CN110957123A - Method for preparing iron-nickel soft magnetic powder core with magnetic conductivity of 125 - Google Patents
Method for preparing iron-nickel soft magnetic powder core with magnetic conductivity of 125 Download PDFInfo
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- CN110957123A CN110957123A CN201911297670.3A CN201911297670A CN110957123A CN 110957123 A CN110957123 A CN 110957123A CN 201911297670 A CN201911297670 A CN 201911297670A CN 110957123 A CN110957123 A CN 110957123A
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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
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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
Abstract
The invention belongs to the technical field of soft magnetic materials, and particularly relates to a preparation method of an iron-nickel soft magnetic powder core with the magnetic conductivity of 125, which comprises the steps of iron-nickel powder preparation, insulation coating, press forming, heat treatment and surface coating; the iron-nickel powder preparation method comprises the following steps of screening iron-nickel powder into three particle sizes of less than 60 mu m, more than or equal to 60 mu m, less than 125 mu m and more than or equal to 125 mu m according to a proportion of 40%: 30%: mixing at a ratio of 30%. The invention adopts gas atomization iron-nickel powder, and prepares the iron-nickel metal soft magnetic powder core with the magnetic permeability of 125 through the procedures of granularity proportioning, insulation coating, press forming, surface spraying and the like.
Description
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to a preparation method of an iron-nickel soft magnetic powder core with the magnetic conductivity of 125.
Background
The metal soft magnetic powder core has high saturation magnetic flux density, high effective magnetic permeability and good magnetic property stability, and is widely applied to the fields of communication, computers, household appliances, transformers, inverters, new energy automobiles and the like. Among them, iron and nickel have the highest DC bias performance, high saturation magnetic induction and low loss, so it has great market application.
Reference patent:
soft magnetic materials of iron-nickel alloys having a permeability of 125 and a method for producing the same are disclosed in application No. 201110133772.9.
Soft magnetic materials of iron-nickel-molybdenum alloys having a permeability of 125 and a method for producing the same are disclosed in application No. 201110130045.7.
A high-magnetic-permeability Ni-Zn soft magnetic ferrite material and its preparing process are disclosed in application No. 201410803723.5.
Disclosure of Invention
The invention aims to provide a preparation method of an iron-nickel soft magnetic powder core with the magnetic conductivity of 125, and the iron-nickel soft magnetic core prepared by the method has low loss and good direct current bias performance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of an iron-nickel soft magnetic powder core with 125 magnetic conductivity comprises the steps of iron-nickel powder preparation, insulation coating, compression molding, heat treatment and surface coating; the method is characterized in that: the iron-nickel powder preparation method comprises the following steps of screening iron-nickel powder into three particle sizes of less than 60 mu m, more than or equal to 60 mu m, less than 125 mu m and more than or equal to 125 mu m according to a proportion of 40%: 30%: mixing at a ratio of 30%.
Further, the iron-nickel powder is gas atomized iron-nickel powder.
Further, the content of nickel in the iron-nickel powder is 40% -60%, and the balance is iron.
Further, the insulation coating is formed by forming a silicon oxide coating layer on the surface of the iron-nickel powder by a sol-gel method for insulation.
Further, the insulation coating by the sol-gel method specifically comprises the following steps: adding a silica sol aqueous solution into the uniformly mixed iron-nickel powder, heating, frying, then mixing kaolin into the mixture, and adding a water glass solution, heating, frying and drying; wherein the dosage of the silica sol is 0.3-0.8% of the weight of the iron-nickel powder, the dosage of the kaolin is 0.2-0.5% of the weight of the iron-nickel powder, the dosage of the water glass is 0.2-0.5% of the weight of the iron-nickel powder, and the temperature is controlled below 100 ℃.
Further, the press forming: and adding a release agent into the insulated powder, and performing compression molding, wherein the molding pressure is 16-21 tons/square centimeter.
Furthermore, microcrystalline wax is selected as the release agent, and the dosage of the microcrystalline wax is 0.1-0.3% of the weight of the iron-nickel powder.
Further, the heat treatment: and (3) putting the pressed and formed magnetic core into a mixed atmosphere of nitrogen and hydrogen for sintering, wherein the ratio of the nitrogen to the hydrogen is 1:3, the sintering temperature is 650-850 ℃, and the heat preservation time is 30-120 min.
Further, the surface coating: and the surface of the magnetic core is spin-coated by adopting epoxy resin powder.
The invention has the beneficial effects that:
(1) the invention adopts gas atomization iron-nickel powder, and prepares the iron-nickel metal soft magnetic powder core with the magnetic permeability of 125 through the procedures of granularity proportioning, insulation coating, press forming, surface spraying and the like.
(2) The invention adopts three kinds of powder with different grain diameters for grain grading, can effectively improve the magnetic permeability, improve the density of the magnetic core and simultaneously reduce the porosity of the magnetic core.
(3) The invention adopts the sol-gel method for insulation, so that the surface of the iron-nickel metal powder is provided with the silicon oxide coating layer, and the iron-nickel magnetic powder has the advantages of higher thermal stability, electrical insulation and the like, so that the loss of the prepared iron-nickel magnetic powder core is lower.
(4) The preparation process is simple, the preparation process is energy-saving and environment-friendly, the prepared product has excellent performance, high magnetic permeability, high direct current bias performance and low power loss, and the product performance is in the leading level of the industry.
Detailed Description
In order to better understand the present invention, the following embodiments are further described.
A preparation method of an iron-nickel soft magnetic powder core with 125 magnetic conductivity comprises the following steps:
s1, iron-nickel powder preparation: sieving gas atomized iron-nickel powder (wherein the content of nickel is 40-60%, and the balance is iron, or the iron and the nickel respectively account for 50%) into three particle sizes of less than 60 mu m, more than or equal to 60 mu m, less than 125 mu m and more than or equal to 125 mu m according to a proportion of 40%: 30%: mixing at a ratio of 30%.
S2, insulating and coating: forming a silicon oxide coating layer on the surface of the iron-nickel powder by adopting a sol-gel method for insulation, and specifically comprising the following steps: adding a silica sol aqueous solution into the uniformly mixed iron-nickel powder, heating, frying, then mixing kaolin into the mixture, and adding a water glass solution, heating, frying and drying; wherein the amount of the silica sol is 0.3-0.8 wt% of the iron-nickel powder, the amount of the kaolin is 0.2-0.5 wt% of the iron-nickel powder, and the amount of the water glass is 0.2-E
0.5%, and the temperature should be controlled below 100 deg.C during insulation.
S3, press forming: adding a release agent into the insulated powder, and performing compression molding, wherein the molding pressure is 16-21 tons/square centimeter; the release agent is microcrystalline wax, and the dosage of the microcrystalline wax is 0.1-0.3% of the weight of the iron-nickel powder. Because the microcrystalline wax has better demoulding effect and less dosage than the traditional stearate, and the microcrystalline wax can reduce the loss of the magnetic core.
S4, heat treatment: and (3) putting the pressed and formed magnetic core into a mixed atmosphere of nitrogen and hydrogen for sintering, wherein the ratio of the nitrogen to the hydrogen is 1:3, the sintering temperature is 650-850 ℃, and the heat preservation time is 30-120 min. Wherein the nitrogen plays a role in protection, and the hydrogen plays a role in reduction.
S5, surface coating: and the surface of the magnetic core is spin-coated by adopting epoxy resin powder.
Example 1
Taking gas atomization iron-nickel powder, wherein the content of nickel is 50%, dividing the powder into three particle sizes of less than 60 μm, more than or equal to 60 μm, less than 125 μm and more than or equal to 125 μm by using a vibrating screen, and then adopting the particle sizes of-60 μm: 60-125 μm: +/-125 μm ═ 40%: 30%: mixing at a ratio of 30%.
Then adding the silica sol aqueous solution into the iron-nickel powder, heating to 90 ℃, roasting to dry, and cooling; adding kaolin, drying, mixing, adding water glass solution, heating to 90 deg.C, and parching to dry. The dosage of the silica sol is 0.4 percent of the weight of the iron-nickel powder, the dosage of the kaolin is 0.4 percent of the weight of the iron-nickel powder, the dosage of the water glass is 0.2 percent of the weight of the iron-nickel powder, and the temperature during insulation is controlled below 100 ℃.
Microcrystalline wax accounting for 0.2 percent of the weight of the iron-nickel powder is added as a release agent before compression molding, and the mixture is uniformly mixed and then compressed into a magnetic ring with the thickness of 26.9mm by 14.8mm by 11.1mm, and the molding pressure is 17 tons/square centimeter.
Placing the molded magnetic core into a heat treatment furnace, introducing nitrogen, introducing hydrogen after 10min, preserving heat at 750 ℃ for 50min, and naturally cooling, wherein the ratio of nitrogen to hydrogen is about 1: 3; and spin-coating epoxy resin powder on the surface of the magnetic ring, and curing to obtain the iron-nickel soft magnetic powder core with the magnetic conductivity of 125. The magnetic properties of the obtained iron-nickel magnetic powder core are shown in table 1.
Example 2
Taking gas atomization iron-nickel powder, wherein the content of nickel is 50%, dividing the powder into three particle sizes of less than 60 μm, more than or equal to 60 μm, less than 125 μm and more than or equal to 125 μm by using a vibrating screen, and then adopting the particle sizes of-60 μm: 60-125 μm: +/-125 μm ═ 40%: 30%: mixing at a ratio of 30%.
Then adding the silica sol water solution into the iron-nickel powder, heating to 80 ℃, roasting to dry, and cooling; adding kaolin, drying, mixing, adding water glass solution, heating to 80 deg.C, and parching to dry. The dosage of the silica sol is 0.3 percent of the weight of the iron-nickel powder, the dosage of the kaolin is 0.3 percent of the weight of the iron-nickel powder, the dosage of the water glass is 0.3 percent of the weight of the iron-nickel powder, and the temperature during insulation is controlled below 100 ℃.
Microcrystalline wax accounting for 0.3 percent of the weight of the iron-nickel powder is added as a release agent before compression molding, and the mixture is uniformly mixed and then compressed into a magnetic ring with the thickness of 26.9mm by 14.8mm by 11.1mm, wherein the molding pressure is 18 tons/square centimeter.
Placing the formed magnetic core into a heat treatment furnace, introducing nitrogen, introducing hydrogen after 10min, preserving heat at 780 ℃ for 40min, and naturally cooling, wherein the ratio of nitrogen to hydrogen is about 1: 3; and spin-coating epoxy resin powder on the surface of the magnetic core, and curing to obtain the iron-nickel soft magnetic powder core with the magnetic permeability of 125. The magnetic properties of the obtained iron-nickel magnetic powder core are shown in table 1.
Example 3
Taking gas atomization iron-nickel powder, wherein the content of nickel is 50%, dividing the powder into three particle sizes of less than 60 μm, more than or equal to 60 μm, less than 125 μm and more than or equal to 125 μm by using a vibrating screen, and then adopting the particle sizes of-60 μm: 60-125 μm: +/-125 μm ═ 40%: 30%: mixing at a ratio of 30%.
Then adding the silica sol water solution into the iron-nickel powder, heating to 70 ℃, roasting to dry, cooling, adding kaolin, drying, mixing uniformly, then adding the water glass solution, heating to 90 ℃, roasting to dry. The dosage of the silica sol is 0.5 percent of the weight of the iron-nickel powder, the dosage of the kaolin is 0.3 percent of the weight of the iron-nickel powder, the dosage of the water glass is 0.4 percent of the weight of the iron-nickel powder, and the temperature during insulation is controlled below 100 ℃.
Microcrystalline wax accounting for 0.2 percent of the weight of the iron-nickel powder is added as a release agent before compression molding, and the mixture is uniformly mixed and then compressed into a magnetic ring with the thickness of 26.9mm by 14.8mm by 11.1mm, wherein the molding pressure is 20 tons/square centimeter.
Placing the molded magnetic core into a heat treatment furnace, introducing nitrogen, introducing hydrogen after 10min, preserving the temperature at 800 ℃ for 30min, and naturally cooling, wherein the ratio of nitrogen to hydrogen is about 1: 3; and spin-coating epoxy resin powder on the surface of the magnetic core, and curing to obtain the iron-nickel soft magnetic powder core with the magnetic permeability of 125. The magnetic properties of the obtained iron-nickel magnetic powder core are shown in table 1.
Example 4
Taking gas atomization iron-nickel powder, wherein the content of nickel is 50%, dividing the powder into three particle sizes of less than 60 μm, more than or equal to 60 μm, less than 125 μm and more than or equal to 125 μm by using a vibrating screen, and then adopting the particle sizes of-60 μm: 60-125 μm: +/-125 μm ═ 40%: 30%: mixing at a ratio of 30%.
Then adding the silica sol water solution into the iron-nickel powder, heating to 80 ℃, roasting to dry, cooling, adding kaolin, drying, mixing uniformly, then adding the water glass solution, heating to 90 ℃, roasting to dry. The dosage of the silica sol is 0.8 percent of the weight of the iron-nickel powder, the dosage of the kaolin is 0.5 percent of the weight of the iron-nickel powder, the dosage of the water glass is 0.5 percent of the weight of the iron-nickel powder, and the temperature during insulation is controlled below 100 ℃.
Microcrystalline wax accounting for 0.3 percent of the weight of the iron-nickel powder is added as a release agent before compression molding, and the mixture is uniformly mixed and then compressed into a magnetic ring with the thickness of 26.9mm by 14.8mm by 11.1mm, wherein the molding pressure is 20 tons/square centimeter.
Placing the molded magnetic core into a heat treatment furnace, introducing nitrogen, introducing hydrogen after 10min, preserving the temperature at 800 ℃ for 30min, and naturally cooling, wherein the ratio of nitrogen to hydrogen is about 1: 3; and spin-coating epoxy resin powder on the surface of the magnetic core, and curing to obtain the iron-nickel soft magnetic powder core with the magnetic permeability of 125. The magnetic properties of the obtained iron-nickel magnetic powder core are shown in table 1.
Example 5
Taking gas atomization iron-nickel powder, wherein the content of nickel is 50%, dividing the powder into three particle sizes of less than 60 μm, more than or equal to 60 μm, less than 125 μm and more than or equal to 125 μm by using a vibrating screen, and then adopting the particle sizes of-60 μm: 60-125 μm: +/-125 μm ═ 40%: 30%: mixing at a ratio of 30%.
Then adding the silica sol water solution into the iron-nickel powder, heating to 80 ℃, roasting to dry, cooling, adding kaolin, drying, mixing uniformly, then adding the water glass solution, heating to 90 ℃, roasting to dry. The dosage of the silica sol is 0.3 percent of the weight of the iron-nickel powder, the dosage of the kaolin is 0.3 percent of the weight of the iron-nickel powder, the dosage of the water glass is 0.3 percent of the weight of the iron-nickel powder, and the temperature during insulation is controlled below 100 ℃.
Microcrystalline wax accounting for 0.1 percent of the weight of the iron-nickel powder is added as a release agent before compression molding, and the mixture is uniformly mixed and then compressed into a magnetic ring with the thickness of 26.9mm by 14.8mm by 11.1mm, and the molding pressure is 20 tons/square centimeter.
Placing the molded magnetic core into a heat treatment furnace, introducing nitrogen, introducing hydrogen after 10min, preserving the temperature at 800 ℃ for 30min, and naturally cooling, wherein the ratio of nitrogen to hydrogen is about 1: 3; and spin-coating epoxy resin powder on the surface of the magnetic core, and curing to obtain the iron-nickel soft magnetic powder core with the magnetic permeability of 125. The magnetic properties of the obtained iron-nickel magnetic powder core are shown in table 1.
Table 1:
as can be seen from Table 1, the iron-nickel soft magnetic powder core with the magnetic permeability of 125 prepared by the method has the direct current bias performance of more than 48 percent under the condition of 100 Oe; the power loss is about 580mW/cm3 at 100KHz and 1000Gs, and the performance is at the leading level of the industry.
The above description is only an application example of the present invention, and certainly, the present invention should not be limited by this application, and therefore, the present invention is still within the protection scope of the present invention by equivalent changes made in the claims of the present invention.
Claims (9)
1. A preparation method of an iron-nickel soft magnetic powder core with 125 magnetic conductivity comprises the steps of iron-nickel powder preparation, insulation coating, compression molding, heat treatment and surface coating; the method is characterized in that: the iron-nickel powder preparation method comprises the following steps of screening iron-nickel powder into three particle sizes of less than 60 mu m, more than or equal to 60 mu m, less than 125 mu m and more than or equal to 125 mu m according to a proportion of 40%: 30%: mixing at a ratio of 30%.
2. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 1, characterized in that: the iron-nickel powder is gas atomized iron-nickel powder.
3. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 1, characterized in that: the nickel content in the iron-nickel powder is 40% -60%, and the balance is iron.
4. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 1, characterized in that: and the insulation coating adopts a sol-gel method to form a silicon oxide coating layer on the surface of the iron-nickel powder for insulation.
5. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 5, characterized in that: the sol-gel method for insulating coating specifically comprises the following steps: adding a silica sol aqueous solution into the uniformly mixed iron-nickel powder, heating, frying, then mixing kaolin into the mixture, and adding a water glass solution, heating, frying and drying; wherein the dosage of the silica sol is 0.3-0.8% of the weight of the iron-nickel powder, the dosage of the kaolin is 0.2-0.5% of the weight of the iron-nickel powder, the dosage of the water glass is 0.2-0.5% of the weight of the iron-nickel powder, and the temperature is controlled below 100 ℃.
6. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 1, characterized in that: and (3) compression molding: and adding a release agent into the insulated powder, and performing compression molding, wherein the molding pressure is 16-21 tons/square centimeter.
7. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 6, characterized in that: the release agent is microcrystalline wax, and the dosage of the microcrystalline wax is 0.1-0.3% of the weight of the iron-nickel powder.
8. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 1, characterized in that: the heat treatment comprises the following steps: and (3) putting the pressed and formed magnetic core into a mixed atmosphere of nitrogen and hydrogen for sintering, wherein the ratio of the nitrogen to the hydrogen is 1:3, the sintering temperature is 650-850 ℃, and the heat preservation time is 30-120 min.
9. The method for preparing an iron-nickel soft magnetic powder core with 125 magnetic permeability according to claim 1, characterized in that: coating the surface: and the surface of the magnetic core is spin-coated by adopting epoxy resin powder.
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