CN102623121A - Method for manufacturing iron-silicon material and Mu-90 iron-silicon magnetic powder core - Google Patents

Method for manufacturing iron-silicon material and Mu-90 iron-silicon magnetic powder core Download PDF

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CN102623121A
CN102623121A CN2012100958558A CN201210095855A CN102623121A CN 102623121 A CN102623121 A CN 102623121A CN 2012100958558 A CN2012100958558 A CN 2012100958558A CN 201210095855 A CN201210095855 A CN 201210095855A CN 102623121 A CN102623121 A CN 102623121A
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iron
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magnetic core
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CN102623121B (en
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柏海明
聂敏
朱小辉
许佳辉
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TDG Holding Co Ltd
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Abstract

The invention relates to a method for manufacturing an iron-silicon material and a Mu-90 iron-silicon magnetic powder core, comprising the following steps of: smelting of alloy, pulverizing, reducing of powder, grading of powder, proportioning of granularity, passivating of powder material, insulation coating, mold-pressing and molding, thermal treatment and surface coating. Small amounts of elements V and Nb are added in the alloy smelting process, and the magnetic performance of the iron-silicon alloy is improved; the powder prepared according to the invention is spherical and is smooth on the surface and easily and uniformly coated; the magnetic powder core has higher quality factors and excellent direct-current superposition characteristics; and meanwhile, de-ionized water is used as a passivation solution thinner and has the advantages of good passivation effect, low cost and convenience in mass production. When the frequency is 100KHz, the magnetic conductivity Mu of the magnetic powder core is 90; when the frequency is 100 KHz, the magnetic powder core is below 100Oe, and the coefficient of the initial magnetic conductivity is not less than 0.39; the loss Pcv (25KHz, 100mT) of volume ratio of the magnetic powder core is not more than 310 mW/cm<3>; and the temperature coefficient Alpha L of the magnetic powder core is less than 520*10-(6 DEG C)-1(-55 to 150 DEG C). The development requirements on low-voltage large-current, high-powder density and high-frequency in the traditional electronics industry are satisfied greatly.

Description

The manufacturing approach of a kind of iron silicon materials and μ 90 iron silica magnetic particle cores
Technical field
The present invention relates to field of powder metallurgy; Especially a kind of manufacturing approach of magnetic permeability μ 90 iron silica magnetic particle cores; This soft magnetic material is not only applicable to make big current power inductance, pfc circuit inductance, DC/DC transducer 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.Owing to one deck dielectric insulating film in the coated with uniform of soft-magnetic alloy powder particle, the resistivity of magnetic core is high, 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, Switching Power Supply as inductance filter, choking-winding, become one of important part of soft magnetic material.
Adopt iron silicon magnetically soft alloy to manufacture the magnetic core; Stabilized operating temperature can reach 200 ℃; Avoided magnetic core when hot operation, to produce the heat ageing problem; Simultaneously, its performance characteristics is just in time filled up between ferrocart core and other three kinds of alloy magnetic powder cores (iron sial, iron nickel, 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 does not have aging, and power loss is lower; Compare with Fe-Si-Al magnetic core, iron silica magnetic particle core has more excellent dc superposition characteristic; Compare with iron nickel, iron nickel molybdenum magnetic core, though its magnetic permeability range of choice is narrower, power loss is higher, and the dc superposition characteristic of iron silicon is more excellent than iron nickel molybdenum, and its cost is far below iron nickel and iron nickel molybdenum magnetic core.So the alloy magnetic powder core that adopts the ferro-silicium material to become 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 90 iron silica magnetic particle cores; This alloy magnetic core is fit to the requirement of present low-voltage, high-current, high power density, high frequencyization very much; 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, solar photovoltaic system; 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 90 iron silica magnetic particle cores; The composition of said iron silicon materials and μ 90 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, comprises 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-100 orders and-60 orders store;
E. grain size proportion: by-100 orders: the mass ratio of-60 orders=3:7 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; The phosphate aqueous solution that phosphoric acid was mixed with that slowly adds by powder quality 0.1%~0.4% in the powder after preheating carries out Passivation Treatment; Subsequently the powder after the passivation is changed in the baking oven and dry 150~200 ℃ of bake out temperatures;
G. insulation coats: in the powder of oven dry, add talcum powder or mica powder, 6.0% sodium metasilicate and 0.5% the zinc stearate of powder quality 0~0.4% successively, mix and dry;
H. compression molding: the briquetting pressure of magnetic core is got 1900~2200MPa, removes the corner burr after the moulding;
I. heat treatment: the magnetic core after the moulding is incubated 30~60min in 600~800 ℃ of inert gas shielding atmosphere; Said inert gas is nitrogen or argon gas;
J. face coat: the magnetic wicking surface carries out coating.
As a kind of preferred, the composition of said iron silicon materials and μ 90 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 deionized water in the said powder passivation, step as phosphoric acid.
As a kind of preferred, adopt talcum powder as insulating compound in the said powder insulation encapsulation steps.
As a kind of preferred, briquetting pressure is 2100MPa in the said compression molding step.
As a kind of preferred, temperature is 720 ℃ in the said 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, is prone to evenly coat, 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 deionized water to make the diluent of phosphoric acid among the present invention, passivation effect is suitable with existing method, and its cost is low, high safety, be convenient to production.
⑶ the physical property of magnetic permeability μ 90 iron silica magnetic particle cores of the present invention with have excellent magnetic characteristics.During 100kHz, magnetic permeability μ=90 of magnetic core; During 100kHz, the magnetic core under 100Oe, the coefficient of initial permeability>=0.39; The volume ratio loss P of magnetic core Cv(25kHz, 100mT)≤310mW/cm 3The temperature coefficient α of magnetic core L<520 * 10 -6-1(55~150 ℃) have satisfied the demand for development of present electron trade low-voltage, high-current, high power density and high frequencyization greatly.
Embodiment
Embodiment 1:
Armco 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, and these powders are inserted cool off after about 1100 ℃ of hydrogen furnace inherences are incubated 2h, be to guarantee the powder reduction quality; Dew point of hydrogen is controlled at below-60 ℃; According to granularity-100 order: the mass ratio of-60 orders=3:7 carries out the powder proportioning, afterwards with the phosphoric acid that is equivalent to alloy powder quality 0.2%, and adds deionized water and is diluted to certain density phosphoric acid solution and carries out Passivation Treatment; Form coating film on alloy powder surface, in alloy powder, add the talcum powder that is equivalent to alloy powder quality 0.4%, 6.0% sodium metasilicate and 0.5% zinc stearate successively and mix and dry; Alloy powder is dropped in the mould of φ 33.00 * φ 19.9 * 10.70 (being that external diameter is that 33.00mm, internal diameter are that 19.9mm, thickness are the ring-shaped magnetic core of 10.70mm) with 2100MPa (21t/cm 2) unit 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 at last gets final product.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic permeability μ=88.9 of magnetic core;
⑵ dc superposition characteristic: during 100kHz, the magnetic core is under the 100Oe magnetic field intensity, and the coefficient of initial permeability is 0.412;
⑶ the volume ratio loss P of magnetic core Cv(25kHz, 100 mT)=303.1mW/cm 3
⑷ the temperature coefficient α of magnetic core L=501 * 10 -6-1(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 permeability μ=89.5 of magnetic core;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability=0.404;
⑶ the volume ratio loss P of magnetic core Cv(25kHz, 100 mT)=293.5mW/cm 3
⑷ the temperature coefficient α of magnetic core L=480 * 10 -6-1(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 permeability μ=90.4 of magnetic core;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability=0.391;
⑶ the volume ratio loss P of magnetic core Cv(25kHz, 100 mT)=284.1mW/cm 3
⑷ the temperature coefficient α of magnetic core L=460 * 10 -6-1(55~150 ℃).
Embodiment 4:
Processing step according to embodiment 1; The powder that proportioning is good carries out Passivation Treatment with being equivalent to alloy powder quality 0.1% phosphoric acid and diluted phosphoric acid solution; Form coating film on the alloy powder surface; Add the talcum powder be equivalent to alloy powder quality 0.3%, 6.0% sodium metasilicate and 0.5% zinc stearate successively and mix, the 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 permeability μ=90.2 of magnetic core;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability=0.406;
⑶ the volume ratio loss P of magnetic core Cv(25kHz, 100 mT)=310mW/cm 3
⑷ the temperature coefficient α of magnetic core L=508 * 10 -6-1(55~150 ℃).
Embodiment 5:
Processing step according to embodiment 1; The powder that proportioning is good carries out Passivation Treatment with being equivalent to alloy powder quality 0.4% phosphoric acid and diluted phosphoric acid solution; Form coating film on the alloy powder surface; Add the mica powder be equivalent to alloy powder quality 0.1%, 6.0% sodium metasilicate and 0.5% zinc stearate successively and mix, alloy powder is dropped in the mould of φ 33.00 * φ 19.9 * 10.70 (being that external diameter is that 33.00mm, internal diameter are that 19.9mm, thickness are the ring-shaped magnetic core of 10.70mm) with 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 at last gets final product.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic permeability μ=89.1 of magnetic core;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability=0.396;
⑶ the volume ratio loss P of magnetic core Cv(25kHz, 100 mT)=321.5mW/cm 3
⑷ the temperature coefficient α of magnetic core L=536 * 10 -6-1(55~150 ℃).
Embodiment 6:
Carry 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 at last gets final product.The physical characteristic and the magnetic property of gained magnetic core:
⑴ during 100kHz, magnetic permeability μ=88.3 of magnetic core;
⑵ dc superposition characteristic: during 100kHz, the magnetic core under the 100Oe magnetic field intensity, the coefficient of initial permeability=0.415;
⑶ the volume ratio loss P of magnetic core Cv(25kHz, 100 mT)=298.3mW/cm 3
⑷ the temperature coefficient α of magnetic core L=493.6 * 10 -6-1(55~150 ℃).

Claims (5)

1. the preparation method of iron silicon materials and μ 90 iron silica magnetic particle cores; The composition of said iron silicon materials and μ 90 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, comprises 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-100 orders and-60 orders store;
E. grain size proportion: by-100 orders: the mass ratio of-60 orders=3:7 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; The phosphate aqueous solution that phosphoric acid was mixed with that slowly adds by powder quality 0.1%~0.4% in the powder after preheating carries out Passivation Treatment; Subsequently the powder after the passivation is changed in the baking oven and dry 150~200 ℃ of bake out temperatures;
G. insulation coats: in the powder of oven dry, add talcum powder or mica powder, 6.0% sodium metasilicate and 0.5% the zinc stearate of powder quality 0~0.4% successively, mix and dry;
H. compression molding: the briquetting pressure of magnetic core is got 1900~2200MPa, removes the corner burr after the moulding;
I. heat treatment: the magnetic core after the moulding is incubated 30~60min in 600~800 ℃ of inert gas shielding atmosphere; Said inert gas is nitrogen or argon gas;
J. face coat: the magnetic wicking surface carries out coating.
2. according to the manufacturing approach of said a kind of iron silicon materials of claim 1 and μ 90 iron silica magnetic particle cores, it is characterized in that: the composition of said iron silicon materials and μ 90 iron silica magnetic particle cores is Si:6.4wt%, V:0.4wt%, and Nb:0.2wt%, surplus is Fe.
3. according to the manufacturing approach of said a kind of iron silicon materials of claim 1 and μ 90 iron silica magnetic particle cores, it is characterized in that: adopt the diluent of deionized water in the said powder passivation, step as phosphoric acid.
4. according to the manufacturing approach of said a kind of iron silicon materials of claim 1 and μ 90 iron silica magnetic particle cores, it is characterized in that: briquetting pressure is 2100MPa in the said compression molding step.
5. according to the manufacturing approach of said a kind of iron silicon materials of claim 1 and μ 90 iron silica magnetic particle cores, it is characterized in that: temperature is 720 ℃ in the said heat treatment step, insulation 50min.
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CN103219119A (en) * 2013-04-18 2013-07-24 安泰科技股份有限公司 Preparation method of mu90 high-permeability Fe-based amorphous magnetic powder core
CN103594219A (en) * 2013-11-28 2014-02-19 四川东阁科技有限公司 Method for manufacturing sendust material and mu173 sendust magnetic powder core
CN104103413A (en) * 2014-06-24 2014-10-15 湖州南浔闻天磁性材料有限公司 Method for preparing magnetic powder core with high-flux magnet ring performance
CN105185560A (en) * 2015-08-24 2015-12-23 北京康普锡威科技有限公司 Preparation method of Fe-based metal soft magnetic powder core
CN105529124A (en) * 2016-01-19 2016-04-27 兆晶股份有限公司 Preparation method of iron-based non-crystal magnetic powder core
CN107369514A (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 90
CN107424706A (en) * 2017-04-28 2017-12-01 武汉钢铁有限公司 Silicon steel powder core and preparation method thereof
CN107578876A (en) * 2017-10-17 2018-01-12 德清森腾电子科技有限公司 A kind of manufacturing process of ferro-silicium soft-magnetic composite material
CN109148071A (en) * 2018-08-02 2019-01-04 浙江东睦科达磁电有限公司 A kind of preparation method of iron silicon materials and 100 iron silica magnetic particle core of μ
CN112071621A (en) * 2020-09-09 2020-12-11 德清鑫晨新材料有限公司 Manufacturing equipment of iron-silicon alloy magnetic powder core material with high direct-current superposition characteristic
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
CN113724958A (en) * 2021-08-31 2021-11-30 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying
CN114068167A (en) * 2021-11-15 2022-02-18 横店集团东磁股份有限公司 Soft magnetic composite material and preparation method and application thereof
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CN103219119A (en) * 2013-04-18 2013-07-24 安泰科技股份有限公司 Preparation method of mu90 high-permeability Fe-based amorphous magnetic powder core
CN103594219A (en) * 2013-11-28 2014-02-19 四川东阁科技有限公司 Method for manufacturing sendust material and mu173 sendust magnetic powder core
CN104103413A (en) * 2014-06-24 2014-10-15 湖州南浔闻天磁性材料有限公司 Method for preparing magnetic powder core with high-flux magnet ring performance
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CN107424706A (en) * 2017-04-28 2017-12-01 武汉钢铁有限公司 Silicon steel powder core and preparation method thereof
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CN107369514A (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 90
CN107578876B (en) * 2017-10-17 2020-05-12 德清森腾电子科技有限公司 Manufacturing process of iron-silicon alloy soft magnetic composite material
CN107578876A (en) * 2017-10-17 2018-01-12 德清森腾电子科技有限公司 A kind of manufacturing process of ferro-silicium soft-magnetic composite material
CN109148071A (en) * 2018-08-02 2019-01-04 浙江东睦科达磁电有限公司 A kind of preparation method of iron silicon materials and 100 iron silica magnetic particle core of μ
CN112071621A (en) * 2020-09-09 2020-12-11 德清鑫晨新材料有限公司 Manufacturing equipment of iron-silicon alloy magnetic powder core material with high direct-current superposition characteristic
CN112071621B (en) * 2020-09-09 2022-08-16 德清鑫晨新材料有限公司 Manufacturing equipment of iron-silicon alloy magnetic powder core material with high direct-current superposition characteristic
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
CN113724958A (en) * 2021-08-31 2021-11-30 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying
CN113724958B (en) * 2021-08-31 2024-04-16 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying
CN114068167A (en) * 2021-11-15 2022-02-18 横店集团东磁股份有限公司 Soft magnetic composite material and preparation method and application thereof
CN114724833A (en) * 2022-03-08 2022-07-08 天通(六安)新材料有限公司 Preparation method of gas-atomized iron-silicon-aluminum magnetic powder core with ultralow magnetic conductivity
CN114724833B (en) * 2022-03-08 2023-05-30 天通(六安)新材料有限公司 Preparation method of ultralow-permeability gas atomization sendust magnetic powder core

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