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CN102294476A - Ferrosilicon material and mu75 ferrosilicon magnetic powder core manufacturing method - Google Patents

Ferrosilicon material and mu75 ferrosilicon magnetic powder core manufacturing method Download PDF

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CN102294476A
CN102294476A CN2011102353748A CN201110235374A CN102294476A CN 102294476 A CN102294476 A CN 102294476A CN 2011102353748 A CN2011102353748 A CN 2011102353748A CN 201110235374 A CN201110235374 A CN 201110235374A CN 102294476 A CN102294476 A CN 102294476A
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powder
magnetic
iron
magnetic core
ferrosilicon
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CN102294476B (en
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杜成虎
柏海明
朱小辉
许佳辉
聂敏
孙蒋平
申志刚
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TDG Holding Co Ltd
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Abstract

The invention relates to a ferrosilicon material and mu75 ferrosilicon magnetic powder core manufacturing method, which comprises the steps of alloy smelting, milling, powder reduction, powder grading, granularity proportioning, powder passivation, insulative cladding, compression molding, heat treatment and surface coating. In the process of alloy smelting, a small number of V and Nb elements are added to improve the magnetic property of ferrosilicon alloy. The prepared powder is in a ball shape, has a smooth surface and is easy to clad uniformly, and the obtained magnetic powder core has a very high quality factor and an excellent direct current superposition characteristic. When the mu75 ferrosilicon magnetic powder core is at 100kHz, the magnetic conductivity mu is 75, Q is 50-60, and the coefficient of the initial magnetic conductivity is larger than or equal to 0.57 under 100Oe; the power loss Pcv (50kHz, 500Gs) is less than or equal to 150mW/cm<3>; and the temperature coefficient alpha T is less than 3.6*10<-4>/DEG C (-55-150 DEG C). The magnetic powder core prepared in the method disclosed by the invention greatly meets the development requirements of low-voltage large current, high power density and high frequency in the present electronic industry; and simultaneously, the magnetic powder core can also be manufactured into a high power density integrated inductor to be widely applied in point of load (POL) and voltage regulator module (VRM) power supplies.

Description

The manufacture method of a kind of iron silicon materials and μ 75 iron silica magnetic particle cores
Technical field
The present invention relates to field of powder metallurgy, especially a kind of manufacture method of magnetic conductivity μ 75 iron silica magnetic particle cores, this soft magnetic materials is not only applicable to make big current power inductance, pfc circuit inductance, DC/DC converter and photovoltaic DC-to-AC converter etc., also is applicable to preparation high power density one inductor.
Background technology
Magnetically soft alloy magnetic core is that soft-magnetic alloy powder is mixed a kind of compound soft magnetic material that compacting forms with dielectric.Since one deck dielectric insulating film in the coated with uniform of soft-magnetic alloy powder particle, the resistivity height of magnetic core, thereby eddy-current loss is very low, is suitable for upper frequency and uses.In addition, the magnetic core also has advantages such as higher saturation induction density, good frequency characteristic and permanent magnetic conduction, make the magnetic core be widely used in fields such as telecommunications, radar, power switch as inductance filter, choking-winding, become one of important part of soft magnetic materials.
Adopt iron silicon magnetically soft alloy to manufacture the magnetic core, operating temperature can reach 200 ℃, avoided the heat ageing problem of magnetic core when hot operation, simultaneously, its performance characteristics is just in time filled up between ferrocart core and other three kinds of alloy magnetic powder cores (high magnetic flux, iron sial, iron nickel molybdenum) with characteristics such as high performance-price ratio and good dc superposition characteristic, high-frequency low-consumption characteristics.Compare with ferrocart core, iron silica magnetic particle core cannot not have agingly, the advantage that power attenuation is low; Compare with Fe-Si-Al magnetic core, iron silica magnetic particle core has more excellent dc superposition characteristic, lower price; Compare with iron nickel magnetic core, the dc superposition characteristic of the two is suitable, and loss ratio iron nickel magnetic core is slightly high, but because nickel is noble metal, costs an arm and a leg, so the cost of iron silica magnetic particle core will be far below iron nickel magnetic core.So the alloy magnetic powder core that adopts the ferro-silicium material to be made into has wide application, has caused the extensive concern of industry.
Summary of the invention
The objective of the invention is to produce a kind of iron silicon materials of preparation and μ 75 iron silica magnetic particle cores, this alloy magnetic core is particularly suitable for the requirement of present low-voltage, high-current, high power density, high frequencyization, can substitute the part ferrocart core, Fe-Si-Al magnetic core, products such as iron nickel magnetic core.The inductor that the magnetic core that uses the present invention to prepare is made can be applied to inverter, electric power active power factor compensating circuit, the filtering of solar photovoltaic system power supply; Also can be made into high power density one inductor, widely apply in POL POL and the VRM power supply.
The present invention takes following technical proposals:
The preparation method of a kind of iron silicon materials and μ 75 iron silica magnetic particle cores, the composition of described iron silicon materials and μ 75 iron silica magnetic particle cores is the binary system ferro-silicium and adds micro-Nb and V element, the content of Si is 6.4wt%~7.0wt%, surplus is Fe, comprise alloy melting, powder process, powder reduction, powder classification, grain size proportion, powder passivation, insulation coating, compression molding, heat treatment and face coat step, wherein:
A. alloy melting: alloy melting carries out in magnesia crucible open type intermediate frequency furnace, and smelting temperature is more than 1400 ℃, and the time of alloy melting is more than 50min;
B. powder process: alloy melting directly carries out nitrogen spray powder process after well, carries out annealing in process after the spraying powder is crossed 60 mesh sieves;
C. powder reduction: adopt hydrogen reducing, dew point of hydrogen is controlled at below-60 ℃;
D. powder classification: powder is carried out classification by-200 orders ,-100 orders ,-60 orders store;
E. grain size proportion: by-200 orders :-100 orders: the mass ratio of-60 orders=3:3:1 carries out the powder proportioning;
F. powder passivation: the powder that proportioning is good changes preheating in the baking oven over to, 100~200 ℃ of preheat temperatures, slowly add powder quality 0.8%~1.2% phosphoric acid solution in the powder after preheating and carry out Passivation Treatment, the powder after the passivation is changed in the baking oven dry subsequently, 150~200 ℃ of bake out temperatures;
G. insulation coats: add the talcum powder of powder quality 0.6%~0.8% or mica powder, 6.0% sodium metasilicate and 0.5% zinc stearate successively in the powder of oven dry, mix and dry;
H. compression molding: the briquetting pressure of magnetic core is got 1800~2000MPa, removes the corner burr after the moulding;
I. heat treatment: the magnetic core after the moulding is incubated 30~60min in 600~800 ℃ nitrogen or ar gas environment;
J. face coat: the magnetic wicking surface carries out coating.
As a kind of preferred, the composition of described iron silicon materials and μ 75 iron silica magnetic particle cores is Si:6.4wt%, V:0.4wt%, and Nb:0.2wt%, surplus is Fe.
As a kind of preferred, adopt the diluent of water for industrial use in the described powder passivation step as phosphoric acid; Described phosphoric acid solution is a phosphate aqueous solution, and its mass concentration is 30%.
As a kind of preferred, briquetting pressure is 1900MPa in the described compression molding step.
As a kind of preferred, temperature is 720 ℃ in the described heat treatment step, insulation 50min.
Advantage of the present invention and good effect:
⑴ the powder that the present invention produces is spherical and smooth surface, easily evenly coats, and gained magnetic core has very high quality factor and excellent dc superposition characteristic.
⑵ among the existing preparation method, adopt acetone and other organic solvent to make the diluent of passivator usually, and adopt water for industrial use to make the diluent of phosphoric acid among the present invention, passivation effect is suitable with existing method, and therefore, cost is low, high safety, be convenient to production.
⑶ the physical property of magnetic conductivity μ 75 iron silica magnetic particle cores of the present invention and having excellent magnetic characteristics.During 100kHz, magnetic conductivity μ=75 of magnetic core, Q=50~60; During 100kHz, the magnetic core under 100Oe, the coefficient of initial permeability 〉=0.57; The volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3Temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃) have satisfied the demand for development of present electron trade low-voltage, high-current, high power density, high frequencyization greatly.
The specific embodiment
Embodiment 1:
Ingot iron, silicon metal, ferro-niobium, vanadium iron are dropped into successively in the intermediate frequency furnace of 50 kilograms of nominals and smelt, composition is Si:6.4wt%, V:0.4wt%, and Nb:0.2wt%, surplus is Fe; Add an amount of titanium sponge simultaneously,, be not present in the alloy of melting for smelting the usefulness of slagging-off; Smelting temperature is about 1400 ℃, the time 1h of alloy melting; Alloy melting directly carries out nitrogen spray powder process after well, the spraying powder is crossed 60 mesh sieves, cool off after these powders are inserted inherent about the 1100 ℃ insulation 2h of hydrogen furnace, for guaranteeing the powder reduction quality, dew point of hydrogen is controlled at below-60 ℃, according to granularity-200 order :-100 orders: the mass ratio of-60 orders=3:3:1 carries out the powder proportioning, be that 30% phosphate aqueous solution carries out Passivation Treatment with the mass concentration that is equivalent to alloy powder quality 0.8% afterwards, form coating film on the alloy powder surface, in alloy powder, add 0.7% talcum powder successively, 6.0% sodium metasilicate and 0.5% zinc stearate mix and dry; It is that external diameter is that 33.00mm, internal diameter are that 19.9mm, thickness are the ring-shaped magnetic core of 10.70mm that alloy powder is dropped into φ 33.00 * φ 19.9 * 10.70() mould in use 1900MPa(19T/cm 2) pressure compression moulding, the magnetic core after the moulding is incubated 50min and carries out destressing heat treatment in 720 ℃ nitrogen environment, the surface that is coated in the magnetic core with the modified form epoxy resin coating gets final product at last.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic conductivity μ=74.9 of magnetic core, Q=56.2;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability 〉=0.57;
⑶ the volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3
⑷ temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃).
Embodiment 2:
The alloy melting composition is Si:6.7wt%, V:0.5wt%, and Nb:0.2wt%, surplus is Fe, subsequent process steps is carried out according to embodiment 1.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic conductivity μ=75.3 of magnetic core, Q=51.9;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability 〉=0.57;
⑶ the volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3
⑷ temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃).
Embodiment 3:
The alloy melting composition is Si:6.92wt%, V:0.4wt%, and Nb:0.2wt%, surplus is Fe, subsequent process steps is carried out according to embodiment 1.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic conductivity μ=75.7 of magnetic core, Q=54.3;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability 〉=0.57;
⑶ the volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3
⑷ temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃).
Embodiment 4:
Processing step according to embodiment 1, powder that proportioning is good is that 30% phosphate aqueous solution carries out Passivation Treatment with the mass concentration that is equivalent to alloy powder quality 1.0%, form coating film on the alloy powder surface, adding the talcum powder be equivalent to alloy powder quality 0.6%, 6.0% sodium metasilicate and 0.5% zinc stearate successively insulate, processing step according to embodiment 1 carries out subsequently, makes the magnetic core.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic conductivity μ=75.2 of magnetic core, Q=59.7;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability 〉=0.57;
⑶ the volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3
⑷ temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃).
Embodiment 5:
Processing step according to embodiment 1, powder that proportioning is good is that 30% phosphate aqueous solution carries out Passivation Treatment with the mass concentration that is equivalent to alloy powder quality 1.2%, form coating film on the alloy powder surface, add 0.8% mica powder, 6.0% sodium metasilicate and 0.5% zinc stearate successively and insulate, it is that external diameter is that 33.00mm, internal diameter are that 19.9mm, thickness are the ring-shaped magnetic core of 10.70mm that alloy powder is dropped into φ 33.00 * φ 19.9 * 10.70() mould in use 2000MPa(20T/cm 2) pressure compression moulding, the magnetic core after the moulding is incubated 50min and carries out destressing heat treatment in 720 ℃ nitrogen environment, the surface that is coated in the magnetic core with the modified form epoxy resin coating gets final product at last.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic conductivity μ=75.1 of magnetic core, Q=52.1;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability 〉=0.57;
⑶ the volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3
⑷ temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃).
Embodiment 6:
Processing step according to embodiment 1, powder that proportioning is good is that 30% phosphate aqueous solution carries out Passivation Treatment with the mass concentration that is equivalent to alloy powder quality 1.2%, form coating film on the alloy powder surface, add 0.8% mica powder, 6.0% sodium metasilicate and 0.5% zinc stearate successively and insulate, alloy powder is dropped in the mould of φ 33.00 * φ 19.9 * 10.70 and use 1800MPa(18T/cm 2) pressure compression moulding, the magnetic core after the moulding is incubated 50min and carries out destressing heat treatment in 720 ℃ nitrogen environment, the surface that is coated in the magnetic core with the modified form epoxy resin coating gets final product at last.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic conductivity μ=74.6 of magnetic core, Q=49.5;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability 〉=0.57;
⑶ the volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3
⑷ temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃).
Embodiment 7:
The alloy melting composition is Si:6.98wt%, V:0.4wt%, Nb:0.2wt%, surplus is Fe, subsequent process steps is carried out according to embodiment 1, place 750 ℃ nitrogen environment insulation 50min to carry out destressing heat treatment in the magnetic core after the compression moulding, the surface that is coated in the magnetic core with the modified form epoxy resin coating gets final product at last.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic conductivity μ=75.0 of magnetic core, Q=58.3;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability 〉=0.57;
⑶ the volume ratio loss P of magnetic core Cv(50kHz, 500Gs)≤150mW/cm 3
⑷ temperature coefficient α T<3.6 * 10 of magnetic core -4/ ℃ (55~150 ℃).

Claims (5)

1. the preparation method of iron silicon materials and μ 75 iron silica magnetic particle cores, the composition of described iron silicon materials and μ 75 iron silica magnetic particle cores is the binary system ferro-silicium and adds micro-Nb and V element, the content of Si is 6.4wt%~7.0wt%, surplus is Fe, comprise alloy melting, powder process, powder reduction, powder classification, grain size proportion, powder passivation, insulation coating, compression molding, heat treatment and face coat step, it is characterized in that:
A. alloy melting: alloy melting carries out in magnesia crucible open type intermediate frequency furnace, and smelting temperature is more than 1400 ℃, and the time of alloy melting is more than 50min;
B. powder process: alloy melting directly carries out nitrogen spray powder process after well, carries out annealing in process after the spraying powder is crossed 60 mesh sieves;
C. powder reduction: adopt hydrogen reducing, dew point of hydrogen is controlled at below-60 ℃;
D. powder classification: powder is carried out classification by-200 orders ,-100 orders ,-60 orders store;
E. grain size proportion: by-200 orders :-100 orders: the mass ratio of-60 orders=3:3:1 carries out the powder proportioning;
F. powder passivation: the powder that proportioning is good changes preheating in the baking oven over to, 100~200 ℃ of preheat temperatures, slowly add powder quality 0.8%~1.2% phosphoric acid solution in the powder after preheating and carry out Passivation Treatment, the powder after the passivation is changed in the baking oven dry subsequently, 150~200 ℃ of bake out temperatures;
G. insulation coats: add the talcum powder of powder quality 0.6%~0.8% or mica powder, 6.0% sodium metasilicate and 0.5% zinc stearate successively in the powder of oven dry, mix and dry;
H. compression molding: the briquetting pressure of magnetic core is got 1800~2000MPa, removes the corner burr after the moulding;
I. heat treatment: the magnetic core after the moulding is incubated 30~60min in 600~800 ℃ nitrogen or ar gas environment;
J. face coat: the magnetic wicking surface carries out coating.
2. according to the manufacture method of described a kind of iron silicon materials of claim 1 and μ 75 iron silica magnetic particle cores, it is characterized in that: the composition of described iron silicon materials and μ 75 iron silica magnetic particle cores is Si:6.4wt%, V:0.4wt%, and Nb:0.2wt%, surplus is Fe.
3. according to the manufacture method of described a kind of iron silicon materials of claim 1 and μ 75 iron silica magnetic particle cores, it is characterized in that: adopt the diluent of water for industrial use in the described powder passivation step as phosphoric acid; Described phosphoric acid solution is a phosphate aqueous solution, and its mass concentration is 30%.
4. according to the manufacture method of described a kind of iron silicon materials of claim 1 and μ 75 iron silica magnetic particle cores, it is characterized in that: briquetting pressure is 1900MPa in the described compression molding step.
5. according to the manufacture method of described a kind of iron silicon materials of claim 1 and μ 75 iron silica magnetic particle cores, it is characterized in that: temperature is 720 ℃ in the described heat treatment step, insulation 50min.
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Cited By (9)

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CN103839642A (en) * 2013-12-19 2014-06-04 横店集团东磁股份有限公司 Neu flux core material with permeability being 75 and preparing method thereof
CN104233055A (en) * 2014-09-03 2014-12-24 湖州南浔闻天磁性材料有限公司 Preparation method of iron-silicon material and iron-silicon magnetic powder core
CN104584150A (en) * 2012-08-31 2015-04-29 株式会社神户制钢所 Iron powder for powder magnetic core and process for producing powder magnetic core
CN106521312A (en) * 2016-11-01 2017-03-22 电子科技大学 Method for preparing FeSiAl-series alloy micro powder electromagnetic absorbent
CN107369516A (en) * 2017-07-20 2017-11-21 天通(六安)新材料有限公司 A kind of manufacture method of the composite magnetic powder cores of μ 75
CN112837919A (en) * 2020-12-30 2021-05-25 深圳市铂科新材料股份有限公司 Antirust alloy magnetic core and preparation method and application thereof
CN113314326A (en) * 2021-04-29 2021-08-27 天通控股股份有限公司 High-permeability low-eddy-current-loss insulating powder and preparation method thereof
CN116013678A (en) * 2023-03-02 2023-04-25 深圳信义磁性材料有限公司 Preparation method of low-loss ferrosilicon magnetic powder core material

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CN104584150B (en) * 2012-08-31 2017-09-22 株式会社神户制钢所 The manufacture method of iron powder for dust core and compressed-core
CN104584150A (en) * 2012-08-31 2015-04-29 株式会社神户制钢所 Iron powder for powder magnetic core and process for producing powder magnetic core
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CN103839642A (en) * 2013-12-19 2014-06-04 横店集团东磁股份有限公司 Neu flux core material with permeability being 75 and preparing method thereof
CN103839642B (en) * 2013-12-19 2016-04-20 横店集团东磁股份有限公司 A kind of μ 75 iron tantnickel powder core material and preparation method thereof
CN104233055A (en) * 2014-09-03 2014-12-24 湖州南浔闻天磁性材料有限公司 Preparation method of iron-silicon material and iron-silicon magnetic powder core
CN106521312A (en) * 2016-11-01 2017-03-22 电子科技大学 Method for preparing FeSiAl-series alloy micro powder electromagnetic absorbent
CN106521312B (en) * 2016-11-01 2018-04-06 电子科技大学 A kind of preparation method of FeSiAl systems alloy powder electromagnetic absorption agent
CN107369516A (en) * 2017-07-20 2017-11-21 天通(六安)新材料有限公司 A kind of manufacture method of the composite magnetic powder cores of μ 75
CN112837919A (en) * 2020-12-30 2021-05-25 深圳市铂科新材料股份有限公司 Antirust alloy magnetic core and preparation method and application thereof
CN113314326A (en) * 2021-04-29 2021-08-27 天通控股股份有限公司 High-permeability low-eddy-current-loss insulating powder and preparation method thereof
CN116013678A (en) * 2023-03-02 2023-04-25 深圳信义磁性材料有限公司 Preparation method of low-loss ferrosilicon magnetic powder core material
CN116013678B (en) * 2023-03-02 2023-10-17 深圳信义磁性材料有限公司 Preparation method of low-loss ferrosilicon magnetic powder core material

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