CN113707401A - Magnetic carbon-coated Fe-based soft magnetic powder core and preparation method thereof - Google Patents
Magnetic carbon-coated Fe-based soft magnetic powder core and preparation method thereof Download PDFInfo
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 76
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 74
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002131 composite material Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 20
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 239000000314 lubricant Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000178 monomer Substances 0.000 claims abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 239000003822 epoxy resin Substances 0.000 claims description 11
- 229920000647 polyepoxide Polymers 0.000 claims description 11
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 5
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910021581 Cobalt(III) chloride Inorganic materials 0.000 claims description 2
- 229910005347 FeSi Inorganic materials 0.000 claims description 2
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000362 cobalt(III) sulfate Inorganic materials 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 229920002050 silicone resin Polymers 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims 1
- 238000000465 moulding Methods 0.000 claims 1
- 238000003825 pressing Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 23
- 239000010410 layer Substances 0.000 description 21
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 150000001299 aldehydes Chemical class 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- QSNSCYSYFYORTR-UHFFFAOYSA-N 4-chloroaniline Chemical compound NC1=CC=C(Cl)C=C1 QSNSCYSYFYORTR-UHFFFAOYSA-N 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000002262 Schiff base Substances 0.000 description 2
- 150000004753 Schiff bases Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- KKOFYQBBUSZDKJ-UHFFFAOYSA-N 4-oxohexanal Chemical compound CCC(=O)CCC=O KKOFYQBBUSZDKJ-UHFFFAOYSA-N 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
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- AFAIELJLZYUNPW-UHFFFAOYSA-N pararosaniline free base Chemical compound C1=CC(N)=CC=C1C(C=1C=CC(N)=CC=1)=C1C=CC(=N)C=C1 AFAIELJLZYUNPW-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 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
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The invention discloses a magnetic carbon-coated Fe-based soft magnetic powder core, which comprises the following steps: (1) adding soluble salt containing magnetic elements, 1,3, 5-mesitylene, 2,4, 6-benzenetriol and rosaniline into 1, 4-dioxyhexane, carrying out ultrasonic treatment, and heating until all monomers are dissolved; (2) dropwise adding an acetic acid solution into the solution, and stirring to obtain a coordination composite material solution; (3) adding the coordination composite material solution into the Fe-based soft magnetic powder, uniformly stirring and drying to obtain insulating Fe-based soft magnetic powder; (4) mixing the insulating Fe-based soft magnetic powder with a binder and a lubricant, then pressing and forming to obtain a blank, carrying out heat treatment in nitrogen, cooling and spraying to obtain the magnetic powder core. The preparation method has simple equipment and simplified working procedures, so that the cost is reduced, and the prepared Fe-based soft magnetic powder core has higher compactness and higher strength.
Description
Technical Field
The invention relates to the technical field of magnetic material manufacturing, in particular to a Fe-based soft magnetic powder core and a preparation method thereof.
Background
Fe-based soft magnetic powder core and its productionIs an important soft magnetic material and is widely applied to an electromagnetic energy conversion device. With the development of power electronic devices toward higher frequency, smaller size, and higher conversion efficiency, higher requirements such as low loss and high magnetic permeability are also placed on soft magnetic composite materials. In the preparation process of the soft magnetic composite material, insulation coating is the most core key process. The insulation coating method commonly used in the industry at present is a phosphoric acid passivation process, the method is low in cost and easy to control, but the loss is increased due to chemical corrosion of magnetic powder, and a phosphate insulation layer is easy to ablate at high temperature, so that the optimization of the performance of the soft magnetic composite material is limited. In order to solve the high temperature instability of the phosphate insulating layer, an oxide having high resistance and high temperature resistance is widely introduced as the insulating coating layer. Patent CN201510621353.8 "preparation method and application of high-strength soft magnetic composite material" discloses a preparation method of high-strength soft magnetic composite material: the passivated iron powder and the refined magnesium oxide powder are uniformly mixed by a mechanical mixing method, and the high-strength soft magnetic composite material is obtained through pressing and heat treatment. Patent CN109848428A "preparation method of metal soft magnetic composite material and metal soft magnetic composite material" discloses a preparation method of metal soft magnetic composite material: carrying out surface micro-oxidation and annealing treatment under the gas phase auxiliary condition to form an insulating coating layer on the surface of the magnetic powder in situ to obtain the metal soft magnetic composite material, wherein the insulating coating layer is Al2O3、SiO2、Cr2O3. The method can solve the problem of high temperature stability effectively, but the insulating layer is nonmagnetic, so that the obvious diluted magnetic effect is caused, and the method is not beneficial to maintaining the high magnetic conductivity and high saturation magnetization of the soft magnetic composite material.
Disclosure of Invention
The invention provides a preparation method of a magnetic carbon-coated Fe-based soft magnetic powder core in order to overcome the problems in the prior art, and the method has the advantages of simple equipment, simplified process, reduced cost and suitability for industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a magnetic carbon-coated Fe-based soft magnetic powder core comprises the following steps:
(1) adding soluble salt containing magnetic elements, 1,3, 5-mesitylene-trimethyl aldehyde, 2,4, 6-benzenetriol and rosaniline into 1, 4-dioxyhexane, carrying out ultrasonic treatment, and heating until all monomers are dissolved to form a solution;
(2) dropwise adding an acetic acid solution into the solution obtained in the step (1) and stirring to obtain a coordination composite material solution;
(3) adding the coordination composite material solution obtained in the step (2) into Fe-based soft magnetic powder, uniformly stirring, and drying to obtain insulating Fe-based soft magnetic powder;
(4) uniformly mixing the insulating Fe-based soft magnetic powder obtained in the step (3) with a binder and a lubricant, and performing compression molding to obtain a blank;
(5) and (4) carrying out heat treatment on the blank obtained in the step (4) in nitrogen, cooling, and spraying insulating paint to obtain the magnetic carbon-coated Fe-based soft magnetic powder core.
In the invention, 1,3, 5-benzenetricarboxylic acid and 2,4, 6-benzenetrisol both contain three hydroxyl groups and a magnetic element (Fe)3+、Ni2+、Co3+) Ions have stronger chelating capacity, and then the magnetic element-organic polymer coordination composite material is formed through Schiff base reaction and coordination. And (2) performing high-temperature heat treatment in a nitrogen atmosphere, so that in the carbonization process, the magnetic element ions trapped in the organic polymer are reduced into magnetic particles in situ to obtain a magnetic carbon insulating layer, wherein a 0.05-2.0 mu M magnetic carbon layer is coated on the surface of the Fe-based soft magnetic powder, and the microstructure of the magnetic carbon is that M @ C (M ═ Fe, Co and Ni) nano particles are embedded into an N-doped carbon matrix. The invention avoids the cracking of the phosphate insulating layer in the pressing process, the magnetic carbon has high temperature resistance, the resistivity of the magnetic powder core is improved, the high-temperature heat treatment is beneficial to releasing the internal stress in the blank, and the loss of the magnetic powder core is greatly reduced; meanwhile, the magnetic carbon insulating layer can relieve the magnetic dilution effect, and the magnetic performance of the composite material is further improved.
Preferably, in step (1), the soluble iron salt is selected from FeCl3、Fe2(SO4)3、Fe(NO3)3、NiCl2、NiSO4、Ni(NO3)2、CoCl3、Co2(SO4)3And Co (NO)3)3One or more of them are mixed.
Preferably, in the step (1), the ultrasonic time is 5-15 min; the heating temperature is 70-100 ℃.
Preferably, in the step (2), the concentration of the acetic acid solution is 1-3 mol/L.
Preferably, in the step (3), the metallic soft magnetic powder is one selected from Fe, FeSi, FeSiAl, and FeSiB.
Preferably, in the step (3), the drying temperature is 60-80 ℃, and the drying time is 12-24 hours.
Preferably, in the step (1), the addition amount of the soluble ferric salt is 0.5-1.0 wt% based on the total mass of the Fe-based soft magnetic powder; the addition amount of the 1,3, 5-mesitylene triformol is 0.5-1.0 wt%; the addition amount of the 2,4, 6-benzenetriol is 0.5-1.0 wt%; the addition amount of the rosaniline is 0.5-1.0 wt%; the addition amount of the 1, 4-dioxyhexane is 0.5-1.0 wt%; the addition amount of the acetic acid is 0.05-0.1 wt%, and the dosage ratio of the soluble magnetic element-containing salt, 1,3, 5-mesitylene, 2,4, 6-benzenetriol, rosaniline and 1, 4-dioxane is 1:1:1:1: 1. The addition amount of the materials is critical, the magnetic element-organic polymer coordination composite material cannot be formed through Schiff base reaction and coordination due to the fact that the addition amount is too low, and the overall magnetic performance of the Fe-based soft magnetic composite material is affected due to the fact that the addition amount is too high.
Preferably, in the step (4), the binder is one or more selected from epoxy resin, silicone resin, silica, glass powder and water glass; the addition amount of the binder is 0.5-1.0 wt% based on the total mass of the Fe-based soft magnetic powder.
Preferably, in the step (4), the lubricant is selected from one or two of zinc stearate and barium stearate; the lubricant is added in an amount of 0.5 to 1.0 wt% based on the total mass of the Fe-based soft magnetic powder.
Preferably, in the step (4), the pressure of the compression molding is 1500-2000 MPa.
Preferably, in the step (5), the heat treatment temperature is 600-750 ℃ and the time is 0.5-2 h. The heat treatment temperature is critical, the internal stress generated in the pressing process cannot be released due to too low heat treatment temperature, the magnetic performance cannot reach the optimal value, and the binding agent is damaged due to too high heat treatment temperature, so that the Fe-based magnetic powder is further oxidized.
The invention also provides the magnetic carbon-coated Fe-based soft magnetic powder core prepared by the preparation method, the magnetic carbon-coated Fe-based soft magnetic powder core has the characteristics of low loss, high magnetic conductivity and good bonding strength, and the prepared magnetic carbon insulating layer reduces the magnetic dilution effect and enhances the high-frequency stability of the metal magnetic powder core.
Compared with the prior art, the invention has the advantages that:
1) the invention synchronously completes the carbonization of the insulating layer and the reduction of magnetic element ions in the necessary process of preparing the magnetic powder core by high-temperature heat treatment in nitrogen atmosphere, simplifies the preparation process flow, reduces the cost and is suitable for industrial large-scale production;
2) compared with the traditional phosphate insulating layer and oxide insulating layer, the magnetic carbon insulating layer has the advantages that the magnetic dilution effect is relieved due to the existence of M @ C (M ═ Fe, Co and Ni) nano particles, and the performance of the product is further improved;
3) the magnetic carbon grows on the surface of the soft magnetic powder in situ, the binding degree between the insulating coating layer and the magnetic powder is high, the coating is uniform and compact, and the prepared Fe-based soft magnetic powder core has high compactness, high strength and good comprehensive performance.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
(1) FeCl is added31,3, 5-mesitylene-trimethyl aldehyde,Adding 2,4, 6-benzenetriol and pararosaniline into an aqueous solution of 1, 4-dioxane, mixing, carrying out ultrasonic treatment for 15min, heating to 100 ℃, completely dissolving to form a solution, and then dropwise adding a 3mol/L acetic acid solution into the obtained solution, and stirring to obtain a coordination composite material solution. Mixing the FeSiAl soft magnetic powder with the coordination composite material solution to form a layer of coordination composite material solution on the surface of the FeSiAl soft magnetic powder, and drying for 24 hours at 80 ℃ to obtain the insulated FeSiAl soft magnetic powder. Taking the total mass of FeSiAl metal soft magnetic powder as a reference, FeCl3The addition amount of (B) is 1 wt%; the addition amount of the 1,3, 5-mesitylene-trimethyl aldehyde is 1.0 wt%; the addition amount of the 2,4, 6-benzenetriol is 1.0 wt%; the adding amount of the parachloroaniline is 1.0 wt%; 1, 4-Dioxohexane was added in an amount of 1.0 wt%; the amount of acetic acid added was 0.05 wt%.
(2) And (2) uniformly mixing the insulating FeSiAl soft magnetic powder obtained in the step (1) with epoxy resin and zinc stearate, and performing compression molding under 2000MPa to obtain 3 annular blanks with the outer diameter of 33.00mm, the inner diameter of 19.90mm and the height of 10.7 mm. Based on the total mass of the FeSiAl metal soft magnetic powder, the addition amount of the epoxy resin is 1.0 wt%, and the addition amount of the zinc stearate is 1.0 wt%.
(3) And (3) carrying out heat treatment on the annular blank obtained in the step (2) in a nitrogen atmosphere, wherein the heat treatment temperature is 800 ℃, the time is 2.0h, cooling, and spraying a layer of epoxy resin insulating paint to obtain a magnetic carbon-coated FeSiAl metal magnetic powder core sample 1, a sample 2 and a sample 3, wherein the microstructure of the magnetic carbon is characterized in that a 0.05-2.0 mu m magnetic carbon layer is coated on the surface of FeSiAl soft magnetic powder, and the microstructure of the magnetic carbon is that Fe @ C nano particles are embedded into an N-doped carbon matrix.
The magnetic parameters tested are as follows:
example 2
(1) Mixing NiCl2Adding 1,3, 5-mesitylene-trimethyl aldehyde, 2,4, 6-benzenetriol and rosaniline into 1, 4-dioxyhexane, performing ultrasonic treatment for 5min, heating to 70 ℃, dissolving completely to form a solution, and then adding the solution into a containerAnd dropwise adding 1mol/L acetic acid solution into the obtained solution, and stirring to obtain a coordination composite material solution. Mixing the FeSiAl soft magnetic powder with the coordination composite material solution to form a layer of coordination composite material solution on the surface of the FeSiAl soft magnetic powder, and drying at 60 ℃ for 12h to obtain the insulated FeSiAl soft magnetic powder. NiCl based on the total mass of FeSiAl metal soft magnetic powder2The addition amount of (B) is 0.5 wt%; the addition amount of the 1,3, 5-mesitylene-trimethyl aldehyde is 0.5 wt%; the addition amount of the 2,4, 6-benzenetriol is 0.5 wt%; the adding amount of the parachloroaniline is 0.5 wt%; the addition amount of 1, 4-dioxahexane was 0.5% by weight; the amount of acetic acid added was 0.1 wt%.
(2) And (2) uniformly mixing the insulating FeSiAl soft magnetic powder obtained in the step (1) with epoxy resin and zinc stearate, and performing compression molding under the pressure of 1500MPa to obtain 3 annular blanks with the outer diameter of 33.00mm, the inner diameter of 19.90mm and the height of 10.7 mm. The addition amount of the epoxy resin is 0.5 wt% and the addition amount of the zinc stearate is 0.5 wt% based on the total mass of the FeSiAl metal soft magnetic powder.
(3) And (3) carrying out heat treatment on the blank obtained in the step (2) in a nitrogen atmosphere, wherein the heat treatment temperature is 600 ℃, the time is 0.5h, cooling, and spraying a layer of epoxy resin insulating paint to obtain a magnetic carbon-coated FeSiAl metal magnetic powder core sample 4, a sample 5 and a sample 6, wherein the microstructure of the magnetic carbon is characterized in that a magnetic carbon layer of 0.05-2.0 mu m is coated on the surface of FeSiAl soft magnetic powder, and the microstructure of the magnetic carbon is that Ni @ C nano particles are embedded into an N-doped carbon matrix.
The magnetic parameters tested are as follows:
example 3
(1) Mixing Co (NO)3)3Adding 1,3, 5-mesitylene-trimethyl aldehyde, 2,4, 6-benzenetriol and rosaniline into 1, 4-dioxyhexane, carrying out ultrasonic treatment for 10min,heating to 90 ℃, completely dissolving to form a solution, and then dropwise adding 2mol/L acetic acid solution into the obtained solution for stirring to obtain a coordination composite material solution. Mixing the FeSiAl soft magnetic powder with the coordination composite material solution to form a layer of coordination composite material solution on the surface of the FeSiAl soft magnetic powder, and drying at 70 ℃ for 18h to obtain the insulated FeSiAl soft magnetic powder. NiCl based on the total mass of FeSiAl metal soft magnetic powder2The addition amount of (B) is 0.7 wt%; the addition amount of the 1,3, 5-mesitylene-trimethyl aldehyde is 0.7 wt%; the addition amount of the 2,4, 6-benzenetriol is 0.7 wt%; the adding amount of the parachloroaniline is 0.7 wt%; the addition amount of 1, 4-dioxahexane was 0.7% by weight; the amount of acetic acid added was 0.07 wt%.
(2) And (2) uniformly mixing the insulating FeSiAl soft magnetic powder obtained in the step (1) with epoxy resin and zinc stearate, and performing compression molding under the pressure of 1800MPa to obtain 3 blanks with the outer diameter of 33.00mm, the inner diameter of 19.90mm and the height of 10.7 mm. Based on the total mass of the FeSiAl metal soft magnetic powder, the addition amount of the epoxy resin is 0.7 wt%, and the addition amount of the zinc stearate is 0.7 wt%.
(3) And (3) carrying out heat treatment on the blank obtained in the step (2) in a nitrogen atmosphere, wherein the heat treatment temperature is 700 ℃, the time is 1.0h, cooling, and spraying a layer of epoxy resin insulating paint to obtain a magnetic carbon-coated FeSiAl metal magnetic powder core sample 7, a sample 8 and a sample 9, wherein the microstructure of the magnetic carbon is characterized in that a magnetic carbon layer of 0.05-2.0 mu m is coated on the surface of FeSiAl soft magnetic powder, and the microstructure of the magnetic carbon is that Co @ C nano particles are embedded into an N-doped carbon matrix.
The magnetic parameters tested are as follows:
the above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention shall fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. A preparation method of a magnetic carbon-coated Fe-based soft magnetic powder core is characterized by comprising the following steps:
(1) adding soluble salt containing magnetic elements, 1,3, 5-mesitylene-trimethyl aldehyde, 2,4, 6-benzenetriol and rosaniline into 1, 4-dioxyhexane, carrying out ultrasonic treatment, and heating until all monomers are dissolved to form a solution;
(2) dropwise adding an acetic acid solution into the solution obtained in the step (1) and stirring to obtain a coordination composite material solution;
(3) adding the coordination composite material solution obtained in the step (2) into Fe-based soft magnetic powder, uniformly stirring, and drying to obtain insulating Fe-based soft magnetic powder;
(4) uniformly mixing the insulating Fe-based soft magnetic powder obtained in the step (3) with a binder and a lubricant, and performing compression molding to obtain a blank;
(5) and (4) carrying out heat treatment on the blank obtained in the step (4) in nitrogen, cooling, and spraying insulating paint to obtain the magnetic carbon-coated Fe-based soft magnetic powder core.
2. The method for preparing a magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein in the step (1), the soluble magnetic element-containing salt is selected from FeCl3、Fe2(SO4)3、Fe(NO3)3、NiCl2、NiSO4、Ni(NO3)2、CoCl3、Co2(SO4)3And Co (NO)3)3One or more of them are mixed.
3. The preparation method of the magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein in the step (1), the ultrasonic time is 5-15 min; the heating temperature is 70-100 ℃.
4. The method for preparing a magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein in the step (2), the concentration of the acetic acid solution is 1 to 3 mol/L.
5. The method for producing a magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein in the step (3), the Fe-based soft magnetic powder is one selected from Fe, FeSi, FeSiAl, and FeSiB.
6. The method for preparing a magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein in the step (3), the drying temperature is 60-80 ℃ and the drying time is 12-24 h.
7. The method for preparing a magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein the soluble magnetic element-containing salt is added in an amount of 0.5 to 1.0 wt% based on the total mass of the Fe-based soft magnetic powder; the addition amount of the 1,3, 5-mesitylene triformal is 0.5-1.0 wt%; the addition amount of the 2,4, 6-benzenetriol is 0.5-1.0 wt%; the addition amount of the rosaniline is 0.5-1.0 wt%; the addition amount of the 1, 4-dioxyhexane is 0.5-1.0 wt%; the addition amount of the acetic acid is 0.05-0.1 wt%, and the dosage ratio of the soluble magnetic element-containing salt, 1,3, 5-mesitylene, 2,4, 6-benzenetriol, rosaniline and 1, 4-dioxane is 1:1:1:1: 1.
8. The method for preparing a magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein in the step (4), the binder is one or more selected from epoxy resin, silicone resin, silica, glass powder and water glass; the lubricant is selected from one or two of zinc stearate and barium stearate; the addition amount of the binder is 0.5-1.0 wt% and the addition amount of the lubricant is 0.5-1.0 wt% based on the total mass of the Fe-based soft magnetic powder.
9. The method for preparing a magnetic carbon-coated Fe-based soft magnetic powder core according to claim 1, wherein in the step (4), the pressure of the press molding is 1500-2000 MPa; in the step (5), the heat treatment temperature is 600-800 ℃, and the time is 0.5-2.0 h.
10. A magnetic carbon-coated Fe-based soft magnetic powder core produced by the production method according to any one of claims 1 to 9.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108579783A (en) * | 2018-03-28 | 2018-09-28 | 中山大学 | A kind of preparation method of the monatomic material of N doping porous carbon carried metal |
| CN109461558A (en) * | 2018-11-26 | 2019-03-12 | 山东汇嘉磁电科技有限公司 | A kind of low-loss Fe-Si-Al magnetic core compound coating method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108579783A (en) * | 2018-03-28 | 2018-09-28 | 中山大学 | A kind of preparation method of the monatomic material of N doping porous carbon carried metal |
| CN109461558A (en) * | 2018-11-26 | 2019-03-12 | 山东汇嘉磁电科技有限公司 | A kind of low-loss Fe-Si-Al magnetic core compound coating method |
Non-Patent Citations (2)
| Title |
|---|
| ZHIFANG LI ET AL.: "Enhanced Aerobic Epoxidation of Styrene with Copper(II), Cobalt(II), Iron(III), or Oxovanadium(IV) Salen Complexes Immobilized onto Carbon-Coated Fe3O4 Nanoparticles Hybridized with Graphene Sheets", CHEMPLUSCHEM, vol. 79, pages 716 * |
| 郭翔: "氮掺杂碳包覆磁性纳米粒子复合微球吸波性能研究", 中国优秀硕士学位论文全文数据库（工程科技I辑）, pages 40 - 46 * |
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