CN113838658A - Preparation method of iron-silicon magnetic powder core - Google Patents
Preparation method of iron-silicon magnetic powder core Download PDFInfo
- Publication number
- CN113838658A CN113838658A CN202111011374.XA CN202111011374A CN113838658A CN 113838658 A CN113838658 A CN 113838658A CN 202111011374 A CN202111011374 A CN 202111011374A CN 113838658 A CN113838658 A CN 113838658A
- Authority
- CN
- China
- Prior art keywords
- magnetic powder
- iron
- silicon
- powder core
- ferrosilicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 102
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 56
- 238000000137 annealing Methods 0.000 claims abstract description 39
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 34
- 229920002050 silicone resin Polymers 0.000 claims abstract description 33
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 20
- 238000009689 gas atomisation Methods 0.000 claims abstract description 16
- 238000000748 compression moulding Methods 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 238000000889 atomisation Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 9
- 229910000859 α-Fe Inorganic materials 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000006698 induction Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 230000007847 structural defect Effects 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000005381 magnetic domain Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 description 1
- 229910017082 Fe-Si Inorganic materials 0.000 description 1
- 229910017133 Fe—Si Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- 229910003962 NiZn Inorganic materials 0.000 description 1
- 229910002796 Si–Al Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000314 poly p-methyl styrene Polymers 0.000 description 1
- 206010063401 primary progressive multiple sclerosis Diseases 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- H01F1/14—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 metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a ferro-silicon magnetic powder core, belonging to the field of magnetic materials. The method comprises the following steps: (1) preparing iron-silicon spherical powder by adopting a gas atomization process; (2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and an organic solvent, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder; (3) placing the composite magnetic powder obtained in the step (2) in a mould, and performing compression molding to obtain a pressed blank of the iron-silicon magnetic powder core; (4) pressing the iron-silicon magnetic powder core obtained in the step (3) at a vacuum degree of 2-8 multiplied by 10‑3And annealing under Pa, wherein the annealing temperature is 700-800 ℃, and the iron-silicon magnetic powder core is obtained. The preparation method of the invention can obviously improve the effective magnetic conductivity of the iron-silicon magnetic powder core and reduce the power loss; simple and easy operation, low cost and suitability for large-scale production.
Description
Technical Field
The invention relates to a preparation method of a ferrosilicon magnetic powder core, belonging to the field of magnetic materials.
Background
Soft Magnetic Composite (SMC) or magnetic powder core has the characteristics of magnetic three-dimensional isotropy, high resistivity, small high-frequency eddy current loss and the like, and is a key base material for preparing electronic components (inductors). According to the magnetic components, the metal magnetic powder core can be divided into Fe, Fe-Si, Fe-Ni, Fe-Si-Al, Fe-Ni-Mo, amorphous and nanocrystalline magnetic powder cores and the like, and the preparation process mainly comprises the steps of soft magnetic metal powder preparation, insulation coating, press forming, annealing heat treatment and the like. The iron-silicon magnetic powder core has the characteristics of high saturation magnetic induction, excellent direct current superposition performance, low material cost and the like, is commonly used for preparing high-power and high-current inductance components, and has important application in the field of new energy such as photovoltaic solar energy, new energy automobiles and charging piles thereof.
In order to improve the energy conversion efficiency of the iron-silicon magnetic powder core and reduce the heat generation of the device, the iron-silicon magnetic powder core is generally required to be subjected to insulation coating treatment so as to reduce the power loss of the iron-silicon magnetic powder core. The loss of the metal magnetic powder core mainly comprises eddy current loss and hysteresis loss. The surface layer of the magnetic powder particles is provided with an insulating coating layer by utilizing organic, inorganic or organic/inorganic compounds with high resistivity, so that the eddy current effect between adjacent magnetic powder particles is blocked, and the high-frequency eddy current loss can be effectively reduced. However, the introduction of a large amount of non-magnetic insulating media can significantly reduce the volume fraction of the magnetic components and increase the internal demagnetizing field, which leads to significant deterioration of saturation induction, permeability and hysteresis loss, and is not favorable for miniaturization and energy saving of electronic components. According to reports, the magnetic permeability of the iron-silicon metal magnetic powder core is not more than 150 at most. In addition, the pressing force of the iron-silicon magnetic powder core can reach 1.5GPa, a great amount of structural defects such as residual stress, dislocation and the like can be introduced to become a pinning center of magnetic domain motion, so that the hysteresis loss is obviously increased, and the effective magnetic permeability is obviously reduced. Therefore, the pressed compact after press molding needs to be annealed to eliminate residual stress and structural defects. The protective atmosphere for the annealing heat treatment is usually selected from nitrogen, argon/hydrogen or a nitrogen/hydrogen mixture.
With the trend of miniaturization, high frequency, high efficiency and energy saving of electronic components, higher requirements are put forward on the comprehensive magnetic properties of the metal magnetic powder core, such as saturation magnetic induction, loss, magnetic conductivity, frequency/temperature characteristics and the like. Annealing treatment after compression molding can effectively eliminate residual stress and structural defects in the compression molding process and improve the mechanical strength of the magnetic powder core. In order to increase the annealing temperature of the metal magnetic powder core while ensuring the integrity and high resistivity of the insulating coating layer, it is necessary to increase the heat resistance stability of the insulating coating medium. The patent CN 103151134B utilizes MnZn or NiZn ferrite to modify silicone resin to prepare an insulating composite coating agent, the insulating composite coating agent with the mass fraction of 1-5% is used for insulating and coating soft magnetic metal particles, cold press molding is carried out at 500-800 MPa, and then treatment at 300-650 ℃ is carried out in high-purity argon or high-purity nitrogen, so that the metal magnetic powder core with high magnetic conductivity, low loss and high strength is obtained. Patent CN 107446352 a discloses a silicone resin, which mainly comprises the following components in parts by weight: 30-50 parts of MQ silicon resin, 30-60 parts of precipitated white carbon black, 2-6 parts of mercaptopropyl methyldimethoxysilane and 10-78 parts of HMPA 5. The silicon resin has high decomposition temperature, can improve the heat resistance of the insulating powder and can improve the heat treatment temperature of the metal magnetic powder core to 900 ℃. In addition, the annealing temperature can be greatly increased by using a non-magnetic/magnetic inorganic insulating coating medium such as silicon dioxide, aluminum oxide, titanium oxide, aluminum nitride, ferrite, or the like. However, the inorganic coating medium has poor binding ability with magnetic powder particles, is brittle, and is easily broken during pressing. The problems of poor heat resistance of an organic medium and poor pressing performance of an inorganic medium can be improved to a certain extent by utilizing organic/inorganic composite coating, but the process complexity of the metal magnetic powder core is greatly increased by the composite coating.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a ferrosilicon magnetic powder core, which can obviously improve the effective magnetic conductivity of the ferrosilicon magnetic powder core.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a ferrosilicon magnetic powder core comprises the following steps:
(1) preparing iron-silicon spherical powder by adopting a gas atomization process;
(2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and an organic solvent, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder;
(3) placing the composite magnetic powder obtained in the step (2) in a mould, and performing compression molding to obtain a pressed blank of the iron-silicon magnetic powder core;
(4) and (4) annealing the pressed blank of the ferrosilicon magnetic powder core obtained in the step (3) under the vacuum degree of 2-8 x 10 < -3 > Pa, wherein the annealing temperature is 700-800 ℃, and the ferrosilicon magnetic powder core is obtained.
According to the invention, the annealing treatment is carried out in vacuum, and the oxygen content in the annealing treatment atmosphere is controlled, so that the decomposition of the silicone resin is effectively inhibited, and the thermal stability of the silicone resin is enhanced; the temperature of the annealing treatment is increased in the annealing treatment, so that the silicone resin can be fully spread on the surface of the iron-silicon spherical powder to form a thin, uniform and continuous insulating coating layer, and the eddy current loss is reduced; and the residual stress introduced in the compression molding process can be fully released, the effective magnetic conductivity of the iron-silicon magnetic powder core is obviously improved, and the power loss is reduced. The preparation method is simple and feasible, has low cost and is suitable for large-scale production.
As a preferred embodiment of the method for preparing the ferrosilicon magnetic powder core of the present invention, in the step (2), the mass ratio of the silicone resin, the organic solvent and the ferrosilicon spherical powder is silicone resin: organic solvent: 0.25-1.0% of spherical silicon powder: 1: 100.
the inventors have conducted extensive studies to find that the saturation magnetic induction of the ferrosilicon magnetic powder core can be effectively retained by controlling the amount of the non-magnetic silicone resin.
In a preferred embodiment of the method for preparing the magnetic ferrite core according to the present invention, the organic solvent is at least one of acetone and ethanol.
As a preferred embodiment of the preparation method of the iron-silicon magnetic powder core, the conditions of the compression molding in the step (3) are unidirectional compression, the compression force is 800-1200 MPa, and the pressure maintaining time is 8-10 s.
The magnetic powder core is formed by pressing under certain pressure, certain internal stress exists, the magnetic domain deflection difficulty is increased due to the existence of the internal stress, the coercive force is increased, the loss of the magnetic powder core is increased, the magnetic conductivity is reduced, and the performance of the magnetic powder core can be effectively improved by removing the internal stress. The invention has smaller pressing force in the pressing and forming process, can reduce the damage of the die, has smaller introduced residual stress, reduces the structural defects of the iron-silicon magnetic powder and enhances the effective magnetic conductivity of the iron-silicon magnetic powder core.
As a preferred embodiment of the preparation method of the iron-silicon magnetic powder core, the temperature rise rate of the annealing treatment in the step (4) is 5-8 ℃/min, the heat preservation time is 2-6h, and the iron-silicon magnetic powder core is naturally cooled to the room temperature after the heat preservation is finished.
As a preferred embodiment of the method for preparing the iron-silicon magnetic powder core of the present invention, the parameters of the gas atomization process in step (1) are as follows: the atomization pressure is 5-7MPa, and the atomization temperature is 1520-1650 ℃.
The invention adopts the gas atomization method to prepare the iron-silicon spherical powder, can reduce the influence caused by impurities, and simultaneously the spherical powder is beneficial to insulating coating.
As a preferred embodiment of the method for preparing the ferrosilicon magnetic powder core of the present invention, the particle size of the ferrosilicon spherical powder is: d10=10.9~15.5μm、D50=25.7~43.8μm、D90=60.7~112.5μm。
The median particle size of the iron-silicon spherical powder selected by the invention is 25.7-43.8 mu m, the boundary effective particle size of the iron-silicon spherical powder is larger, and the prepared iron-silicon magnetic powder core has higher effective magnetic conductivity. Meanwhile, the powder with different particle sizes is mixed, the small particles can occupy the gap positions of the large particles, after the powder is pressed and formed, the gaps of the powder are reduced, the density is increased, and the good magnetic performance of the magnetic powder core can be ensured.
As a preferred embodiment of the preparation method of the iron-silicon magnetic powder core, the content of Si in the iron-silicon spherical powder is 4.5-6.5% of the total mass in percentage by mass.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the annealing treatment is carried out in vacuum, so that the oxygen content in the annealing treatment atmosphere is reduced, the decomposition of the silicone resin is inhibited, and the stability of the silicone resin is increased; the annealing temperature is increased, the residual stress introduced in the compression molding process is fully released, the hysteresis loss is reduced, the power loss is reduced, and the effective magnetic conductivity of the iron-silicon magnetic powder core is obviously increased;
(2) the invention controls the quantity of the non-magnetic silicone resin to ensure that the saturation magnetic induction of the iron-silicon magnetic powder core is at a higher value;
(3) the invention adopts the unidirectional pressing method to press the model, the pressing force in the pressing process is lower, the damage of the mould can be reduced, the introduced residual stress is smaller, and the performance of the iron-silicon magnetic powder core can be better ensured.
Drawings
FIG. 1 is a graph showing the morphology and elemental analysis of the ferrite core obtained in example 1.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following detailed description and accompanying drawings.
Example 1
The embodiment provides a preparation method of a ferrosilicon magnetic powder core, which comprises the following steps:
(1) preparing iron-silicon spherical powder by adopting a gas atomization process, wherein the gas atomization process comprises the following parameters: the atomization pressure is 6MPa, and the atomization temperature is 1580 ℃; the particle size of the iron-silicon spherical powder is as follows: d10=12.7μm、D50=31.5μm、D9068.5 μm; the Si content in the iron-silicon spherical powder is 6.5 percent of the total mass by mass fraction;
(2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and acetone, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder; the mass ratio of the silicone resin to the acetone to the iron-silicon spherical powder is that the silicone resin: acetone: silicon sphere powder 0.5: 1: 100, respectively;
(3) uniformly distributing the composite magnetic powder obtained in the step (2) in a cavity of a die, and performing 1200MPa one-way compression molding for 8s to obtain a pressed blank of the iron-silicon magnetic powder core;
(4) placing the pressed compact of the ferrosilicon magnetic powder core obtained in the step (3) in a high vacuum furnace, wherein the vacuum degree is 5 multiplied by 10-3And (3) annealing under Pa, wherein the heating rate of the annealing is 8 ℃/min, the annealing temperature is 700 ℃, the heat preservation time is 4h, and the ferrosilicon magnetic powder core is obtained after furnace cooling.
Example 2
The embodiment provides a preparation method of a ferrosilicon magnetic powder core, which comprises the following steps:
(1) preparing iron-silicon spherical powder by adopting a gas atomization process, wherein the gas atomization process comprises the following parameters: the atomization pressure is 6MPa, and the atomization temperature is 1580 ℃; the particle size of the iron-silicon spherical powder is as follows: d10=12.7μm、D50=31.5μm、D9068.5 μm; the Si content in the iron-silicon spherical powder is 6.5 percent of the total mass by mass fraction;
(2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and an organic solvent, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder; the mass ratio of the silicone resin, the organic solvent and the iron-silicon spherical powder is that the silicone resin: organic solvent: silicon sphere powder 1.0: 1: 100, respectively;
(3) uniformly distributing the composite magnetic powder obtained in the step (2) in a cavity of a die, and performing 1200MPa one-way compression molding for 8s to obtain a pressed blank of the iron-silicon magnetic powder core;
(4) placing the pressed compact of the ferrosilicon magnetic powder core obtained in the step (3) in a high vacuum furnace, wherein the vacuum degree is 5 multiplied by 10-3And (3) annealing under Pa, wherein the heating rate of the annealing is 8 ℃/min, the annealing temperature is 700 ℃, the heat preservation time is 4h, and the ferrosilicon magnetic powder core is obtained after furnace cooling.
Example 3
The embodiment provides a preparation method of a ferrosilicon magnetic powder core, which comprises the following steps:
(1) preparing iron-silicon spherical powder by adopting a gas atomization process, wherein the gas atomization process comprises the following parameters: the atomization pressure is 6MPa, and the atomization temperature is 1580 ℃; the particle size of the iron-silicon spherical powder is as follows: d10=12.7μm、D50=31.5μm、D9068.5 μm; the Si content in the iron-silicon spherical powder is 6.5 percent of the total mass by mass fraction;
(2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and an organic solvent, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder; the mass ratio of the silicone resin, the organic solvent and the iron-silicon spherical powder is that the silicone resin: organic solvent: silicon sphere powder 0.25: 1: 100, respectively;
(3) uniformly distributing the composite magnetic powder obtained in the step (2) in a cavity of a die, and performing 800MPa one-way compression molding for 8s to obtain a pressed blank of the iron-silicon magnetic powder core;
(4) placing the pressed compact of the ferrosilicon magnetic powder core obtained in the step (3) in a high vacuum furnace, wherein the vacuum degree is 5 multiplied by 10-3Annealing under Pa, wherein the heating rate of the annealing is 8 ℃/min, the annealing temperature is 800 ℃, the heat preservation time is 6h, and the ferrosilicon magnetic powder core is obtained after furnace cooling.
Example 4
The embodiment provides a preparation method of a ferrosilicon magnetic powder core, which comprises the following steps:
(1) preparing iron-silicon spherical powder by adopting a gas atomization process, wherein the gas atomization process comprises the following parameters: the atomization pressure is 7MPa, and the atomization temperature is 1520 ℃; the particle size of the iron-silicon spherical powder is as follows: d10=11.2μm、D50=26.8μm、D9063.5 μm; the Si content in the iron-silicon spherical powder is 6.5 percent of the total mass by mass fraction;
(2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and an organic solvent, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder; the mass ratio of the silicone resin, the organic solvent and the iron-silicon spherical powder is that the silicone resin: organic solvent: silicon sphere powder 0.3: 1: 100, respectively; wherein the organic solvent is a mixed solution of ethanol and acetone;
(3) uniformly distributing the composite magnetic powder obtained in the step (2) in a cavity of a die, and performing unidirectional compression molding at 1000MPa for 9s to obtain a pressed blank of the iron-silicon magnetic powder core;
(4) placing the pressed compact of the ferrosilicon magnetic powder core obtained in the step (3) in a high vacuum furnace, wherein the vacuum degree is 2 multiplied by 10-3Annealing under Pa, wherein the heating rate of the annealing is 5 ℃/min, the annealing temperature is 750 ℃, the heat preservation time is 2h, and the ferrosilicon magnetic powder core is obtained after furnace cooling.
Example 5
The embodiment provides a preparation method of a ferrosilicon magnetic powder core, which comprises the following steps:
(1) preparing iron-silicon spherical powder by adopting a gas atomization process, wherein the gas atomization process comprises the following parameters: the atomization pressure is 5MPa, and the atomization temperature is 1650 ℃; the particle size of the iron-silicon spherical powder is as follows: d10=14.5μm、D50=42.3μm、D9097.5 μm; the Si content in the iron-silicon spherical powder is 6.5 percent of the total mass by mass fraction;
(2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and an organic solvent, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder; the mass ratio of the silicone resin, the ethanol and the iron-silicon spherical powder is that the silicone resin: ethanol: silicon sphere powder 0.5: 1: 100, respectively;
(3) uniformly distributing the composite magnetic powder obtained in the step (2) in a cavity of a die, and performing 800MPa one-way compression molding for 10s to obtain a pressed blank of the iron-silicon magnetic powder core;
(4) putting the pressed compact of the ferrosilicon magnetic powder core obtained in the step (3) into a high vacuum furnace, wherein the vacuum degree is 8 multiplied by 10-3Annealing under Pa, wherein the heating rate of the annealing is 6 ℃/min, the annealing temperature is 700 ℃, the heat preservation time is 4h, and the ferrosilicon magnetic powder core is obtained after furnace cooling.
Comparative example 1
The only difference between this comparative example and example 1 is that: the annealing treatment is carried out in a tube furnace without vacuum pumping, and the annealing atmosphere is air.
Comparative example 2
The only difference between this comparative example and example 1 is that: the annealing treatment is carried out in a tube furnace, the tube furnace is not vacuumized, flowing argon is continuously introduced, and the purity of the argon is 99.99 percent.
Comparative example 3
The only difference between this comparative example and example 1 is that: the temperature of the annealing treatment was 500 ℃.
Comparative example 4
The only difference between this comparative example and example 1 is that: the mass ratio of the silicone resin to the acetone to the iron-silicon spherical powder is that the silicone resin: acetone: silicon sphere powder 1.5: 1: 100.
the magnetic performance parameters such as volume ratio loss, permeability, saturation induction, residual stress, resistivity and the like of the iron-silicon magnetic powder cores of examples 1 to 5 and comparative examples 1 to 5 were measured by using a Japanese Kawasaki SY-8219 type B-H analyzer, a comprehensive physical measurement system PPMS, an iXRD X-ray residual stress analyzer and an SZT-2C four-probe resistivity tester, and the measurement results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the effective permeability of the iron-silicon magnetic powder core prepared by the invention is as high as 150, and the functional loss is as low as 650mW/cm3。
FIG. 1 is a graph showing the morphology and elemental analysis of the ferrite core obtained in example 1; wherein (a) is SEM picture of iron silicon magnetic powder core, (b) is Si element distribution diagram, (c) is O element distribution diagram, and (d) is Fe element distribution diagram. As can be seen from fig. 1, a thin Si-rich and O-rich insulating coating is attached to the surface layer of the magnetic powder particles.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The preparation method of the iron-silicon magnetic powder core is characterized by comprising the following steps:
(1) preparing iron-silicon spherical powder by adopting a gas atomization process;
(2) adding the iron-silicon spherical powder prepared in the step (1) into a mixed solution of silicone resin and an organic solvent, uniformly mixing, and then ultrasonically stirring until the mixture is dried to obtain the insulation coated composite magnetic powder;
(3) placing the composite magnetic powder obtained in the step (2) in a mould, and performing compression molding to obtain a pressed blank of the iron-silicon magnetic powder core;
(4) pressing the iron-silicon magnetic powder core obtained in the step (3) at a vacuum degree of 2-8 multiplied by 10-3And annealing under Pa, wherein the annealing temperature is 700-800 ℃, and the iron-silicon magnetic powder core is obtained.
2. The method for preparing the ferrosilicon magnetic powder core as claimed in claim 1, wherein the mass ratio of the silicone resin, the organic solvent and the ferrosilicon spherical powder in the step (2) is silicone resin: organic solvent: 0.25-1.0% of iron-silicon spherical powder: 1: 100.
3. the method of manufacturing a ferrite core according to claim 1 or 2, wherein the organic solvent is at least one of acetone and ethanol.
4. The method for preparing the ferrosilicon magnetic powder core as claimed in claim 1, wherein the conditions of the press molding in the step (3) are a one-way press method, a pressing force is 800 to 1200MPa, and a pressure holding time is 8 to 10 s.
5. The method for preparing the ferrosilicon magnetic powder core as recited in claim 1, wherein the annealing treatment in the step (4) has a temperature rise rate of 5 to 8 ℃/min and a heat preservation time of 2 to 6 hours, and the ferrosilicon magnetic powder core is naturally cooled to room temperature after the heat preservation.
6. The method for preparing the ferrosilicon magnetic powder core as recited in claim 1, wherein the parameters of the gas atomization process in the step (1) are as follows: the atomization pressure is 5-7MPa, and the atomization temperature is 1520-1650 ℃.
7. The method of preparing a ferrite powder core according to claim 1, wherein said ferrite powder is spherical powderThe particle size is as follows: d10=10.9~15.5μm、D50=25.7~43.8μm、D90=60.7~112.5μm。
8. The method of producing a ferrosilicon magnetic powder core as claimed in claim 1, wherein the content of Si in the ferrosilicon spherical powder is 4.5 to 6.5% by mass of the total mass.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111011374.XA CN113838658A (en) | 2021-08-31 | 2021-08-31 | Preparation method of iron-silicon magnetic powder core |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111011374.XA CN113838658A (en) | 2021-08-31 | 2021-08-31 | Preparation method of iron-silicon magnetic powder core |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113838658A true CN113838658A (en) | 2021-12-24 |
Family
ID=78961772
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111011374.XA Pending CN113838658A (en) | 2021-08-31 | 2021-08-31 | Preparation method of iron-silicon magnetic powder core |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113838658A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114582616A (en) * | 2022-01-27 | 2022-06-03 | 武汉科技大学 | Fe/FeSi composite iron powder core with layered structure and preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104036902A (en) * | 2014-05-28 | 2014-09-10 | 浙江明贺钢管有限公司 | Preparing method of metal magnetic powder core |
CN108987022A (en) * | 2018-06-26 | 2018-12-11 | 华南理工大学 | A kind of FeSiAl powder core and preparation method thereof |
CN110085385A (en) * | 2019-06-03 | 2019-08-02 | 马鞍山新康达磁业有限公司 | A kind of high magnetic permeability composite powder and preparation method thereof |
-
2021
- 2021-08-31 CN CN202111011374.XA patent/CN113838658A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104036902A (en) * | 2014-05-28 | 2014-09-10 | 浙江明贺钢管有限公司 | Preparing method of metal magnetic powder core |
CN108987022A (en) * | 2018-06-26 | 2018-12-11 | 华南理工大学 | A kind of FeSiAl powder core and preparation method thereof |
CN110085385A (en) * | 2019-06-03 | 2019-08-02 | 马鞍山新康达磁业有限公司 | A kind of high magnetic permeability composite powder and preparation method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114582616A (en) * | 2022-01-27 | 2022-06-03 | 武汉科技大学 | Fe/FeSi composite iron powder core with layered structure and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108565109B (en) | Preparation method of soft magnetic composite material | |
CN111739730B (en) | Preparation method of organic-coated high-performance metal magnetic powder core | |
WO2021142974A1 (en) | Metal soft magnetic powder coated with insulation and preparation method therefor and use thereof | |
CN111696746A (en) | Crushing-method Fe-Si-Al soft magnetic powder core and preparation method thereof | |
CN111451515B (en) | Low-power-consumption soft magnetic alloy material, preparation method thereof and electronic device | |
CN114334416B (en) | Method for preparing high-performance neodymium-iron-boron magnet by solid-liquid phase separation diffusion process | |
CN113744948B (en) | Amorphous magnetic powder core precursor particle, amorphous magnetic powder core, preparation method of amorphous magnetic powder core and inductance device | |
CN113838658A (en) | Preparation method of iron-silicon magnetic powder core | |
CN113380483B (en) | Composite soft magnetic material and preparation method thereof | |
CN112216460A (en) | Nanocrystalline neodymium-iron-boron magnet and preparation method thereof | |
CN112735721B (en) | High-frequency low-loss composite soft magnetic material and preparation method and application thereof | |
CN112017835B (en) | Low-heavy rare earth high-coercivity sintered neodymium-iron-boron magnet and preparation method thereof | |
CN113077953A (en) | Method for improving magnetic conductivity of iron-based magnetic powder core based on magnetic exchange length and product | |
CN112712992A (en) | FeSi/Ni composite magnetic powder core and preparation method thereof | |
CN116190093A (en) | Soft magnetic powder core and preparation method thereof | |
CN113628824B (en) | High-strength ceramic-coated iron-based composite soft magnetic material and preparation method thereof | |
CN112216500B (en) | Method for processing neodymium magnet added with yttrium element | |
US20240038421A1 (en) | Soft magnetic powder, preparation method therefor, and use thereof | |
CN113299451A (en) | FeNi nano particle/epoxy resin composite coated iron-silicon magnetic powder core and preparation method thereof | |
CN111383810A (en) | Preparation method of amorphous alloy magnetic powder core | |
WO2023106221A1 (en) | PRODUCTION METHOD FOR ANISOTROPIC Nd-Fe-B MAGNETIC POWDER | |
CN117936217B (en) | High-permeability low-loss nanocrystalline composite magnetic powder core and preparation method thereof | |
CN108538533B (en) | Preparation method of soft magnetic composite material by interface diffusion | |
CN113921220B (en) | Mixed soft magnetic powder and application thereof in preparation of soft magnetic powder core | |
CN117153515A (en) | Iron-based amorphous and nanocrystalline soft magnetic alloy powder, nanocrystalline magnetic powder core and application thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |