CN116130237B - Preparation method of carbonyl iron powder magnetic core with 35 magnetic permeability and high Q value - Google Patents
Preparation method of carbonyl iron powder magnetic core with 35 magnetic permeability and high Q value Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 230000035699 permeability Effects 0.000 title claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 67
- 239000000843 powder Substances 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000003822 epoxy resin Substances 0.000 claims abstract description 20
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 20
- 239000006247 magnetic powder Substances 0.000 claims abstract description 19
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 239000003973 paint Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 13
- 239000000314 lubricant Substances 0.000 claims abstract description 12
- 238000007873 sieving Methods 0.000 claims abstract description 12
- 238000001723 curing Methods 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 54
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 27
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 229920001568 phenolic resin Polymers 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 235000019353 potassium silicate Nutrition 0.000 claims description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000005011 phenolic resin Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical group [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 5
- 239000005007 epoxy-phenolic resin Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 10
- 235000019580 granularity Nutrition 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 4
- 239000011810 insulating material Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000000306 component Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
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- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical class [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- ZPLUZNXSYCCJOE-UHFFFAOYSA-N phosphoric acid;propan-2-one Chemical compound CC(C)=O.OP(O)(O)=O ZPLUZNXSYCCJOE-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
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
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a preparation method of a carbonyl iron powder magnetic core with high Q value and magnetic permeability of 35, which comprises the following steps: the carbonyl iron powder is proportioned according to different granularity and is uniformly mixed; chemical film forming, drying; adding an insulating binding material, uniformly mixing, drying, granulating and sieving; adding lubricant into the sieved powder, uniformly mixing, and then performing compression molding; carrying out heat treatment on the pressed magnetic powder core in a furnace, and adopting a gradient heating mode; the heat treatment temperature is controlled between 600 ℃ and 160 ℃ and the heat treatment time is 2h to 4h; and coating the surface of the magnetic powder core after heat treatment with epoxy resin paint by adopting a paint spraying process, and heating by an oven for curing. The preparation method only adopts three or four auxiliary materials, and has the advantages of simple steps, simple equipment, strong operability and low production cost; the carbonyl iron powder magnetic core with high Q value, low power consumption and good DC superposition characteristic is obtained.
Description
Technical Field
The invention relates to a preparation method of a carbonyl iron powder magnetic core with a high Q value and a magnetic conductivity of 35, belonging to the technical field of material preparation.
Background
The high-frequency inductor is taken as an indispensable basic component, is widely applied to oscillators, crystal oscillator circuits, high-frequency transceiver modules, communication equipment and other module high-frequency circuits, and plays roles in filtering, rectifying, transforming, electromagnetic interference suppression and the like in the circuits. The core, which is the core component of the inductor, has a decisive influence on the performance of the inductor, such as the operating frequency band, the Q-value, etc. The loss of the high-frequency magnetic core mainly comes from eddy current loss, and the common metal magnetic powder core has large particle size and large eddy current and can only be applied to the frequency range of tens of KHz and hundreds of KHz. Carbonyl iron powder is very fine in granularity and small in vortex, and is often uniformly mixed with various inorganic and organic insulating materials to prepare magnetic powder cores with various magnetic permeability, so that the carbonyl iron powder is applied to high-frequency bands above MHz.
At present, the domestic patents related to carbonyl iron powder are complicated in powder insulation coating steps, such as the powder insulation coating steps in the Chinese patent invention of preparation method of carbonyl iron powder core with magnetic permeability of 35 (publication No. CN 111524697A): mixing carbonyl iron powder, water of chromic acid aqueous solution phosphoric acid and alcohol solution, forming a layer of oxide film on the surface of carbonyl iron, then performing secondary coating treatment, and coating mica powder, kaolin and other clay powder on the surface again; and then coating the powder surface for three times, wherein the substances coated for three times are silica-alumina sol, silica sol and alumina sol. The coating method has the advantages that powder particles can be completely coated as far as possible and isolated from the outside air, but the coating materials are more, the required forming pressure is larger, and the insulating layer can be damaged due to the excessively high pressure in the compression forming process, so that the loss is increased; and nitrogen atmosphere is adopted in the heat treatment process to prevent oxidation, so that the cost is increased. In addition, compared with similar products of the American Micrometals company, the carbonyl iron powder magnetic core with the magnetic conductivity of 35 in the domestic market has the problems of low Q value, large power consumption and poor direct current superposition characteristics.
Disclosure of Invention
First, the technical problem to be solved
In order to solve the problems in the prior art, the invention provides a preparation method of a carbonyl iron powder magnetic core with high Q value, low power consumption and magnetic permeability mu=35.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
a preparation method of a carbonyl iron powder magnetic core with 35 magnetic permeability and high Q value comprises the following steps:
(1) The carbonyl iron powder is proportioned according to different granularity and is uniformly mixed;
(2) Chemical film forming: pouring the phosphoric acid solution into the carbonyl iron powder which is uniformly mixed, mixing and stirring until the reaction is completed, and then drying;
(3) Granulating: after powder is chemically formed into a film, adding an insulating binding material, uniformly mixing, drying, granulating and sieving;
(4) And (5) press forming: adding lubricant into the sieved powder, uniformly mixing, and then performing compression molding;
(5) Core heat treatment: carrying out heat treatment on the pressed magnetic powder core in a furnace, and adopting a gradient heating mode; the heat treatment temperature is controlled between 600 ℃ and 160 ℃ and the heat treatment time is 2h to 4h;
(6) Surface coating: and coating the surface of the magnetic powder core with epoxy resin paint by adopting a paint spraying process, and heating by an oven for curing.
In the above-described production method, preferably, in the step (1), the content of C in the carbonyl iron powder is 0.1% or less, the content of O is 0.4% or less, the content of N is 0.1% or less, and the balance is Fe.
In the above-described production method, it is preferable that in the step (1), the particle size ratio of the carbonyl iron powder is d10=3.5 to 5 μm, d50=9 to 12 μm, d90=21 to 25 μm.
In the preparation method, preferably, in the step (2), the solvent of the phosphoric acid solution is acetone, alcohol or water, and the solution is prepared according to the volume ratio of phosphoric acid to the solvent of 1:20-100;
the consumption of the phosphoric acid is 0.3 to 0.6 percent of the weight of the carbonyl iron powder.
In the preparation method as described above, preferably, in the step (2), the reaction condition is 40 to 85 ℃, and the completion of the reaction means drying the powder; the drying temperature is 80-150 ℃ and the drying time is 15-60 min.
In the preparation method as described above, preferably, in the step (3), the insulating adhesive material is one or more of epoxy resin, silicone resin, phenolic resin or water glass; the consumption of the insulating binding material is 0.4-0.7% of the weight of the carbonyl iron powder.
Further preferably, in the step (3), the insulating adhesive material is epoxy resin and phenolic resin, and the weight ratio of the epoxy resin to the phenolic resin is 3:1-4: 1, a step of;
or the insulating bonding material is water glass and organic silicon resin, and the weight ratio of the water glass to the organic silicon resin is 1:5.
In the above preparation method, preferably, in the step (3), the granulation is carried out by sieving with a 40-80 mesh sieve, and then drying at 80-100 ℃ for 15-30 min.
In the preparation method, preferably, in the step (4), the lubricant is zinc stearate, and the amount of the lubricant is 0.2-0.4% of the weight of the powder after sieving treatment.
In the above-mentioned production method, preferably, in the step (4), the pressure of the press molding is 600 to 800MPa.
In the preparation method, in the step (5), the temperature is preferably raised from normal temperature to 60-80 ℃ and then is maintained, the temperature is raised at a speed of 5-10 ℃/min, the temperature is maintained after 20-30 ℃ each time, the temperature is maintained for 20-60 min, and the temperature is maintained for 4-5 stages.
Specifically, the gradient heating mode is that the temperature is raised to 60-80 ℃ at the temperature rising rate of 5 ℃/min, and the temperature is kept at 60-80 ℃ for 20-30 min; heating from 60-80 ℃ to 80-120 ℃, heating up at a speed of 5-10 ℃/min, and preserving heat for 30-60 min at 80-120 ℃; heating from 80-120 ℃ to 120-150 ℃, heating up at a rate of 8-10 ℃/min, and preserving heat at 120-150 ℃ for 30-60 min; heating from 120-150 ℃ to 150-160 ℃, heating up at a speed of 8-10 ℃/min, and preserving heat for 30-60 min at 150-160 ℃.
In the above-mentioned preparation method, preferably, in the step (6), the magnetic core is chamfered after the heat treatment, the magnetic core is heated to 120 ℃, the surface of the magnetic core is coated with the epoxy resin paint by a paint spraying process, and the magnetic core is cured by heating in an oven.
In the invention, the material with the magnetic permeability in the range of 35+/-10% is called 35, namely the material with the magnetic permeability in the range of 31.5-38.5 is called 35.
(III) beneficial effects
The beneficial effects of the invention are as follows:
(1) The invention provides a preparation method of a carbonyl iron powder magnetic core with a magnetic conductivity of 35, which utilizes the characteristics of fine granularity and high activity of carbonyl iron powder, adopts diluted phosphoric acid solution to perform in-situ reaction on the surface of the powder, precisely controls the reaction time and the uniformity of a surface insulating layer by controlling the concentration of phosphoric acid and the temperature in the reaction process, so that a compact insulating layer with strong bonding force with the powder is formed on the surface of the powder, and the main component of the insulating layer is various ferric phosphate salts, and can be subjected to heat treatment at the temperature of 600 ℃ without decomposing or crystallizing the insulating layer.
(2) The preparation method of the carbonyl iron powder magnetic core with the high Q value and the magnetic permeability of 35 provided by the invention has the advantages that the used molding pressure is small, and the possibility of insulating damage of the powder surface in the pressing process is reduced.
(3) The preparation method of the carbonyl iron powder magnetic core with the high Q value and the magnetic permeability of 35 provided by the invention adopts the stepped heating heat treatment magnetic core, which is beneficial to complete reaction in the curing process of the organic binder.
(4) The preparation method of the carbonyl iron powder magnetic core with the high Q value and the magnetic permeability of 35 only adopts three or four auxiliary materials, and has the advantages of simple steps, simple equipment, strong operability and low production cost; the carbonyl iron powder magnetic core with high Q value, low power consumption and good DC superposition characteristic is obtained.
Detailed Description
A preparation method of a carbonyl iron powder magnetic core with 35 magnetic permeability and high Q value comprises the following steps:
(1) Particle size ratio: selecting carbonyl iron powder, wherein the content of C is less than or equal to 0.1%, the content of O is less than or equal to 0.4%, the content of N is less than or equal to 0.1%, and the balance is Fe;
the carbonyl iron powder is proportioned according to different granularities and is uniformly mixed.
(2) Chemical film forming: pouring the diluted phosphoric acid solution into the uniformly mixed powder, mixing and stirring until the reaction is completed, and then drying, wherein the weight of phosphoric acid is 0.3-0.6% of the weight of carbonyl iron powder. The carbonyl iron powder has fine granularity and high activity, and phosphoric acid can also react with the carbonyl iron powder rapidly. When the phosphoric acid is too low, it may cause the insulating layer on the surface of the powder particles to be too thin or some of the surface of the powder particles may not be entirely formed with the insulating layer, and the weight of the phosphoric acid is preferably 0.3 to 0.6% of the weight of the carbonyl iron powder.
(3) Granulating: after powder chemical film forming, adding one or more of the following insulating binding materials, such as epoxy resin, organic silicon resin, phenolic resin, water glass and the like, uniformly mixing, drying, granulating and sieving; the weight of the insulating binding material accounts for 0.4-0.7% of the weight of the carbonyl iron powder.
(4) And (5) press forming: adding the lubricant into the heat-treated granular powder, uniformly mixing, and then performing compression molding under the pressure of 600-800 MPa. The weight of the lubricant is 0.2-0.4% of the weight of the granule powder after heat treatment.
(5) Core heat treatment: the pressed magnetic powder core is heat treated in a furnace in a gradient heating mode. Preferably, the heat treatment temperature is controlled between 60 ℃ and 160 ℃ and the heat treatment time is 2h to 4h.
(6) Surface coating: and (3) heating the magnetic core obtained in the step (5) to 120 ℃, coating the surface of the magnetic powder core with epoxy resin paint by adopting a paint spraying process, and heating by using an oven to cure.
In the above method, preferably, in the step (2), the particle size ratio d10=3.5 to 5 μm, d50=9 to 12 μm, d90=21 to 25 μm. The weight of the insulating binding material accounts for 0.4-0.7% of the weight of the powder, and the heat treatment temperature is controlled between 140 ℃ and 160 ℃. Through a great deal of experimental researches, the weight of the insulating bonding material accounts for 0.4 to 0.7 percent of the weight of the powder, and the magnetic permeability of the insulating bonding material is lower than 0.4 percent of the weight of the powder. The heat treatment temperature is preferably 140-160 ℃, because the temperature range can lead to the solidification temperature of the insulating material, especially the organic insulating material, and the temperature is higher than the solidification temperature of the insulating material, so that the bonding material can be damaged to a certain extent, the eddy current among particles is increased, and the Q value is reduced.
The present invention will be described in detail below by way of specific embodiments for better explanation of the present invention, and raw materials, equipment, etc. used in examples may be commercially available products, without being specifically explained.
Example 1
(1) Taking carbonyl iron powder with the content of C less than or equal to 0.1%, the content of O less than or equal to 0.4%, the content of N less than or equal to 0.1% and the balance of Fe;
taking carbonyl iron powder according to the granularity proportion of d10=4.2 μm, d50=9.5 μm and d90=22.6 μm; the powders were mixed homogeneously.
(2) Diluting phosphoric acid in acetone, wherein the volume ratio of phosphoric acid to acetone is 1:50, adding an acetone phosphate solution into carbonyl iron powder according to the weight of phosphoric acid being 0.5% of the weight of carbonyl iron powder, heating to 40 ℃, and stirring and insulating until the powder is dried. And then placing the insulated carbonyl iron powder into an oven, wherein the drying temperature is 80 ℃ and the drying time is 60min.
(3) Epoxy resin and phenolic resin are dissolved in acetone, and then added into the insulated carbonyl iron powder in turn after being completely dissolved, and the mixture is stirred uniformly at normal temperature. Wherein the dosage of the epoxy resin and the phenolic resin is 0.6% of the weight of the carbonyl iron powder, and the weight ratio of the epoxy resin to the phenolic resin is 3:1.
Stirring until the mixture is dried, sieving with a 60-mesh sieve, granulating, and drying in a drying oven at 80 ℃ for 30min; after drying, the small particles of 400 mesh or less were removed (it was found that the small particles of 400 mesh or less affect the flowability of the powder and the uniformity of the product properties, so the small particles of 400 mesh or less were removed in this step).
(4) And adding 0.2% of zinc stearate lubricant into the granulated powder, and pressing and forming the granules under 800MPa.
(5) Carrying out heat treatment on the pressed magnetic powder core in air, and adopting a step heating mode, wherein the method specifically comprises the following steps: the temperature is kept at the normal temperature to 80 ℃ at the heating rate of 5 ℃/min and the temperature is kept at the temperature of 80 ℃ for 30min; the temperature is kept at 80 ℃ to 120 ℃ at a heating rate of 5 ℃/min and is kept at 120 ℃ for 60min; the temperature is raised at 120-160 deg.c and 8 deg.c/min for 60min at 160 deg.c.
(6) Chamfering the heat-treated magnetic powder core (namely removing burrs), heating the magnetic core to 120 ℃, coating the surface of the magnetic powder core with epoxy resin paint by adopting a paint spraying process, and heating and curing by an oven.
Example 2
(1) Taking carbonyl iron powder with the content of C less than or equal to 0.1%, the content of O less than or equal to 0.3%, the content of N less than or equal to 0.05% and the balance of Fe.
Particle size ratio, powder with particle size d10=3.8 μm, d50=10.2 μm, d90=21.7 μm was mixed homogeneously.
(2) Phosphoric acid is diluted in alcohol, the volume ratio of the phosphoric acid to the alcohol is 1:100, and the weight of the phosphoric acid is 0.6% of that of carbonyl iron powder. Adding phosphoric acid alcohol solution into carbonyl iron powder, heating to 65 ℃, stirring and insulating until the powder is dried. And then placing the insulated carbonyl iron powder into an oven, wherein the drying temperature is 100 ℃ and the drying time is 30min.
(3) Epoxy resin and phenolic resin are dissolved in acetone and then added into the insulated carbonyl iron powder in turn, and the mixture is stirred uniformly at normal temperature. Wherein the weight of the epoxy resin and the phenolic resin is 0.4% of the weight of the carbonyl iron powder, and the weight ratio of the epoxy resin to the phenolic resin is 4:1.
Stirring until the mixture is dried, sieving with a 40-mesh sieve, granulating, and drying in a drying oven at 80 ℃ for 30min. The granularity ratio after drying is 0% -5% below 400 meshes, 10% -20% between-400 meshes and-200 meshes, and the balance between-200 meshes and-40 meshes.
(4) And adding 0.25% of zinc stearate lubricant into the granulated powder, and pressing and forming the granules under 600 MPa.
(5) And carrying out heat treatment on the pressed magnetic powder core in air, and adopting a step heating mode. The temperature is kept between normal temperature and 60 ℃ at a heating rate of 5 ℃/min and at 60 ℃ for 20min; the temperature is increased by 5 ℃/min at 60 ℃ to 80 ℃ and the temperature is kept for 30min at 80 ℃; the temperature is increased by 10 ℃/min at the temperature of 80 ℃ to 120 ℃ and the temperature is kept for 60min at the temperature of 120 ℃; the temperature is raised at 120-150 ℃ at a rate of 10 ℃/min, and the temperature is kept at 150 ℃ for 60min.
(6) Chamfering the heat-treated magnetic powder core, heating the magnetic core to 120 ℃, coating the surface of the magnetic powder core with epoxy resin paint by adopting a paint spraying process, and heating by an oven for curing.
Example 3
(1) Taking carbonyl iron powder with the content of C less than or equal to 0.05%, the content of O less than or equal to 0.4%, the content of N less than or equal to 0.08% and the balance of Fe;
particle size ratio, d10=4.5 μm, d50=11.4 μm, d90=23.2 μm, and powder was mixed uniformly.
(2) Phosphoric acid was diluted in deionized water at a ratio of phosphoric acid to deionized water of 1:20, with the weight of phosphoric acid being 0.3% of the weight of carbonyl iron powder. The aqueous phosphoric acid solution was added to carbonyl iron powder, heated to 85 ℃, and stirred for insulation until the powder dried. And then placing the insulated carbonyl iron powder into an oven, wherein the drying temperature is 150 ℃ and the drying time is 15min.
(3) Dissolving water glass in water, dissolving organic silicon resin in alcohol, adding the completely dissolved water glass into the insulated carbonyl iron powder, and uniformly stirring at 80 ℃ until the mixture is dried; then adding the organic silicon resin dissolved in alcohol into the powder for stirring. The weight of the water glass and the weight of the organic silicon resin are 0.35 percent of the weight of the carbonyl iron powder, and the weight ratio of the water glass to the organic silicon resin is 1:5.
Stirring until the mixture is dried, sieving with 80 mesh sieve, granulating, and drying in a drying oven at 100deg.C for 30min. The granularity ratio after drying is 5-25% between-400 mesh and-200 mesh, and the rest is-200 mesh to-40 mesh.
(4) Adding 0.3% zinc stearate lubricant into the granulated powder, mixing uniformly, and compacting the granules under 750 MPa.
(5) And carrying out heat treatment on the pressed magnetic powder core in air, and adopting a step heating mode. The method comprises the following steps: the temperature is kept at the normal temperature to 80 ℃ and the heating rate is 10 ℃/min, and the temperature is kept at 80 ℃ for 60min; the temperature is increased by 8 ℃/min at 80 ℃ to 100 ℃, and the temperature is kept for 60min at 100 ℃; the temperature is kept at 100 ℃ to 120 ℃ at a heating rate of 8 ℃/min and is kept at 120 ℃ for 60min; the temperature is raised at 120-160 deg.c and 10 deg.c/min for 60min at 160 deg.c.
(6) Chamfering the heat-treated magnetic powder core, heating the magnetic core to 120 ℃, coating the surface of the magnetic powder core with epoxy resin paint by adopting a paint spraying process, heating by a baking oven for curing, and coating and curing the surface with paint for moisture and humidity resistance and attractive surface.
The magnetic ring was pressed in the above-described embodiment to have a size of Φ46.7mm×Φ24.1mm×18.0mm, and 30 turns were wound on the magnetic ring with an enamel wire of Φ0.51 mm. Measuring inductance value and Q value by adopting an Agilent E4980A LCR table, and calculating magnetic permeability by the inductance value; measuring the direct current superposition characteristics of the magnetic core by adopting an Agilent E4980A LCR table and an Agilent 42841A bias current source; the core power consumption was measured using a SY-8232B-H analyzer.
At the same time, for the commercially available products: products of different lot numbers of Shenzhen Jun Bright electronics Limited and American Micrometals were tested simultaneously as above and the results are shown in Table 1 below.
TABLE 1 detection results
The result shows that the carbonyl iron powder magnetic core with the magnetic permeability of mu=35 prepared by the method has the advantages of higher Q value, small power loss and good direct current superposition characteristic compared with the existing product.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any person skilled in the art may make modifications or alterations to the above disclosed technical content to equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (4)
1. The preparation method of the carbonyl iron powder magnetic core with the high Q value and the magnetic permeability of 35 is characterized by comprising the following steps:
(1) The carbonyl iron powder is proportioned according to different granularity and is uniformly mixed;
(2) Chemical film forming: pouring the phosphoric acid solution into the carbonyl iron powder which is uniformly mixed, mixing and stirring until the reaction is completed, and then drying;
(3) Granulating: after powder is chemically formed into a film, adding an insulating binding material, uniformly mixing, drying, granulating and sieving;
(4) And (5) press forming: adding lubricant into the sieved powder, uniformly mixing, and then performing compression molding;
(5) Core heat treatment: carrying out heat treatment on the pressed magnetic powder core in a furnace, and adopting a gradient heating mode; the heat treatment temperature is controlled between 60 ℃ and 160 ℃ and the heat treatment time is 2h to 4h;
(6) Surface coating: coating the surface of the magnetic powder core with epoxy resin paint by adopting a paint spraying process, and heating by an oven for curing;
in the step (1), the content of C in the carbonyl iron powder is less than or equal to 0.1 percent, the content of O is less than or equal to 0.4 percent, the content of N is less than or equal to 0.1 percent, and the balance is Fe;
the granularity proportion of the carbonyl iron powder is d10=3.5-5 mu m, d50=9-12 mu m, d90=21-25 mu m;
in the step (3), the insulating bonding material is epoxy resin and phenolic resin, and the weight ratio of the epoxy resin to the phenolic resin is 3:1-4: 1, a step of;
or the insulating bonding material is water glass and organic silicon resin, and the weight ratio of the water glass to the organic silicon resin is 1:5; the consumption of the insulating binding material is 0.4-0.7% of the weight of the carbonyl iron powder; granulating and sieving, namely sieving by a 40-80-mesh sieve, granulating, and drying in a drying oven at 80-100 ℃ for 15-30 min;
in the step (4), the lubricant is zinc stearate, and the dosage of the lubricant is 0.2-0.4% of the weight of the powder after sieving treatment;
in the step (5), the gradient heating mode is that after the temperature is raised from normal temperature to 60-80 ℃, the heating rate is 5 ℃/min, and the temperature is kept for 20-30 min at 60-80 ℃; heating from 60-80 ℃ to 80-120 ℃, heating up at a speed of 5-10 ℃/min, and preserving heat for 30-60 min at 80-120 ℃; heating from 80-120 ℃ to 120-150 ℃, heating up at a rate of 8-10 ℃/min, and preserving heat at 120-150 ℃ for 30-60 min; heating from 120-150 ℃ to 150-160 ℃, heating up at a speed of 8-10 ℃/min, and preserving heat for 30-60 min at 150-160 ℃.
2. The preparation method of claim 1, wherein in the step (2), the solvent of the phosphoric acid solution is acetone, alcohol or water, and the solution is prepared according to the volume ratio of phosphoric acid to the solvent of 1:20-100;
the consumption of the phosphoric acid is 0.3 to 0.6 percent of the weight of the carbonyl iron powder.
3. The process according to claim 1, wherein in the step (2), the reaction conditions are 40 to 85 ℃, and the completion of the reaction means drying the powder; the drying temperature is 80-150 ℃ and the drying time is 15-60 min.
4. The method according to claim 1, wherein in the step (4), the pressure of the press molding is 600 to 800MPa.
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| CN114496544A (en) * | 2022-02-24 | 2022-05-13 | 北京七星飞行电子有限公司 | Method for manufacturing low-power-consumption iron-nickel-molybdenum magnetic powder core |
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