CN104036905A - Soft magnetic composite material and preparation method thereof - Google Patents
Soft magnetic composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a soft magnetic composite material and a preparation method thereof. An alloy component of the soft magnetic composite material is iron-based amorphous alloy. Represented by the atomic ratio, the components of the alloy satisfy the formula of Fe100-a-b-cTaMbDc, wherein 15<=a<=30, 0<b<=5, and 0<c<=3; T is one or more of Si, B and C, M is one or more of Mo, Zr, Y, Ni, Ti and Cr, and D is one or more of rare earth elements. The preparation method comprises the steps of alloy smelting, atomization pulverization, passivating treatment, compression moulding, heat treatment and solidification. According to the preparation method, spherical powder is obtained through an atomization method, the power is passivated through a phosphoric acid diluent, and a uniform insulating coating layer can be formed; resistivity is improved effectively, loss is reduced effectively, the quantity of added nonmagnetic substance is small in a preparation process, and the soft magnetic composite material is high in magnetic conductivity and excellent in direct-current bias characteristic.
Description
Technical field
The present invention relates to a kind of amorphous soft magnet composite material and preparation method thereof, belong to soft magnetic material technical field.
Background technology
Soft magnetic material, as a kind of magnetic functional material, has the magnetic characteristics such as high saturation and magnetic intensity, high magnetic permeability, low-coercivity, is widely used in power electronics industry.Since being developed application from late nineteenth century, soft magnetic material has had the developing history of more than 100 year.The soft magnetic material of initial application only has electrical pure iron and carbon steel, has in succession developed subsequently the soft magnetic materials such as silicon steel, iron-nickel alloy, ferroaluminium, soft magnetic ferrites, amorphous nano-crystalline, soft-magnetic composite material.At present, soft magnetic material is mainly divided three classes, metal soft magnetic material, soft magnetic ferrites, soft-magnetic composite material.The saturation magnetization of metal soft magnetic material is high, magnetic permeability is large, but resistivity is low, in the time of frequency applications loss higher, so be only applicable to low frequency occasion.Soft magnetic ferrites resistivity is high, high-frequency loss is low, be mainly used in high frequency or hyperfrequency occasion, but ferrite is ferrimagnetism material, and saturation magnetization is relatively low, and when application, volume is larger.Soft-magnetic composite material refers to that the magnetic being coated by dielectric suppresses the soft magnetic material forming, and because dielectric has intercepted the contact between magnetic, soft-magnetic composite material has the resistivity higher than conventional metals soft magnetic material, can be applied to high frequency occasion.Soft-magnetic composite material has again the saturation magnetization higher than ferrite, can miniaturization in the time of application.In addition, soft-magnetic composite material is that magnetic compacting forms, and can be processed into various shape, as annular, U-shaped, E type etc., can meet different application scenarios.
The wider soft-magnetic composite material of application at present, divide according to the kind of magnetic, mainly contain following a few class: the soft-magnetic composite materials such as iron, iron sial, iron nickel molybdenum, iron nickel, soft-magnetic composite material loss prepared by straight iron powder is higher, iron-silicon-aluminum soft magnet composite material direct current biasing poor-performing, and iron nickel or iron nickel molybdenum powder are expensive, corresponding soft-magnetic composite material cost is too high.Therefore, exploitation have simultaneously excellent magnetic can and cheaply soft-magnetic composite material become the study hotspot in soft magnetism field.
Amorphous alloy refers to that the atomic arrangement obtaining by rapid cooling mode presents that long-range is unordered, the alloy of shortrange order, and amorphous alloy does not have other crystal defects such as crystal boundary, has the character that is better than conventional metals alloy.Fe-based amorphous soft magnetic material has the advantages such as high saturation and magnetic intensity, low-coercivity, high magnetic permeability and high resistivity, and with low cost.The amorphous soft magnet composite material of being prepared by amorphous soft magnetic material also has excellent magnetic property and low cost, becomes research direction popular in soft-magnetic composite material.
In current research, mainly adopt the mode of broken amorphous band powder process to prepare amorphous soft magnet composite material, preparation technology is comparatively complicated, and has added a large amount of namagnetic substances, causes prepared soft-magnetic composite material magnetic permeability lower.In addition, comparatively out-of-flatness of the powder surface that band crush method makes, is difficult to form uniform insulating coating, cause eddy current loss higher, and magnetic is brought internal stress in shattering process, due to the restriction of amorphous soft magnet composite material annealing temperature, be difficult to remove completely internal stress.So the broken amorphous soft magnet composite material comprehensive magnetic of sending out preparation of traditional band can be poor, magnetic permeability is low, loss is high.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of soft-magnetic composite material and preparation method thereof is provided, improve the combination property of amorphous soft magnet composite material, reduce the wastage, improve magnetic permeability and direct current biasing characteristic.
The present invention realizes the technical scheme that above-mentioned technical purpose adopts:
The alloying component that forms this soft-magnetic composite material is Fe-based amorphous alloy, and the composition of Fe-based amorphous alloy represents to meet following formula: Fe with atomic ratio
100-a-b-ct
am
bd
c, wherein, 15≤a≤30,0<b≤5,0<c≤3, T is selected from one or more in Si, B or C, M is selected from one or more in Mo, Zr, Y, Ni, Ti or Cr, and D is selected from one or more in rare earth element.
The preparation method of described soft-magnetic composite material comprises following steps:
1) alloy melting: Fe-based amorphous alloy carries out melting in vacuum melting furnace;
2) powder by atomization: melted Fe-based amorphous alloy is carried out to inert gas spraying and make amorphous soft magnet powder, screening obtains and is less than 100 object amorphous soft magnet powder;
3) grain size proportion: obtained amorphous soft magnet powder is carried out mixing after-400 orders ,-300 orders ,-200 orders ,-100 order classifications processing, the mass percentage content of mixed-powder is :-100 ~+200 orders account for 20 ~ 40%,-200 ~+300 orders account for 25 ~ 50%,-300 ~+400 orders account for 10 ~ 30%, and all the other are-400 orders;
4) Passivation Treatment: amorphous soft magnet powder good grain size proportion is mixed with phosphoric acid dilution, and the consumption of sour dilution is 10 ~ 50% of amorphous soft magnet powder weight, carries out the Passivation Treatment of 0.5 ~ 2h at 50 ~ 150 DEG C;
5) compressing: in the powder after Passivation Treatment, to add binding agent, lubricant, under the pressure of 1500 ~ 2200MPa, be pressed into amorphous soft magnet composite material;
6) heat treatment: compressing amorphous soft magnet composite material is carried out to annealing in process 0.5 ~ 2h at 300 ~ 450 DEG C, and annealing atmosphere is vacuum or non-oxidizing atmosphere;
7) solidify: the binding agent dilution of the amorphous soft magnet composite material after annealing being put into 80 ~ 100 DEG C solidifies 0.5 ~ 2h, obtains amorphous soft magnet composite material.
More excellent, described inert gas is nitrogen or argon gas.The solvent of described phosphoric acid dilution is selected from one or more in water, alcohol or acetone, and the consumption of phosphoric acid is 0.2 ~ 1% of amorphous soft magnet powder weight.Described binding agent is one or more in epoxy resin, silicone resin, silicon dioxide, glass dust, aluminium oxide, boron oxide or waterglass, and the consumption of binding agent is 1 ~ 5% of amorphous soft magnet powder quality.Described lubricant is one or more in zinc stearate and barium stearate, and the consumption of lubricant is powder quality 0.1 ~ 1%.Described binding agent dilution is acetone or alcohol.Described amorphous soft magnet composite material is E type, U-shaped or ring-like.
The present invention has following beneficial effect: obtained spherical magnetic by atomization, be conducive to form uniform insulating coating; Passivation technology used can carry out effective insulating wrapped to magnetic, improves resistivity, reduces eddy current loss; Preparation process does not insert other insulating compound, can effectively improve magnetic permeability.Compared with prior art, the present invention adopts the amorphous soft magnet composite material magnetic permeability prepared of method is high, loss is low, has excellent direct current biasing characteristic.
Embodiment
The alloying component that forms this soft-magnetic composite material is Fe-based amorphous alloy, and the composition of Fe-based amorphous alloy represents to meet following formula: Fe with atomic ratio
100-a-b-ct
am
bd
c, wherein, 15≤a≤30,0<b≤5,0<c≤3, T is selected from one or more in Si, B or C, M is selected from one or more in Mo, Zr, Y, Ni, Ti or Cr, and D is selected from one or more in rare earth element.
More excellent, described inert gas is nitrogen or argon gas.The solvent of described phosphoric acid dilution is selected from one or more in water, alcohol or acetone, and the consumption of phosphoric acid is 0.2 ~ 1% of amorphous soft magnet powder weight.Described binding agent is one or more in epoxy resin, silicone resin, silicon dioxide, glass dust, aluminium oxide, boron oxide or waterglass, and the consumption of binding agent is 1 ~ 5% of amorphous soft magnet powder quality.Described lubricant is one or more in zinc stearate and barium stearate, and the consumption of lubricant is powder quality 0.1 ~ 1%.Described binding agent dilution is acetone or alcohol.Described amorphous soft magnet composite material is E type, U-shaped or ring-like.
Further describe technical scheme of the present invention below in conjunction with embodiment.
Embodiment 1:
In the present embodiment, the alloy molecular formula that forms soft-magnetic composite material is Fe
76si
9b
12cr
2dy
1, be below concrete preparation process:
(1) alloy melting: magnetically soft alloy carries out melting in vacuum melting furnace;
(2) powder by atomization: melted alloy is directly carried out to nitrogen spray and make amorphous soft magnet powder, screening obtains and is less than 100 object powder;
(3) grain size proportion: obtained amorphous powder is carried out mixing after-400 orders ,-300 orders ,-200 orders ,-100 order classifications processing, the mass percentage content of mixed-powder is :-100 ~+200 orders account for 30%,-200 ~+300 orders account for 50%, and-300 ~+400 orders account for 15%, and-400 orders account for 5%;
(4) Passivation Treatment: amorphous powder good grain size proportion is mixed with phosphoric acid alcohol dilution, and the consumption of phosphoric acid alcohol dilution is 10% of magnetic weight, and the consumption of phosphoric acid is 0.4% of magnetic weight, carries out the Passivation Treatment of 1h at 80 DEG C;
(5) compressing: the epoxy resin that adds acetone diluted in the powder after Passivation Treatment, the addition of epoxy resin is 2% of magnetic weight, add again the zinc stearate of magnetic weight 0.25%, under the pressure of 1700MPa, be pressed into annular soft-magnetic composite material;
(6) heat treatment: compressing amorphous soft magnet composite material is carried out to annealing in process 1h at 400 DEG C, and annealing atmosphere is argon gas atmosphere;
(7) solidify: the epoxy resin acetone diluted liquid of the amorphous soft magnet composite material after annealing being put into 80 DEG C solidifies 2h, obtains amorphous soft magnet composite material.
After tested, the electromagnetic parameter of gained soft-magnetic composite material is as shown in the table.
Embodiment 2:
In the present embodiment, the alloy molecular formula that forms soft-magnetic composite material is Fe
69.7si
18b
12y
0.2dy
0.1, be below concrete preparation process:
(1) alloy melting: magnetically soft alloy carries out melting in vacuum melting furnace;
(2) powder by atomization: melted alloy is directly carried out to nitrogen spray and make amorphous soft magnet powder, screening obtains and is less than 100 object powder;
(3) grain size proportion: obtained amorphous powder is carried out mixing after-400 orders ,-300 orders ,-200 orders ,-100 order classifications processing, the mass percentage content of mixed-powder is :-100 ~+200 orders account for 20%,-200 ~+300 orders account for 30%, and-300 ~+400 orders account for 30%, and-400 orders account for 20%;
(4) Passivation Treatment: amorphous powder good grain size proportion is mixed with phosphate aqueous solution, and the consumption of phosphate aqueous solution is 30% of magnetic weight, and the consumption of phosphoric acid is 0.2% of magnetic weight, carries out the Passivation Treatment of 0.5h at 150 DEG C;
(5) compressing: in the powder after Passivation Treatment, add waterglass, the addition of waterglass is 1% of magnetic weight, then add the zinc stearate of magnetic weight 0.1%, under the pressure of 2200MPa, be pressed into annular soft-magnetic composite material;
(6) heat treatment: compressing amorphous soft magnet composite material is carried out to annealing in process 2h at 300 DEG C, and annealing atmosphere is argon gas atmosphere;
(7) solidify: the epoxy resin acetone diluted liquid of the amorphous soft magnet composite material after annealing being put into 90 DEG C solidifies 1h, obtains amorphous soft magnet composite material.
After tested, the electromagnetic parameter of gained soft-magnetic composite material is as shown in the table.
Embodiment 3:
In the present embodiment, the alloy molecular formula that forms soft-magnetic composite material is Fe
77si
9b
6cr
5ho
3, be below concrete preparation process:
(1) alloy melting: magnetically soft alloy carries out melting in vacuum melting furnace;
(2) powder by atomization: melted alloy is directly carried out to nitrogen spray and make amorphous soft magnet powder, screening obtains and is less than 100 object powder;
(3) grain size proportion: obtained amorphous powder is carried out mixing after-400 orders ,-300 orders ,-200 orders ,-100 order classifications processing, the mass percentage content of mixed-powder is :-100 ~+200 orders account for 40%,-200 ~+300 orders account for 25%, and-300 ~+400 orders account for 10%, and-400 orders account for 25%;
(4) Passivation Treatment: amorphous powder good grain size proportion is mixed with phosphoric acid acetone diluted liquid, and the consumption of phosphoric acid acetone diluted liquid is 50% of magnetic weight, and the consumption of phosphoric acid is 1% of magnetic weight, carries out the Passivation Treatment of 2h at 50 DEG C;
(5) compressing: in the powder after Passivation Treatment, to add silicone resin and silicon dioxide with alcohol dilution, the addition of silicone resin and silicon dioxide is respectively 2.5% of magnetic weight, add again the barium stearate of magnetic weight 1%, under the pressure of 1500MPa, be pressed into annular soft-magnetic composite material;
(6) heat treatment: compressing amorphous soft magnet composite material is carried out to annealing in process 0.5h at 450 DEG C, and annealing atmosphere is argon gas atmosphere;
(7) solidify: the epoxy resin acetone diluted liquid of the amorphous soft magnet composite material after annealing being put into 100 DEG C solidifies 0.5h, obtains amorphous soft magnet composite material.
After tested, the electromagnetic parameter of gained soft-magnetic composite material is as shown in the table.
Claims (8)
1. a soft-magnetic composite material, is characterized in that: the alloying component that forms this soft-magnetic composite material is Fe-based amorphous alloy, and the composition of Fe-based amorphous alloy represents to meet following formula: Fe with atomic ratio
100-a-b-ct
am
bd
c, wherein, 15≤a≤30,0<b≤5,0<c≤3, T is selected from one or more in Si, B or C, M is selected from one or more in Mo, Zr, Y, Ni, Ti or Cr, and D is selected from one or more in rare earth element.
2. a preparation method for soft-magnetic composite material as claimed in claim 1, is characterized in that comprising following steps:
1) alloy melting: Fe-based amorphous alloy carries out melting in vacuum melting furnace;
2) powder by atomization: melted Fe-based amorphous alloy is carried out to inert gas spraying and make amorphous soft magnet powder, screening obtains and is less than 100 object amorphous soft magnet powder;
3) grain size proportion: obtained amorphous soft magnet powder is carried out mixing after-400 orders ,-300 orders ,-200 orders ,-100 order classifications processing, the mass percentage content of mixed-powder is :-100 ~+200 orders account for 20 ~ 40%,-200 ~+300 orders account for 25 ~ 50%,-300 ~+400 orders account for 10 ~ 30%, and all the other are-400 orders;
4) Passivation Treatment: amorphous soft magnet powder good grain size proportion is mixed with phosphoric acid dilution, and the consumption of phosphoric acid dilution is 10 ~ 50% of amorphous soft magnet powder weight, carries out the Passivation Treatment of 0.5 ~ 2h at 50 ~ 150 DEG C;
5) compressing: in the amorphous soft magnet powder after Passivation Treatment, to add binding agent, lubricant, under the pressure of 1500 ~ 2200MPa, be pressed into amorphous soft magnet composite material;
6) heat treatment: compressing amorphous soft magnet composite material is carried out to annealing in process 0.5 ~ 2h at 300 ~ 450 DEG C, and annealing atmosphere is vacuum or non-oxidizing atmosphere;
7) solidify: the binding agent dilution of the amorphous soft magnet composite material after annealing being put into 80 ~ 100 DEG C solidifies 0.5 ~ 2h, obtains amorphous soft magnet composite material.
3. the preparation method of soft-magnetic composite material according to claim 2, is characterized in that: described inert gas is nitrogen or argon gas.
4. the preparation method of soft-magnetic composite material according to claim 2, is characterized in that: the solvent of described phosphoric acid dilution is selected from one or more in water, alcohol or acetone, and the consumption of phosphoric acid is 0.2 ~ 1% of amorphous soft magnet powder weight.
5. the preparation method of soft-magnetic composite material according to claim 2, it is characterized in that: described binding agent is one or more in epoxy resin, silicone resin, silicon dioxide, glass dust, aluminium oxide, boron oxide or waterglass, the consumption of binding agent is 1 ~ 5% of amorphous soft magnet powder quality.
6. the preparation method of soft-magnetic composite material according to claim 2, is characterized in that: described lubricant is one or more in zinc stearate and barium stearate, and the consumption of lubricant is powder quality 0.1 ~ 1%.
7. the preparation method of soft-magnetic composite material according to claim 2, is characterized in that: described binding agent dilution is acetone or alcohol.
8. the preparation method of soft-magnetic composite material according to claim 2, is characterized in that: described amorphous soft magnet composite material is E type, U-shaped or ring-like.
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Application publication date: 20140910 |