CN103426580B - A kind of composite magnetic powder core and preparation method thereof - Google Patents
A kind of composite magnetic powder core and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of composite magnetic powder core and preparation method thereof.Technical scheme is: hydro-thermal method prepares the Nano-Ferrite Particle of particle size uniformity, repressed, Technology for Heating Processing at soft-magnetic alloy powder surface in situ, prepares novel ferrite composite magnetic powder core.The invention have the advantage that (1) is owing to using hydro-thermal method in-situ method to prepare MnZn, nickel-zinc ferrite, in that context it may be convenient to prepare the nano-particle that particle size size is uniform, controlled；(2) ferrite is as the insulating wrapped agent of soft-magnetic alloy powder, the shortcoming causing matrix magnetic property to reduce when overcoming tradition namagnetic substance as covering, it is possible to obtain higher pcrmeability and saturation magnetization.
Description
Technical field
The present invention relates to a kind of composite magnetic powder core and preparation method thereof, belong to field of material preparation.
Background technology
Soft magnetic materials is a class material with ferromagnetic ferromagnetism or ferrimagnetism, and easily magnetization is the most easily demagnetized.The huge number of soft magnetic materials, can be divided into metal soft magnetic material, soft magnetic ferrite and powder core.Soft magnetic ferrites have high resistivity, therefore with the obvious advantage in medium-high frequency section, but owing to being ferrimagnetism material, therefore saturation magnetization is relatively low, it is impossible to meet the power requirement that electronic equipment increases day by day, therefore cannot apply in numerous high-grade, precision and advanced fields.Soft magnetic metal advantage is that saturation magnetization is high, but has the prominent shortcoming that resistivity is low, and when causing using in high frequency, eddy-current loss is very big, and pcrmeability drastically declines, and therefore cannot use under high frequency, and this is fatal shortcoming for soft magnetic materials.
Powder core is a kind of soft magnetic materials being mixed compacting by ferromagnetism powder with dielectric.Owing to ferromagnetic particle is the least, being separated by non magnetic electrical insulating film material again, therefore, on the one hand can completely cut off eddy current, material is applicable to upper frequency；On the other hand due to the channel effect between granule, material is caused to have low permeability and permanent permeance；Little due to particle size again, the most do not occur to collect skin phenomenon, pcrmeability is also the most relatively stable with the change of frequency.It is mainly used in high-frequency inductor.The magnetic electricity performance of powder core depends primarily on the permeability of powder material, the size and shape of powder, their activity coefficient, the content of dielectric, briquetting pressure and Technology for Heating Processing etc..Metal soft magnetic powder core, had both remained some good characteristics of soft magnetic metal and ferrite soft magnetic, overcame some defects of the two the most to greatest extent simultaneously, was the best a kind of soft magnetic materials of combination property.
Powder core is commonly used preparation process and is included: powder passivation, insulating wrapped, compacting, heat treatment etc..Insulating wrapped is a most important link in soft-magnetic powder core preparation process, and the quality of clad directly influences the quality of soft-magnetic powder core magnetic property.Conventional cladding medium has: the high resistivity medium such as Kaolin, silicon oxide.This kind of medium can effectively improve system insulating properties, reduces the eddy-current loss under high frequency.But this type of medium is all non magnetic, while improving material high-frequency work characteristic, reduce the magnetic property of matrix, including pcrmeability and the intensity of magnetization.
In the preparation process for magnetic powder core that a series of patents such as Chinese patent 97102244.5,200480021670.6,200680001781.2 use, insulating barrier is namagnetic substance, and their addition result in the reduction of powder core pcrmeability.
Chinese patent 200610124964.2,201310096126.9 is all that the mode using iron-based magnetic powder directly to mix with ferrite powder obtains powder core.Manganese-zinc ferrite in patent 200610124964.2 does not introduce preparation method, and a size of 200 mesh, suitable with the granular size of iron-based magnetic powder, it is impossible to be effectively coated with magnetic powder.Patent 201310096126.9 is then to use sol-gal process to obtain ferrite particle.The present invention is with they district's otherwises: the present invention uses hydro-thermal method directly at soft-magnetic alloy powder superficial growth ferrite particle, it is thus achieved that ferrite particle dimensional uniformity good, covered effect is good.
Chinese patent 201010297482.3 uses and controls oxidizing process at ferrous powder granules surface in situ generation Fe3O4Shell, is then mixed with soft-magnetic powder core with appropriate silicones, can weaken the non-magnetic media infringement to matrix magnetic property to a certain extent.This invention is the method by chemical reaction, in-situ preparation magnetic dielectric, and the parameter of chemical reaction should strictly control.Present invention phase region otherwise therewith is: the present invention is at soft-magnetic alloy powder superficial growth ferrite particle by hydro-thermal reaction, it is thus achieved that ferrite particle have excellent magnetic characteristics.
Summary of the invention
For the problem that presently, there are, the present invention uses hydro-thermal method to prepare the Nano-Ferrite Particle of particle size uniformity, repressed, Technology for Heating Processing at soft-magnetic alloy powder surface in situ, prepares novel ferrite composite magnetic powder core.
Technical scheme is as follows: (a) is passivated: take a certain amount of phosphoric acid, heating in water bath to 85 DEG C.Being slowly added to the magnetically soft alloy that need to be passivated, stirring makes the two be sufficiently mixed reaction, is passivated 30min, and phosphoric acid consumption is 0.2 wt.% ~ 6 wt.%.B () pioneer liquid prepares: by Fe3+Salt, Zn2+Salt and Ni2+(or Mn2+) salt Ni in molar ratioxZn1-x Fe2O4(or Mn x Zn1-x Fe2O4,x=0.2 ~ 0.8), it is distributed in the ethylene glycol of 50ml, Fe3+Salt is fixed as 0.5mmol, and stirring is until being completely dissolved.Add 1.54gCH3COONH4With 0.8ml Polyethylene Glycol, stir 30 minutes.(c) powder in-stiu coating: the soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 2h 24h at 160 DEG C ~ 220 DEG C.Products therefrom by washing with alcohol for several times, at 80 DEG C be dried.Magnetically soft alloy consumption can determine according to ferritic theoretical growing amount, and making magnetically soft alloy in product is 70 ~ 99.9wt.%, and ferrite is 0.1 ~ 30wt.%.D () adds bonding agent: take the W-6C of 0.1 ~ 4wt.% of the mixed-powder quality that step (c) obtains, pouring stirring in 50ml acetone into makes it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 1.5-2h to mixture be evaporated, powder uniformly mixes.(e) molding: under 0.4 ~ 1.9GPa pressure, powder is pressed into fine and close annulus.F () heat treatment: carry out heat treatment of annealing in the protective atmosphere of nitrogen or argon, to eliminate the internal stress that compacting produces, heat treatment temperature is 480 ~ 700 DEG C.
The invention have the advantage that (1) is owing to using hydro-thermal method in-situ method to prepare MnZn, nickel-zinc ferrite, in that context it may be convenient to prepare the nano-particle that particle size size is uniform, controlled；(2) ferrite is as the insulating wrapped agent of soft-magnetic alloy powder, the shortcoming causing matrix magnetic property to reduce when overcoming tradition namagnetic substance as covering, it is possible to obtain higher pcrmeability and saturation magnetization.
Detailed description of the invention
Embodiment 1
Take 0.2g phosphoric acid, heating in water bath to 85 DEG C.Being slowly added to 100gFeSiAl magnetically soft alloy, stirring makes the two be sufficiently mixed reaction, is passivated 30min.By FeCl3、NiCl2Salt and ZnCl2Salt Ni in molar ratio x Zn1-x Fe2O4(x=0.8) it is distributed in the ethylene glycol of 50ml, FeCl3For 0.5mmol, stirring is until being completely dissolved.Add 1.54gCH3COONH4With 0.8ml Polyethylene Glycol, stir 30 minutes.
Soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 24h at 160 DEG C.Products therefrom by washing with alcohol for several times, at 80 DEG C be dried.
Take the W-6C of 0.1wt.%, pour in 50ml acetone stirring into and make it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 1.5h to mixture be evaporated, powder uniformly mixes.
Under 1.9GPa pressure, powder is pressed into fine and close annulus.Carrying out heat treatment of annealing in the protective atmosphere of nitrogen, to eliminate the internal stress that compacting produces, heat treatment temperature is 700 DEG C.
Embodiment 2
Take the phosphoric acid of 0.6g, heating in water bath to 85 DEG C.Being slowly added to 10gFeSi magnetically soft alloy, stirring makes the two be sufficiently mixed reaction, is passivated 30min.By Fe(NO3)3, Ni(NO3)2And Zn(NO3)2Ni in molar ratio x Zn1-x Fe2O4(x=0.5) it is distributed in the ethylene glycol of 50ml, Fe(NO3)3Salt is 0.5mmol, and stirring is until being completely dissolved.Add 1.54gCH3COONH4With 0.8ml Polyethylene Glycol, stir 30 minutes.
Soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 12h at 180 DEG C.Products therefrom by washing with alcohol for several times, at 80 DEG C be dried.
Take the W-6C of 4wt.%, pour in 50ml acetone stirring into and make it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 2h to mixture be evaporated, powder uniformly mixes.
Under 1.4GPa pressure, powder is pressed into fine and close annulus.Carrying out heat treatment of annealing in the protective atmosphere of argon, to eliminate the internal stress that compacting produces, heat treatment temperature is 640 DEG C.
Embodiment 3
Take the phosphoric acid of 0.09g, heating in water bath to 85 DEG C.Being slowly added to 2.8gFeNi magnetically soft alloy, stirring makes the two be sufficiently mixed reaction, is passivated 30min.By Fe2(SO4)3、Ni SO4And ZnSO4Ni in molar ratio x Zn1-x Fe2O4(x=0.6) it is distributed in the ethylene glycol of 500ml, Fe2(SO4)3For 5mmol, stirring is until being completely dissolved.Add 15.4gCH3COONH4With 8ml Polyethylene Glycol, stir 30 minutes.
Soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 8h at 200 DEG C.Products therefrom by washing with alcohol for several times, at 80 DEG C be dried.
Take the W-6C of 2wt.%, pour in 50ml acetone stirring into and make it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 2h to mixture be evaporated, powder uniformly mixes.
Under 0.4GPa pressure, powder is pressed into fine and close annulus.Carrying out heat treatment of annealing in the protective atmosphere of argon, to eliminate the internal stress that compacting produces, heat treatment temperature is 480 DEG C.
Embodiment 4
Take the phosphoric acid of 1.5g, heating in water bath to 85 DEG C.Being slowly added to 50gFeNiMo magnetically soft alloy, stirring makes the two be sufficiently mixed reaction, is passivated 30min.By FeCl3、MnCl2Salt and ZnCl2Salt Mn in molar ratio x Zn1-x Fe2O4(x=0.4) it is distributed in the ethylene glycol of 50ml, FeCl3For 0.5mmol, stirring is until being completely dissolved.Add 1.54gCH3COONH4With 0.8ml Polyethylene Glycol, stir 30 minutes.
Soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 2h at 220 DEG C.Products therefrom by washing with alcohol for several times, at 80 DEG C be dried.
Take the W-6C of 0.3wt.%, pour in 50ml acetone stirring into and make it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 1.5h to mixture be evaporated, powder uniformly mixes.
Under 0.8GPa pressure, powder is pressed into fine and close annulus.Carrying out heat treatment of annealing in the protective atmosphere of nitrogen, to eliminate the internal stress that compacting produces, heat treatment temperature is 520 DEG C.
Embodiment 5
Take the phosphoric acid of 0.8g, heating in water bath to 85 DEG C.Being slowly added to 100gFeSiAl magnetically soft alloy, stirring makes the two be sufficiently mixed reaction, is passivated 30min.By Fe(NO3)3, Mn(NO3)2And Zn(NO3)2Mn in molar ratio x Zn1-x Fe2O4(x=0.2) it is distributed in the ethylene glycol of 50ml, Fe(NO3)3Salt is 0.5mmol, and stirring is until being completely dissolved.Add 1.54gCH3COONH4With 0.8ml Polyethylene Glycol, stir 30 minutes.
Soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 10h at 200 DEG C.Products therefrom by washing with alcohol for several times, at 80 DEG C be dried.
Take the W-6C of 0.5%, pour in 50ml acetone stirring into and make it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 1.5h to mixture be evaporated, powder uniformly mixes.
Under 1.3GPa pressure, powder is pressed into fine and close annulus.Carrying out heat treatment of annealing in the protective atmosphere of nitrogen, to eliminate the internal stress that compacting produces, heat treatment temperature is 600 DEG C.
Embodiment 6
Take the phosphoric acid of 0.6g, heating in water bath to 85 DEG C.Being slowly added to 20gFeCuNbSiB non-crystaline amorphous metal, stirring makes the two be sufficiently mixed reaction, is passivated 30min.By Fe2(SO4)3、Ni SO4And ZnSO4Ni in molar ratio x Zn1-x Fe2O4(x=0.3) it is distributed in the ethylene glycol of 50ml, Fe2(SO4)3For 0.5mmol, stirring is until being completely dissolved.Add 1.54gCH3COONH4With 0.8ml Polyethylene Glycol, stir 30 minutes.
Soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 12h at 180 DEG C.Products therefrom by washing with alcohol for several times, at 80 DEG C be dried.
Take the W-6C of 1.6wt.%, pour in 50ml acetone stirring into and make it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 1.5h to mixture be evaporated, powder uniformly mixes.
Under 1.6GPa pressure, powder is pressed into fine and close annulus.Carrying out heat treatment of annealing in the protective atmosphere of nitrogen, to eliminate the internal stress that compacting produces, heat treatment temperature is 680 DEG C.
Claims (1)
1. the preparation method of a composite magnetic powder core, it is characterised in that the method includes the steps of:
A () is passivated: take a certain amount of phosphoric acid, heating in water bath to 85 DEG C；Being slowly added to the magnetically soft alloy that need to be passivated, stirring makes the two be sufficiently mixed reaction, is passivated 30min, and phosphoric acid consumption is 0.2 wt.% ~ 6 wt.%；
B () pioneer liquid prepares: by Fe3+Salt, Zn2+Salt and Mn2+Salt Mn in molar ratio x Zn1-x Fe2O4(x=0.2 ~ 0.8), it is distributed in the ethylene glycol of 50ml, Fe3+Salt is 0.5mmol, and stirring is until being completely dissolved；Add 1.54gCH3COONH4With 0.8ml Polyethylene Glycol, stir 30 minutes；
(c) powder in-stiu coating: the soft-magnetic alloy powder after pioneer's liquid and passivation is transferred in the stainless steel autoclave of band agitating function, agitating heating 2h24h at 160 DEG C ~ 220 DEG C；Products therefrom by washing with alcohol for several times, at 80 DEG C be dried；Magnetically soft alloy consumption can determine according to ferritic theoretical growing amount, and making magnetically soft alloy in product is 70 ~ 99.9wt.%, and ferrite is 0.1 ~ 30wt.%；
D () adds bonding agent: take the W-6C of 0.1 ~ 4wt.% of the mixed-powder quality that step (c) obtains, pouring stirring in 50ml acetone into makes it dissolve, be poured in above-mentioned mixed-powder under 75 DEG C of water bath condition, be sufficiently stirred for 1.5-2h to mixture be evaporated, powder uniformly mixes；
(d) molding: under 0.4 ~ 1.9GPa pressure, powder is pressed into fine and close annulus；
E () heat treatment: carry out heat treatment of annealing in the protective atmosphere of nitrogen or argon, to eliminate the internal stress that compacting produces, heat treatment temperature is 480 ~ 700 DEG C.
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| CN108987062A (en) * | 2018-07-05 | 2018-12-11 | 浙江大学 | A kind of ferrite-magnetically soft alloy composite cores and preparation method thereof |
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| CN110835269A (en) * | 2019-10-30 | 2020-02-25 | 安徽朗基新材料科技有限公司 | Production process of high-strength high-performance soft magnetic ferrite material |
| CN111696745A (en) * | 2020-07-15 | 2020-09-22 | 中钢集团南京新材料研究院有限公司 | Composite Fe-Si-Al soft magnetic powder core and preparation method thereof |
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