CN113674979A - Preparation method and material of metal soft magnetic core applied to ultrahigh frequency - Google Patents
Preparation method and material of metal soft magnetic core applied to ultrahigh frequency Download PDFInfo
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/33—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/255—Magnetic cores made from particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/34—Special means for preventing or reducing unwanted electric or magnetic effects, e.g. no-load losses, reactive currents, harmonics, oscillations, leakage fields
Abstract
The invention provides a preparation method of a metal soft magnetic core applied to ultrahigh frequency and a material thereof. According to the invention, the metal magnetic powder is activated by the surface treatment agent through the powder material selection, the magnetic powder with small particle size is preferably selected, a layer of coating layer is formed on the surface of the metal magnetic powder, then the coating agent is coated, and under the activation action of the surface treatment agent, the coating agent can uniformly coat the metal magnetic powder, so that the coating uniformity is higher, the insulation effect of the magnetic powder is improved, the resistivity of the magnetic powder is improved, the loss of the magnetic powder core under the high-frequency condition is effectively reduced, and the problem of the high-frequency use of the material in the 5G communication aspect can be effectively solved.
Description
Technical Field
The invention belongs to the technical field of soft magnetic materials and powder metallurgy, relates to soft magnetic powder, and particularly relates to a preparation method and a material thereof, wherein the preparation method is applied to a metal soft magnetic core under ultrahigh frequency, and the preparation method can be used for improving the insulation effect of the magnetic powder, improving the resistivity of the magnetic powder and effectively reducing the loss of a magnetic powder core under a high-frequency condition.
Background
The metal magnetic powder core is used as one of soft magnetic materials in magnetic materials, has low playing force, low loss and excellent permanent magnetic property, and is widely applied to power electronic equipment. The intelligent power grid power factor correction device is mainly applied to frequency conversion air conditioners, electric vehicle charging mould block power factor correction circuit reactors and rear-stage LC filter reactors, intelligent power grid power quality management, cloud computing center dynamic servers, machine room UPS power factor reactors, photovoltaic power generation grid-connected inverters and the like. Is an important soft magnetic material, and is particularly suitable for the aspect of high-end electronic industry. Recently, electronic devices are developed towards high frequency, large current, high efficiency and high power density, and the performance of metal soft magnetism is just following the development trend.
The main technological process of the metal soft magnetic powder core includes mixing metal soft magnetic powder and insulating material, coating one layer of compact insulating material on the surface of the powder, drying the powder, adding lubricating powder, molding in the mold of a press to form product in required shape, and final sintering in certain atmosphere and temperature condition to eliminate the internal stress in the product, reduce magnetic hysteresis loss, improve product performance and raise product strength to obtain product with excellent comprehensive performance. The surface of the product is coated with a layer of insulating material, so that the surface resistivity of the powder can be improved, and the eddy current among particles can be reduced, thereby reducing the eddy current loss of the magnetic powder core.
With the development of 5G communication, the high frequency use of materials becomes a leading problem in the soft magnetic industry, and the ultrahigh frequency inevitably causes ultrahigh magnetic core loss, so that most of materials can reduce the use efficiency of the whole machine when in use, and the problem of realizing high frequency low loss can only be solved from the materials.
Disclosure of Invention
The invention aims to overcome the defect that the loss of the existing soft magnetic powder is large under the application of ultrahigh frequency, and provides the preparation method of the metal soft magnetic core applied under the ultrahigh frequency, which has the advantages of simple process, low requirement on equipment, improvement on the insulation effect of the magnetic powder, improvement on the resistivity of the magnetic powder and effective reduction of the loss of the magnetic powder core under the high-frequency condition.
The invention also provides the metal soft magnetic core material prepared by the preparation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a metal soft magnetic core applied to ultrahigh frequency is characterized by comprising the following steps:
1) preparing powder: taking Fe-Si-Al magnetic powder, wherein the ratio of the particle size of 5-20 mu m is more than 95%;
2) surface treatment: dissolving a surface treating agent in a solvent to prepare a surface treating solution, adding the surface treating solution into the Fe-Si-Al magnetic powder obtained in the step 1), uniformly stirring, and drying for later use;
3) coating: preparing a coating agent solution; adding the Fe-Si-Al magnetic powder obtained in the step 2) into a coating agent solution, uniformly stirring to form magnetic powder slurry, heating and continuously stirring until the magnetic powder slurry is dried to obtain primary magnetic powder;
4) preparing magnetic powder slurry: adding an adhesive into an organic solvent to prepare an adhesive solution, adding the primary magnetic powder obtained in the step 3) into the adhesive solution to form magnetic powder slurry, heating and continuously stirring until the magnetic powder slurry is dried to obtain intermediate-grade magnetic powder;
5) mixing: adding a release agent into the medium-grade magnetic powder obtained in the step 4) and uniformly mixing to obtain magnetic powder to be molded;
6) and (3) pressing and forming: pressing the magnetic powder to be molded obtained in the step 5) into a magnetic powder core blank;
7) annealing: annealing the magnetic powder core blank obtained in the step 6) to obtain a semi-finished magnetic powder core;
8) and (3) coating epoxy resin on the surface of the semi-finished magnetic powder core obtained in the step (7), and heating and curing to obtain the metal soft magnetic core applied to ultrahigh frequency.
According to the technical scheme, the eddy current loss of the magnetic powder core is large under the high-frequency application condition, so that the traditional metal magnetic powder core cannot be applied to the high-frequency field.
In a preferable embodiment of the present invention, in step 1), the oxygen content of the sendust powder is less than 400 ppm.
In a preferable embodiment of the present invention, in step 2), the surface treatment agent includes at least one of a silane coupling agent, phosphoric acid, aluminum dihydrogen phosphate, or an organoaluminum resin, the solvent is ethanol or methyl acetate, the weight ratio of the surface treatment agent to the solvent is 1/15-1/4, and the addition amount of the surface treatment agent is 0.05-0.5% of the weight of the sendust powder.
As a preferable scheme of the invention, in the step 3), the coating agent comprises one or a mixture of more of phosphoric acid, aluminum dihydrogen phosphate, organic aluminum resin or aluminum phosphate, the solvent is water, the weight ratio of the coating agent to the solvent is 1/20-1/30, and the coating agent solution accounts for 3-10% of the weight of the sendust magnetic powder.
As a preferable scheme of the invention, in the step 4), the adhesive comprises one or a mixture of several of modified epoxy resin, phenolic resin or silicone resin, the weight ratio of the adhesive to the solvent is 1/10-1/3, and the adhesive solution accounts for 3-10% of the weight of the sendust magnetic powder.
In a preferred embodiment of the present invention, in step 5), the release agent is stearic acid amide powder.
In a preferable embodiment of the present invention, in step 6), the pressure for press forming is 18 to 22 tons/cm2。
As a preferred embodiment of the present invention, in step 7), the annealing conditions are: keeping the temperature at 650-750 ℃ for 30-55min under the nitrogen atmosphere.
As a preferable scheme of the invention, in the step 8), the semi-finished magnetic powder core is heated to 180-220 ℃ before the epoxy resin is coated.
On the other hand, the invention provides the metal soft magnetic core material prepared by the preparation method and applied to ultrahigh frequency, thereby improving the insulation effect of magnetic powder, improving the resistivity of the magnetic powder and effectively reducing the loss of the magnetic powder core under the high-frequency condition.
Compared with the prior art, the invention has the following beneficial effects:
1) the preparation method has simple process and low requirement on equipment, and can be used for batch production;
2) the invention adopts the coating process of the surface treating agent and the coating agent, so that the coating uniformity is higher, the solvent is not discharged and wasted, the use effect is good, the cost is low and no pollution is caused;
3) the metal soft magnetic powder core prepared by the preparation method provided by the invention has the advantage that the loss is greatly reduced under a high-frequency condition.
Drawings
FIG. 1 is a diagram of the morphology of the insulated SiFe-Si-Al powder prepared in example 1 of the present invention.
FIG. 2 is a surface topography of a shaped blank made in accordance with example 1 of 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 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.
The Fe-Si-Al powder used in the invention is commercially available ordinary gas atomization powder, wherein the Si-Al powder comprises 7.5-10% of Si, 4-7% of Al and the balance of Fe.
The surface treating agent, the coating agent, the adhesive, the organic solvent, the release agent and the epoxy resin used in the invention can be purchased from the market.
Example 1
The iron-silicon-aluminum powder used in the embodiment contains 7.5-10% of silicon, 4-7% of aluminum and the balance of iron, wherein the powder with the granularity of 5-20 mu m is preferably used as a magnetic powder core raw material, and the oxygen content is within 400 ppm; selecting a silane coupling agent as a surface treatment agent, dissolving the silane coupling agent in ethanol, wherein the weight ratio of a solute to the solvent is 1/4, pouring the uniformly mixed surface treatment agent solution into a container containing magnetic powder after the solution is prepared, wherein the surface treatment agent accounts for 0.2 percent of the weight of the magnetic powder, stirring for about 30min, standing and airing; preparing a coating agent solution, and dissolving aluminum phosphate in water, wherein the coating agent aluminum phosphate accounts for 0.15% of the weight of the magnetic powder, and the ratio of the aluminum phosphate to the water is 1/20; adding a coating agent solution into the surface-treated Fe-Si-Al powder, uniformly stirring to form magnetic powder slurry, heating to 100 ℃, and continuously stirring until the magnetic powder slurry is dried; preparing an adhesive solution, wherein methyl acetate is used as a solvent, the ratio of the adhesive to the solvent is 1/3, and the adhesive is modified epoxy resin; adding an adhesive solution into the coated sendust magnetic powder, wherein the adhesive accounts for 3.5% of the weight of the magnetic powder, uniformly stirring the magnetic powder to form magnetic powder slurry, heating the slurry to 80 ℃, preserving heat, and stirring until the magnetic powder slurry is dried; adding a release agent stearic acid amide accounting for 0.4 percent of the weight of the coated magnetic powder and 0.1 percent of nano silicon dioxide powder (for adjusting inductance) into the insulated and coated magnetic powder, and uniformly mixing; preparing magnetic powder to be molded into magnetic powder core blank by a press, wherein the pressure of the press is 20 tons/cm2(ii) a Taking nitrogen as protective atmosphere, and placing the magnetic powder core blank in an environment of 725 ℃ for heat preservation for 30min to prepare a semi-finished magnetic powder core; baking the magnetic powder core to 200 ℃, performing electrostatic spraying on epoxy resin powder, then heating the resin for curing, and performing winding test.
The appearance of the powder after the iron-silicon-aluminum insulation is shown in figure 1, and the surface appearance of the formed blank is shown in figure 2.
Example 2, the only difference from example 1 is that the capping agent is an organoaluminum resin.
Example 3, the only difference from example 1 is that the coating agent is aluminum dihydrogen phosphate.
The metallic soft magnetic core windings obtained in examples 1-3 were tested and the results are shown in table 1.
TABLE 1 test results
Example 4
The iron-silicon-aluminum powder used in the embodiment contains 7.5-10% of silicon, 4-7% of aluminum and the balance of iron, wherein the powder with the granularity of 5-20 mu m is preferably used as a magnetic powder core raw material, and the oxygen content is within 400 ppm; selecting a silane coupling agent as a surface treatment agent, dissolving the silane coupling agent in ethanol, wherein the weight ratio of a solute to the solvent is 1/15, pouring the uniformly mixed surface treatment agent solution into a container containing magnetic powder after the solution is prepared, wherein the coating agent accounts for 0.2 percent of the weight of the magnetic powder, stirring for about 30min, standing and airing; preparing a coating agent solution, and dissolving aluminum phosphate in water, wherein the coating agent aluminum phosphate accounts for 0.2% of the weight of the magnetic powder, and the ratio of the aluminum phosphate to the water is 1/20; adding a coating agent solution into the surface-treated Fe-Si-Al powder, uniformly stirring to form magnetic powder slurry, heating to 100 ℃, and continuously stirring until the magnetic powder slurry is dried; preparing an adhesive agent solution, wherein ethanol or methyl acetate is used as a solvent, the ratio of the adhesive to the solvent is 1/10, and the adhesive is modified epoxy resin; adding an adhesive solution into the coated sendust magnetic powder, wherein the adhesive accounts for 3.5% of the weight of the magnetic powder, uniformly stirring the magnetic powder to form magnetic powder slurry, heating the slurry to 80 ℃, preserving heat, and stirring until the magnetic powder slurry is dried; adding a release agent stearic acid amide accounting for 0.4 percent of the weight of the coated magnetic powder, 0.1 percent of nano silicon dioxide powder (for regulating inductance) and 0.2 percent of kaolin powder (for regulating inductance) into the insulated and coated magnetic powder, and uniformly mixing; preparing magnetic powder to be molded into magnetic powder core blank by a press, wherein the pressure of the press is 20 tons/cm2(ii) a Taking nitrogen as protective atmosphere, and placing the magnetic powder core blank in an environment of 725 ℃ for heat preservation for 30min to prepare a semi-finished magnetic powder core; magnetic fieldBaking the powder core to 200 ℃, performing electrostatic spraying on epoxy resin powder, then heating the resin for curing, and performing winding test;
example 5, the only difference from example 4 is that the surface treating agent is an organoaluminum resin.
Example 6, the only difference from example 4 is that the surface treatment agent is aluminum dihydrogen phosphate.
The metallic soft magnetic core windings obtained in examples 4-6 were tested and the results are shown in table 2.
TABLE 2 test results
According to the invention, the metal magnetic powder is activated by the surface treatment agent through the powder material selection, the magnetic powder with small particle size is preferably selected, a layer of coating layer is formed on the surface of the metal magnetic powder, then the coating agent is coated, and under the activation action of the surface treatment agent, the coating agent can uniformly coat the metal magnetic powder, so that the coating uniformity is higher, the insulation effect of the magnetic powder is improved, the resistivity of the magnetic powder is improved, the loss of the magnetic powder core under the high-frequency condition is effectively reduced, and the problem of the high-frequency use of the material in the 5G communication aspect can be effectively solved.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a metal soft magnetic core applied to ultrahigh frequency is characterized by comprising the following steps:
1) preparing powder: taking Fe-Si-Al magnetic powder, wherein the ratio of the particle size of 5-20 mu m is more than 95%;
2) surface treatment: dissolving a surface treating agent in a solvent to prepare a surface treating solution, adding the surface treating solution into the Fe-Si-Al magnetic powder obtained in the step 1), uniformly stirring, and drying for later use;
3) coating: preparing a coating agent solution; adding the Fe-Si-Al magnetic powder obtained in the step 2) into a coating agent solution, uniformly stirring to form magnetic powder slurry, heating and continuously stirring until the magnetic powder slurry is dried to obtain primary magnetic powder;
4) preparing magnetic powder slurry: adding an adhesive into an organic solvent to prepare an adhesive solution, adding the primary magnetic powder obtained in the step 3) into the adhesive solution to form magnetic powder slurry, heating and continuously stirring until the magnetic powder slurry is dried to obtain intermediate-grade magnetic powder;
5) mixing: adding a release agent into the medium-grade magnetic powder obtained in the step 4) and uniformly mixing to obtain magnetic powder to be molded;
6) and (3) pressing and forming: pressing the magnetic powder to be molded obtained in the step 5) into a magnetic powder core blank;
7) annealing: annealing the magnetic powder core blank obtained in the step 6) to obtain a semi-finished magnetic powder core;
8) and (3) coating epoxy resin on the surface of the semi-finished magnetic powder core obtained in the step (7), and heating and curing to obtain the metal soft magnetic core applied to ultrahigh frequency.
2. The method for preparing a metal soft magnetic core applied to ultrahigh frequency according to claim 1, wherein in the step 1), the oxygen content of the sendust powder is less than 400 ppm.
3. The method of claim 1, wherein in the step 2), the surface treatment agent comprises at least one of a silane coupling agent, phosphoric acid, aluminum dihydrogen phosphate or an organic aluminum resin, the solvent is ethanol or methyl acetate, the weight ratio of the surface treatment agent to the solvent is 1/15-1/4, and the addition amount of the surface treatment agent is 0.05-0.5% of the weight of the sendust powder.
4. The method as claimed in claim 1, wherein in the step 3), the coating agent comprises one or more of phosphoric acid, aluminum dihydrogen phosphate, organic aluminum resin or aluminum phosphate, the solvent is water, the weight ratio of the coating agent to the solvent is 1/20-1/30, and the coating agent solution accounts for 3-10% of the weight of the sendust powder.
5. The method for preparing a metal soft magnetic core applied to ultrahigh frequency according to claim 1, wherein in the step 4), the adhesive comprises one or a mixture of several of modified epoxy resin, phenolic resin or silicone resin, the weight ratio of the adhesive to the solvent is 1/10-1/3, and the adhesive solution accounts for 3-10% of the weight of the sendust.
6. The method for preparing a metallic soft magnetic core for use at ultrahigh frequencies according to claim 1, wherein in step 5), the release agent comprises zinc stearate, calcium stearate, stearic acid amide, EBS wax or polyvinyl ether.
7. The method for preparing a metallic soft magnetic core for use at ultra-high frequencies according to claim 1, wherein the pressure for the press-forming in step 6) is 18 to 22 tons/cm2。
8. The method for preparing a metallic soft magnetic core applied to ultra-high frequencies according to claim 1, wherein in the step 7), the annealing conditions are as follows: keeping the temperature at 650-750 ℃ for 30-55min under the nitrogen atmosphere.
9. The method as claimed in claim 1, wherein the semi-finished magnetic powder core is heated to 180-220 ℃ before the epoxy resin is coated in step 8).
10. A metallic soft magnetic core material for use at ultra-high frequencies, characterized in that it is produced by the production method according to any one of claims 1 to 9.
Priority Applications (1)
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