CN111739730B - Preparation method of organic-coated high-performance metal magnetic powder core - Google Patents
Preparation method of organic-coated high-performance metal magnetic powder core Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 41
- 239000002184 metal Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 110
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 230000001050 lubricating effect Effects 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000011368 organic material Substances 0.000 claims abstract description 4
- 238000000889 atomisation Methods 0.000 claims abstract description 3
- 238000011049 filling Methods 0.000 claims abstract description 3
- 239000011812 mixed powder Substances 0.000 claims abstract description 3
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 239000004927 clay Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000009689 gas atomisation Methods 0.000 claims description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000010445 mica Substances 0.000 claims description 4
- 229910052618 mica group Inorganic materials 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 3
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 3
- 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 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- VAWNDNOTGRTLLU-UHFFFAOYSA-N iron molybdenum nickel Chemical compound [Fe].[Ni].[Mo] VAWNDNOTGRTLLU-UHFFFAOYSA-N 0.000 claims description 3
- -1 iron silicon aluminum Chemical compound 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- RVDLHGSZWAELAU-UHFFFAOYSA-N 5-tert-butylthiophene-2-carbonyl chloride Chemical compound CC(C)(C)C1=CC=C(C(Cl)=O)S1 RVDLHGSZWAELAU-UHFFFAOYSA-N 0.000 claims description 2
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 claims description 2
- CRGZYKWWYNQGEC-UHFFFAOYSA-N magnesium;methanolate Chemical compound [Mg+2].[O-]C.[O-]C CRGZYKWWYNQGEC-UHFFFAOYSA-N 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 239000011863 silicon-based powder Substances 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 125000000468 ketone group Chemical group 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 11
- 238000000465 moulding Methods 0.000 abstract description 2
- 239000011241 protective layer Substances 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 16
- 230000035699 permeability Effects 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 239000000696 magnetic material Substances 0.000 description 5
- 238000000748 compression moulding Methods 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 102220043159 rs587780996 Human genes 0.000 description 3
- UCOXGMHKZNIXKW-UHFFFAOYSA-N butan-2-ylalumane Chemical compound C(C)(CC)[AlH2] UCOXGMHKZNIXKW-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- 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
- H01F1/20—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 in the form of particles, e.g. powder
- H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—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 in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
-
- 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
- H01F1/20—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 in the form of particles, e.g. powder
- H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—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 in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
- H01F1/26—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 in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a high-performance metal magnetic powder core coated with organic materials, which comprises the following steps of (1) selecting metal soft magnetic powder obtained by an air atomization process, mixing an organic film forming material and an organic solvent to prepare an organic solution, and mixing and stirring the organic solution and the metal soft magnetic powder; (2) annealing the powder obtained in the step (1) at high temperature in a non-oxidizing atmosphere; (3) mixing the powder obtained in the step (2) with a passivating agent, stirring and mixing uniformly, (4) adding lubricating powder into the powder obtained in the step (3), mixing uniformly, filling the mixed powder into a die cavity of a press, and molding to prepare a blank; (5) and annealing the formed blank in a non-oxidizing atmosphere. According to the invention, before high-temperature treatment, an organic film forming material is adopted to carry out coating pretreatment on the metal soft magnetic powder, a layer of organic film is formed on the surface of the powder, a primary insulating protective layer is formed on the surface of a product after high-temperature heat treatment, and meanwhile, the lapping phenomenon among the powder is inhibited.
Description
Technical Field
The invention relates to the field of preparation of soft magnetic materials, in particular to a preparation method of a high-performance metal magnetic powder core coated with organic materials.
Background
The metal magnetic powder core is used as one of soft magnetic materials in magnetic materials, has low playing force, low loss and excellent permanent magnetic property, and is widely applied to power electronic equipment. The intelligent power grid power factor correction device is mainly applied to frequency conversion air conditioners, electric vehicle charging mould block power factor correction circuit reactors and rear-stage LC filter reactors, intelligent power grid power quality management, cloud computing center dynamic servers, machine room UPS power factor reactors, photovoltaic power generation grid-connected inverters and the like. Is an important soft magnetic material, and is particularly suitable for the aspect of high-end electronic industry. Recently, electronic devices are developed towards high frequency, large current, high efficiency and high power density, and the performance of metal soft magnetism is just following the development trend.
The main technological process of the metal soft magnetic powder core includes mixing metal soft magnetic powder and insulating material, coating one layer of compact insulating material on the surface of the powder, drying the powder, adding lubricating powder, molding in the mold of a press to form product in required shape, and final sintering in certain atmosphere and temperature condition to eliminate the internal stress in the product, reduce magnetic hysteresis loss, improve product performance and raise product strength to obtain product with excellent comprehensive performance. The surface of the product is coated with a layer of insulating material, so that the surface resistivity of the powder can be improved, and the eddy current among particles can be reduced, thereby reducing the eddy current loss of the magnetic powder core.
In order to better match the development direction of power electronics and adapt to the trend of high power density, high frequency, small size and large current, the performance of the metal soft magnetic powder core needs to be further improved, the inductance is improved, and the magnetic loss is reduced. The surface insulation coating of the metal soft magnetic powder has great effect on the product performance. The coating layer on the surface of the powder is required to be difficult to damage an insulating layer when the powder is molded under high pressure, and the insulating layer is also not damaged when the powder is subjected to heat treatment at a temperature higher than 700 ℃ in the subsequent sintering process, so that the product can be ensured to have a complete insulating layer after the heat treatment, and the product is ensured to have good eddy current loss. It is very important that the effective insulating film has good properties for the metallic soft magnetic powder core.
The loss of the metal soft magnet is composed of hysteresis loss and eddy current loss, and the method for reducing the eddy current loss is mentioned above. The hysteresis loss can be reduced by the following method. The powder is subjected to high-temperature heat treatment under a certain atmosphere before insulation coating, and the higher the heat treatment temperature is, the more helpful is in eliminating the internal stress of the powder and improving the hysteresis loss. Meanwhile, high-temperature heat treatment can soften the powder, improve the formability of the powder and improve the magnetic permeability of the powder. However, if the heat treatment temperature is too high, the powder tends to stick together. The powder is bonded together, which is not favorable for the performance of the metal soft magnetic powder core and can further increase the eddy current loss of the magnetic powder core. The heat treatment temperature is therefore generally limited and new stresses may be introduced if the heat treatment temperature is increased to cause the powders to bond, requiring a crushing process such as ball milling to separate the powders that are stuck together. There is therefore a need for a method that can solve the high temperature powder heat treatment problem.
Disclosure of Invention
The present invention is directed to a method for preparing a high performance metal magnetic powder core using an organic cladding to solve the problems set forth in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a high-performance metal magnetic powder core coated with organic materials comprises the following steps:
(1) selecting metal soft magnetic powder obtained by an air atomization process, mixing an organic film forming material and an organic solvent to prepare an organic solution, mixing and stirring the prepared solution and the metal soft magnetic powder for 30-60 minutes, and then drying;
(2) annealing the powder obtained in the step (1) at high temperature in a non-oxidizing atmosphere to form a compact oxide film on the surface of the powder;
(3) mixing the powder obtained in the step (2) with a passivating agent, stirring and uniformly mixing for 60-120 minutes, drying, and sieving with a 60-100-mesh sieve;
(4) adding lubricating powder into the powder obtained in the step (3), uniformly mixing, filling the mixed powder into a die cavity of a press, forming to prepare a blank, wherein the forming pressure is 18-22T/cm2；
(5) Annealing the formed blank in a non-oxidizing atmosphere, wherein the annealing conditions are as follows: heating to 500 ℃ at 300-.
Further: the drying treatment in the step (1) and the step (3) is drying for 2-9 hours at room temperature or drying in an oven.
Further, the metal soft magnetic powder is one or a mixture of iron-nickel powder, iron-nickel-molybdenum powder, iron-silicon powder and iron-silicon-aluminum powder obtained by a gas atomization process, the powder is spherical, the oxygen content is 200-900PPm, and the particle size range is D10: 6-15 microns, D50: 20-38 microns, D90: 45-80 microns.
Further, the organic film-forming substance in the step (1) is one or a mixture of more of aluminum sec-butoxide, magnesium methoxide, magnesium ethoxide, methyl organic silicon resin and phenyl organic silicon resin, and the mass ratio of the organic film-forming substance to the metal soft magnetic powder is 1-4%.
Further, the organic film-forming material described in the step (1) needs to be dissolved by an organic solvent to form an organic solution, and the solvent adopted in the invention is a ketone material, wherein the mass ratio of the ketone solvent to the iron-nickel powder is as follows: 8 to 15 percent.
Further, the high temperature in the step (2) is 800-950 ℃, and the heat treatment time is 60-120 minutes.
Further, the powder annealing atmosphere in the step (2) is nitrogen, hydrogen or a mixture of hydrogen and nitrogen.
Further, the passivating agent in the step (3) is formed by mixing an acidic substance, an oxide, clay powder and a solvent, wherein the acidic substance is phosphoric acid, oxalic acid, chromic acid, aluminum dihydrogen phosphate or a mixture of a plurality of substances, the oxide is 3-10nm of silicon dioxide, aluminum oxide or a mixture of silicon dioxide and aluminum oxide, and the clay powder is one or a mixture of 800-plus 1500-mesh kaolin, mica powder and diatomite powder; the solvent is organic solvent or water; the mass ratio of the passivating agent to the metal soft magnetic powder is 0.2-1.5%; the mass ratio of the acidic substance to the metal soft magnetic powder in the passivating agent is 0.05-0.6%; the mass ratio of the nano oxide to the metal soft magnetic powder in the passivating agent is 0.1-0.6%; the mass ratio of the clay powder to the metal soft magnetic powder in the passivating agent is 0.1-1.3%.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, before high-temperature treatment at 800-950 ℃, an organic film forming substance is adopted to carry out coating pretreatment on the metal soft magnetic powder, the metal powder and the organic metal are uniformly mixed and dried in a solution state, a layer of organic film is formed on the surface of the powder, a primary insulating protective layer is formed on the surface of a product after the high-temperature heat treatment condition, and meanwhile, the lapping phenomenon among the powder is inhibited. After the powder is subjected to high-temperature heat treatment, the internal stress of the powder is fully released, the formability of the powder can be improved, the product can reach higher density during forming, the product with better direct-current superposition characteristic can be obtained, and the magnetic powder core loss can be reduced.
After one-step high-temperature heat treatment film forming is finished, secondary insulation treatment is carried out on the product, and the adopted passivator consists of oxides and acid substances with different particle sizes. The oxide with different particle sizes can form a compact oxide film on the surface of the powder, and meanwhile, the oxide has a certain particle size, namely a layer of skeleton substances exists between the powder, so that the direct current superposition characteristic of the product is favorably improved, and the improvement of the constant magnetic property of the product is facilitated. The magnetic permeability of the product produced by the invention can reach more than 130, and the sintering temperature can reach more than 750 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Taking iron-nickel powder produced by a gas atomization process, wherein D50=35 and the oxygen content is 900 ppm. Taking the mass ratio of sec-butyl aluminum to iron-nickel powder to be 2 percent, the mass ratio of acetone to iron-nickel powder to be 10 percent, uniformly mixing the sec-butyl aluminum and acetone to prepare a solution, uniformly mixing the solution and the iron-nickel powder, stirring for 30-60 minutes at room temperature, forming a layer of uniform organic film on the surface of the powder, standing for 2-9 hours at room temperature until the powder is dried, sieving by using a 80-mesh sieve, and then carrying out heat treatment on the sieved powder under the condition of 850 ℃ and hydrogen atmosphere, wherein the obtained powder has no bonding phenomenon.
Preparing a passivating agent: according to the mass ratio of the oxalic acid to the iron-nickel powder, 0.03 percent of oxalic acid, 0.02 percent of aluminum dihydrogen phosphate, 0.006 percent of chromic acid, 0.1 percent of silica with the particle size of 3mm, 0.2 percent of mica powder and 8 percent of water are added into the powder, and the mixture is stirred for 30 minutes, dried at the temperature of 100 ℃ and sieved by a sieve with 80 meshes. Adding 0.35% lubricating powder into the powder subjected to secondary coating, mixing, and compression molding in a press at 20T/cm2Annealing the blank in a high temperature sintering furnaceAnd (4) treating, wherein the sintering conditions are 400 ℃ for 40 minutes, 730 ℃ for 60 minutes and hydrogen in the atmosphere. The magnetic core of the iron-nickel magnetic powder prepared by the process has magnetic permeability of 131, and power loss of 148mW/cm under the conditions of 50kHz and 100mT3。
Comparative example: under the same other conditions, the iron-nickel powder is not mixed with an aluminum sec-butoxide and an acetone solution, high-temperature treatment is not carried out, the magnetic permeability of the prepared iron-nickel magnetic powder core is 119, the power loss is 251mW/cm under the conditions of 50kHz and 100mT3。
Example 2:
taking iron-nickel powder produced by a gas atomization process, wherein D50=25 and the oxygen content is 400 ppm. Taking the organic silicon resin and iron-nickel powder in a mass ratio of 2%, the aluminum sec-butoxide and iron-nickel powder in a mass ratio of 2% and the acetone and iron-nickel powder in a mass ratio of 15%, uniformly mixing the solution and the iron-nickel powder to prepare a solution, stirring the solution and the iron-nickel powder at room temperature until the powder is dried, forming a layer of uniform organic film on the surface of the powder, drying the powder in an oven at the temperature of 80 ℃, sieving the powder with a sieve of 80 ℃, and then carrying out heat treatment on the sieved powder at the temperature of 950 ℃ in the atmosphere of mixed nitrogen and hydrogen gas.
Preparing a passivating agent: calculated according to the mass ratio of the iron-nickel powder, 0.05 percent of phosphoric acid, 0.1 percent of alumina, 0.3 percent of mica powder and 12 percent of propanol. Adding a passivating agent into the powder, stirring for 30 minutes, drying at 80 ℃, and sieving by a 80-mesh sieve. Adding 0.35% lubricating powder into the powder subjected to secondary coating, mixing, and compression molding in a press at 22T/cm2And annealing the blank in a high-temperature sintering furnace under the conditions of 400 ℃ for 40 minutes, 730 ℃ for 60 minutes and hydrogen atmosphere. The magnetic core permeability of the iron-nickel magnetic powder manufactured by the process is 125, and the power loss is 118mW/cm under the conditions of 50kHz and 100mT3。
Example 3:
taking iron-nickel powder produced by a gas atomization process, wherein D50=25 and the oxygen content is 900 ppm. Taking methyl organic silicon and iron-nickel powder in a mass ratio of 3.0 percent and acetone and iron-nickel powder in a mass ratio of 15 percent, uniformly mixing the methyl organic silicon and the acetone to prepare a solution, uniformly mixing the solution and the iron-nickel powder, stirring at room temperature until the powder is dried, forming a layer of uniform organic film on the surface of the powder, drying the powder in an oven at the temperature of 80 ℃, sieving by a sieve of 80 meshes, and then carrying out heat treatment on the sieved powder at the temperature of 800 ℃ in a nitrogen-hydrogen mixed gas atmosphere.
Preparing a passivating agent: according to the mass ratio of the oxalic acid to the iron-nickel powder, the oxalic acid is 0.4 percent, the phosphoric acid is 0.20 percent, the 10nm silicon dioxide is 0.2 percent, the kaolin is 1 percent, and the acetone is 8 percent. Adding a passivating agent into the powder, stirring for 30 minutes, drying at 100 ℃, and sieving by a 80-mesh sieve. Adding 0.4% lubricating powder into the powder subjected to secondary coating, mixing, and compression molding in a press at 20T/cm2And annealing the blank in a high-temperature sintering furnace under the conditions of 400-40 minutes at 700-60 minutes in hydrogen atmosphere. The magnetic core has magnetic permeability of 62, power loss of 188mW/cm at 50kHz and 100mT3。
Comparative example: under the same other conditions, the iron-nickel powder is not mixed with acetone solution without methyl organosilicon, and is not subjected to high-temperature treatment, the magnetic permeability of the prepared iron-nickel magnetic powder core is 54, the power loss is 262mW/cm under the conditions of 50kHz and 100mT3。
The method can also be applied to other soft magnetic materials, such as iron nickel molybdenum powder, iron silicon aluminum powder and the like.
The basic principles of the invention and the advantages of the invention have been shown and described above, and the properties of the powder heat treated at high temperatures according to the invention are significantly improved compared to the non-heat treated powder.
The passivation solution prepared by the invention is matched with the heat treatment powder, and the prepared metal soft magnetic powder core has lower loss.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (3)
1. A preparation method of a high-performance metal magnetic powder core coated with organic materials is characterized by comprising the following steps:
(1) selecting metal soft magnetic powder obtained by an air atomization process, mixing an organic film forming material and an organic solvent to prepare an organic solution, mixing and stirring the prepared solution and the metal soft magnetic powder for 30-60 minutes, and then drying; wherein the organic film forming substance is one or a mixture of more of aluminum sec-butoxide, magnesium methoxide, magnesium ethoxide, methyl organic silicon resin and phenyl organic silicon resin, and the mass ratio of the organic film forming substance to the metal soft magnetic powder is 1-4%; the organic solvent is a ketone substance, and the mass ratio of the ketone substance to the metal soft magnetic powder is 8-15%;
(2) annealing the powder obtained in the step (1) at high temperature in a non-oxidizing atmosphere to form a compact oxide film on the surface of the powder; wherein the high temperature is 800-950 ℃, the heat treatment time is 60-120 minutes, and the powder annealing atmosphere is nitrogen, hydrogen or mixed gas of hydrogen and nitrogen;
(3) mixing the powder obtained in the step (2) with a passivating agent, stirring and uniformly mixing for 60-120 minutes, drying, and sieving with a 60-100-mesh sieve; wherein the passivating agent is formed by mixing an acidic substance, an oxide, clay powder and a solvent; the acidic substance is phosphoric acid, oxalic acid, chromic acid, aluminum dihydrogen phosphate or a mixture of a plurality of substances, the oxide is silicon dioxide with the granularity of 3-10nm, aluminum oxide or a mixture of the silicon dioxide and the aluminum oxide, and the clay powder is one or a mixture of 800-plus-1500-mesh kaolin, mica powder and diatomite powder; the solvent is organic solvent or water; the mass ratio of the passivating agent to the metal soft magnetic powder is 0.2-1.5%; the mass ratio of the acidic substance to the metal soft magnetic powder in the passivating agent is 0.05-0.6%; the mass ratio of the oxide to the metal soft magnetic powder in the passivating agent is 0.1-0.6%; the mass ratio of the clay powder to the metal soft magnetic powder in the passivating agent is 0.1-1.3%;
(4) adding lubricating powder into the powder obtained in the step (3), uniformly mixing, filling the mixed powder into a die cavity of a press, forming to prepare a blank, wherein the forming pressure is 18-22T/cm2；
(5) Annealing the formed blank in a non-oxidizing atmosphere, wherein the annealing conditions are as follows: heating to 500 ℃ at 300 ℃, keeping the temperature for 30-60 minutes, then heating to 780 ℃ at 720 ℃, and keeping the temperature for 40-80 minutes, wherein the non-oxidizing atmosphere is at least one gas of nitrogen, argon and hydrogen.
2. The method for preparing a high-performance metal magnetic powder core by using organic coating according to claim 1, wherein the drying treatment in the step (1) and the step (3) is drying at room temperature for 2-9 hours or drying in an oven.
3. The method for preparing a high-performance metal magnetic powder core using organic coating as claimed in claim 1, wherein the metal soft magnetic powder in step (1) is one or more of iron nickel powder, iron nickel molybdenum powder, iron silicon powder and iron silicon aluminum powder obtained by gas atomization process, the powder is spherical, the oxygen content is 200-900PPm, the particle size range is D10: 6-15 microns, D50: 20-38 microns or D90: 45-80 microns.
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| JP2023552401A (en) * | 2020-12-04 | 2023-12-15 | 横店集団東磁股▲ふん▼有限公司 | Integrated co-firing inductor and its manufacturing method |
| CN113470915B (en) * | 2021-06-02 | 2024-04-05 | 昆山磁通新材料科技有限公司 | Soft magnetic composite material and preparation method and application thereof |
| CN114284014A (en) * | 2021-12-24 | 2022-04-05 | 东莞市铭燕电子有限公司 | High-temperature non-aging iron powder core and preparation method thereof |
| CN114255981B (en) * | 2021-12-29 | 2023-04-28 | 西南科技大学 | Preparation method of iron-nickel-molybdenum/silicon dioxide soft magnetic powder core composite material |
| CN115938718B (en) * | 2023-03-09 | 2023-05-30 | 天通控股股份有限公司 | Direct-insert integrated cofiring inductor and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004319652A (en) * | 2003-04-15 | 2004-11-11 | Tamura Seisakusho Co Ltd | Core and method of manufacturing the same |
| JP2007273929A (en) * | 2006-03-31 | 2007-10-18 | Dowa Holdings Co Ltd | Insulation coating soft magnetic metallic powder, pressed powder core, and their manufacturing method |
| CN103377786A (en) * | 2013-07-10 | 2013-10-30 | 浙江大学 | Preparation method for iron-silicon-aluminum alloy magnetic powder core |
| CN104028749A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-thermal-stability insulated coating treatment method of metal soft magnetic composite material |
| CN104028751A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-insulativity insulated coating treatment method of metal soft magnetic composite material |
| CN105225783A (en) * | 2015-11-05 | 2016-01-06 | 东莞铭普光磁股份有限公司 | The preparation method of the coated powder core of a kind of epoxy modified silicone resin |
| CN107578874A (en) * | 2017-09-14 | 2018-01-12 | 横店集团东磁股份有限公司 | A kind of preparation method of the iron nickel powder core of magnetic permeability μ=200 |
-
2020
- 2020-08-27 CN CN202010875571.5A patent/CN111739730B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004319652A (en) * | 2003-04-15 | 2004-11-11 | Tamura Seisakusho Co Ltd | Core and method of manufacturing the same |
| JP2007273929A (en) * | 2006-03-31 | 2007-10-18 | Dowa Holdings Co Ltd | Insulation coating soft magnetic metallic powder, pressed powder core, and their manufacturing method |
| CN103377786A (en) * | 2013-07-10 | 2013-10-30 | 浙江大学 | Preparation method for iron-silicon-aluminum alloy magnetic powder core |
| CN104028749A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-thermal-stability insulated coating treatment method of metal soft magnetic composite material |
| CN104028751A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | High-insulativity insulated coating treatment method of metal soft magnetic composite material |
| CN105225783A (en) * | 2015-11-05 | 2016-01-06 | 东莞铭普光磁股份有限公司 | The preparation method of the coated powder core of a kind of epoxy modified silicone resin |
| CN107578874A (en) * | 2017-09-14 | 2018-01-12 | 横店集团东磁股份有限公司 | A kind of preparation method of the iron nickel powder core of magnetic permeability μ=200 |
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