resin and epoxy resin composite adhesive is formed by compounding thermoplastic resin, epoxy resin and an epoxy resin curing agent;
2) pressing and molding the coated magnetic powder by using a cold press to obtain an annular powder core blank;
3) and (3) curing the annular powder core blank in a vacuum oven, and cooling to room temperature to obtain the magnetic powder core.
Preferably, the passivating agent in the step 1) is one of phosphoric acid and chromic acid, and the adding amount of the passivating agent is 0.6 wt% -1.0 wt% of the total mass of the magnetic powder.
Preferably, the coupling agent in the step 1) is a silane coupling agent, the silane coupling agent is one of KH792, KH550, KH560 or KH580, and the addition amount is 0.3 wt% -0.6 wt% of the total mass of the magnetic powder; the lubricant in the step 1) is zinc stearate, and the addition amount of the lubricant is 0.1-0.3 wt% of the total mass of the magnetic powder.
Preferably, the thermoplastic resin is selected from one of phenoxy resin, polyvinyl formal copolymerized acrylic acid, epoxidized thermoplastic elastomer AT501 or MBS resin;
the addition amount of the thermoplastic resin is 0.05 wt% -0.45 wt% of the total mass of the magnetic powder; the epoxy resin is selected from one of NPES-902, NPES-901, NPES-907, NPES-904 or NPCN-704, and the addition amount of the epoxy resin is 2 wt% -4 wt% of the total mass of the magnetic powder.
Preferably, the epoxy resin curing agent is one of Dicyandiamide and Diaminodiphenyl Sulfone (DDS).
Preferably, the method for compounding the thermoplastic resin and the epoxy resin compound adhesive comprises the following steps: firstly, dissolving thermoplastic resin, epoxy resin and epoxy resin curing agent by organic solvent, mixing, and stirring in water bath at 50-80 ℃ for 30-60min to obtain the uniformly mixed composite adhesive.
Preferably, the organic solvent is one or more of butanone, tetrahydrofuran or xylene.
Preferably, the drying after the passivation treatment in the step 1) is drying under the stirring of water bath at the temperature of 60-80 ℃, and the drying after the coupling treatment by adding the coupling agent is drying under the stirring of water bath at the temperature of 80-100 ℃;
the pressing pressure of the hydraulic press in the step 2) is 10-30MPa, and the pressure maintaining time is 60-120s
In the step 3), the curing temperature is 150-180 ℃, and the curing time is 1-2 h.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the composite effect of the thermoplastic resin adhesive and the epoxy resin adhesive is improved, the respective advantages of the thermoplastic resin and the epoxy resin are integrated, the thermoplastic resin provides toughness which the epoxy resin lacks, the epoxy resin provides strength which the thermoplastic resin does not have and more effective cladding performance on the magnetic powder core, the cladding effect of the magnetic powder core can be well improved by integrating the two adhesives, and the magnetic performance and the mechanical performance of the magnetic powder core are improved.
(2) The manufacturing process is simple, and the used equipment is simple;
(3) the magnetic powder core is suitable for metal magnetic powder cores such as iron-silicon-aluminum cores and the like, and can greatly improve the high-frequency performance and quality factors of the magnetic powder cores.
(4) The magnetic powder core can maintain excellent magnetic performance and greatly improve the mechanical performance of the magnetic powder core.
Drawings
FIG. 1 is a cross-sectional profile of a composite adhesive coated sendust core prepared in example 1 with a thermoplastic resin and an epoxy resin.
FIG. 2 is a cross-sectional profile of a composite adhesive coated sendust core prepared in example 2 with a thermoplastic resin and an epoxy resin.
FIG. 3 is a cross-sectional profile of a sendust core coated with a composite adhesive of thermoplastic resin and epoxy resin prepared in example 3.
FIG. 4 is a cross-sectional profile of a composite adhesive coated sendust core prepared in example 4 with a thermoplastic resin and an epoxy resin.
FIG. 5 is a cross-sectional profile of a composite adhesive coated sendust core prepared in example 5 with a thermoplastic resin and an epoxy resin.
FIG. 6 is a cross-sectional profile of a composite adhesive coated sendust core prepared in example 6 with a thermoplastic resin and an epoxy resin.
FIG. 7 is a cross-sectional profile of a composite adhesive coated sendust core prepared in example 7 with a thermoplastic resin and an epoxy resin.
Detailed Description
The invention will now be further described by way of example with reference to the accompanying drawings. In the embodiment of the present invention, the technical solutions in the embodiments of the present invention are clearly and completely described, and obviously, the described embodiments are only a part of the embodiments of the present invention, and not all embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The relevant test methods involved in the embodiments of the present invention are described below:
tensile strength: and testing the tensile strength of the magnetic powder core by using an electric table tensile testing machine. The electric table tensile testing machine has three optional mechanical units, namely N, kgf and lbf, the unit is selected as N during measurement, and the tensile strength of the magnetic powder core can be calculated by calculating the cross-sectional area of the magnetic powder core when the magnetic powder core is broken.
Effective magnetic permeability: and measuring the effective magnetic conductivity of the magnetic powder core by using an impedance analyzer, wherein the measuring frequency is 1 MHz. The effective magnetic conductivity can be calculated by winding 37.5 turns of coil on the magnetic powder core magnetic ring, then testing, and testing the inductance value of the coil and combining the frequency and the sample size.
Magnetic powder core density: the invention adopts a weighing method to measure the mass of a magnetic powder core sample, and then measures the thickness of 5 positions of the sample to obtain an average value. The magnetic powder core adopts a uniform die during compression molding, so that the inner diameter and the outer diameter of the magnetic powder core can be considered to be consistent, the volume of the magnetic powder core sample can be calculated, and the density of the magnetic powder core sample can be finally calculated.
Resistivity: and testing the resistivity of the sample by using a four-probe resistivity tester. The testing step is that the magnetic powder core sample is placed in a test bench, the four probe heads are pressed down by operating the probe bench, so that the sample is connected with a power supply, and the resistivity value is tested and read. And selecting different positions on the surface of the sample for testing, and averaging.
Quality factor: and measuring the quality factor of the magnetic powder core by adopting an impedance analyzer, winding 37.5 turns of coils on the magnetic ring of the magnetic powder core, and then testing, wherein the testing frequency is 1 MHz.
Loss: and testing the loss of the magnetic powder core by adopting a B-H analyzer, and then testing by winding 37.5 turns of coils on the magnetic powder core magnetic ring. In the test, the magnetic flux density BmThe frequency f is 1MHz at 20mT, and the test temperature T is 25 deg.C, which is used to measure the loss of magnetic powder core.
Example 1:
the thermoplastic resin and epoxy resin composite adhesive coated magnetic powder core is prepared by the following steps:
(1) passivating the sendust magnetic powder with phosphoric acid, and drying the sendust magnetic powder under the stirring of water bath at 60 ℃ to obtain passivated sendust magnetic powder, wherein the adding amount of the phosphoric acid is 0.6 wt% of the weight of the sendust magnetic powder;
(2) performing coupling treatment on passivated iron-silicon-aluminum magnetic powder by using a silane coupling agent KH-792, and stirring and drying in water bath at 80 ℃ to obtain coupled iron-silicon-aluminum magnetic powder, wherein the using amount of KH792 is 0.3 wt% of the mass of the iron-silicon-aluminum magnetic powder;
(3) dissolving epoxy resin NPES-901, phenoxy resin and epoxy resin curing agent dicyandiamide in butanone, stirring for 30min in a water bath at50 ℃ to obtain a uniformly mixed composite adhesive, then stirring and mixing the uniformly mixed composite adhesive with the coupled ferrum-silicon-aluminum magnetic powder, uniformly mixing, drying, grinding and sieving to obtain coated magnetic powder; the mass of the NPES-901 is 2.65 wt% of the mass of the sendust magnetic powder, the mass of the phenoxy resin is 0.35 wt% of the mass of the sendust magnetic powder, and the mass of the dicyandiamide is 10 wt% of the mass of the NPES-901;
(4) adding 0.3 wt% of zinc stearate lubricant (the amount of the added zinc stearate lubricant is 0.3 wt% of the coated Fe-Si-Al magnetic powder) into the coated Fe-Si-Al magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded;
(5) adding magnetic powder to be molded into a mold, pressing into an annular powder core blank by using a cold press under the pressure of 30MPa, keeping the pressure for 120s, wherein the size of the annular powder core blank is as follows: phi 20X 16X 2, namely 20mm of outer diameter, 16mm of inner diameter and 2mm of height.
(6) And (3) putting the annular powder core blank into a vacuum oven, curing for 2 hours at 180 ℃, and naturally cooling to room temperature to obtain the sendust magnetic powder core.
The cross-sectional profile of the iron-silicon-aluminum magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive prepared in this embodiment is shown in fig. 1. Therefore, the internal structure of the sendust magnetic powder core is compact, the thermoplastic resin and the epoxy resin composite adhesive are uniformly coated on the surface of the sendust magnetic powder, the tensile strength of the prepared magnetic powder core is higher, and meanwhile, the magnetic powder core also has excellent magnetic performance.
The performance of the sendust core obtained in this example was tested and shown in table 1 below:
TABLE 1
Figure BDA0003075983410000061
As can be seen from table 1, the magnetic powder core prepared in example 1 has high tensile strength and good electromagnetic properties, such as high resistivity and low loss. Therefore, the magnetic powder core prepared by the embodiment has high mechanical property, and the electromagnetic property of the magnetic powder core cannot be reduced. In the prior art, the tensile strength of the magnetic powder core prepared in Chinese invention patent 201410230405.4 and Chinese invention patent 201410230351.1 is 7.04MPa and 5.81MPa respectively, the mechanical property is poor, and the prepared magnetic powder core is easy to crack and the like, but the tensile strength of the magnetic powder core prepared in the embodiment reaches 17.04MPa, the mechanical property is good, the cracking of the magnetic powder core can be effectively reduced, and the magnetic powder core is convenient to transport and wind coils.
Example 2:
(1) passivating the sendust magnetic powder with phosphoric acid, and drying the sendust magnetic powder under the stirring of water bath at 60 ℃ to obtain the passivated sendust magnetic powder, wherein the adding amount of the phosphoric acid is 0.6 wt% of the total mass of the sendust magnetic powder;
(2) performing coupling treatment on passivated iron-silicon-aluminum magnetic powder by using a silane coupling agent KH-792, and stirring and drying in water bath at 80 ℃ to obtain coupled iron-silicon-aluminum magnetic powder, wherein the mass of the KH792 is 0.6 wt% of the total mass of the iron-silicon-aluminum magnetic powder;
(3) dissolving epoxy resin NPES-901, phenoxy resin and epoxy resin curing agent dicyandiamide in butanone, stirring for 30min in a water bath at50 ℃ to obtain a uniformly mixed composite adhesive, then stirring and mixing with coupled ferrum-silicon-aluminum magnetic powder, uniformly mixing, drying, and then grinding and sieving to obtain coated magnetic powder; the mass of the NPES-901 is 2.95 wt% of the total mass of the iron-silicon-aluminum magnetic powder, the mass of the phenoxy resin is 0.05 wt% of the total mass of the iron-silicon-aluminum magnetic powder, and the mass of the dicyandiamide is 10 wt% of the mass of the NPES-901;
(4) adding 0.3 wt% of zinc stearate lubricant into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded;
(5) adding magnetic powder to be molded into a mold, pressing into a ring-shaped powder core blank by using a cold press under the pressure of 30MPa, and keeping the pressure for 120s, wherein the size of the ring-shaped powder core blank is as follows: phi 20 is multiplied by 16 is multiplied by 2, namely the outer diameter is 20mm, the inner diameter is 16mm, and the height is 2 mm;
(6) and (3) putting the annular powder core blank into a vacuum oven, curing for 2 hours at 180 ℃, and naturally cooling to room temperature to obtain the sendust magnetic powder core.
The cross-sectional profile of the iron-silicon-aluminum magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive prepared in this embodiment is shown in fig. 2. Therefore, the internal structure of the sendust magnetic powder core is compact, the thermoplastic resin and the epoxy resin composite adhesive are uniformly coated on the surface of the sendust magnetic powder, the tensile strength of the prepared magnetic powder core is higher, and meanwhile, the magnetic powder core also has excellent magnetic performance. The final sendust core was tested for properties as shown in table 2 below:
TABLE 2
Figure BDA0003075983410000071
Figure BDA0003075983410000081
As can be seen from table 2, the magnetic powder core prepared in example 2 has high tensile strength and good electromagnetic properties, such as high resistivity and low loss. This also shows that the magnetic powder core prepared by the method has high mechanical property and does not reduce the electromagnetic property of the magnetic powder core. Compared with the prior art, the tensile strength of the magnetic powder core prepared in Chinese invention patent 201410230405.4 and Chinese invention patent 201410230351.1 is 7.04MPa and 5.81MPa respectively, the mechanical property is poor, the prepared magnetic powder core is easy to crack and the like, the tensile strength of the magnetic powder core prepared by the method reaches 14.37MPa, the mechanical property is good, the cracking of the magnetic powder core can be effectively reduced, and the magnetic powder core is convenient to transport and wind coils.
Example 3:
(1) passivating the sendust magnetic powder with phosphoric acid, and drying the sendust magnetic powder under the stirring of water bath at the temperature of 80 ℃ to obtain the passivated sendust magnetic powder, wherein the adding amount of the phosphoric acid is 1.0 wt% of the total mass of the sendust magnetic powder;
(2) performing coupling treatment on passivated iron-silicon-aluminum magnetic powder by using a silane coupling agent KH792, stirring and drying in water bath at 100 ℃ to obtain coupled iron-silicon-aluminum magnetic powder, wherein the mass of the KH792 is 0.3 wt% of the total mass of the iron-silicon-aluminum magnetic powder;
(3) dissolving epoxy resin NPES-901, phenoxy resin and epoxy resin curing agent dicyandiamide with butanone, stirring for 30min at50 ℃ in water bath to obtain a uniformly mixed composite adhesive, stirring and mixing with coupled sendust magnetic powder, uniformly mixing, drying, grinding and sieving to obtain coated magnetic powder, wherein the mass of NPES-901 is 2.95 wt% of the total mass of the sendust magnetic powder, the mass of the phenoxy resin is 0.45 wt% of the total mass of the sendust magnetic powder, and the mass of dicyandiamide is 10 wt% of the mass of NPES-901;
(4) adding 0.1 wt% of zinc stearate lubricant into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded;
(5) adding magnetic powder to be molded into a mold, pressing into a ring-shaped powder core blank by using a cold press under the pressure of 30MPa, keeping the pressure for 60s, wherein the size of the ring-shaped powder core blank is as follows: phi 20 is multiplied by 16 is multiplied by 2, namely the outer diameter is 20mm, the inner diameter is 16mm, and the height is 2 mm;
(6) and (3) putting the annular powder core blank into a vacuum oven, curing for 2 hours at 180 ℃, and naturally cooling to room temperature to obtain the sendust magnetic powder core.
The cross-sectional profile of the iron-silicon-aluminum magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive prepared in this embodiment is shown in fig. 3. Therefore, the internal structure of the sendust magnetic powder core is compact, the thermoplastic resin and the epoxy resin composite adhesive are uniformly coated on the surface of the sendust magnetic powder, the tensile strength of the prepared magnetic powder core is higher, and meanwhile, the magnetic powder core also has excellent magnetic performance. The final sendust core was tested for properties as shown in table 3 below:
TABLE 3
Figure BDA0003075983410000091
As can be seen from table 3, the magnetic powder core prepared in example 3 has high tensile strength and good electromagnetic properties, such as high resistivity and low loss. This also shows that the magnetic powder core prepared by the method has high mechanical property and does not reduce the electromagnetic property of the magnetic powder core. Compared with the prior art, the tensile strength of the magnetic powder core prepared in Chinese invention patent 201410230405.4 and Chinese invention patent 201410230351.1 is 7.04MPa and 5.81MPa respectively, the mechanical property is poor, the prepared magnetic powder core is easy to crack and the like, the tensile strength of the magnetic powder core prepared by the method reaches 15.37MPa, the mechanical property is good, the cracking of the magnetic powder core can be effectively reduced, and the magnetic powder core is convenient to transport and wind coils.
Example 4:
(1) passivating the sendust magnetic powder with phosphoric acid, and drying the sendust magnetic powder under the stirring of water bath at 60 ℃ to obtain the passivated sendust magnetic powder, wherein the adding amount of the phosphoric acid is 0.6 wt% of the total mass of the sendust magnetic powder;
(2) performing coupling treatment on passivated iron-silicon-aluminum magnetic powder by using a silane coupling agent KH792, stirring and drying in water bath at 80 ℃, so as to obtain coupled iron-silicon-aluminum magnetic powder, wherein the mass of the KH792 is 0.6 wt% of the total mass of the iron-silicon-aluminum magnetic powder;
(3) dissolving epoxy resin NPCN-704, phenoxy resin and epoxy resin curing agent dicyandiamide with butanone, stirring for 30min in a water bath at50 ℃ to obtain a uniformly mixed composite adhesive, stirring and mixing with coupled ferrum-silicon-aluminum magnetic powder, uniformly mixing, drying, grinding and sieving to obtain coated magnetic powder, wherein the mass of the NPCN-704 is 2.65 wt% of the total mass of the ferrum-silicon-aluminum magnetic powder, the mass of the phenoxy resin is 0.35 wt% of the total mass of the ferrum-silicon-aluminum magnetic powder, and the mass of the dicyandiamide is 15 wt% of the mass of the NPCN-704;
(4) adding 0.3 wt% of zinc stearate lubricant into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded;
(5) adding magnetic powder to be molded into a mold, pressing into a ring-shaped powder core blank by using a cold press under the pressure of 30MPa, and keeping the pressure for 120s, wherein the size of the ring-shaped powder core blank is as follows: phi 20 is multiplied by 16 is multiplied by 2, namely the outer diameter is 20mm, the inner diameter is 16mm, and the height is 2 mm;
(6) and (3) putting the annular powder core blank into a vacuum oven, curing for 1h at 180 ℃, and naturally cooling to room temperature to obtain the sendust magnetic powder core.
The cross-sectional profile of the iron-silicon-aluminum magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive prepared in this embodiment is shown in fig. 4. Therefore, the internal structure of the sendust magnetic powder core is compact, the thermoplastic resin and the epoxy resin composite adhesive are uniformly coated on the surface of the sendust magnetic powder, the tensile strength of the prepared magnetic powder core is higher, and meanwhile, the magnetic powder core also has excellent magnetic performance. The final sendust core was tested for properties as shown in table 4 below:
TABLE 4
Figure BDA0003075983410000101
As can be seen from table 4, the magnetic powder core prepared in example 4 has high tensile strength and good electromagnetic properties, such as high resistivity and low loss. This also shows that the magnetic powder core prepared by the method has high mechanical property and does not reduce the electromagnetic property of the magnetic powder core. Compared with the prior art, the tensile strength of the magnetic powder core prepared in Chinese invention patent 201410230405.4 and Chinese invention patent 201410230351.1 is 7.04MPa and 5.81MPa respectively, the mechanical property is poor, the prepared magnetic powder core is easy to crack and the like, the tensile strength of the magnetic powder core prepared by the method reaches 15.52MPa, the mechanical property is good, the cracking of the magnetic powder core can be effectively reduced, and the magnetic powder core is favorable for transportation and coil winding.
Example 5:
(1) passivating the sendust magnetic powder with phosphoric acid, and drying the sendust magnetic powder under the stirring of water bath at 60 ℃ to obtain the passivated sendust magnetic powder, wherein the adding amount of the phosphoric acid is 0.6 wt% of the total mass of the sendust magnetic powder;
(2) performing coupling treatment on passivated iron-silicon-aluminum magnetic powder by using a silane coupling agent KH792, stirring and drying in water bath at 80 ℃, so as to obtain coupled iron-silicon-aluminum magnetic powder, wherein the mass of the KH792 is 0.6 wt% of the total mass of the iron-silicon-aluminum magnetic powder;
(3) dissolving epoxy resin NPES-901, polyvinyl formal copolymer acrylic acid and epoxy resin curing agent dicyandiamide in tetrahydrofuran, stirring for 30min in water bath at50 ℃ to obtain a uniformly mixed composite adhesive, stirring and mixing with coupled ferrum-silicon-aluminum magnetic powder, uniformly mixing, drying, grinding and sieving to obtain coated magnetic powder, wherein the mass of NPES-901 is 2.75 wt% of the total mass of the ferrum-silicon-aluminum magnetic powder, the mass of polyvinyl formal copolymer acrylic acid is 0.25 wt% of the total mass of the ferrum-silicon-aluminum magnetic powder, and the mass of dicyandiamide is 10 wt% of the mass of NPES-901;
(4) adding 0.3 wt% of zinc stearate lubricant into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded;
(5) adding magnetic powder to be molded into a mold, pressing into a ring-shaped powder core blank by using a cold press under the pressure of 30MPa, and keeping the pressure for 120s, wherein the size of the ring-shaped powder core blank is as follows: phi 20 is multiplied by 16 is multiplied by 2, namely the outer diameter is 20mm, the inner diameter is 16mm, and the height is 2 mm;
(6) and (3) putting the annular powder core blank into a vacuum oven, curing for 2 hours at 180 ℃, and naturally cooling to room temperature to obtain the sendust magnetic powder core.
The cross-sectional profile of the iron-silicon-aluminum magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive prepared in this embodiment is shown in fig. 5. Therefore, the internal structure of the sendust magnetic powder core is compact, the thermoplastic resin and the epoxy resin composite adhesive are uniformly coated on the surface of the sendust magnetic powder, the tensile strength of the prepared magnetic powder core is higher, and meanwhile, the magnetic powder core also has excellent magnetic performance. The final sendust core was tested for properties as shown in table 5 below:
TABLE 5
Figure BDA0003075983410000121
As can be seen from table 5, the magnetic powder core prepared in example 5 has high tensile strength and good electromagnetic properties, such as high resistivity and low loss. This also shows that the magnetic powder core prepared by the method has high mechanical property and does not reduce the electromagnetic property of the magnetic powder core. Compared with the prior art, the tensile strength of the magnetic powder core prepared in Chinese invention patent 201410230405.4 and Chinese invention patent 201410230351.1 is 7.04MPa and 5.81MPa respectively, the mechanical property is poor, the prepared magnetic powder core is easy to crack and the like, the tensile strength of the magnetic powder core prepared by the method reaches 16.16MPa, the mechanical property is good, the cracking of the magnetic powder core can be effectively reduced, and the magnetic powder core is convenient to transport and wind coils.
Example 6:
(1) passivating the sendust magnetic powder with phosphoric acid, and drying the sendust magnetic powder under the stirring of water bath at 60 ℃ to obtain the passivated sendust magnetic powder, wherein the adding amount of the phosphoric acid is 0.6 wt% of the total mass of the sendust magnetic powder;
(2) performing coupling treatment on passivated iron-silicon-aluminum magnetic powder by using a silane coupling agent KH550, stirring and drying in water bath at 80 ℃, and thus obtaining the coupled iron-silicon-aluminum magnetic powder, wherein the mass of the KH550 is 0.3 wt% of the total mass of the iron-silicon-aluminum magnetic powder;
(3) dissolving epoxy resin NPES-901, phenoxy resin and epoxy resin curing agent dicyandiamide in butanone, stirring for 30min at50 ℃ in water bath to obtain a uniformly mixed composite adhesive, then stirring and mixing with coupled ferrum-silicon-aluminum magnetic powder, uniformly mixing, drying, grinding and sieving to obtain coated magnetic powder. The mass of the NPES-901 is 2.75 wt% of the total mass of the iron-silicon-aluminum magnetic powder, the mass of the polyvinyl formal copolymerized acrylic acid is 0.25 wt% of the total mass of the iron-silicon-aluminum magnetic powder, and the mass of the dicyandiamide is 10 wt% of the mass of the NPES-901;
(4) adding 0.3 wt% of zinc stearate lubricant into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded;
(5) adding magnetic powder to be molded into a mold, pressing into a ring-shaped powder core blank by using a cold press under the pressure of 30MPa, and keeping the pressure for 120s, wherein the size of the ring-shaped powder core blank is as follows: phi 20 is multiplied by 16 is multiplied by 2, namely the outer diameter is 20mm, the inner diameter is 16mm, and the height is 2 mm;
(6) and (3) putting the annular powder core blank into a vacuum oven, curing for 2 hours at 180 ℃, and naturally cooling to room temperature to obtain the sendust magnetic powder core.
The cross-sectional profile of the iron-silicon-aluminum magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive prepared in this embodiment is shown in fig. 6. Therefore, the internal structure of the sendust magnetic powder core is compact, the thermoplastic resin and the epoxy resin composite adhesive are uniformly coated on the surface of the sendust magnetic powder, the tensile strength of the prepared magnetic powder core is higher, and meanwhile, the magnetic powder core also has excellent magnetic performance. The final sendust core was tested for properties as shown in table 6 below:
TABLE 6
Figure BDA0003075983410000131
As can be seen from table 6, the magnetic powder core prepared in example 6 has high tensile strength and good electromagnetic properties, such as high resistivity and low loss. This also shows that the magnetic powder core prepared by the method has high mechanical property and does not reduce the electromagnetic property of the magnetic powder core. Compared with the prior art, the tensile strength of the magnetic powder core prepared in Chinese invention patent 201410230405.4 and Chinese invention patent 201410230351.1 is 7.04MPa and 5.81MPa respectively, the mechanical property is poor, the prepared magnetic powder core is easy to crack and the like, the tensile strength of the magnetic powder core prepared by the method reaches 16.55MPa, the mechanical property is good, the cracking of the magnetic powder core can be effectively reduced, and the magnetic powder core is convenient to transport and wind coils.
Example 7:
(1) passivating the sendust magnetic powder with phosphoric acid, and drying the sendust magnetic powder under the stirring of water bath at 60 ℃ to obtain the passivated sendust magnetic powder, wherein the adding amount of the phosphoric acid is 0.6 wt% of the total mass of the sendust magnetic powder;
(2) and (3) coupling the passivated iron-silicon-aluminum magnetic powder by using a silane coupling agent KH792, and stirring and drying in water bath at 80 ℃ to obtain the coupled iron-silicon-aluminum magnetic powder. KH792 accounts for 0.6 wt% of the total mass of the Fe-Si-Al magnetic powder;
(3) dissolving epoxy resin NPES-901, MBS and epoxy resin curing agent dicyandiamide with butanone, stirring for 30min in 50 ℃ water bath to obtain a uniformly mixed composite adhesive, then stirring and mixing with coupled ferrosilicon-aluminum magnetic powder, uniformly mixing, drying, grinding and sieving to obtain coated magnetic powder, wherein the mass of NPES-901 is 2.55 wt% of the total mass of the ferrosilicon-aluminum magnetic powder, the mass of polyvinyl formal copolymerized acrylic acid is 0.45 wt% of the total mass of the ferrosilicon-aluminum magnetic powder, and the mass of dicyandiamide is 10 wt% of the mass of NPES-901;
(4) adding 0.3 wt% of zinc stearate lubricant into the coated magnetic powder, and uniformly mixing to obtain the magnetic powder to be molded;
(5) adding magnetic powder to be molded into a mold, pressing into a ring-shaped powder core blank by using a cold press under the pressure of 30MPa, and keeping the pressure for 120s, wherein the size of the ring-shaped powder core blank is as follows: phi 20 is multiplied by 16 is multiplied by 2, namely the outer diameter is 20mm, the inner diameter is 16mm, and the height is 2 mm;
(6) and (3) putting the annular powder core blank into a vacuum oven, curing for 2 hours at 180 ℃, and naturally cooling to room temperature to obtain the sendust magnetic powder core.
The cross-sectional profile of the iron-silicon-aluminum magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive prepared in this embodiment is shown in fig. 7. Therefore, the internal structure of the sendust magnetic powder core is compact, the thermoplastic resin and the epoxy resin composite adhesive are uniformly coated on the surface of the sendust magnetic powder, the tensile strength of the prepared magnetic powder core is higher, and meanwhile, the magnetic powder core also has excellent magnetic performance. The final sendust cores were tested for properties as shown in table 7 below:
TABLE 7
Figure BDA0003075983410000141
Figure BDA0003075983410000151
As can be seen from table 7, the magnetic powder core prepared in example 7 has high tensile strength and good electromagnetic properties, such as high resistivity and low loss. This also shows that the magnetic powder core prepared by the method has high mechanical property and does not reduce the electromagnetic property of the magnetic powder core. Compared with the prior art, the tensile strength of the magnetic powder core prepared in Chinese invention patent 201410230405.4 and Chinese invention patent 201410230351.1 is 7.04MPa and 5.81MPa respectively, the mechanical property is poor, the prepared magnetic powder core is easy to crack and the like, the tensile strength of the magnetic powder core prepared by the method reaches 15.52MPa, the mechanical property is good, the cracking of the magnetic powder core can be effectively reduced, and the magnetic powder core is convenient to transport and wind coils.
It will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. A thermoplastic resin and epoxy resin composite adhesive coated magnetic powder core is characterized in that a powder core blank is obtained by curing at the temperature of 150-180 ℃, the powder core blank is obtained by cold press molding of coated magnetic powder, and the coated magnetic powder is obtained by drying passivated magnetic powder after treatment of a coupling agent, and coating with a thermoplastic resin, epoxy resin composite adhesive and a lubricant; the thermoplastic resin and epoxy resin composite adhesive is formed by compounding thermoplastic resin, epoxy resin and an epoxy resin curing agent.
2. The thermoplastic resin and epoxy resin composite binder coated magnetic powder core of claim 1, wherein the magnetic powder is sendust.
3. The method for preparing the thermoplastic resin and epoxy resin composite adhesive coated magnetic powder core according to claim 1 or 2, characterized by comprising the following steps:
1) passivating the magnetic powder by using a passivating agent, drying, adding a coupling agent for coupling, drying, and adding a thermoplastic resin, an epoxy resin composite adhesive and a lubricant for coating; the thermoplastic resin and epoxy resin composite adhesive is formed by compounding thermoplastic resin, epoxy resin and an epoxy resin curing agent;
2) pressing and molding the coated magnetic powder by using a cold press to obtain an annular powder core blank;
3) and (3) curing the annular powder core blank in a vacuum oven, and cooling to room temperature to obtain the magnetic powder core.
4. The method for preparing the magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive according to claim 3, wherein the passivating agent in the step 1) is one of phosphoric acid and chromic acid, and the adding amount of the passivating agent is 0.6 wt% -1.0 wt% of the total mass of the magnetic powder.
5. The method for preparing the magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive according to claim 3, wherein the coupling agent in the step 1) is a silane coupling agent, the silane coupling agent is one of KH792, KH550, KH560 or KH580, and the addition amount is 0.3 wt% to 0.6 wt% of the total mass of the magnetic powder; the lubricant in the step 1) is zinc stearate, and the addition amount of the lubricant is 0.1-0.3 wt% of the total mass of the magnetic powder.
6. The method for preparing the magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive according to claim 3, wherein the thermoplastic resin is one selected from phenoxy resin, polyvinyl formal copolymerized acrylic acid, epoxidized thermoplastic elastomer AT501 or MBS resin;
the addition amount of the thermoplastic resin is 0.05 wt% -0.45 wt% of the total mass of the magnetic powder; the epoxy resin is selected from one of NPES-902, NPES-901, NPES-907, NPES-904 or NPCN-704, and the addition amount of the epoxy resin is 2 wt% -4 wt% of the total mass of the magnetic powder.
7. The method for preparing the magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive according to claim 1, wherein the epoxy resin curing agent is one of dicyandiamide and diaminodiphenyl sulfone.
8. The method for preparing the magnetic powder core coated by the thermoplastic resin and epoxy resin composite adhesive according to claim 7, wherein the method for compounding the thermoplastic resin and epoxy resin composite adhesive comprises the following steps: firstly, dissolving thermoplastic resin, epoxy resin and epoxy resin curing agent by organic solvent, mixing, and stirring in water bath at 50-80 ℃ for 30-60min to obtain the uniformly mixed composite adhesive.
9. The method for preparing the magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive according to claim 8, wherein the organic solvent is one or more of butanone, tetrahydrofuran, and xylene.
10. The method for preparing the magnetic powder core coated with the thermoplastic resin and epoxy resin composite adhesive according to claim 1, wherein the drying after the passivation treatment in the step 1) is drying under water bath stirring at a temperature of 60 ℃ to 80 ℃, and the drying after the coupling treatment by adding the coupling agent is drying under water bath stirring at a temperature of 80 ℃ to 100 ℃;
the pressing pressure of the hydraulic press in the step 2) is 10-30MPa, and the pressure maintaining time is 60-120s
In the step 3), the curing temperature is 150-180 ℃, and the curing time is 1-2 h.
CN202110552565.0A 2021-05-20 2021-05-20 Coated magnetic powder core of thermoplastic resin and epoxy resin composite adhesive and preparation method thereof Pending CN113410021A (en)

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