CN101871071B - Manufacturing method of soft magnet silicon-aluminum alloy magnetic powder core with small amounts of rare earth element cerium or lanthanum - Google Patents
Manufacturing method of soft magnet silicon-aluminum alloy magnetic powder core with small amounts of rare earth element cerium or lanthanum Download PDFInfo
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- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 22
- 229910052746 lanthanum Inorganic materials 0.000 title claims abstract description 20
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 12
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims description 14
- 229910000838 Al alloy Inorganic materials 0.000 title abstract 2
- 239000006247 magnetic powder Substances 0.000 title abstract 2
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 36
- 239000000956 alloy Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 6
- 229910000640 Fe alloy Inorganic materials 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000314 lubricant Substances 0.000 claims abstract description 5
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 4
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 4
- GSVIBLVMWGSPRZ-UHFFFAOYSA-N cerium iron Chemical compound [Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Ce].[Ce] GSVIBLVMWGSPRZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002161 passivation Methods 0.000 claims abstract description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims abstract description 4
- 238000005507 spraying Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 241001062472 Stokellia anisodon Species 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical group S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920005591 polysilicon Polymers 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical group [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 229910001021 Ferroalloy 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
- 230000035699 permeability Effects 0.000 abstract description 15
- 238000003723 Smelting Methods 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000006698 induction Effects 0.000 abstract description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 abstract 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 230000007423 decrease Effects 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- NNLJGFCRHBKPPJ-UHFFFAOYSA-N iron lanthanum Chemical compound [Fe].[La] NNLJGFCRHBKPPJ-UHFFFAOYSA-N 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 229910000702 sendust Inorganic materials 0.000 description 7
- 229910002796 Si–Al Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a manufacturing method of a soft magnet silicon-aluminum alloy magnetic powder core with small amounts of rare earth element cerium or lanthanum, which comprises the following steps: 1) smelting industrial pure iron, polycrystalline silicon, pure aluminum, cerium-iron alloy or lanthanum-iron alloy in a vacuum induction furnace into FeSiAl alloy cast ingots with small amounts of cerium or lanthanum, wherein the alloy cast ingots comprise the components of 9.0-9.8% of Si, 5.4-6.0% of Al, 0.02-0.25% of Ce or La, 0.006-0.015% of C, 0.008-0.010% of O2, 0.008-0.028% of S, 0.03-0.035% of P and balance of Fe; and mechanically crushing into FeSiAl alloy powder, carrying out high-heat treatment in a shielding gas atmosphere, and then screening; 2) carrying out surface passivation treatment on the FeSiAl alloy powder with phosphoric acid and alcohol, then adding 0.20% of kaolin, 0.20% of lubricant and 0.50% of parting compound, uniformly mixing, and carrying out pressure forming; and 3) carrying out heat treatment and surface spraying. The invention can increase the resistivity of the magnetic core and reduce the high-frequency eddy current loss, and has lower magnetic core loss. Besides, the invention improves the temperature stability of the magnetic permeability, and enables the decline of the magnetic permeability to be less than 3% when the working temperature rises to 125 DEG C.
Description
Technical field
The present invention relates to the manufacture method of magnetic bodies, relate in particular to a kind of manufacture method of adding the soft magnet silicon-aluminum magnetic core of a small amount of rare-earth element cerium or lanthanum.This magnetic core scope of application is very extensive, mainly is applicable in PFC inductance and output inductor among LED power supply, Switching Power Supply and the UPS, the electromagnetic interface filter main transformer and other pulse transformer etc. in differential mode inductance, the anti exciting converter.
Background technology
Sendust has good soft magnetic characteristic, as far back as last century the '30s just found by the Japanese, particularly special component Si～9.6%, Al～5.4%, surplus is the alloy of Fe, μ m value can reach 160,000, is named as the Sendust alloy.For no other reason than that silicon, aluminium are easy to generate segregation and scaling loss and are not widely used when smelting.Last century, the nineties was because the progress of smelting technique and the growth requirement of electronics industry have promoted the development of sendust magnetic core.Japanese subsequently gold show husband adds neodymium (Nd) in the Sendust alloy, improved its processability, magnetic (μ
0, μ
m, Hc, Bs), resistance to wear all do not reduce.The researcher's additional element that has (Sn, Be, Ti, V, Y, B, Mo, W, Cr etc.) back alloy rigidity has improved, and the resistance to wear that has has improved.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of manufacture method of adding the soft magnet silicon-aluminum magnetic core of a small amount of rare-earth element cerium or lanthanum is provided.
The manufacture method of adding the soft magnet silicon-aluminum magnetic core of a small amount of rare-earth element cerium or lanthanum comprises the steps:
1) will smelt in Armco iron, polysilicon, fine aluminium, cerium-iron alloy or the lanthanum ferroalloy input vaccum sensitive stove, be smelted into the FeSiAl alloy cast ingot that contains a small amount of rare-earth element cerium or lanthanum, the mass percentage content that its alloy cast ingot is formed is: Si 9.0～9.8%, Al 5.4～6.0%, Ce or La 0.02～0.25%, C 0.006～0.015%, O
20.008～0.010%, S 0.008～0.028%, P 0.03～0.035%, all the other are Fe.
2) alloy cast ingot is become the FeSiAl alloy powder with Mechanical Crushing; after the protective atmosphere high-temperature heat treatment, sieve; make the mass percentage content of FeSiAl alloy powder granularmetric composition be :-100～+ 140 orders account for 5%;-140～+ 200 orders account for 15%;-200～+ 300 orders account for 45%, and-300 orders account for 35%.
3) after above-mentioned FeSiAl alloy powder carries out the surface passivation processing with the phosphoric acid alcoholic solution, add 0.2% kaolin again, 0.2% lubricant, 0.5% release agent mixes; Use the dry powder automatic forming hydraulic press compression molding, pressure is 22～25T/cm
2, compacting is shaped as annular.
4) press-formed product heat treatment under nitrogen protection, heat treatment temperature is: 640～690 ℃, at last with the soft magnet silicon-aluminum magnetic core that obtains adding a small amount of rare-earth element cerium or lanthanum after the spraying of epoxy resin paint.
Described release agent is zinc stearate or barium stearate.Described lubricant is a molybdenum sulfide.The present invention compared with prior art has following beneficial effect:
1) improved the resistance coefficient of sendust magnetic core,, made the resistance coefficient of alloy can reach 82-85x10 owing to add a small amount of rare-earth element cerium or lanthanum in the alloy
-6Ω m;
2) reduced the power loss of Fe-Si-Al magnetic core, the sendust magnetic core made from this alloy is 125 ± 5 at magnetic permeability, frequency is that 50KHz, magnetic flux density are that power loss unshakable in one's determination under the 500Gs condition can be reduced to 70mw/cm
3Below;
3) improved the temperature stability of magnetic core magnetic permeability, making magnetic permeability with this alloy is 125 Fe-Si-Al magnetic core, and the temperature stability of its magnetic permeability is strong, and the fall of magnetic permeability was less than 3% when working temperature rose to 125 ℃.
Embodiment
Embodiment 1:
1) sendust is smelted the vacuum medium frequency induction furnace of selecting nominal 100Kg for use, earlier Armco iron is melted, successively polysilicon, fine aluminium, cerium-iron alloy are dropped in the vaccum sensitive stove then and smelt, adopt electromagnetic agitation to be smelted into the FeSiAl alloy cast ingot, the mass percentage content that its FeSiAl alloy cast ingot is formed is: Si9%, and Al 6.0%, and Ce 0.02%, C 0.015%, O
20.010%, S 0.008%, and P 0.035%, and surplus is Fe.
2) alloy cast ingot is become the FeSiAl alloy powder with Mechanical Crushing; after the protective atmosphere high-temperature heat treatment, sieve; make the mass percentage content of FeSiAl alloy powder granularmetric composition be :-100～+ 140 orders account for 5%;-140～+ 200 orders account for 15%;-200～+ 300 orders account for 45%, and-300 orders account for 35%.
3) powder being carried out surface passivation handles, extract above-mentioned FeSiAl alloy powder 1000g, pour with 5g phosphoric acid again that proportioning becomes the phosphoric acid alcoholic solution in the 80g alcohol into, the phosphoric acid alcoholic solution is poured into to stir in the FeSiAl alloy powder of this 1000g makes its drying, and then add kaolin 2g, molybdenum sulfide 2g, zinc stearate 5g mix; Use the dry powder automatic forming hydraulic press compression molding, pressure is 22T/cm
2, compacting annular size: external diameter Φ 26.90mm, internal diameter Φ 14.70mm, height 11.20mm.；
4) press-formed product is in nitrogen protection heat treatment, and heat treatment temperature is: 670 ℃, and at last with the soft magnet silicon-aluminum magnetic core that obtains adding a small amount of rare-earth element cerium after the spraying of epoxy resin paint.The resistance alloys coefficient reaches 82.5 * 10
-6Ω m.Sample detects and adopts coiling inductance coil enamelled wire Φ 0.5mm, 26 circles.Its magnetic parameter such as table 1.
Table 1
The corresponding inductance coefficent 159nH/N of inductance value 107.5 μ H
2, meet magnetic permeability 125.
Magnetic permeability varies with temperature as table 2:
Table 2
Embodiment 2:
Manufacture method is with embodiment 1, and alloy composition is Si 9.56%, and Al 5.4%, and Ce 0.125%, C0.012%, O
20.010%, S 0.025%, and P 0.032%, and surplus is Fe, compacting pressure 23T/cm
2, 690 ℃ of heat treatment temperatures.
The resistance alloys coefficient is 83.8 * 10
-6Ω m.
The magnetic parameter such as the table 3 of embodiment 2 goods.
Compacting annular size: external diameter Φ 16.50mm, internal diameter Φ 10.15mm, height 6.35mm.Coiling inductance coil enamelled wire Φ 0.5mm, 17 circles.
Table 3
The corresponding inductance coefficent 74nH/N of inductance value 21.4 μ H
2Meet magnetic permeability 125.
Magnetic permeability varies with temperature rate such as table 4
Table 4
Embodiment 3:
Manufacture method is with embodiment 1, and chemical composition is Si 9.80%, and Al 5.62%, and Ce 0.250%, and C 0.008%, O
20.008%, S 0.028%, and P 0.030%, and surplus is Fe, compacting pressure 25T/cm
2, 640 ℃ of heat treatment temperatures
The resistance alloys coefficient is 85.2 * 10
-6Ω m.
The magnetic parameter such as the table 5 of magnetic core goods
Compacting size: external diameter Φ 33.0mm, internal diameter Φ 19.95mm, height 11.20mm.Coiling inductance coil enamelled wire Φ 0.5mm, 33 circles.
Table 5
The corresponding inductance coefficent 137nH/N of inductance value 149.2 μ H
2Corresponding magnetic permeability 125.
Magnetic permeability varies with temperature rate such as table 6
Table 6
Embodiment 4:
Manufacture method is with embodiment 1, and main chemical compositions such as table 7, remainder are Fe (being mass percent).
Table 7
Suppress annular size with embodiment 1, resistance alloys coefficient such as table 7.
The magnetic parameter such as the table 8 of magnetic core goods
Table 8
DC Bias 20 Oe, 100KHz, all greater than 74%, on show the corresponding magnetic permeability 125 ± 5% of inductance value
Magnetic permeability varies with temperature as table 9
Table 9
Claims (3)
1. a manufacture method of adding the soft magnet silicon-aluminum magnetic core of a small amount of rare-earth element cerium or lanthanum is characterized in that comprising the steps:
1) will smelt in Armco iron, polysilicon, fine aluminium, cerium-iron alloy or the lanthanum ferroalloy input vaccum sensitive stove, be smelted into the FeSiAl alloy cast ingot that contains a small amount of rare-earth element cerium or lanthanum, the mass percentage content that its alloy cast ingot is formed is: Si9.0～9.8%, Al 5.4～6.0%, Ce or La 0.02～0.25%, C 0.006～0.015%, O 0.008～0.010%, S 0.008～0.028%, P 0.03～0.035%, all the other are Fe;
2) alloy cast ingot is become the FeSiAl alloy powder with Mechanical Crushing, after the protective atmosphere high-temperature heat treatment, sieve, make the mass percentage content of FeSiAl alloy powder granularmetric composition be :-100～+ 140 orders account for 5%,-140～+ 200 orders account for 15%,-200～+ 300 orders account for 45%, and-300 orders account for 35%;
3) after above-mentioned FeSiAl alloy powder carries out the surface passivation processing with the phosphoric acid alcoholic solution, add 0.2% kaolin again, 0.2% lubricant, 0.5% release agent mixes; Use the dry powder automatic forming hydraulic press compression molding, pressure is 22～25T/cm
2, compacting is shaped as annular;
4) press-formed product heat treatment under nitrogen protection, heat treatment temperature is: 640～690 ℃, at last with the soft magnet silicon-aluminum magnetic core that obtains adding a small amount of rare-earth element cerium or lanthanum after the spraying of epoxy resin paint.
2. a kind of manufacture method of adding the soft magnet silicon-aluminum magnetic core of a small amount of rare-earth element cerium or lanthanum according to claim 1 is characterized in that described release agent is zinc stearate or barium stearate.
3. a kind of manufacture method of adding the soft magnet silicon-aluminum magnetic core of a small amount of rare-earth element cerium or lanthanum according to claim 1 is characterized in that described lubricant is a molybdenum sulfide.
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| CN102360661A (en) * | 2011-05-19 | 2012-02-22 | 浙江科达磁电有限公司 | Iron-silicon alloy soft magnetic material with magnetic permeability μ=75 and its manufacturing method |
| CN102314986A (en) * | 2011-05-19 | 2012-01-11 | 浙江科达磁电有限公司 | A kind of iron-silicon alloy magnetic powder core and its manufacturing method |
| CN102268605B (en) * | 2011-08-11 | 2013-10-16 | 广东省钢铁研究所 | Method for preparing iron silicon soft magnetic alloy |
| CN102744403A (en) * | 2012-06-19 | 2012-10-24 | 同济大学 | Preparation method of nanocrystalline magnetic powder cores |
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| CN103456479A (en) * | 2013-03-24 | 2013-12-18 | 广州市德珑电子器件有限公司 | Method for manufacturing high-temperature-resistant metal soft magnetic powder core |
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| CN103578736A (en) * | 2013-10-28 | 2014-02-12 | 任静儿 | Soft-magnetic inductive iron core manufacturing method |
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| CN107633931A (en) * | 2017-09-15 | 2018-01-26 | 安徽信息工程学院 | A kind of alloy for magnetic composite and preparation method thereof |
| CN107644722A (en) * | 2017-09-15 | 2018-01-30 | 安徽信息工程学院 | A kind of alloy for permanent-magnet material and preparation method thereof |
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| CN112233870A (en) * | 2020-10-26 | 2021-01-15 | 江苏智仁景行新材料研究院有限公司 | Nanoscale Fe-Si-Al soft magnetic alloy powder and preparation method thereof |
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| CN100367421C (en) * | 2004-12-14 | 2008-02-06 | 王�锋 | Method for manufacturing soft magnet silicon-aluminium magnetic powder core |
| CN101090019A (en) * | 2007-04-26 | 2007-12-19 | 王忠强 | Manufacturing method of high magnetoconductivity FcSiAl magnetic powder core |
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