CN113744989A - Metal magnetic powder core and preparation method and application thereof - Google Patents
Metal magnetic powder core and preparation method and application thereof Download PDFInfo
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- CN113744989A CN113744989A CN202111027349.0A CN202111027349A CN113744989A CN 113744989 A CN113744989 A CN 113744989A CN 202111027349 A CN202111027349 A CN 202111027349A CN 113744989 A CN113744989 A CN 113744989A
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 149
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 146
- 239000002184 metal Substances 0.000 title claims abstract description 146
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 98
- 239000002245 particle Substances 0.000 claims abstract description 43
- 229940024546 aluminum hydroxide gel Drugs 0.000 claims abstract description 38
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 38
- 238000009413 insulation Methods 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000007873 sieving Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 238000000465 moulding Methods 0.000 claims abstract description 12
- 230000001050 lubricating effect Effects 0.000 claims abstract description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 229910000702 sendust Inorganic materials 0.000 claims description 31
- 238000002161 passivation Methods 0.000 claims description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 15
- 229940063655 aluminum stearate Drugs 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 11
- 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 11
- 239000007787 solid Substances 0.000 claims description 9
- 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 8
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 8
- 235000019359 magnesium stearate Nutrition 0.000 claims description 6
- 239000000696 magnetic material Substances 0.000 claims description 3
- 239000000314 lubricant Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002923 metal particle Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 15
- 239000010410 layer Substances 0.000 description 49
- 239000007789 gas Substances 0.000 description 33
- 230000000052 comparative effect Effects 0.000 description 17
- 238000000576 coating method Methods 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- VAWNDNOTGRTLLU-UHFFFAOYSA-N iron molybdenum nickel Chemical compound [Fe].[Ni].[Mo] VAWNDNOTGRTLLU-UHFFFAOYSA-N 0.000 description 7
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- XEVZIAVUCQDJFL-UHFFFAOYSA-N [Cr].[Fe].[Si] Chemical compound [Cr].[Fe].[Si] XEVZIAVUCQDJFL-UHFFFAOYSA-N 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- -1 for example Substances 0.000 description 6
- 229920002050 silicone resin Polymers 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009689 gas atomisation Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000003929 acidic solution Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F3/00—Cores, Yokes, or armatures
- H01F3/08—Cores, Yokes, or armatures made from powder
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a metal magnetic powder core and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing metal magnetic powder and a passivating agent into slurry; mixing the aluminum hydroxide gel with the slurry, and then sequentially drying and sieving; and mixing the lubricating powder with the powder obtained by sieving, pressing and molding, and then carrying out heating treatment to obtain the metal magnetic powder core. The surface of the metal magnetic powder particles is passivated by adopting a passivating agent, then aluminum hydroxide gel is added, and the passivating agent and the aluminum hydroxide gel react on the surfaces of the metal magnetic powder particles to generate the aluminum oxide insulating layer. The metal magnetic powder core provided by the invention has better insulation effect and high temperature resistance, and ensures the insulation effect among metal magnetic powder particles, thereby greatly reducing the eddy current loss.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, relates to a magnetic powder core, and particularly relates to a metal magnetic powder core and a preparation method and application thereof.
Background
The metal magnetic powder core has high saturation magnetic field intensity and soft package characteristic, can be used for reducing the volume of a magnetic core device, but has low resistivity, and when the metal magnetic powder core is used under a high-frequency circuit, the eddy current loss is high, so that the device is easy to generate heat. Therefore, reducing eddy current loss becomes a key to solve the application of the metal magnetic powder core in high frequency circuits. One of the effective methods for reducing eddy current loss is to perform insulation coating on the surface of the metal magnetic powder particles.
The existing insulation coating method has two modes, one mode is passivation insulation by using a pure acidic solution, for example, passivation treatment by using an acidic solution such as phosphoric acid, chromic acid and the like. And the other is to add organic resin or water glass to cover and increase the insulation effect after the passivation of the acid solution, for example, phosphoric acid and silicon resin are utilized, and phosphoric acid and phenolic resin are used for the covering after the passivation. Although the two methods have certain insulation effect, the defects are obvious, for example, when pure phosphoric acid solution is used for passivating insulation, the insulation effect is insufficient due to the single insulation layer, and meanwhile, the insulation layer is easy to peel off under stress when metal magnetic powder is pressed. Although the insulation effect is improved by the insulation mode of phosphoric acid and organic resin, the problem of binder removal cracking exists in the metal magnetic powder core during heat treatment, and the addition of too much organic resin can reduce the product density and reduce the stacking characteristic due to larger volume of the organic resin.
CN 111029076a discloses a gas atomized sendust soft magnetic composite material with low intermediate frequency loss, which is made of three gas atomized sendust powders with different particle size ranges. The preparation method disclosed by the invention comprises the steps of firstly mixing absolute ethyl alcohol with silicon dioxide to obtain mixed insulating slurry and then drying the mixed insulating slurry; and crushing and sieving the dried powder, and then adding organic silicon resin for insulation coating. Silicon dioxide is adopted for insulation coating, because the silicon dioxide is a powder material and has no cohesiveness, the soft magnetic metal powder cannot be coated, and the soft magnetic metal powder and the silicon dioxide are powder with different particle sizes, so that particle size segregation is easily generated during mixing, and the insulation effect is influenced; in addition, the addition of silicone resin can cause the problem of binder removal cracking during heat treatment.
CN 107464650A discloses a high-temperature heat-resistant metal soft magnetic powder core, which is composed of metal soft magnetic powder and silicone resin, wherein the mass ratio of the metal soft magnetic powder to the silicone resin is (0.5-5): 100. The method for insulating and coating by using the silicone resin is disclosed, and the silicone resin and the metal soft magnetic powder are difficult to be uniformly mixed, and the silicone resin powder and the metal soft magnetic powder have large particle density difference and are easy to segregate to further cause uneven coating; in addition, the addition of the organic silicon resin requires low-temperature air heat treatment once and then annealing in an inert gas atmosphere, so that the preparation method is complex, the cost is high, and the problem of heat treatment glue discharge is caused.
CN 101089108A discloses an inorganic insulating adhesive for a metal soft magnetic powder core and a preparation method thereof, wherein the inorganic insulating adhesive is made of SiO2、Al2O3、ZrO2Mica powder and water. Although the disclosed method does not use an organic binder, and can avoid the problem of binder removal caused by heat generation of the metal soft magnetic powder core in the using process, the inorganic insulating binder is only attached to the surface of the powder in a physical adsorption mode, and the inorganic insulating binder is unevenly distributed on the surface of the soft magnetic metal powder in the processes of press forming and the like, so that the insulating effect is poor.
Based on the above research, how to provide a metal magnetic powder core, the insulating layer with better insulating effect is provided on the surface of the powder particles to ensure the insulating effect among the powder particles, and meanwhile, the metal magnetic powder core has high temperature resistance, and can reduce the eddy current loss phenomenon when being used under a high-frequency circuit, thereby becoming a problem which needs to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a metal magnetic powder core and a preparation method and application thereof, wherein the metal magnetic powder core has better insulating effect and high temperature resistance, can ensure the insulating effect among metal magnetic powder particles, and greatly reduces eddy current loss.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a metal magnetic powder core, comprising the steps of:
(1) mixing metal magnetic powder and a passivating agent into slurry;
(2) mixing the aluminum hydroxide gel with the slurry obtained in the step (1), and then drying and sieving the mixture in sequence;
(3) and (3) mixing the lubricating powder with the powder obtained by sieving in the step (2), pressing and molding, and then performing heating treatment to obtain the metal magnetic powder core.
Firstly, passivating the surface of metal magnetic powder particles by adopting a passivating agent to generate a primary insulating layer; then adding aluminum hydroxide gel for secondary coating, wherein the primary coating passivator and the secondary coating material aluminum hydroxide gel react on the surfaces of the metal magnetic powder particles and uniformly precipitate and separate out an aluminum oxide insulating layer. Therefore, the coating layer of the metal magnetic powder core is the passivation layer and the aluminum oxide insulating layer, the coating layer makes up the defects of easy peeling and high-temperature decomposition of a pure passivation layer coating, and the high-temperature resistance and high-insulation characteristics of aluminum oxide are utilized, so that the obtained metal magnetic powder core has better insulation effect and high-temperature resistance, the insulation effect among metal magnetic powder particles is ensured, and the eddy current loss is greatly reduced.
Preferably, the metal magnetic powder in step (1) is atomized metal magnetic powder.
Preferably, the average particle size of the metal magnetic powder in step (1) is 1 to 100 μm, for example, 1 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the metal magnetic powder in step (1) comprises any one or a combination of at least two of sendust, sendust or sendust, and typical but non-limiting combinations include sendust and sendust, and sendust or a combination of sendust and sendust.
Preferably, the passivating agent in step (1) is added in an amount of 0.1 to 3 wt% of the metal magnetic powder, for example, 0.1 wt%, 0.25 wt%, 0.5 wt%, 0.75 wt%, 1 wt%, 1.25 wt%, 1.5 wt%, 1.75 wt%, 2 wt%, 2.25 wt%, 2.5 wt%, 2.75 wt%, or 3 wt%, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the metal magnetic powder, the passivating agent and the aqueous slurry are mixed in the step (1), and the water is added in an amount of 1-10 wt% of the metal magnetic powder, for example, 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt% or 10 wt%, but not limited to the recited values, and other values in the range of the recited values are also applicable.
Preferably, the passivating agent comprises any one or a combination of at least two of phosphoric acid, chromic acid or aluminium dihydrogen phosphate, typical but non-limiting combinations include a combination of phosphoric acid and chromic acid, a combination of phosphoric acid and aluminium dihydrogen phosphate or a combination of chromic acid and aluminium dihydrogen phosphate, preferably phosphoric acid.
Preferably, the mixing in step (1) is stirring mixing for 3-10 min, such as 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, but not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, the solid content of the aluminum hydroxide gel in the step (2) is 15 to 35 wt%, for example, 15 wt%, 17.5 wt%, 20 wt%, 22.5 wt%, 25 wt%, 27.5 wt%, 30 wt%, 32.5 wt% or 35 wt%, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the aluminum hydroxide gel of step (2) is added in an amount of 0.1 to 3 wt% of the metal magnetic powder, for example, 0.1 wt%, 0.25 wt%, 0.5 wt%, 0.75 wt%, 1 wt%, 1.25 wt%, 1.5 wt%, 1.75 wt%, 2 wt%, 2.25 wt%, 2.5 wt%, 2.75 wt%, or 3 wt%, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the mixing in step (2) is stirring mixing for 3-10 min, such as 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, but not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, the temperature of the drying in step (2) is 150 to 250 ℃, for example, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃ or 250 ℃, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the drying time in step (2) is 1.5 to 2.5 hours, such as 1.5 hours, 1.6 hours, 1.7 hours, 1.8 hours, 1.9 hours, 2.0 hours, 2.1 hours, 2.2 hours, 2.3 hours, 2.4 hours or 2.5 hours, but not limited to the recited values, and other values in the range of the recited values are also applicable.
Preferably, the mesh size of the screen in step (2) is 50 to 100 meshes, such as 50 meshes, 55 meshes, 60 meshes, 65 meshes, 70 meshes, 75 meshes, 80 meshes, 85 meshes, 90 meshes, 95 meshes or 100 meshes, but not limited to the listed values, and other values not listed in the range of values are also applicable.
Preferably, the lubricant powder added in step (3) is 0.1 to 1.0 wt% of the metal magnetic powder, and may be, for example, 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.6 wt%, 0.7 wt%, 0.8 wt%, 0.9 wt%, or 1.0 wt%, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the lubricating powder of step (3) comprises any one of, or a combination of at least two of, aluminum stearate, zinc stearate, or magnesium stearate, with typical but non-limiting combinations comprising a combination of aluminum stearate and zinc stearate, a combination of aluminum stearate and magnesium stearate, or a combination of zinc stearate and magnesium stearate, preferably aluminum stearate.
Preferably, the pressure of the compression molding in the step (3) is 10-22 t/cm2For example, it may be 10t/cm2、11t/cm2、12t/cm2、13t/cm2、14t/cm2、15t/cm2、16t/cm2、17t/cm2、18t/cm2、19t/cm2、20t/cm2、21t/cm2Or 22t/cm2But are not limited to the recited values, and other values within the numerical range not recited are equally applicable.
Preferably, the temperature of the heat treatment in step (3) is 600 to 800 ℃, for example, 600 ℃, 625 ℃, 650 ℃, 675 ℃, 700 ℃, 725 ℃, 750 ℃, 775 ℃ or 800 ℃, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the time of the heat treatment in the step (3) is 1 to 2 hours, for example, 1 hour, 1.1 hour, 1.2 hours, 1.3 hours, 1.4 hours, 1.5 hours, 1.6 hours, 1.7 hours, 1.8 hours, 1.9 hours or 2 hours, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) stirring mixed metal magnetic powder, a passivating agent and water for 3-10 min to obtain slurry; the addition amount of the passivating agent is 0.1-3 wt% of the metal magnetic powder, and the addition amount of the water is 1-10 wt% of the metal magnetic powder;
(2) stirring and mixing aluminum hydroxide gel with a solid content of 15-35 wt% and the slurry in the step (1) for 3-10 min, drying at 150-250 ℃ for 1.5-2.5 h in sequence, and sieving with a 50-100-mesh sieve; the addition amount of the aluminum hydroxide gel is 0.1-3 wt% of the metal magnetic powder;
(3) mixing the lubricating powder with the powder obtained by sieving in the step (2) at the speed of 10-22 t/cm2Pressing and forming under pressure, and then carrying out heating treatment at 600-800 ℃ for 1-2 h to obtain the metal magnetic powder core; the addition amount of the lubricating powder is 0.1-1.0 wt% of the metal magnetic powder.
In a second aspect, the present invention provides a metal magnetic powder core obtained by the preparation method according to the first aspect.
Preferably, the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an alumina insulation layer.
In a third aspect, the present invention provides a use of the metal magnetic powder core according to the first aspect as a magnetic material.
Compared with the prior art, the invention has the following beneficial effects:
the invention firstly passivates the surface of the metal magnetic powder particles, then adds aluminum hydroxide gel for coating, and the passivator reacts with the aluminum hydroxide gel to generate an aluminum oxide insulating layer, the coating overcomes the defects of easy peeling and high-temperature decomposition of a pure passivation layer coating.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a metal magnetic powder core, the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an alumina insulation layer, and the preparation method of the metal magnetic powder core comprises the following steps:
(1) stirring the mixed gas to atomize iron-silicon-aluminum (FeSiAl-85-9.5-5.5, trade mark: sendust) powder, phosphoric acid and water for 5min to obtain slurry; the average grain size of the gas atomized sendust powder is 50 microns, the addition amount of the phosphoric acid is 1.5 wt% of the gas atomized sendust powder, and the addition amount of the water is 5 wt% of the gas atomized sendust powder;
(2) stirring and mixing 25 wt% of aluminum hydroxide gel with the slurry obtained in the step (1) for 5min, drying at 200 ℃ for 2h, and sieving with a 70-mesh sieve; the addition amount of the aluminum hydroxide gel is 1.5 wt% of the gas atomized ferrosilicon aluminum powder;
(3) mixing the aluminum stearate with the powder sieved in the step (2) at 15t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 700 ℃ for 1.5h to obtain the metal magnetic powder core; the addition amount of the aluminum stearate is 5 wt% of the gas atomized ferrum-silicon-aluminum powder.
Example 2
The embodiment provides a metal magnetic powder core, the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an alumina insulation layer, and the preparation method of the metal magnetic powder core comprises the following steps:
(1) stirring the mixed gas to atomize iron-nickel (FeNi-50-50, High-Flux) powder, chromic acid and water for 10min to obtain slurry; the average particle size of the gas atomized iron-nickel powder is 75 micrometers, the addition amount of chromic acid is 2 wt% of the gas atomized iron-nickel powder, and the addition amount of water is 7.5 wt% of the gas atomized iron-nickel powder;
(2) stirring and mixing the aluminum hydroxide gel with the solid content of 20 wt% and the slurry in the step (1) for 3min, drying at 150 ℃ for 2.5h in sequence, and sieving by a 50-mesh sieve; the addition amount of the aluminum hydroxide gel is 1 wt% of the gas atomized iron-nickel powder;
(3) mixing zinc stearate with the powder sieved in the step (2) at 20t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 750 ℃ for 1h to obtain the metal magnetic powder core; the addition amount of the zinc stearate is 1.0 wt% of the gas atomized iron-nickel powder.
Example 3
The embodiment provides a metal magnetic powder core, the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an alumina insulation layer, and the preparation method of the metal magnetic powder core comprises the following steps:
(1) stirring and mixing iron-nickel-molybdenum (Fe-Ni-Mo-17-81-2, trade mark: MPP) powder atomized by water, aluminium dihydrogen phosphate and water for 3min to obtain slurry; the average particle size of the water atomized iron nickel molybdenum powder is 25 micrometers, the addition amount of the aluminum dihydrogen phosphate is 1 wt% of the water atomized iron nickel molybdenum powder, and the addition amount of the water is 2.5 wt% of the water atomized iron nickel molybdenum powder;
(2) stirring and mixing the aluminum hydroxide gel with the solid content of 30 wt% and the slurry in the step (1) for 10min, drying at 250 ℃ for 1.5h, and sieving with a 100-mesh sieve; the addition amount of the aluminum hydroxide gel is 2 wt% of the water atomized iron-nickel-molybdenum powder;
(3) mixing magnesium stearate with the powder sieved in the step (2) at 10t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 650 ℃ for 2h to obtain the metal magnetic powder core; the addition amount of the magnesium stearate is 0.1 wt% of the water atomized iron-nickel-molybdenum powder.
Example 4
The embodiment provides a metal magnetic powder core, the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an alumina insulation layer, and the preparation method of the metal magnetic powder core comprises the following steps:
(1) stirring and mixing the iron-silicon-chromium (Fe-Si-Cr-92-4.5-3.5) powder, chromic acid and water for 10min to obtain slurry; the average particle size of the water atomized iron-silicon-chromium powder is 100 micrometers, the addition amount of chromic acid is 3 wt% of the water atomized iron-silicon-chromium powder, and the addition amount of water is 10 wt% of the water atomized iron-silicon-chromium powder;
(2) stirring and mixing aluminum hydroxide gel with the solid content of 15 wt% and the slurry in the step (1) for 3min, drying at 150 ℃ for 2.5h in sequence, and sieving by a 50-mesh sieve; the addition amount of the aluminum hydroxide gel is 0.1 wt% of the water atomized iron-silicon-chromium powder;
(3) mixing zinc stearate with the powder sieved in the step (2) at 22t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 800 ℃ for 2h to obtain the metal magnetic powder core; the addition amount of the zinc stearate is 1.0 wt% of the water atomized iron-silicon-chromium powder.
Example 5
The embodiment provides a metal magnetic powder core, the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an alumina insulation layer, and the preparation method of the metal magnetic powder core comprises the following steps:
(1) stirring the mixed gas to atomize iron-silicon-aluminum (FeSiAl-85-9.5-5.5, trade mark: sendust) powder, phosphoric acid and water for 3min to obtain slurry; the average grain size of the gas atomized sendust powder is 1 mu m, the addition amount of the phosphoric acid is 0.1 wt% of the gas atomized sendust powder, and the addition amount of the water is 1 wt% of the gas atomized sendust powder;
(2) stirring and mixing aluminum hydroxide gel with the solid content of 35 wt% and the slurry in the step (1) for 10min, drying at 250 ℃ for 1.5h in sequence, and sieving by a 100-mesh sieve; the addition amount of the aluminum hydroxide gel is 3 wt% of the gas atomized ferrosilicon aluminum powder;
(3) mixing the aluminum stearate with the powder sieved in the step (2) at the ratio of 10t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 600 ℃ for 2h to obtain the metal magnetic powder core; the addition amount of the aluminum stearate is 0.1 wt% of the gas atomized ferrum-silicon-aluminum powder.
Example 6
The embodiment provides a metal magnetic powder core, wherein the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an aluminum oxide insulating layer.
The preparation method of the metal magnetic powder core is different from that of the embodiment 1 only in that the metal magnetic powder is gas atomized iron-nickel (FeNi-50-50, brand: High-Flux) powder, and the rest is the same as that of the embodiment 1
Example 7
The embodiment provides a metal magnetic powder core, wherein the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an aluminum oxide insulating layer.
The preparation method of the metal magnetic powder core is different from that of the example 1 only in that the metal magnetic powder is gas atomized iron nickel molybdenum (Fe-Ni-Mo-17-81-2, trade mark: MPP) powder, and the rest is the same as that of the example 1.
Example 8
The embodiment provides a metal magnetic powder core, wherein the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an aluminum oxide insulating layer.
The preparation method of the metal magnetic powder core is different from that of the embodiment 1 only in that chromic acid is used as a passivating agent, namely, the quality of phosphoric acid and the like is replaced by chromic acid, and the rest is the same as that of the embodiment 1.
Example 9
The embodiment provides a metal magnetic powder core, wherein the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an aluminum oxide insulating layer.
The preparation method of the metal magnetic powder core is different from that of the embodiment 1 only in that aluminum dihydrogen phosphate is used as a passivating agent, namely, the mass of phosphoric acid is replaced by that of aluminum dihydrogen phosphate, and the rest is the same as that of the embodiment 1.
Example 10
The embodiment provides a metal magnetic powder core, wherein the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an aluminum oxide insulating layer.
The preparation method of the metallic magnetic powder core is different from that of example 1 only in that the aluminum hydroxide gel is added in an amount of 0.08 wt% based on the weight of the gas atomized sendust powder, and the rest is the same as example 1.
Example 11
The embodiment provides a metal magnetic powder core, wherein the surface of the powder particle of the metal magnetic powder core is coated with a passivation layer and an aluminum oxide insulating layer.
The preparation method of the metallic magnetic powder core is different from that of example 1 only in that the aluminum hydroxide gel is added in an amount of 4 wt% of the gas atomized sendust powder, and the rest is the same as example 1.
Comparative example 1
The present comparative example provides a metal magnetic powder core, the surface of the powder particle of which is coated with a passivation layer, and the preparation method of the metal magnetic powder core comprises the following steps:
(1) gas atomization iron silicon aluminum (FeSiAl-85-9.5-5.5, trade mark: sendust) powder, phosphoric acid and water are stirred and mixed for 5min, and then are dried for 2h at 200 ℃; the particle size of the gas atomized sendust powder is 50 microns, the addition amount of the phosphoric acid is 1.5 wt% of the gas atomized sendust powder, and the addition amount of the water is 5 wt% of the gas atomized sendust powder;
(2) mixing the aluminum stearate with the powder obtained by drying in the step (1) at 15t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 700 ℃ for 1.5h to obtain the metal magnetic powder core; the addition amount of the aluminum stearate is 5 wt% of the gas atomized ferrum-silicon-aluminum powder.
Comparative example 2
The comparative example provides a metal magnetic powder core, the surface of which is coated with an aluminum hydroxide gel layer, and the preparation method of the metal magnetic powder core comprises the following steps:
(1) gas atomization iron silicon aluminum (FeSiAl-85-9.5-5.5, trade mark: sendust) powder and aluminum hydroxide gel with the solid content of 25 wt% are stirred and mixed for 5min, and then are dried for 2h at 200 ℃ in sequence, and are sieved by a 70-mesh sieve; the addition amount of the aluminum hydroxide gel is 1.5 wt% of the gas atomized ferrosilicon aluminum powder;
(2) mixing the aluminum stearate with the powder sieved in the step (1) at 15t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 700 ℃ for 1.5h to obtain the metal magnetic powder core; the addition amount of the aluminum stearate is 5 wt% of the gas atomized ferrum-silicon-aluminum powder.
Comparative example 3
The present comparative example provides a metal magnetic powder core coated with an alumina layer, and a method for preparing the metal magnetic powder core includes the steps of:
(1) gas atomization iron silicon aluminum (FeSiAl-85-9.5-5.5, trade mark: sendust) powder, aluminum oxide and water are stirred and mixed for 5min, and then are dried for 2h at 200 ℃ in sequence, and are sieved by a 70-mesh sieve; the addition amount of the alumina is 1.5 wt% of the gas atomized sendust powder, and the addition amount of the water is 5 wt% of the gas atomized sendust powder;
(2) mixing the aluminum stearate with the powder sieved in the step (1) at 15t/cm2Pressing and molding under pressure, and then carrying out heating treatment at 700 ℃ for 1.5h to obtain the metal magnetic powder core; the addition amount of the aluminum stearate is 5 wt% of the gas atomized ferrum-silicon-aluminum powder.
The test conditions and test results of the above examples and comparative examples are as follows:
and (3) testing conditions are as follows: the metal magnetic powder cores provided in the above examples and comparative examples were made into annular magnetic rings with dimensions of o.d: 29.90mm, I.D: 14.70mm, HT: 11.20 mm; permeability was tested using an HP-8248A LCR analyzer under conditions of 100khz x 1V 36 Ts.
The electromagnetic property test results are shown in table 1:
TABLE 1
From table 1, the following points can be seen:
(1) the surface of the metal magnetic powder core powder particles is coated with a passivation layer and an aluminum oxide insulating layer; passivating the surface of the metal magnetic powder core powder particles by adopting a passivating agent, adding aluminum hydroxide gel to react with the passivating agent, and generating an aluminum oxide insulating layer on the surface of the metal magnetic powder core powder particles. The metal magnetic powder core provided by the invention has good insulation effect and high temperature resistance, the magnetic conductivity is 58-62 mu, the direct current bias percentage of the 100Oe magnetic conductivity is 56.8-60%, and the loss under 50kHz/100mt is 180-198 mw/cc.
(2) By combining the embodiment 1 and the embodiments 8-9, the phosphoric acid is used as a preferable passivating agent, so that the insulating property of the metal magnetic powder core can be better improved, and the loss is reduced; it is understood from the combination of example 1 and examples 10 to 11 that when the amount of aluminum hydroxide gel added is too small or too large, the insulating property of the metal magnetic powder core is slightly lowered, and the loss is increased.
(3) As can be seen from the combination of example 1 and comparative example 1, the cladding layer of the metallic magnetic powder core provided in comparative example 1 includes only the passivation layer, and since the single passivation layer is easily peeled off and decomposed at high temperature, the insulating property of the metallic magnetic powder core provided in comparative example 1 is poor and the loss is high compared to example 1.
(4) Combining example 1 with comparative example 2, it can be seen that the cladding layer of the metal magnetic powder core provided in comparative example 2 only comprises the aluminum hydroxide gel layer, and the aluminum hydroxide gel layer cannot uniformly clad the metal magnetic powder, and the surface of the metal magnetic powder particle is not passivated, so that the metal magnetic powder core provided in comparative example 2 has poor insulating property and high loss.
(5) It can be seen from the combination of example 1 and comparative example 3 that the cladding layer of the metal magnetic powder core provided in comparative example 3 only comprises an alumina layer, and since the alumina powder body has no cohesiveness, the alumina powder body can only be attached to the surface of the metal magnetic powder particles in a physical adsorption manner, and is unevenly distributed on the surface of the metal magnetic powder particles, the insulating property of the metal magnetic powder core provided in comparative example 3 is poor, and the loss is high.
In summary, the invention provides a metal magnetic powder core and a preparation method and application thereof, the surface of metal magnetic powder particles is passivated by adopting a passivating agent, then aluminum hydroxide gel is added, and the passivating agent and the aluminum hydroxide gel react on the surface of the metal magnetic powder particles to generate an aluminum oxide insulating layer. Therefore, the metal magnetic powder core provided by the invention has better insulation effect and high temperature resistance, and ensures the insulation effect among metal magnetic powder particles, thereby greatly reducing the eddy current loss.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a metal magnetic powder core is characterized by comprising the following steps:
(1) mixing metal magnetic powder and a passivating agent into slurry;
(2) mixing the aluminum hydroxide gel with the slurry obtained in the step (1), and then drying and sieving the mixture in sequence;
(3) and (3) mixing the lubricating powder with the powder obtained by sieving in the step (2), pressing and molding, and then performing heating treatment to obtain the metal magnetic powder core.
2. The method according to claim 1, wherein the metal magnetic powder of step (1) is atomized metal magnetic powder;
preferably, the average particle size of the metal magnetic powder in the step (1) is 1-100 μm;
preferably, the metal magnetic powder in step (1) comprises any one or a combination of at least two of sendust, sendust or sendust.
3. The preparation method according to claim 1 or 2, wherein the passivating agent in the step (1) is added in an amount of 0.1-3 wt% of the metal magnetic powder;
preferably, metal magnetic powder, a passivating agent and water are mixed in the step (1) to form slurry, and the addition amount of the water is 1-10 wt% of the metal magnetic powder;
preferably, the passivating agent comprises any one or a combination of at least two of phosphoric acid, chromic acid or aluminium dihydrogen phosphate, preferably phosphoric acid;
preferably, the mixing in the step (1) is stirring and mixing for 3-10 min.
4. The method according to any one of claims 1 to 3, wherein the solid content of the aluminum hydroxide gel in the step (2) is 15 to 35 wt%;
preferably, the addition amount of the aluminum hydroxide gel in the step (2) is 0.1-3 wt% of the metal magnetic powder;
preferably, the mixing in the step (2) is stirring and mixing for 3-10 min;
preferably, the drying temperature in the step (2) is 150-250 ℃;
preferably, the drying time in the step (2) is 1.5-2.5 h;
preferably, the mesh number of the screen in the step (2) is 50-100 meshes.
5. The method according to any one of claims 1 to 4, wherein the lubricant powder in the step (3) is added in an amount of 0.1 to 1.0 wt% based on the metal magnetic powder;
preferably, the lubricating powder of step (3) comprises any one of or a combination of at least two of aluminum stearate, zinc stearate, or magnesium stearate.
6. The method according to any one of claims 1 to 5, wherein the pressure for the press molding in the step (3) is 10 to 22t/cm2；
Preferably, the temperature of the heating treatment in the step (3) is 600-800 ℃;
preferably, the time of the heating treatment in the step (3) is 1-2 h.
7. The production method according to any one of claims 1 to 6, characterized by comprising the steps of:
(1) stirring mixed metal magnetic powder, a passivating agent and water for 3-10 min to obtain slurry; the addition amount of the passivating agent is 0.1-3 wt% of the metal magnetic powder, and the addition amount of the water is 1-10 wt% of the metal magnetic powder;
(2) stirring and mixing aluminum hydroxide gel with a solid content of 15-35 wt% and the slurry in the step (1) for 3-10 min, drying at 150-250 ℃ for 1.5-2.5 h in sequence, and sieving with a 50-100-mesh sieve; the addition amount of the aluminum hydroxide gel is 0.1-3 wt% of the metal magnetic powder;
(3) mixing the lubricating powder with the powder obtained by sieving in the step (2) at the speed of 10-22 t/cm2Pressing and forming under pressure, and then carrying out heating treatment at 600-800 ℃ for 1-2 h to obtain the metal magnetic powder core; the addition amount of the lubricating powder is 0.1-1.0 wt% of the metal magnetic powder.
8. A metal magnetic powder core, which is obtained by the preparation method of any one of claims 1 to 7.
9. The metal magnetic powder core according to claim 8, wherein the surface of the powder particles of the metal magnetic powder core is coated with a passivation layer and an alumina insulation layer.
10. Use of a metal magnetic powder core according to claim 8 or 9 as a magnetic material.
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