WO2023165096A1 - 一种一体成型电感用低损耗粉末及其制备方法 - Google Patents
一种一体成型电感用低损耗粉末及其制备方法 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 156
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 claims abstract description 16
- 239000000835 fiber Substances 0.000 claims abstract description 15
- 239000010453 quartz Substances 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007822 coupling agent Substances 0.000 claims abstract description 14
- 239000004014 plasticizer Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000003822 epoxy resin Substances 0.000 claims abstract description 10
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 10
- 239000000314 lubricant Substances 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 34
- 239000011812 mixed powder Substances 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 21
- 102220043159 rs587780996 Human genes 0.000 claims description 18
- -1 iron-silicon-aluminum Chemical compound 0.000 claims description 17
- 229910000838 Al alloy Inorganic materials 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 12
- 229910019142 PO4 Inorganic materials 0.000 claims description 9
- 239000010452 phosphate Substances 0.000 claims description 9
- NXQMCAOPTPLPRL-UHFFFAOYSA-N 2-(2-benzoyloxyethoxy)ethyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCCOCCOC(=O)C1=CC=CC=C1 NXQMCAOPTPLPRL-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 7
- ZPLUZNXSYCCJOE-UHFFFAOYSA-N phosphoric acid;propan-2-one Chemical compound CC(C)=O.OP(O)(O)=O ZPLUZNXSYCCJOE-UHFFFAOYSA-N 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical group CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 claims description 6
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims description 5
- JDSQBDGCMUXRBM-UHFFFAOYSA-N 2-[2-(2-butoxypropoxy)propoxy]propan-1-ol Chemical compound CCCCOC(C)COC(C)COC(C)CO JDSQBDGCMUXRBM-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000005461 lubrication Methods 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 229910000702 sendust Inorganic materials 0.000 claims description 4
- PZTAGFCBNDBBFZ-UHFFFAOYSA-N tert-butyl 2-(hydroxymethyl)piperidine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCCCC1CO PZTAGFCBNDBBFZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 235000019359 magnesium stearate Nutrition 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 claims description 2
- 239000010410 layer Substances 0.000 claims 6
- 239000011247 coating layer Substances 0.000 claims 1
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 abstract description 2
- 239000006247 magnetic powder Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 39
- 230000035699 permeability Effects 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910000599 Cr alloy Inorganic materials 0.000 description 5
- XEVZIAVUCQDJFL-UHFFFAOYSA-N [Cr].[Fe].[Si] Chemical compound [Cr].[Fe].[Si] XEVZIAVUCQDJFL-UHFFFAOYSA-N 0.000 description 5
- 239000000788 chromium alloy Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 2
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- SVKYAACJXKSYTO-UHFFFAOYSA-N iron;nickel;oxozinc Chemical compound [Ni].[Zn].[Fe]=O SVKYAACJXKSYTO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000126 substance Substances 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
- H01F1/147—Alloys characterised by their composition
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
-
- 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
-
- 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
Definitions
- the invention belongs to the field of magnetic functional materials, and in particular relates to an integrally formed low-loss powder for inductors and a preparation method thereof.
- One-piece inductors are mostly made of carbonyl iron powder or iron-silicon-chromium alloy powder, which is pressed with the coil embedded in it after insulating coating.
- Carbonyl iron powder is characterized by good DC superposition characteristics, low powder hardness, and high density after pressing, but its magnetic permeability is low.
- High DC resistance R DC ; FeSiCr alloy powder has the advantages of good anti-rust properties and adjustable magnetic permeability range, but the powder is relatively hard, difficult to compact and compact, and has high loss.
- the Chinese patent with the notification number CN111063501B has announced a preparation method for producing low-loss powders for integrally formed inductors, that is, after mixing carbonyl iron powder with iron silicon powder or amorphous powder Coating granulation, but the loss of iron-silicon powder is the highest among commonly used soft magnetic metal powders.
- Amorphous powder has no grain boundaries, which makes it difficult to effectively coat, and its hardness is relatively high, so it is difficult to compress, so the obtained powder is still difficult to achieve Aim for low loss.
- the Chinese patent with the publication number CN113380487A discloses a magnetic core powder for integrally formed inductors and its preparation method. Its core is still iron-silicon-chromium alloy powder for inorganic and organic coating. Although the obtained magnetic core has a stable structure and is not easy to crack , but still failed to solve the problem of excessive loss.
- the purpose of the present invention is to overcome the deficiencies of the prior art and provide a low-loss powder for integrally formed inductors and its preparation method, which can not only reduce the loss caused by magnetic substances, but also reduce the use of copper wires in integrally formed inductors In turn, the resistance and the loss caused by the heating of the copper wire are reduced, and the overall efficiency is improved.
- the low-loss powder for integrated molding inductors of the present invention is mainly composed of carbonyl iron powder, gas-atomized iron-silicon-aluminum alloy powder, phosphate coating agent, composite coating agent and lubricant, and carbonyl iron powder and gas-atomized iron
- the mass of the mixed powder after mixing the silicon-aluminum alloy powder is the basis for calculation, where:
- the phosphate coating agent is produced by the reaction of mixed powder and phosphate-acetone solution, wherein the mass of phosphoric acid is 0.1-0.3% of the mass of the mixed powder, and the acetone is 8-10% of the mass of the mixed powder;
- the composite coating agent consists of 0.3-1.2% nickel-zinc ferrite powder, 0.2-0.6% quartz fiber powder, 0.1-0.3% film-forming agent, 0.1-0.4% plasticizer, 1.5-2.8% ring Oxygen resin, 0.3-0.5% of curing agent and 0.1-0.4% of coupling agent are mixed in acetone solvent to form; the lubricant accounts for 0.2-0.4% of the mass of the mixed powder.
- the agent is an epoxy curing agent;
- the coupling agent is ethyltriethoxysilane;
- the lubricant is one or more mixtures of stearic acid, paraffin wax powder and magnesium stearate.
- the outermost layer of the powder is a net-shaped coating film layer composed of a composite coating agent
- the second outer layer is a phosphate film layer composed of a phosphate coating agent
- the innermost layer is a matrix composed of sendust and carbonyl iron powder , and finally formed a double-layer coating structure.
- a method for preparing low-loss powder for integrated molding inductors comprising the following steps:
- Lubrication and sieving Weigh the lubricant and mix it with the granulated powder, and then sieve it with a mesh size of 50-270.
- the powder with an intermediate particle size is the powder for low-loss integrated molding inductors.
- the present invention has the following advantages:
- the selection of original powder is carbonyl iron powder and gas atomized iron silicon aluminum powder, and its principle is that carbonyl iron is easy to press and form, and has better direct-current superposition characteristic, and powder particle size is little, and in the device
- the eddy current loss is proportional to the particle size of the powder, so the eddy current loss generated is lower than that of the conventional powder, and the gas-atomized iron-silicon-aluminum powder is due to its high sphericity, low oxygen content, magnetostriction coefficient close to zero, and magnetic crystals.
- the anisotropy constant is close to zero, which is the lowest loss among conventional soft magnetic materials.
- the overall loss after mixing the two powders of the present invention is much lower than that of conventional powders, while maintaining the DC superposition characteristics close to conventional powders;
- the inductance value of the integrally formed inductor is proportional to the square of the powder magnetic permeability and the number of turns of the coil. Since the magnetic permeability of the pressed powder in the present invention is higher than that of the conventional carbonyl iron powder, the integrally formed inductor with the same inductance value The amount of copper wire used will be reduced, which can reduce the loss caused by the heating of the copper wire in the integrated inductor, and the reduction in the number of copper wires will also help reduce production costs;
- quartz fiber powder is Under the bonding action of film-forming agent, plasticizer, epoxy resin, curing agent, coupling agent and other materials, it can be evenly coated on the surface of the powder.
- the quartz fiber powder has a certain aspect ratio, under microscopic conditions , can form a net-like coating film layer based on quartz fiber powder, the net-like structure helps to increase the toughness of the coating film layer, and is not easily damaged during the pressing process, thereby maintaining the powder with high insulation resistance, so The film layer has good insulation and reliability, and reduces the overall loss by reducing eddy current loss.
- Lubrication and sieving Weigh 2g of stearic acid and mix it with the powder, and then sieve it with 50-270 meshes.
- Example 1 The difference between this comparative example and Example 1 is that all the original powders used are carbonyl iron powders.
- Example 1 The difference between this comparative example and Example 1 is that all the original powders used are iron-silicon-chromium alloy powders.
- Example 1 The difference between this comparative example and Example 1 is that the composite coating agent used is to mix 1g plasticizer diethylene glycol dibenzoate, 24g epoxy resin, 5.5g curing agent, 1.5g ethyl triethoxy The base silane coupling agent is dissolved in the solvent of 100g acetone.
- Example 1 and Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4 was pressed into a magnetic ring with an outer diameter of 10.15 mm, an inner diameter of 5.1 mm, and a height of 3.98 ⁇ 0.02 mm, and after baking, the magnetic ring was made into a coil.
- Embodiment 1 and comparative example 1, comparative example 2, comparative example 3, comparative example 4 characteristic test results are as shown in table 1:
- Example 1 By comparing Example 1 with Comparative Examples 1-3, it can be seen from Table 1 that the present invention uses the mixed powder of sendust powder and carbonyl iron as the original powder, and the magnetic permeability of the prepared material is significantly improved, because the gas mist The magnetostriction coefficient and magnetic anisotropy constant of iron silicon aluminum powder are close to 0, so it has lower loss than iron silicon chromium alloy powder and carbonyl iron powder after mixing.
- Example 1 and Comparative Example 4 it can be seen that after the composite coating of the present invention, the magnetic permeability of the material is higher than that of the ordinary coating process, and the loss is significantly lower than that of the ordinary coating process.
- the spherical nickel-zinc-iron Oxygen powder is magnetic, and after coating and pressing, it can be filled into the gaps between carbonyl iron powders, so the performance has been improved.
- the addition of quartz fiber powder, film-forming agent, and plasticizer can greatly improve the uniformity of coating and the insulation and toughness of the film layer, so that the film layer will not be easily damaged during the pressing process, and the coupling agent can improve The connection between the film layer and the powder matrix, so the coating effect of the film layer is better, the resistivity between the powder and the powder is greatly improved, and the eddy current loss generated between the particles is reduced, so the overall loss is reduced.
- Lubrication and sieving Weigh 3g of magnesium stearate and mix it with the powder. After mixing, sieve it with a mesh size of 50-270. The powder with an intermediate particle size is the powder for low-loss integral molding inductors.
- Example 2 The difference between this comparative example and Example 2 is that the composite coating agent used is an acetone solution mixed with 19g of nickel-zinc ferrite powder, 25g of epoxy resin, 5g of curing agent, and 3g of ethyltriethoxysilane coupling agent.
- the composite coating agent used is an acetone solution mixed with 19g of nickel-zinc ferrite powder, 25g of epoxy resin, 5g of curing agent, and 3g of ethyltriethoxysilane coupling agent.
- Example 2 The difference between this comparative example and Example 2 is that the composite coating agent used is to mix 6g film-forming agent tripropylene glycol n-butyl ether (TPnB), 4g plasticizer dipropylene glycol dibenzoate, 30g epoxy resin, 9g curing Agent, 3g ethyltriethoxysilane coupling agent in acetone solution.
- TPnB tripropylene glycol n-butyl ether
- plasticizer dipropylene glycol dibenzoate 30g epoxy resin
- 9g curing Agent 9g curing Agent
- 3g ethyltriethoxysilane coupling agent in acetone solution.
- Example 2 The difference between this comparative example and Example 2 is that the composite coating agent used is to mix 10g nickel-zinc ferrite powder, 4g quartz fiber powder, 5g film-forming agent tripropylene glycol n-butyl ether (TPnB), 28g epoxy resin, 5g Acetone solution of curing agent.
- the composite coating agent used is to mix 10g nickel-zinc ferrite powder, 4g quartz fiber powder, 5g film-forming agent tripropylene glycol n-butyl ether (TPnB), 28g epoxy resin, 5g Acetone solution of curing agent.
- Embodiment 2 and comparative example 5 are as shown in table 2:
- Example 2 By comparing Example 2 with Comparative Examples 5-8, it can be seen from Table 2 that the present invention uses the mixed powder of sendust powder and carbonyl iron as the original powder, and uses a composite coating agent to coat it.
- the magnetic permeability of the prepared material is obviously improved, and the loss is obviously reduced.
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- Dispersion Chemistry (AREA)
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- Electromagnetism (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
Abstract
一种一体成型电感用低损耗粉末及其制备方法，采用大粒径的气雾化铁硅铝合金粉末与小粒径的羰基铁粉末混合为磁粉主体进行磷化处理，得到磷化粉末，再混入由镍锌铁氧体粉末、石英纤维粉、成膜剂、增塑剂、环氧树脂、固化剂、偶联剂组成的复合包覆剂，待搅拌均匀后进行造粒、烘烤，冷却至室温后，加入润滑剂混合，经50-270目分筛，得到一体成型电感用低损耗粉末。所制得的粉末具有高磁导率、低损耗的特性，利用该粉末压制的一体成型电感具有成本低、损耗低、发热小、效率高等优点。
Description
本发明属于磁性功能材料领域，具体涉及一种一体成型电感用低损耗粉末及其制备方法。
作为电子产品的重要组成部件，新型电子元器件正向着片式化、微型化、高频化、宽频化、高精度化、集成化和绿色环保的方向发展，对功率电感产品尺寸和性能提出了更高的要求，要求其同时具有小尺寸、大电流、较低功耗的特点，因此，为了满足该目的，对一体成型电感用材料的研发成为目前研究的重点。
一体成型电感多采用羰基铁粉或铁硅铬合金粉为材料，经过绝缘包覆后与埋在其中的线圈压制而成。羰基铁粉的特点为直流叠加特性好，粉末硬度低，压制成型后密度高，但其磁导率较低，制作高感值电感时需要增加线圈匝数，导致电感尺寸大、铜线成本高、直流电阻R
DC高；铁硅铬合金粉末的优点是防锈特性好、磁导率范围可调，但是粉末硬度较大、难以压制密实，且其损耗较高。为了提升一体成型电感密度、降低其整体损耗，公告号为CN111063501B的中国专利公布了一种生产一体成型电感用低损耗粉末的制备方法，即将羰基铁粉与铁硅粉或非晶粉进行混合后包覆造粒，但是铁硅粉末损耗是常用软磁金属粉末中损耗最高的，非晶粉末没有晶界、难以有效包覆，且其硬度较大，很难压制，因此得到的粉末依然难以达到低损耗的目标。公开号为CN113380487A的中国专利公布了一种一体成型电感用磁芯粉末及其制备方法，其核心依然是铁硅铬合金粉末进行无机、有机包覆，所得到的磁芯虽然结构稳定、不易开裂，但是仍然未能解决损耗过高的问题。
因此，十分有必要研发出一种一体成型电感用低损耗粉末及其制备方法。
发明内容
本发明的目的是为了克服现有技术的不足，提供一种一体成型电感用低损耗粉末及其制备方法，其不仅可以降低磁性物质带来的损耗，还可以降低一体成型电感内铜线的使用量， 继而降低电阻，以及因铜线发热而带来的损耗，提升整体效率。
本发明的一体成型电感用低损耗粉末，材料主要由羰基铁粉、气雾化铁硅铝合金粉末、磷酸盐包覆剂、复合包覆剂和润滑剂组成，以羰基铁粉和气雾化铁硅铝合金粉末混合后的混合粉末质量为计算基础，其中：
羰基铁粉粒径为D50＝4-8um，占混合粉末质量的45-55％，气雾化铁硅铝合金粉末粒径为D50＝15-20um，占混合粉末质量的55-45％；
磷酸盐包覆剂是由混合粉末与磷酸丙酮溶液反应后产生，其中，磷酸质量为混合粉末质量的0.1-0.3％，丙酮为混合粉末质量的8-10％；
复合包覆剂由0.3-1.2％的镍锌铁氧体粉末、0.2-0.6％的石英纤维粉、0.1-0.3％的成膜剂、0.1-0.4％的增塑剂、1.5-2.8％的环氧树脂、0.3-0.5％的固化剂、0.1-0.4％的偶联剂混合于丙酮溶剂中形成；润滑剂占混合粉末质量的0.2-0.4％。
优选的，羰基铁粉粒径为D50＝5um，气雾化铁硅铝合金粉末粒径为D50＝15um。
优选的，所用的镍锌铁氧体粉末为D50＝0.9-1.1um的球状粉末；石英纤维粉长径比为2:1，目数为7000目；成膜剂为二丙二醇单丁醚(DPnB)、三丙二醇正丁醚(TPnB)中的一种或二者混合；增塑剂为二乙二醇二苯甲酸酯、二丙二醇二苯甲酸酯中的一种或二者混合；固化剂为环氧固化剂；偶联剂为乙基三乙氧基硅烷；润滑剂为硬脂酸、石蜡微粉、硬脂酸镁中的一种或几种混合。
进一步优选的，镍锌铁氧体粉末为粒径为D50＝1.0um的球状粉末。
粉末的最外层是由复合包覆剂构成的网状包覆膜层，次外层是由磷酸盐包覆剂构成的磷酸盐膜层，最内部是铁硅铝与羰基铁粉组成的基体，最终形成了双膜层包覆结构。
一种一体成型电感用低损耗粉末的制备方法，包括如下步骤：
(1)原始粉末混合：将羰基铁粉与气雾化铁硅铝合金粉末均匀混合，得到混合粉末；
(2)原始粉末的磷化：将步骤1得到的混合粉末加入磷酸丙酮溶液内进行混合搅拌20-30min， 之后于100-120℃条件下烘烤15-30min，冷却至室温得到磷化粉末，此时在混合粉末表面包覆磷酸盐膜层，其中磷酸质量为混合粉末质量的0.1-0.3％，丙酮为混合粉末质量的8-10％；
(3)制备复合包覆剂：混合镍锌铁氧体粉末、石英纤维粉、成膜剂、增塑剂、环氧树脂、固化剂、偶联剂于丙酮溶剂内搅拌均匀；
(4)造粒烘干：将磷化粉末混入复合包覆剂内搅拌均匀后进行造粒，后置于烘箱内进行60-80℃条件下40-60min烘烤，得到造粒粉；
(5)润滑与分筛：称取润滑剂与造粒粉混合，混合后进行50-270目分筛，中间粒径粉末即为低损耗一体成型电感用粉末。
本发明与现有技术相比，具有以下优点：
1.本发明中，原始粉末的选择为羰基铁粉与气雾化铁硅铝粉末，其原理在于羰基铁易于压制成型、且有较好的直流叠加特性，而且粉粒径小，器件中的涡流损耗与粉末的粒径成正比关系，因此产生的涡流损耗低于常规粉末，而气雾化铁硅铝粉末因为其球形度高、氧含量低、磁致伸缩系数接近于零、磁晶各向异性常数接近于零，是常规软磁材料中损耗最低的，本发明的两种粉末混合后整体损耗远低于常规粉末、同时保持接近常规粉末的直流叠加特性；
2.调节两种粉末的粒径配比，在一体成型电感压制的过程中，大颗粒气雾化铁硅铝粉末之间在三维空间上存在间隙，这些间隙可以被粒径较小的羰基铁粉末填充，从而提升压制密度、进一步提升磁导率，而羰基铁粉末之间的三维空隙又可以由更细小的球状镍锌铁氧体粉末进行填充，因为镍锌铁氧体粉末具有良好的绝缘性，而磁性材料的涡流损耗又与粉末绝缘电阻的平方成正比，因此镍锌铁氧体粉末的添加能有效降低涡流损耗；
3.一体成型电感的电感值与粉末磁导率、线圈匝数的平方成正比，由于本发明中粉末压制后磁导率高于常规的羰基铁粉，因此在相同电感值的一体成型电感中所用铜线量会减少，从而可以降低一体成型电感中因铜线发热带来的损耗，铜线数量减少还有助于降低生产成本；
4.采用镍锌铁氧体粉末、石英纤维粉、成膜剂、增塑剂、环氧树脂、固化剂、偶联剂所组成 的复合包覆剂，在搅拌造粒后，石英纤维粉在成膜剂、增塑剂、环氧树脂、固化剂、偶联剂等材料的粘结作用下，可以均匀的包覆在粉体表面，由于石英纤维粉具有一定长径比，在微观条件下，可以形成以石英纤维粉为基体的网状包覆膜层，网状结构有助于增加包覆膜层的韧性，在压制过程中不轻易被破坏，从而保持粉末具有高的绝缘电阻，因此该膜层具有良好的绝缘性与可靠性，通过降低涡流损耗而降低整体损耗。
下面通过具体实施例，对本发明的技术方案作进一步具体的说明。
在本发明中，若非特指，所有原料均可从市场购得或是本行业常用的，下述实施例中的方法，如无特别说明，均为本领域常规方法。
实施例1
(1)原始粉末混合：将羰基铁粉450g与气雾化铁硅铝合金粉末550g均匀混合，羰基铁粉粒径为D50＝5um，气雾化铁硅铝合金粉末粒径为D50＝15um；
(2)原始粉末的传统磷化：将原始粉末加入磷酸丙酮溶液内进行混合搅拌25min，之后于100℃条件下烘烤25min，冷却至室温得到磷化粉末，其中磷酸质量为2g，丙酮质量为100g；
(3)制备复合包覆剂：混合4g镍锌铁氧体粉末、2g石英纤维粉、1g成膜剂二丙二醇单丁醚(DPnB)、1g增塑剂二乙二醇二苯甲酸酯、18g环氧树脂、3.5g固化剂、1.5g乙基三乙氧基硅烷偶联剂于100g丙酮溶剂内搅拌均匀；
(4)造粒烘干：将磷化粉末混入复合包覆剂内搅拌均匀后进行造粒，后置于烘箱内进行60℃条件下60min烘烤，得到造粒粉；
(5)润滑与分筛：称取2g硬脂酸与粉末混合，混合后进行50-270目分筛，中间粒剂即为低损耗一体成型电感用粉末。
对比例1
本对比例与实施例1的区别在于，使用的原始粉末全部为羰基铁粉末。
对比例2
本对比例与实施例1的区别在于，使用原始粉末全部为铁硅铬合金粉末。
对比例3
本对比例与实施例1的区别在于，使用原始粉末为质量比1:1的铁硅铬合金粉末与羰基铁混合粉末。
对比例4
本对比例与实施例1的区别在于，使用的复合包覆剂为混合1g增塑剂二乙二醇二苯甲酸酯、24g环氧树脂、5.5g固化剂、1.5g乙基三乙氧基硅烷偶联剂溶解于100g丙酮的溶剂。
将实施例1与对比例1、对比例2、对比例3、对比例4所得粉末压制外径10.15mm、内径5.1mm、高3.98±0.02mm的磁环，烘烤后将磁环绕制线圈，使用WK6500B LCR测试测试磁环电感值，根据公式μe＝(L*Le)/(4*3.14*Ae*N2)计算磁环有效磁导率，其中，μe:有效磁导率，L:电感量(μH)，Le:有效磁路长度(mm)，Ae:有效截面积(mm2)，N:线圈匝数，最后测试磁环损耗。
实施例1与对比例1、对比例2、对比例3、对比例4特性测试结果如表1所示：
表1：实施例1与对比例1、对比例2、对比例3、对比例4特性测试结果
通过对比实施例1与对比例1-3，根据表1可以看出，本发明使用铁硅铝合金粉末与羰基铁的混合粉末作为原始粉末，所制备材料的磁导率明显提高，因为气雾化铁硅铝粉末磁致伸 缩系数与磁各向异性常数接近于0，所以混合后具有比铁硅铬合金粉、羰基铁粉等更低的损耗。通过对比实施例1与对比例4可以看到，经过本发明的复合包覆后，材料磁导率高于普通包覆工艺，损耗明显低于普通包覆工艺，这是因为球状的镍锌铁氧体粉末具有磁性，在包覆、压制后，又可以填充到羰基铁粉末之间的空隙内部，因此性能得到了升高。而石英纤维粉、成膜剂、增塑剂的加入，可以大幅提升包覆的均匀性与膜层的绝缘性与韧性，使膜层在压制过程中不会被轻易破坏，偶联剂可以提升膜层与粉末基体之间的联结，因此膜层包覆效果更好，粉体与粉体之间的电阻率大幅提升，降低了颗粒之间产生的涡流损耗，因此整体损耗得到降低。
实施例2
(1)原始粉末混合：将羰基铁粉500g与气雾化铁硅铝合金粉末500g均匀混合，其中羰基铁粉粒径为D50＝5um，气雾化铁硅铝合金粉末粒径为D50＝15um；
(2)原始粉末的传统磷化：将原始粉末加入磷酸丙酮溶液内进行混合搅拌30min，之后于120℃条件下烘烤15min，冷却至室温得到磷化粉末，其中磷酸质量为3g，丙酮质量为100g；
(3)制备复合包覆剂：混合10g镍锌铁氧体粉末、4g石英纤维粉、2g成膜剂三丙二醇正丁醚(TPnB)、3g增塑剂二丙二醇二苯甲酸酯、25g环氧树脂、5g固化剂、3g乙基三乙氧基硅烷偶联剂于100g丙酮溶剂内搅拌均匀；
(4)造粒烘干：将磷化粉末混入复合包覆剂内搅拌均匀后，进行造粒，后置于烘箱内进行80℃条件下60min烘烤，得到造粒粉；
(5)润滑与分筛：称取3g硬脂酸镁与粉末混合，混合后进行50-270目分筛，中间粒径粉末即为低损耗一体成型电感用粉末。
对比例5
本对比例与实施例2的区别在于原始粉末中羰基铁粉粒径为D50＝10um，气雾化铁硅铝合金粉末粒径为D50＝22um。
对比例6
本对比例与实施例2的区别在于使用的复合包覆剂为混合19g镍锌铁氧体粉末、25g环氧树脂、5g固化剂、3g乙基三乙氧基硅烷偶联剂的丙酮溶液。
对比例7
本对比例与实施例2的区别在于使用的复合包覆剂为混合6g成膜剂三丙二醇正丁醚(TPnB)、4g增塑剂二丙二醇二苯甲酸酯、30g环氧树脂、9g固化剂、3g乙基三乙氧基硅烷偶联剂的丙酮溶液。
对比例8
本对比例与实施例2的区别在于使用的复合包覆剂为混合10g镍锌铁氧体粉末、4g石英纤维粉、5g成膜剂三丙二醇正丁醚(TPnB)、28g环氧树脂、5g固化剂的丙酮溶液。
实施例2与对比例5、对比例6、对比例7、对比例8特性测试结果如表2所示：
表2：实施例2与对比例5、对比例6、对比例7、对比例8特性测试结果
通过对比实施例2与对比例5-8，根据表2可以看出，本发明使用铁硅铝合金粉末与羰基铁的混合粉末作为原始粉末，并采用复合包覆剂将其进行包覆，所制备材料的磁导率明显提高，损耗明显降低。
最后应说明的是，以上实施例仅用以说明本发明的技术方案，而非对其限制，尽管参照上述实施例对本发明进行了详细的说明，所属领域的普通技术人员应当理解，依然可以对本发明的具体实施方式进行修改或者等同替换，而未脱离本发明精神和范围的任何修改或者等同替换，其均应涵盖在本发明的权利要求范围当中。
Claims (10)
- 一种一体成型电感用低损耗粉末，其特征在于，材料主要由羰基铁粉、气雾化铁硅铝合金粉末、磷酸盐包覆剂、复合包覆剂和润滑剂组成，以羰基铁粉和气雾化铁硅铝合金粉末混合后的混合粉末质量为计算基础，其中：羰基铁粉粒径为D50＝4-8um，占混合粉末质量的45-55％，气雾化铁硅铝合金粉末粒径为D50＝15-20um，占混合粉末质量的55-45％；磷酸盐包覆剂是由混合粉末与磷酸丙酮溶液反应后产生，其中，磷酸质量为混合粉末质量的0.1-0.3％，丙酮为混合粉末质量的8-10％；复合包覆剂由0.3-1.2％的镍锌铁氧体粉末、0.2-0.6％的石英纤维粉、0.1-0.3％的成膜剂、0.1-0.4％的增塑剂、1.5-2.8％的环氧树脂、0.3-0.5％的固化剂、0.1-0.4％的偶联剂混合于丙酮溶剂中形成；润滑剂占混合粉末质量的0.2-0.4％。
- 根据权利要求1所述的一种一体成型电感用低损耗粉末，其特征在于，所述羰基铁粉粒径为D50＝5um，气雾化铁硅铝合金粉末粒径为D50＝15um，镍锌铁氧体粉末粒径为D50＝0.9-1.1um。
- 根据权利要求2所述的一种一体成型电感用低损耗粉末，其特征在于，所述镍锌铁氧体粉末为粒径是D50＝1.0um的球状粉末。
- 根据权利要求1所述的一种一体成型电感用低损耗粉末，其特征在于，所述石英纤维粉长径比为2:1，目数为7000目。
- 根据权利要求1所述的一种一体成型电感用低损耗粉末，其特征在于，所述成膜剂为二丙二醇单丁醚、三丙二醇正丁醚中的一种或二种混合；增塑剂为二乙二醇二苯甲酸酯、二丙二醇二苯甲酸酯中的一种或二种混合；固化剂为环氧固化剂；偶联剂为乙基三乙氧基硅烷；润滑剂为硬脂酸、石蜡微粉、硬脂酸镁中的一种或几种混合。
- 根据权利要求1-5任一所述的一种一体成型电感用低损耗粉末，其特征在于，所述低损耗 粉末的最外层是由复合包覆剂构成的网状包覆膜层，次外层是磷酸盐膜层，最内部是铁硅铝与羰基铁粉组成的基体，最终形成了双膜层包覆结构。
- 权利要求1所述一体成型电感用低损耗粉末的制备方法，其特征在于，包括如下步骤：(1)原始粉末混合：将羰基铁粉与气雾化铁硅铝合金粉末均匀混合得到混合粉末；(2)原始粉末的磷化：将步骤1得到的混合粉末加入磷酸丙酮溶液内进行混合搅拌、烘烤、冷却至室温得到磷化粉末，即在混合粉末表面形成磷酸盐膜层；(3)制备复合包覆剂：将镍锌铁氧体粉末、石英纤维粉、成膜剂、增塑剂、环氧树脂、固化剂、偶联剂于丙酮溶剂内混合均匀；(4)造粒烘干：将磷化粉末混入复合包覆剂内搅拌均匀后进行造粒，烘烤后得到造粒粉；(5)润滑与分筛：将润滑剂与造粒粉混合，混合后进行50-270目分筛，中间粒径的粉末为低损耗一体成型电感用粉末。
- 根据权利要求7所述一种一体成型电感用低损耗粉末的制备方法，其特征在于，所述步骤(2)中，将混合粉末加入磷酸丙酮溶液内进行混合搅拌20-30min，之后于100-120℃条件下烘烤15-30min，冷却至室温得到磷化粉末，其中磷酸质量为混合粉末质量的0.1-0.3％，丙酮为混合粉末质量的8-10％。
- 根据权利要求7所述一种一体成型电感用低损耗粉末的制备方法，其特征在于，所述步骤(3)中，丙酮溶剂质量为混合粉末质量的10-12％。
- 根据权利要求7所述一种一体成型电感用低损耗粉末的制备方法，其特征在于，所述步骤(4)中，烘烤温度为60-80℃，烘烤时间为40-60min。
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| CN114582580B (zh) * | 2022-05-06 | 2022-07-29 | 天通控股股份有限公司 | 一种软磁金属粉末及其制备方法 |
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