CN113223843A - Insulation coating method of composite soft magnetic powder - Google Patents

Insulation coating method of composite soft magnetic powder Download PDF

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CN113223843A
CN113223843A CN202110448966.1A CN202110448966A CN113223843A CN 113223843 A CN113223843 A CN 113223843A CN 202110448966 A CN202110448966 A CN 202110448966A CN 113223843 A CN113223843 A CN 113223843A
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soft magnetic
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alloy powder
magnetic alloy
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CN113223843B (en
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霍利山
郭海
黄嘉翔
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Ningbo Zhongke B Plus New Materials Technology Co ltd
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    • 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
    • H01F41/0253Apparatus 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 for manufacturing permanent magnets
    • 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
    • H01F1/33Magnets 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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin
    • 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
    • H01F41/0253Apparatus 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 for manufacturing permanent magnets
    • H01F41/026Apparatus 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 for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment

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Abstract

The invention discloses an insulation coating method of composite soft magnetic powder, which comprises the following steps: step S1, screening soft magnetic alloy powder; step S2, uniformly dispersing the soft magnetic ferrite fine powder into an ethanol solution of a silane coupling agent to obtain a first dispersion liquid; step S3, adding soft magnetic alloy powder into the first dispersion liquid for pretreatment; step S4, adding ammonia water and ethyl orthosilicate into the composite powder dispersion liquid to generate a composite coating layer; step S5, dissolving the binder and the lubricant in acetone, and then uniformly dispersing the ferrite fine powder into the solution to obtain a second dispersion liquid; and step S6, uniformly mixing the coated soft magnetic alloy powder into the second dispersion liquid, granulating and drying. The invention has the beneficial effects that: the silicon dioxide coating layer and the binding agent are doped with a proper amount of soft magnetic ferrite fine powder, so that the magnetic conductivity of the magnetic part formed by pressing is improved, and meanwhile, the high-frequency loss is low, so that a rear-end device of the magnetic part has more excellent comprehensive performance.

Description

Insulation coating method of composite soft magnetic powder
Technical Field
The invention relates to the field of magnetic materials, in particular to an insulation coating method of composite soft magnetic powder.
Background
The amorphous nanocrystalline soft magnetic material has excellent comprehensive properties such as high saturation magnetization, high magnetic conductivity, low coercive force, low loss, good strong hardness, wear resistance and corrosion resistance, good temperature and environmental stability and the like, embodies the advantages of small volume, high efficiency, energy conservation and the like in the power electronic technology, and has better performance price in all metal soft magnetic materials.
In the preparation process of the amorphous nanocrystalline magnetic powder core, the performance of the insulating coating layer is an important factor influencing the high-frequency loss of the magnetic powder core, and if the insulating coating layer is not completely coated or damaged, the eddy current loss among magnetic powder particles is sharply increased, so that the high-frequency loss of the magnetic powder core is increased. The insulation coating is divided into organic coating and inorganic coating, and common organic insulation coating agents include epoxy resin, phenolic resin, organic silicon resin and the like. The organic coating agent has good bonding property, but has poor heat resistance, is difficult to eliminate the internal stress of the magnetic core, and limits the heat treatment temperature of the magnetic powder core. The inorganic coating agent is mainly mineral powder, silicate and various oxides with high resistivity. It is widely used for insulating coated magnetic powder core due to its advantages of high heat treatment temperature, high resistivity, low cost, etc. At present, most of the magnetic powder cores are mainly prepared by inorganic coating, and although the coating agents have good insulation effect, most of the coating agents are non-magnetic substances, so that the magnetic performance of the magnetic powder cores is greatly reduced.
In the prior art, an acid solution is generally used for corrosive insulation coating treatment in the insulation coating process, for example, patent documents such as prior applications CN110181036A and CN104078180B disclose that passivation treatment is performed on powder by using a phosphoric acid solution, and then an insulating agent and a binder are added for insulation coating of the powder, wherein the acid solution is generally diluted by volatile organic matters, which causes cost increase and environmental damage; the reaction control difficulty in the corrosion process is high, and the amorphous nanocrystalline structure on the surface of the powder particles is easy to change due to nonuniform coating and excessive local heat release of the powder particles; the corrosion of powder particles can cause the adverse effects of the reduction of powder magnetic conductivity and the increase of hysteresis loss, so that in order to solve the problems, an insulation coating method of the composite soft magnetic powder is urgently needed to be designed so as to meet the requirements of practical use.
Disclosure of Invention
In view of the above problems in the prior art, a method for insulating and coating composite soft magnetic powder is provided, which can prepare a powder material with high magnetic permeability and low eddy current loss.
The specific technical scheme is as follows:
an insulating coating method for composite soft magnetic powder features that a chemical reaction is used to form a compact and uniform composite coating layer of silicon dioxide and soft magnetic ferrite particles on the surface of soft magnetic alloy powder, and the ferrite particles are uniformly mixed in adhesive. The method comprises the following steps:
step S1, powder screening: screening soft magnetic alloy powder with a preset particle size, and weighing according to a preset mass;
step S2, preparing a first dispersion of ferrite fine powder: mixing a silane coupling agent, absolute ethyl alcohol and deionized water according to a certain proportion, fully stirring to uniformly mix the silane coupling agent, the absolute ethyl alcohol and the deionized water, then adding the soft magnetic ferrite micro powder into the solution, fully stirring to uniformly disperse the soft magnetic ferrite micro powder into the solution, and obtaining a first dispersion liquid of the soft magnetic ferrite micro powder;
step S3, soft magnetic alloy powder pretreatment: adding the soft magnetic alloy powder obtained in the step S1 into the first dispersion liquid of the soft magnetic ferrite fine powder obtained in the step S2, and fully stirring to obtain a composite powder dispersion liquid;
step S4, generating a coating layer: adding a certain amount of ammonia water into the composite powder dispersion liquid prepared in the step S3 to adjust the pH value of the mixed solution to be alkalescent, adding a certain amount of tetraethoxysilane, carrying out water bath, keeping the temperature for a certain time, and finally repeatedly cleaning and drying the composite powder to obtain soft magnetic alloy powder with a silicon dioxide and soft magnetic ferrite fine particle composite coating layer;
step S5, preparing a second dispersion of ferrite fine powder: completely dissolving a binder and a lubricant in acetone to form an acetone solution, doping the soft magnetic ferrite fine powder into the acetone solution, and uniformly dispersing the soft magnetic ferrite fine powder into the acetone solution to obtain a second dispersion liquid of the soft magnetic ferrite fine powder;
step S6, insulating coating: and (4) uniformly mixing the soft magnetic alloy powder with the composite coating layer obtained in the step (S4) and the second dispersion liquid of the soft magnetic ferrite micro-fine powder obtained in the step (S5), stirring to obtain composite soft magnetic slurry, stirring, kneading and granulating the composite soft magnetic slurry on granulating equipment, and drying in an oven to obtain the composite soft magnetic powder with good insulation coating.
Preferably, in step S1, the soft magnetic alloy powder is at least one of amorphous soft magnetic alloy powder, nanocrystalline soft magnetic alloy powder, iron-silicon-aluminum alloy powder, iron-silicon-chromium alloy powder, iron-silicon-nickel alloy powder, iron-silicon-aluminum-nickel alloy powder, iron-nickel-aluminum alloy powder, and carbonyl iron powder.
Preferably, in step S1, the grain size of the soft magnetic alloy powder is less than 100 μm.
Preferably, in the step S2, the mass of the soft magnetic ferrite fine powder is 0.5% to 3% of the preset mass of the soft magnetic alloy powder;
the content of the silane coupling agent is 0.5-5% of the preset mass of the soft magnetic alloy powder.
Preferably, the particle diameters of the soft magnetic ferrite fine powder are less than 1 μm in both the step S2 and the step S5.
Preferably, in the step S4, the content of the tetraethoxysilane is 1% to 10% of the preset mass of the soft magnetic alloy powder.
Preferably, in the step S5, the mass of the soft magnetic ferrite fine powder is 0.5% to 5% of the predetermined mass of the soft magnetic alloy powder.
Preferably, in the step S5, the content of the binder is 1% to 5% of the total mass of the soft magnetic alloy powder with the composite coating layer obtained in the step S4;
the content of the lubricant is 0.5-1% of the total mass of the soft magnetic alloy powder with the composite coating layer.
Preferably, in step S4, a water bath is performed in a water bath kettle;
the temperature of the water bath is 30-70 ℃, and the stirring is carried out for 1-12h at a preset speed.
Preferably, in the step S6, drying is performed in a vacuum oven;
the temperature is set to be 50-100 ℃, and the drying time is more than 1 h.
The invention utilizes a chemical reaction method to form a compact and uniform silicon dioxide and soft magnetic ferrite fine particle composite coating layer outside the soft magnetic alloy powder particles, and uniformly mixes ferrite fine particles into a binder. The beneficial effects of this technical scheme lie in:
firstly, the solution is alkalescent in the process of preparing the composite coating layer, so that the problems of magnetic performance reduction and the like caused by corrosion of powder particles are avoided, and the soft magnetic ferrite has higher high-frequency magnetic conductivity and good insulativity, so that compared with the existing soft magnetic alloy powder insulation coating technology, the technical scheme obviously improves the high-frequency magnetic conductivity of a magnetic part formed by pressing composite soft magnetic powder, simultaneously keeps lower high-frequency loss, and ensures that the rear-end magnetic part, an inductor and other devices have more excellent comprehensive performance;
secondly, because the technical scheme avoids the corrosion to the powder particles, the prepared insulating coating has better uniformity and compactness, and the composite coating is made of stable silicon dioxide and ferrite materials, so that the prepared magnetic part, inductor and other devices have higher electric breakdown resistance and better stability.
Drawings
FIG. 1 is a schematic flow chart of a method for insulation coating of composite soft magnetic powder according to the present invention.
Fig. 2 is a schematic diagram of a powder microstructure of a magnetic ring component compression molded using composite soft magnetic powder in accordance with the present invention.
The figures are numbered: 1. soft magnetic alloy powder particles; 2. fine particles of soft magnetic ferrite; 3. a composite coating layer; 4. and (3) a binder.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
The invention provides an insulation coating method of composite soft magnetic powder, belonging to the field of magnetic materials, as shown in figure 1, comprising the following steps:
step S1, powder screening: screening soft magnetic alloy powder with a preset particle size by using an ultrasonic vibration screen, and weighing according to a preset mass, wherein the particle size of the soft magnetic alloy powder is preferably less than 100 micrometers;
step S2, preparing a first dispersion of ferrite fine powder: weighing a silane coupling agent which is 0.5-5% of the preset mass of the soft magnetic alloy powder, weighing soft magnetic ferrite micro powder which is 0.5-3% of the preset mass of the soft magnetic alloy powder, mixing the silane coupling agent, absolute ethyl alcohol and deionized water according to a certain proportion, fully stirring to uniformly mix the soft magnetic ferrite micro powder, adding the soft magnetic ferrite micro powder into the solution, fully stirring to uniformly disperse the soft magnetic ferrite micro powder in the solution, and obtaining a first dispersion liquid of the soft magnetic ferrite micro powder;
step S3, soft magnetic alloy powder pretreatment: adding the soft magnetic alloy powder obtained in the step S1 into the first dispersion liquid of the soft magnetic ferrite fine powder obtained in the step S2, and fully stirring to obtain a composite powder dispersion liquid;
step S4, generating a coating layer: adding a certain amount of ammonia water into the composite powder dispersion liquid prepared in the step S3 to adjust the pH value of the mixed solution to be alkalescent, adding a certain amount of ethyl orthosilicate, carrying out water bath through a water bath kettle at the temperature of 30-70 ℃, stirring for 1-12h at a preset constant speed, preserving heat for a certain time, and finally repeatedly cleaning and drying the composite powder to obtain the soft magnetic alloy powder with the silicon dioxide and soft magnetic ferrite fine powder composite coating layer;
step S5, preparing a second dispersion of ferrite fine powder: weighing a binder and a lubricant, wherein the binder is 1% -5% of the total mass of the soft magnetic alloy powder with the composite coating layer obtained in the step S4, the lubricant is 0.5% -1% of the total mass of the soft magnetic alloy powder with the composite coating layer, weighing soft magnetic ferrite micro powder again, the soft magnetic ferrite micro powder is 0.5% -5% of the preset mass of the soft magnetic alloy powder, completely dissolving the binder and the lubricant in acetone to form an acetone solution, doping the soft magnetic ferrite micro powder into the acetone solution, and uniformly dispersing the soft magnetic ferrite micro powder into the acetone solution to obtain a second dispersion liquid of the soft magnetic ferrite micro powder;
step S6, insulating coating: and (3) uniformly mixing the soft magnetic alloy powder with the composite coating layer obtained in the step (S4) and the second dispersion liquid of the soft magnetic ferrite micro-fine powder obtained in the step (S5), stirring to obtain composite soft magnetic slurry, stirring, kneading, granulating the composite soft magnetic slurry on granulating equipment, drying in a vacuum oven at the set temperature of 50-100 ℃ for more than 1h to obtain the insulated and coated composite soft magnetic powder.
The invention utilizes a chemical reaction method to form a compact and uniform silicon dioxide and soft magnetic ferrite fine particle composite coating layer outside the soft magnetic alloy powder particles, and uniformly mixes ferrite fine particles into a binder to improve the magnetic conductivity of a magnetic part formed by pressing the soft magnetic alloy powder.
The first embodiment is as follows:
the soft magnetic alloy powder in the embodiment is Fe-Si-B-C-Cr amorphous soft magnetic alloy powder with the particle size of 7-15 mu m, wherein the median particle size D50 is about 10 mu m; the ferrite fine powder is Mn-Zn soft magnetic ferrite powder, and the median particle size D50 is about 750 nm; the insulation coating method comprises the following steps:
step S1, powder screening: screening soft magnetic alloy powder with proper particle size by using an ultrasonic vibration screen, and weighing according to preset mass;
step S2, preparing a first dispersion of ferrite fine powder: respectively weighing a silane coupling agent according to 1.5% of the preset mass of the soft magnetic alloy powder in the step S1, weighing Mn-Zn soft magnetic ferrite fine powder according to 1% of the preset mass of the soft magnetic alloy powder in the step S1, fully stirring and mixing the silane coupling agent, absolute ethyl alcohol and deionized water, then adding the Mn-Zn soft magnetic ferrite fine powder into the solution, fully stirring for 1h at room temperature, and uniformly dispersing the Mn-Zn soft magnetic ferrite fine powder into the solution to obtain a first dispersion liquid of the Mn-Zn soft magnetic ferrite fine powder;
step S3, soft magnetic alloy powder pretreatment: adding the soft magnetic alloy powder obtained in the step S1 into the first dispersion liquid of the soft magnetic ferrite fine powder obtained in the step S2, and fully stirring to obtain a composite powder dispersion liquid;
step S4, generating a coating layer: adding a certain amount of ammonia water into the composite powder dispersion liquid prepared in the step S3, adjusting the pH value of the mixed solution to 9-10, weighing tetraethoxysilane according to 5% of the preset mass of the soft magnetic alloy powder, adding the tetraethoxysilane into the mixed solution, then placing the mixture into a water bath kettle, keeping the water bath temperature at 40 ℃, stirring at a constant speed for 3 hours, keeping the temperature for 0.5 hour, finally repeatedly cleaning and drying the composite powder to obtain the soft magnetic alloy powder with the silicon dioxide and Mn-Zn soft magnetic ferrite fine powder composite coating layer;
step S5, preparing a second dispersion of ferrite fine powder: respectively weighing a binder and a lubricant according to 3% and 0.8% of the total mass of the soft magnetic alloy powder with the composite coating layer prepared in the step S4, completely dissolving the binder and the lubricant in acetone to form an acetone solution, weighing Mn-Zn soft magnetic ferrite fine powder again according to 1% of the preset mass of the soft magnetic alloy powder in the step S1, doping the Mn-Zn soft magnetic ferrite fine powder into the acetone solution, and fully stirring for 1 hour at room temperature to uniformly disperse the Mn-Zn soft magnetic ferrite fine powder into the acetone solution to obtain a second dispersion liquid of the Mn-Zn soft magnetic ferrite fine powder;
step S6, insulating coating: and (3) uniformly mixing the soft magnetic alloy powder with the composite coating layer obtained in the step (S4) and the second dispersion liquid of the Mn-Zn soft magnetic ferrite micro-fine powder obtained in the step (S5), stirring to obtain composite soft magnetic slurry, then stirring, kneading and granulating the composite soft magnetic slurry on a granulating device, drying in a vacuum oven at the set temperature of 80 ℃ for more than 1h, screening out powder with the particle size of-80 meshes to +200 meshes by using an ultrasonic vibration sieve, and thus obtaining the Fe-Si-B-C-Cr composite soft magnetic powder material with good insulation coating.
The Fe-Si-B-C-Cr composite soft magnetic powder coated with insulation in the embodiment is used for preparing a magnetic component, and then a performance test is carried out, and the specific steps are as follows:
step A1, weighing the prepared composite soft magnetic powder material, wherein the mass of the composite soft magnetic powder material is 3g, placing the weighed composite soft magnetic powder material in an annular die, and performing cold pressing to form a magnetic ring blank, preferably, the outer diameter of the annular die is 20mm, and the inner diameter of the annular die is 12 mm; ultrasonic vibration is applied in the cold pressing process, the vibration frequency is 20KHz, and the pressure maintaining pressure is 6t/cm2Keeping the pressure for 60s, and demolding to obtain a magnetic ring blank;
and step A2, placing the magnetic ring blank in a vacuum oven, keeping the temperature at 180 ℃ for 2 hours, and taking out the magnetic ring blank after the magnetic ring blank is cooled to normal temperature to obtain a solidified magnetic ring component. As shown in fig. 2, fig. 2 is a schematic view of a microstructure of the powder inside the magnetic ring component, a compact and uniform composite coating layer 3 of silica and soft magnetic ferrite fine particles 2 is formed outside the soft magnetic alloy powder particles 1 by using a chemical reaction method, and the soft magnetic ferrite fine particles 2 are uniformly doped in a binder 4, so as to achieve the purpose of improving the magnetic permeability of the magnetic ring component.
Step a3, primary magnetic property test: winding 15 turns of enameled copper wires on the cured magnetic ring component prepared in the step A2, testing the inductance of the cured magnetic ring component through an impedance analyzer under the test condition of 1MHz, and calculating the magnetic conductivity mu' according to the inductance; the loss value is tested by a B-H analyzer under the test condition of 1MHz/20 mT.
Table 1 performance parameters of magnetic ring parts obtained in example one and comparative examples one and two
Figure BDA0003037868370000071
In the above table 1, 1 indicates that the Mn — Zn ferrite is added in the corresponding step, and the addition amount is 1% of the predetermined mass of the soft magnetic alloy powder in step S1; 0 means that no Mn-Zn ferrite was added in the corresponding step.
When the magnetic component is prepared from the Fe-Si-B-C-Cr composite soft magnetic powder with good insulation coating prepared in the embodiment, the magnetic permeability mu' under the condition of 1MHz is measured to be 28 by an impedance analyzer; the loss Pcv measured by a B-H analyzer under the condition of 1MHz/20mT was 805kW/m3
The first comparative example adopts the same preparation process and parameters as those of the first example, except that no Mn-Zn soft magnetic ferrite fine powder is added in step S5, and the magnetic permeability μ' of the magnetic ring component finally prepared in the first comparative example is 25; the loss Pcv is 816kW/m3
The second comparative example adopts the same preparation process and parameters as the first example, and is different in that fine Mn-Zn soft magnetic ferrite powder is not added in the whole preparation process, and the magnetic permeability mu' of the magnetic ring component finally prepared in the second comparative example is 21; the loss Pcv is 830kW/m3
Example two:
the soft magnetic alloy powder in the embodiment is Fe-Si-B-Cu-Nb nanocrystalline soft magnetic alloy powder with the particle size of 5-22 μm, wherein the median particle size D50 is about 10 μm; the ferrite fine powder is Mn-Zn soft magnetic ferrite powder, and the median particle size D50 is about 750 nm.
The preparation process of the insulated and coated soft magnetic alloy powder and the preparation process and parameters of the magnetic ring blank obtained in the embodiment are the same as those of the embodiment one, and the differences are that the composition of the nanocrystalline soft magnetic alloy powder is different, the particle size is different, and the parameters of the magnetic ring part are shown in table 2.
Table 2 performance parameters of magnetic ring parts obtained in example two, comparative example three, and comparative example four
Figure BDA0003037868370000081
When the magnetic component is prepared from the Fe-Si-B-Cu-Nb composite soft magnetic powder with good insulation coating prepared in the embodiment, the magnetic permeability mu' under the condition of 1MHz is measured to be 36 by an impedance analyzer; the loss Pcv under the condition of 1MHz/20mT is 465kW/m measured by a B-H analyzer3
The preparation process of the insulated and coated soft magnetic alloy powder and the preparation process and parameters of the magnetic ring blank obtained in the third comparative example are the same as those of the second example, except that only the fine powder of the Mn-Zn soft magnetic ferrite is removed in step S4, and the magnetic permeability μ' of the finally prepared magnetic ring component under the same test condition is 31; the loss Pcv measured by a B-H analyzer under the condition of 1MHz/20mT was 470kW/m3
The preparation process of the insulated and coated soft magnetic alloy powder and the preparation process and parameters of the magnetic ring blank obtained in the fourth comparative example are the same as those of the second embodiment, except that fine Mn-Zn soft magnetic ferrite powder is not added in the whole preparation process, and the magnetic permeability mu' of the finally prepared magnetic ring component is 27; the loss Pcv under the condition of 1MHz/20mT measured by a B-H analyzer is 482kW/m3
As can be seen from tables 1 and 2 above: compact and uniform silicon dioxide and soft magnetic ferrite fine particle composite coating layers are formed outside the soft magnetic alloy powder particles, and the ferrite fine particles are uniformly mixed into the binder, so that on one hand, eddy current paths among the ferromagnetic particles can be effectively blocked, magnetic fields among the ferromagnetic particles can be well coupled, eddy current loss is effectively reduced, and iron loss is reduced; on the other hand, the ferrite has higher high-frequency magnetic conductivity, the magnetic conductivity of the magnetic part formed by pressing soft magnetic powder is improved to more than 30%, and meanwhile, lower high-frequency loss is kept, thereby being very beneficial to high-frequency miniaturization and miniaturization of inductance devices.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.

Claims (10)

1. A method of insulating and coating a composite soft magnetic powder, comprising:
step S1, powder screening: screening soft magnetic alloy powder with a preset particle size, and weighing according to a preset mass;
step S2, preparing a first dispersion of ferrite fine powder: mixing a silane coupling agent, absolute ethyl alcohol and deionized water according to a certain proportion, fully stirring to uniformly mix the silane coupling agent, the absolute ethyl alcohol and the deionized water, then adding the soft magnetic ferrite micro powder into the solution, fully stirring to uniformly disperse the soft magnetic ferrite micro powder into the solution, and obtaining a first dispersion liquid of the soft magnetic ferrite micro powder;
step S3, soft magnetic alloy powder pretreatment: adding the soft magnetic alloy powder obtained in the step S1 into the first dispersion liquid of the soft magnetic ferrite fine powder obtained in the step S2, and fully stirring to obtain a composite powder dispersion liquid;
step S4, generating a coating layer: adding a certain amount of ammonia water into the composite powder dispersion liquid prepared in the step S3 to adjust the pH value of the mixed solution to be alkalescent, adding a certain amount of tetraethoxysilane, carrying out water bath, keeping the temperature for a certain time, and finally repeatedly cleaning and drying the composite powder to obtain soft magnetic alloy powder with a silicon dioxide and soft magnetic ferrite fine particle composite coating layer;
step S5, preparing a second dispersion of ferrite fine powder: completely dissolving a binder and a lubricant in acetone to form an acetone solution, doping the soft magnetic ferrite fine powder into the acetone solution, and uniformly dispersing the soft magnetic ferrite fine powder into the acetone solution to obtain a second dispersion liquid of the soft magnetic ferrite fine powder;
step S6, insulating coating: and (4) uniformly mixing the soft magnetic alloy powder with the composite coating layer obtained in the step (S4) and the second dispersion liquid of the soft magnetic ferrite micro-fine powder obtained in the step (S5), stirring to obtain composite soft magnetic slurry, stirring, kneading and granulating the composite soft magnetic slurry on granulating equipment, and drying in an oven to obtain the composite soft magnetic powder with good insulation coating.
2. The method as claimed in claim 1, wherein the soft magnetic alloy powder is at least one of amorphous soft magnetic alloy powder, nanocrystalline soft magnetic alloy powder, sendust powder, and carbonyl iron powder in step S1.
3. The insulation coating method of composite soft magnetic powder as recited in claim 1, wherein said soft magnetic alloy powder has a particle size of less than 100 μm in said step S1.
4. The insulation coating method of a composite soft magnetic powder as recited in claim 1, wherein in said step S2, the mass of said soft magnetic ferrite fine powder is 0.5-3% of the predetermined mass of said soft magnetic alloy powder;
the content of the silane coupling agent is 0.5-5% of the preset mass of the soft magnetic alloy powder.
5. The insulation coating method of a composite soft magnetic powder as set forth in claim 1, wherein the particle size of the soft magnetic ferrite fine powder is less than 1 μm in both of said step S2 and said step S5.
6. The insulation coating method of composite soft magnetic powder as claimed in claim 1, wherein the content of said tetraethoxysilane is 1% to 10% by mass of the predetermined soft magnetic alloy powder in said step S4.
7. The insulation coating method of composite soft magnetic powder as claimed in claim 1, wherein the mass of the soft magnetic ferrite fine powder is 0.5-5% of the predetermined mass of the soft magnetic alloy powder in the step S5.
8. The method of claim 1, wherein in step S5, the binder is present in an amount of 1-5% by mass based on the total mass of the soft magnetic alloy powder with the composite clad layer obtained in step S4;
the content of the lubricant is 0.5-1% of the total mass of the soft magnetic alloy powder with the composite coating layer.
9. The insulation coating method of composite soft magnetic powder as claimed in claim 1, wherein said step S4, a water bath is performed using a water bath;
the temperature of the water bath is 30-70 ℃, and the stirring is carried out for 1-12h at a preset speed.
10. The insulation coating method of composite soft magnetic powder as claimed in claim 1, wherein said step S6, drying in a vacuum oven;
the temperature is set to be 50-100 ℃, and the drying time is more than 1 h.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113968730A (en) * 2021-11-11 2022-01-25 横店集团东磁股份有限公司 Z-type ferrite composite material and preparation method and application thereof
CN114082943A (en) * 2021-11-23 2022-02-25 成都佳驰电子科技股份有限公司 Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004014613A (en) * 2002-06-04 2004-01-15 Mitsubishi Materials Corp PROCESS FOR PRODUCING Fe-Co BASED COMPOSITE SOFT MAGNETIC SINTERED ALLOY HAVING HIGH DENSITY AND HIGH PERMEABILITY
US20040161600A1 (en) * 2001-04-02 2004-08-19 Kazunori Igarashi Composite soft magnetic sintered material having high density and high magnetic permeability and method for preparation thereof
JP2011214026A (en) * 2010-03-31 2011-10-27 Doshisha Magnetic nanocomposite and method for producing the same
US20160071637A1 (en) * 2013-03-27 2016-03-10 Hitachi Chemical Company, Ltd. Powder magnetic core for reactor
CN105810383A (en) * 2016-05-12 2016-07-27 宁波中科毕普拉斯新材料科技有限公司 Preparation method for iron-based nanocrystalline magnetic powder core
CN110181036A (en) * 2019-05-14 2019-08-30 合肥博微田村电气有限公司 A kind of composite soft-magnetic metal powder, preparation method and integrated inductance
CN110405201A (en) * 2019-08-15 2019-11-05 中南大学 A kind of surface graded clad structure of magnetic powder, method for coating and soft-magnetic composite material
US20210060642A1 (en) * 2018-02-20 2021-03-04 Dowa Electronics Materials Co., Ltd. Silicon oxide-coated soft magnetic powder and method for producing same

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040161600A1 (en) * 2001-04-02 2004-08-19 Kazunori Igarashi Composite soft magnetic sintered material having high density and high magnetic permeability and method for preparation thereof
JP2004014613A (en) * 2002-06-04 2004-01-15 Mitsubishi Materials Corp PROCESS FOR PRODUCING Fe-Co BASED COMPOSITE SOFT MAGNETIC SINTERED ALLOY HAVING HIGH DENSITY AND HIGH PERMEABILITY
JP2011214026A (en) * 2010-03-31 2011-10-27 Doshisha Magnetic nanocomposite and method for producing the same
US20160071637A1 (en) * 2013-03-27 2016-03-10 Hitachi Chemical Company, Ltd. Powder magnetic core for reactor
CN105810383A (en) * 2016-05-12 2016-07-27 宁波中科毕普拉斯新材料科技有限公司 Preparation method for iron-based nanocrystalline magnetic powder core
US20210060642A1 (en) * 2018-02-20 2021-03-04 Dowa Electronics Materials Co., Ltd. Silicon oxide-coated soft magnetic powder and method for producing same
CN110181036A (en) * 2019-05-14 2019-08-30 合肥博微田村电气有限公司 A kind of composite soft-magnetic metal powder, preparation method and integrated inductance
CN110405201A (en) * 2019-08-15 2019-11-05 中南大学 A kind of surface graded clad structure of magnetic powder, method for coating and soft-magnetic composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘国忠等: "金属磁粉芯绝缘包覆研究进展", 《磁性材料及器件》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113968730A (en) * 2021-11-11 2022-01-25 横店集团东磁股份有限公司 Z-type ferrite composite material and preparation method and application thereof
CN113968730B (en) * 2021-11-11 2023-01-10 横店集团东磁股份有限公司 Z-type ferrite composite material and preparation method and application thereof
CN114082943A (en) * 2021-11-23 2022-02-25 成都佳驰电子科技股份有限公司 Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system
CN114082943B (en) * 2021-11-23 2024-01-05 成都佳驰电子科技股份有限公司 Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system

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