CN113223845B - Insulating coating method of soft magnetic alloy powder - Google Patents
Insulating coating method of soft magnetic alloy powder Download PDFInfo
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Abstract
The invention discloses an insulation coating method of soft magnetic alloy powder, which comprises the following steps: step S1, mixing powder: doping soft magnetic ferrite fine powder into the soft magnetic alloy powder, and fully and uniformly mixing; step S2, powder heat treatment: carrying out heat treatment on the mixed powder to obtain first mixed powder; and step S3, passivation treatment: mixing the first mixed powder with a passivating agent solution, stirring for full reaction, and cleaning and drying to obtain second mixed powder; step S4, preparing ferrite fine powder dispersion liquid: completely dissolving the binder and the lubricant in acetone, doping the soft magnetic ferrite fine powder into the acetone solution, and uniformly dispersing the mixture in the solution; and S5, insulating and coating. The beneficial effects of this technical scheme lie in: the soft magnetic ferrite micro powder with proper amount is uniformly doped in the surface passivation layer and the insulating coating layer of the soft magnetic alloy powder, so that the magnetic conductivity of the magnetic part formed by pressing is obviously improved, lower iron loss is realized, and the overall performance of the product is improved.
Description
Technical Field
The invention relates to the field of magnetic materials, in particular to an insulating coating method of soft magnetic alloy 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, is applied to the power electronic technology, has the advantages of small volume, high efficiency, energy conservation and the like, and has the best cost performance.
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 adhesive 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 and coating 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 application of the prior art, the powder is generally subjected to simple passivation treatment by using an acidic solution for powder insulation coating, and then the powder is subjected to insulation coating by adding a binder. For example, the prior application CN201710167796.3 discloses an iron-based magnetic powder insulation coating method, the prior application CN201910400535.0 discloses a composite soft magnetic metal powder, a preparation method and an integrally formed inductor, the prior application CN201410230330.x discloses a nanocrystalline soft magnetic composite material and a preparation method thereof, the prior application CN201310134332.4 discloses a preparation method of a mu 90 high-permeability Fe-based amorphous magnetic powder core, the prior applications all adopt the process, and the process sacrifices the soft magnetic property of the powder while improving the insulation property of the soft magnetic powder; the insulating coating layer is a non-magnetic substance, and reduces the magnetic conductivity and the magnetic flux density of the magnetic powder core, so that in order to solve the problems, an insulating coating method of the soft magnetic alloy powder is urgently needed to be designed so as to meet the requirement of practical use.
Disclosure of Invention
In view of the above problems in the prior art, a method for insulating and coating a soft magnetic alloy powder is provided, which can prepare a soft magnetic powder material with high magnetic permeability.
The specific technical scheme is as follows:
an insulation coating method of soft magnetic alloy powder is characterized in that a proper amount of soft magnetic ferrite fine powder is doped in two stages of surface passivation and insulation coating of the soft magnetic alloy powder to obtain the soft magnetic alloy powder uniformly doped with the soft magnetic ferrite fine powder in a surface passivation layer and an insulation coating layer, so that the purpose of improving the magnetic conductivity of a magnetic part formed by pressing the soft magnetic alloy powder is achieved, and the method comprises the following steps of:
step S1, mixing powder: screening soft magnetic alloy powder with a preset particle size, doping soft magnetic ferrite micro powder into the screened soft magnetic alloy powder, and fully and uniformly mixing the soft magnetic alloy powder and the soft magnetic ferrite micro powder to obtain mixed powder;
step S2, powder heat treatment: carrying out heat treatment on the mixed powder to obtain a first mixed powder;
and step S3, passivation treatment: mixing the first mixed powder subjected to the heat treatment in the step S2 with a passivating agent solution, stirring to enable the first mixed powder to fully react with the passivating agent solution, and then cleaning and drying to obtain a second mixed powder;
step S4, preparing ferrite fine powder dispersion liquid: 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 ferrite fine powder dispersion liquid;
step S5, insulating and coating: and (4) uniformly mixing the ferrite fine powder dispersion liquid obtained in the step (S4) with the second mixed powder obtained in the step (S3), stirring to obtain composite soft magnetic slurry, stirring, kneading and granulating the composite soft magnetic slurry on a granulating device, and drying in an oven to obtain the insulated and coated soft magnetic alloy powder.
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 alloy powder, and iron-nickel-aluminum alloy powder.
Preferably, in the step S1, the predetermined particle size of the soft magnetic alloy powder is less than 100 μm.
Preferably, in the step S1, the content of the soft magnetic ferrite fine powder is 0.2 to 3% of the total weight of the soft magnetic alloy powder.
Preferably, in step S1, the soft magnetic alloy powder and the soft magnetic ferrite fine powder are fully and uniformly mixed by using a powder ball mill or a mixer.
Preferably, the particle size of the soft magnetic ferrite fine powder is less than 1 μm in both the step S1 and the step S4.
Preferably, in step S3, the passivating agent solution is phosphoric acid.
Preferably, in the step S4, the content of the binder is 1% -5% of the total mass of the second mixed powder;
the content of the lubricant is 0.5 to 1 percent of the total mass of the second mixed powder;
the content of the soft magnetic ferrite fine powder is 0.5-5% of the total mass of the second mixed powder.
Preferably, in step S4, the binder is at least one of epoxy resin, polyurethane, silicone resin, amino resin, polyimide, phenolic resin, cyanate ester, and acrylic resin.
Preferably, in the step S4, the lubricant is at least one of zinc stearate, magnesium stearate, aluminum stearate, calcium stearate, graphite powder, and graphene.
Compared with the prior art, the technical scheme has the beneficial effects that:
according to the invention, soft magnetic ferrite micro powder is doped in the surface passivation and insulation coating processes of the soft magnetic alloy powder, on one hand, because the ferrite resistivity is higher, particularly for a magnetic component used in a high frequency band, the eddy current loss can be effectively reduced, so that the iron loss is reduced; on the other hand, the ferrite has higher high-frequency magnetic conductivity, the magnetic conductivity of the magnetic component formed by pressing the soft magnetic powder coated by the method of the invention is improved by more than 30 percent, and simultaneously, the low high-frequency loss is kept, thereby being very beneficial to the high-frequency and miniaturization of the inductance device and leading the inductance device at the rear end thereof to have more excellent performance and wider application prospect.
Drawings
FIG. 1 is a schematic flow chart of a method for insulation coating of soft magnetic alloy powder according to the present invention.
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 insulating coating method of soft magnetic alloy powder, which belongs to the field of magnetic materials and comprises the following steps as shown in figure 1:
step S1, mixing powder materials: screening soft magnetic alloy powder with a preset particle size, wherein the preset particle size of the soft magnetic alloy powder is smaller than 100 microns, weighing a proper amount of soft magnetic ferrite micro powder, wherein the content of the soft magnetic ferrite micro powder is 0.2% -3% of the total mass of the soft magnetic alloy powder obtained by screening, then doping the weighed soft magnetic ferrite micro powder into the soft magnetic alloy powder, and fully and uniformly mixing the soft magnetic alloy powder and the soft magnetic ferrite micro powder through a powder ball mill to obtain mixed powder;
step S2, powder heat treatment: carrying out heat treatment on the powder mixed in the step S1 through a vacuum heat treatment furnace to obtain a first mixed powder, wherein the heat treatment temperature is 300-580 ℃, and the heat treatment time is 0.5-2h;
step S3, passivation treatment: stirring the first mixed powder subjected to the heat treatment in the step S2 and a passivating agent solution for more than 30min so as to fully mix and react the first mixed powder and the passivating agent solution, and then cleaning and drying to obtain second mixed powder;
step S4, preparing ferrite fine powder dispersion liquid: respectively weighing a binder and a lubricant, wherein the mass of the binder is 1% -5% of the total mass of the second mixed powder in the step S3, the mass of the lubricant is 0.5% -1% of the total mass of the second mixed powder in the step S3, then completely dissolving the binder and the lubricant in acetone to form an acetone solution, weighing a proper amount of soft magnetic ferrite fine powder, preferably, the content of the soft magnetic ferrite fine powder is 0.5% -5% of the total mass of the second mixed powder, doping the weighed 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 ferrite fine powder dispersion liquid;
s5, insulating and coating: and (3) uniformly mixing the ferrite fine powder dispersion liquid obtained in the step (S4) with the second mixed powder obtained in the step (S3), stirring for more than 30min to obtain composite soft magnetic slurry, then stirring, kneading and granulating the composite soft magnetic slurry on a granulating device, and drying in a vacuum oven to obtain the insulated and coated soft magnetic alloy powder.
In the powder mixing stage, the soft magnetic alloy powder and a proper amount of soft magnetic ferrite micro powder are fully and uniformly mixed, so that the soft magnetic alloy powder uniformly doped with the soft magnetic ferrite micro powder in a surface passivation layer is obtained in the subsequent passivation treatment stage; doping a proper amount of soft magnetic ferrite fine powder again in the stage of preparing the ferrite fine powder dispersion liquid, and fully and uniformly mixing the soft magnetic ferrite fine powder with an acetone solution so as to obtain soft magnetic alloy powder uniformly doped with the soft magnetic ferrite fine powder in the insulating coating layer in the subsequent insulating coating stage;
by adopting the technical scheme, the soft magnetic alloy powder uniformly doped with the soft magnetic ferrite fine powder in the surface passivation layer and the insulating coating layer is obtained by respectively doping the soft magnetic ferrite fine powder with a proper amount twice so as to improve the magnetic conductivity of the magnetic part formed by pressing the soft magnetic alloy powder.
The first embodiment is as follows:
in the embodiment, the soft magnetic alloy powder material is Fe-Si-B-C-Cr amorphous soft magnetic alloy powder with the particle size of 7-13 microns, wherein the median particle size D is 50-10 microns; the ferrite fine powder is Mn-Zn soft magnetic ferrite powder, and the median particle size D50 is about 750nm; the insulation coating method comprises the following steps:
step S1, mixing powder materials: selecting an ultrasonic vibration screen to screen Fe-Si-B-C-Cr amorphous soft magnetic alloy powder with a proper particle size, weighing Mn-Zn soft magnetic ferrite micro powder according to 1% of the total mass of the Fe-Si-B-C-Cr amorphous soft magnetic alloy powder, and putting the Fe-Si-B-C-Cr amorphous soft magnetic alloy powder and the Mn-Zn soft magnetic ferrite micro powder into a powder ball mill for fully and uniformly mixing to obtain mixed powder of the Mn-Zn soft magnetic ferrite micro powder and the Fe-Si-B-C-Cr amorphous soft magnetic alloy powder;
step S2, powder heat treatment: placing the powder subjected to ball milling and mixing in the step S1 into a vacuum heat treatment furnace, and carrying out heat treatment for 1h at 350 ℃ to obtain first mixed powder;
step S3, passivation treatment: mixing the first mixed powder subjected to the heat treatment in the step S2 with a phosphoric acid solution, stirring for more than 30min to enable the first mixed powder to fully react with the phosphoric acid solution, and then cleaning and drying to obtain second mixed powder;
step S4, preparing ferrite micro powder dispersion liquid: respectively weighing a binder and a lubricant according to 3% and 0.8% of the total mass of the second mixed powder in the step S3, weighing Mn-Zn soft magnetic ferrite fine powder according to 1% of the total mass of the second mixed powder, completely dissolving the binder and the lubricant in acetone to form an acetone solution, doping the Mn-Zn soft magnetic ferrite fine powder into the acetone solution, and uniformly dispersing the Mn-Zn soft magnetic ferrite fine powder into the acetone solution to obtain Mn-Zn soft magnetic ferrite fine powder dispersion liquid;
s5, insulating and coating: and (3) uniformly mixing the Mn-Zn soft magnetic ferrite micro-fine powder dispersion liquid obtained in the step (S4) with the second mixed powder obtained in the step (S3), stirring for more than 30min to obtain composite soft magnetic slurry, then stirring, kneading and granulating the composite soft magnetic slurry on a granulating device, drying for more than 1h in a vacuum oven at 80 ℃, screening the powder with the particle size of-80 meshes to +200 meshes by using an ultrasonic vibration sieve, and thus obtaining the composite soft magnetic powder material with the good insulation coating.
The 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, wherein preferably, the outer diameter of the annular die is 20mm, and the inner diameter of the annular die is 12mm; ultrasonic vibration is applied in the cold pressing process, the vibration frequency is 20KHz, and the pressure maintaining pressure is 6t/cm 2 Keeping the pressure for 60s, and demolding to obtain a magnetic ring blank;
and step A2, placing the magnetic ring blank in a vacuum oven at 180 ℃, keeping the temperature 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.
Step A3, testing the main magnetic property: winding 15 turns of enameled copper wires on the cured magnetic ring component prepared in the step A3, testing the inductance of the cured magnetic ring component through an impedance analyzer under the test condition of 1MHz, and calculating to obtain the magnetic conductivity mu' according to the inductance; the loss value is tested by a B-H analyzer under the test condition of 1MHz/20mT.
Table 1 performance parameters of amorphous magnetic rings prepared in example one and comparative examples one to two
In table 1 above, 1 represents that Mn — Zn ferrite was added in the corresponding step, and the addition amount was 1% of the total mass of the first soft magnetic powder obtained in step S1; 0 indicates 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 which is prepared and well coated in an insulating way, the magnetic permeability mu' of the magnetic component under the condition of 1MHz is measured to be 26 by an impedance analyzer; the loss Pcv measured by a B-H analyzer under the condition of 1MHz/20mT is 815kW/m 3 。
The first comparative example adopts the same preparation process and parameters as the first example, and is only different in that fine powder of the Mn-Zn soft magnetic ferrite is not added in the step S4, and the magnetic permeability mu' of the magnetic ring component finally prepared in the first comparative example is 24.5; the loss Pcv is 820kW/m 3 。
In the second comparative example, the same preparation process and parameters as those in the first example are adopted, and the difference is that Mn-Zn soft magnetic ferrite fine powder is not added in the whole preparation process, and the magnetic permeability mu' of the magnetic ring part finally prepared in the second comparative example is 20.1; the loss Pcv is 830kW/m 3 。
Example two:
in the embodiment, the soft magnetic alloy powder is Fe-Si-B-Cu-Nb nanocrystalline soft magnetic alloy powder, the grain diameter is 5-20 μm, and the median grain diameter D50 is about 10 μm; the ferrite fine powder is Mn-Zn soft magnetic ferrite powder, and the median grain diameter D50 is about 750nm.
The same addition amount of Mn-Zn soft magnetic ferrite fine powder, the same binder and lubricant, and the same binder and lubricant ratio as those in the first embodiment were selected, the preparation process of the insulated coated soft magnetic alloy powder and the preparation process and parameters of the magnetic ring blank obtained in the present embodiment are the same as those in the first embodiment, and the performance parameters of the magnetic ring components are shown in table 2.
TABLE 2 Properties of nanocrystalline magnet rings obtained in example two and comparative examples three-four
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 34 by an impedance analyzer; the loss Pcv measured by a B-H analyzer under the condition of 1MHz/20mT is 480kW/m 3 。
Comparative example III and implementationThe second embodiment adopts the same soft magnetic alloy powder, the same binder and lubricant ratio, and the other preparation processes and parameters are the same as those of the second embodiment, except that the Mn-Zn soft magnetic ferrite fine powder is removed in the step S4, and the magnetic permeability mu' of the finally prepared magnetic ring component under the same test condition is 30; the loss Pcv under the condition of 1MHz/20mT is 483kW/m measured by a B-H analyzer 3 。
The fourth comparative example and the second example adopt the same soft magnetic alloy powder, the same binder and lubricant ratio, and the other preparation processes and parameters are the same as those of the second example, except that Mn-Zn soft magnetic ferrite fine powder is not added in the whole preparation process, and the magnetic permeability mu' of the finally prepared magnetic ring component is 26; the loss Pcv measured by a B-H analyzer was 490kW/m under the condition of 1MHz/20mT 3 。
As can be seen from tables 1 and 2 above: the soft magnetic powder is added with the soft magnetic ferrite micro powder in two stages of surface passivation and insulation coating, so that on one hand, the eddy current path among ferromagnetic particles can be effectively blocked, the magnetic field among the ferromagnetic particles can be well coupled, the eddy current loss is effectively reduced, and the iron loss is reduced; on the other hand, the ferrite has higher magnetic conductivity, the magnetic conductivity of the magnetic part formed by pressing the soft magnetic powder is improved to more than 30%, and meanwhile, lower high-frequency loss is kept, so that the high-frequency and miniaturization of the inductance device are greatly facilitated, and the inductance device at the rear end of the inductance device has wide application prospect.
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 for insulating and coating soft magnetic alloy powder is characterized by comprising the following steps:
step S1, mixing powder: screening soft magnetic alloy powder with a preset particle size, doping soft magnetic ferrite micro powder into the screened soft magnetic alloy powder, and fully and uniformly mixing the soft magnetic alloy powder and the soft magnetic ferrite micro powder to obtain mixed powder;
step S2, powder heat treatment: carrying out heat treatment on the mixed powder to obtain a first mixed powder;
and step S3, passivation treatment: mixing the first mixed powder subjected to the heat treatment in the step S2 with a passivating agent solution, stirring to enable the first mixed powder to fully react with the passivating agent solution, and then cleaning and drying to obtain a second mixed powder;
step S4, preparing ferrite fine powder dispersion liquid: 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 ferrite fine powder dispersion liquid;
step S5, insulating coating: and (4) uniformly mixing the ferrite fine powder dispersion liquid obtained in the step (S4) with the second mixed powder obtained in the step (S3), stirring to obtain composite soft magnetic slurry, stirring, kneading and granulating the composite soft magnetic slurry on a granulating device, and drying in an oven to obtain the insulated and coated soft magnetic alloy powder.
2. The method of claim 1, wherein 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-nickel alloy powder, and carbonyl iron powder.
3. The method for insulation coating of soft magnetic alloy powder as claimed in claim 1, wherein the predetermined grain size of the soft magnetic alloy powder in step S1 is less than 100 μm.
4. The method for insulation-coating of soft magnetic alloy powder as claimed in claim 1, wherein in step S1, the content of the soft magnetic ferrite fine powder is 0.2-3% of the total weight of the soft magnetic alloy powder.
5. The insulation coating method for the soft magnetic alloy powder according to claim 1, wherein in the step S1, the soft magnetic alloy powder and the soft magnetic ferrite fine powder are fully and uniformly mixed by using a ball mill or a mixer.
6. The method for insulation-coating a powder of a soft magnetic alloy as recited in claim 1, wherein the particle size of the fine powder of the soft magnetic ferrite is less than 1 μm in each of the step S1 and the step S4.
7. The method for insulation coating of soft magnetic alloy powder as claimed in claim 1, wherein in step S3, the passivating agent solution is phosphoric acid.
8. The method for insulation coating of soft magnetic alloy powder according to claim 1, wherein in step S4, the content of the binder is 1% -5% of the total mass of the second mixed powder;
the content of the lubricant is 0.5-1% of the total mass of the second mixed powder;
the content of the soft magnetic ferrite fine powder is 0.5-5% of the total mass of the second mixed powder.
9. The method for insulation-coating of a soft magnetic alloy powder according to claim 1, wherein in step S4, the binder is at least one of epoxy resin, polyurethane, silicone resin, amino resin, polyimide, phenolic resin, cyanate resin, and acrylic resin.
10. The method for insulation coating of soft magnetic alloy powder as claimed in claim 1, wherein in step S4, the lubricant is at least one of zinc stearate, magnesium stearate, aluminum stearate, calcium stearate, graphite powder and graphene.
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| CN113223845A (en) | 2021-08-06 |
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