CN104036901A - High-permeability low-loss metal soft-magnetism composite material and preparing method thereof - Google Patents
High-permeability low-loss metal soft-magnetism composite material and preparing method thereof Download PDFInfo
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- CN104036901A CN104036901A CN201410229878.2A CN201410229878A CN104036901A CN 104036901 A CN104036901 A CN 104036901A CN 201410229878 A CN201410229878 A CN 201410229878A CN 104036901 A CN104036901 A CN 104036901A
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- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 239000002184 metal Substances 0.000 title claims abstract 5
- 229910052751 metal Inorganic materials 0.000 title claims abstract 5
- 238000000034 method Methods 0.000 title abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 5
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 5
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 5
- 238000005275 alloying Methods 0.000 claims abstract 2
- 229910045601 alloy Inorganic materials 0.000 claims description 64
- 239000000956 alloy Substances 0.000 claims description 64
- 239000000843 powder Substances 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims 1
- 229910000640 Fe alloy Inorganic materials 0.000 claims 1
- 238000003723 Smelting Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 claims 1
- 230000001681 protective effect Effects 0.000 claims 1
- 229920002050 silicone resin Polymers 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 20
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 229920001296 polysiloxane Polymers 0.000 description 8
- 238000002161 passivation Methods 0.000 description 7
- 229920005591 polysilicon Polymers 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000002905 metal composite material Substances 0.000 description 6
- 229910017082 Fe-Si Inorganic materials 0.000 description 4
- 229910017133 Fe—Si Inorganic materials 0.000 description 4
- 239000000696 magnetic material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a high-permeability low-loss metal soft-magnetism composite material and a preparing method thereof. The composite material is expressed through the atomic ratio satisfying the formula that Fe100-x-y-zSixPyMz, M is one or more of Cr, V, Al and Mn, and the subscripts x, y and z express the atomic percent of corresponding alloying elements and meet the conditions that x is greater than or equal to 2 and less than or equal to 15, y is greater than or equal to 0 and less than or equal to 5, and z is greater than or equal to 0 and less than or equal to 5. The obtained metal soft-magnetism composite material has the advantages of being high in permeability, low in loss, simple in process and low in cost and facilitating forming.
Description
Technical field
The present invention relates to field of magnetic material, relate in particular to a kind of high magnetic conductivity and low loss soft magnetic metal composite material and preparation method thereof.
Background technology
Fe-Si magnetically soft alloy has good soft magnet performance, and when the content of silicon is during at 6.5wt%, its saturation magnetostriction constant goes to zero, and is conducive to improve magnetic permeability and reduces coercive force, and the interpolation of silicon simultaneously also can improve resistance alloys rate, reduces the wastage.Therefore it become current purposes the most extensively, the maximum soft magnetic material of consumption.Along with developing rapidly of electronic technology, the high frequency of electronic device, high power density, miniaturization and high jamproof requirement are increased day by day.But it is on the low side that traditional Fe-Si is associated golden resistivity, limited its use under high frequency, so we need to be pressed into soft-magnetic composite material by Fe-Si powder insulating wrapped, it can be used under high frequency.
To Fe-Si, be at present that the research of powder core is mainly in the optimization of the improvement with composition and technological parameter.The composition of magnetic is determining the intrinsic performance of obtained composite material, so the improvement of composition is the emphasis of research.
Chinese patent 200710051454.1 discloses a kind of manufacture method that adds the powder core of 0.3 ~ 0.5wt%Ti in Fe-6.5%Si alloy, by Optimization Technology, made the powder core of higher magnetic permcability, but by changing Ti content, magnetic permeability does not have significant change.
Chinese patent 201010209010.8 discloses a kind of manufacture method that adds the powder core of a small amount of P in Fe-6.5%Si alloy, and by changing the content of P and technological parameter, to have made magnetic permeability be 60,75,90 powder core.But this patent does not systematically contrast the impact of P content on soft magnet performance.
L. (the Preparation of soft magnetic alloys Fe such as Anestiev
100-x-ysi
xp
y(0 ﹤ x ﹤ 9,0 ﹤ y ﹤ 0.6wt%), using solid phase diffusion-sintering method, Journal of Magnetism and Magnetic Materials 281 (2004) 124 – 134) with powder metallurgy, prepared Fe
100-x-ysi
xp
yblock alloy, has studied the impact of the variation alloy soft magnet performance of Si and P content, finds that Si content is at 4wt%, and P content is when 0.6wt%, and magnetic permeability is the highest, has compared with low-loss simultaneously.But this research is the alloy obtaining with powder metallurgy sintered, consuming time longer, and easily produce hole, the density of alloy is lower, can reduce magnetic permeability.The method of diffusion
S. Jafari etc. (Microstructural and magnetic properties study of Fe – P rolled sheet alloys, Journal of Magnetism and Magnetic Materials 358-359 (2014) 38 – 43) has studied the Fe of sheet
1-xp
x(x=0.36,0.7,1,1at%), find the increase along with P, maximum permeability is increased to 6200 from 4600, and resistivity is increased to 25 μ Ω cm from 15 μ Ω cm.But in the composition of this research, do not add Si, can make the magnetic permeability of alloy and resistivity on the low side.
Summary of the invention
The object of the invention is to overcome the deficiency of existing composition system, soft magnetic metal composite material of a kind of high magnetic conductivity and low loss and preparation method thereof is provided.
The composition of soft magnetic metal composite material represents to meet following formula: Fe with atomic ratio
100-x-y-zsi
xp
ym
zwherein M is selected from one or more in Cr, V, Al, Mn, and subscript x, y, z represents the atomic percent of respective alloy element, meets the following conditions: 2≤x≤15,0≤y≤5,0 < z≤5.
The preparation method of soft magnetic metal composite material is as follows:
(1) by described atomic ratio, Armco iron, polysilicon, ferrorphosphorus and alloy M are dropped in vaccum sensitive stove and smelted, obtain alloy cast ingot;
(2) alloy cast ingot Mechanical Crushing is become to alloy powder, in nitrogen or argon shield atmosphere, after 600 ℃ of high-temperature heat treatment, sieve, make the mass percentage content of alloy powder granularmetric composition be :+100 orders account for 5% ~ 10%,-100 ~+200 orders account for 40% ~ 50%,-200 ~+300 orders account for 30% ~ 40%, and-300 orders account for 10% ~ 20%;
(3) above-mentioned alloy powder is with after 0.2 ~ 1.0wt% phosphoric acid solution Passivation Treatment, fully mix with one or more in the epoxy resin of 1 ~ 3wt%, phenolic resins, silicones, glass powder with low melting point, waterglass, and be pressed into powder core under 1.3 ~ 1.9GPa pressure;
(4) by the powder core suppressing at N
2the lower heat treatment of protection, nitrogen flow is 200mL/min, and heating rate is 30 ℃/min, and heat treatment temperature is 600 ~ 720 ℃, and heat treatment time is 30 ~ 60min.
The present invention compared with prior art has following advantage: in alloy powder of the present invention, contain a large amount of iron, so saturation induction density is higher; Contain nonmetalloid Si simultaneously, can improve resistance alloys rate, magnetic permeability; Contain nonmetalloid P simultaneously, can form substitutional solid solution with Fe, increase the resistivity of alloy, reduce eddy current loss, P can reduce the hole of alloy in the process of melting, increases crystallite dimension, the texture that contributes to crystallization, this is highly beneficial for carrying heavy alloyed magnetic permeability; Contain M(simultaneously and be selected from least one in Cr, V, Al, Mn), increased the processing characteristics of alloy, and technique is simple, is beneficial to moulding, and there is certain cost advantage.
Embodiment
Soft magnetic metal composite material of the present invention consists of: Fe
100-x-y-zsi
xp
ym
z, wherein M is selected from least one in Cr, V, Al, Mn, and subscript x, y, z represents the atomic percent of respective alloy element, meets the following conditions: 2≤x≤15,0≤y≤5,0 < z≤5.
Specifically for silicone content 2% ~ 15%, phosphorus content, 0 ~ 5%, contains a small amount of alloy M simultaneously, its magnetic permeability can be higher, and loss is low, has good soft magnet performance.
Embodiment 1
(1) choose composition Fe
97-xsi
xp
1v
2x=3 wherein, 6,9,12,15, Armco iron, polysilicon, ferrorphosphorus and alloy M are dropped in vaccum sensitive stove and smelted, obtain alloy cast ingot;
(2) alloy cast ingot Mechanical Crushing is become to alloy powder, in nitrogen or argon shield atmosphere, after 600 ℃ of high-temperature heat treatment, sieve, make the mass percentage content of alloy powder granularmetric composition be :+100 orders account for 10% ,-100 ~+200 orders account for 40%,-200 ~+300 orders account for 40%, and-300 orders account for 10%;
(3) above-mentioned alloy powder, with after 0.2wt% phosphoric acid solution Passivation Treatment, fully mixes with 1% silicones, and be pressed into powder core under 1.3GPa pressure;
(4) by the powder core suppressing at N
2the lower heat treatment of protection, nitrogen flow is 200mL/min, and heating rate is 30 ℃/min, and heat treatment temperature is 600 ℃, and heat treatment time is 30min.The soft-magnetic composite material performance obtaining is as shown in the table.
When the content of Si is increased to 12at% from 3at% as can be seen from the table, effective permeability has risen to 105 from 84, and loss is from 430KW/m
3be reduced to 325KW/m
3, continuation increases the content of Si, can reduce the magnetic permeability of soft-magnetic composite material.
Embodiment 2
Concrete implementation step is identical with embodiment 1, and in an example of the present invention, composition is chosen Fe
86-ysi
12p
yal
2, y=0 wherein, 0.5,1,1.5,2,2.5,3,3.5,4.
As can be seen from the table when P content is increased to 1.5at% from 0, effective permeability has been increased to 115 from 82, and loss has simultaneously reached minimum 278KW/m
3, continuing increases P content, can reduce the magnetic permeability of soft-magnetic composite material.
Embodiment 3
(1) choose composition Fe
84.5si
12p
1.5al
2, Armco iron, polysilicon, ferrorphosphorus and alloy M are dropped in vaccum sensitive stove and smelted, obtain alloy cast ingot;
(2) alloy cast ingot Mechanical Crushing is become to alloy powder, in nitrogen or argon shield atmosphere, after 600 ℃ of high-temperature heat treatment, sieve, make the mass percentage content of alloy powder granularmetric composition be :+100 orders account for 5% ,-100 ~+200 orders account for 50%,-200 ~+300 orders account for 35%, and-300 orders account for 10%;
(3) above-mentioned alloy powder, with after 0.2wt% phosphoric acid solution Passivation Treatment, fully mixes with 1% silicones, and be pressed into powder core under 1.9GPa pressure;
(4) by the powder core suppressing at N
2the lower heat treatment of protection, nitrogen flow is 200mL/min, and heating rate is 30 ℃/min, and heat treatment temperature is 600 ℃, and heat treatment time is 30min.The soft-magnetic composite material effective permeability obtaining is 126, and loss is 264KW/m
3.
Embodiment 4
(1) choose composition Fe
84.5si
12p
1.5al
2, Armco iron, polysilicon, ferrorphosphorus and alloy M are dropped in vaccum sensitive stove and smelted, obtain alloy cast ingot;
(2) alloy cast ingot Mechanical Crushing is become to alloy powder, in nitrogen or argon shield atmosphere, after 600 ℃ of high-temperature heat treatment, sieve, make the mass percentage content of alloy powder granularmetric composition be :+100 orders account for 5% ,-100 ~+200 orders account for 50%,-200 ~+300 orders account for 30%, and-300 orders account for 15%;
(3) above-mentioned alloy powder, with after 0.6wt% phosphoric acid solution Passivation Treatment, fully mixes with 2% silicones, and be pressed into powder core under 1.9GPa pressure;
(4) by the powder core suppressing at N
2the lower heat treatment of protection, nitrogen flow is 200mL/min, and heating rate is 30 ℃/min, and heat treatment temperature is 600 ℃, and heat treatment time is 30min.The soft-magnetic composite material effective permeability obtaining is 118, and loss is 246KW/m
3.
Embodiment 5
(1) choose composition Fe
84.5si
12p
1.5al
2, Armco iron, polysilicon, ferrorphosphorus and alloy M are dropped in vaccum sensitive stove and smelted, obtain alloy cast ingot;
(2) alloy cast ingot Mechanical Crushing is become to alloy powder, in nitrogen or argon shield atmosphere, after 600 ℃ of high-temperature heat treatment, sieve, make the mass percentage content of alloy powder granularmetric composition be :+100 orders account for 5% ,-100 ~+200 orders account for 50%,-200 ~+300 orders account for 30%, and-300 orders account for 15%;
(3) above-mentioned alloy powder, with after 1.0wt% phosphoric acid solution Passivation Treatment, fully mixes with 3% silicones, and be pressed into powder core under 1.9GPa pressure;
(4) by the powder core suppressing at N
2the lower heat treatment of protection, nitrogen flow is 200mL/min, and heating rate is 30 ℃/min, and heat treatment temperature is 600 ℃, and heat treatment time is 30min.The soft-magnetic composite material effective permeability obtaining is 103, and loss is 258KW/m
3.
Embodiment 6
(1) choose composition Fe
84.5si
12p
1.5al
2, Armco iron, polysilicon, ferrorphosphorus and alloy M are dropped in vaccum sensitive stove and smelted, obtain alloy cast ingot;
(2) alloy cast ingot Mechanical Crushing is become to alloy powder, in nitrogen or argon shield atmosphere, after 600 ℃ of high-temperature heat treatment, sieve, make the mass percentage content of alloy powder granularmetric composition be :+100 orders account for 5% ,-100 ~+200 orders account for 50%,-200 ~+300 orders account for 30%, and-300 orders account for 15%;
(3) above-mentioned alloy powder, with after 0.6wt% phosphoric acid solution Passivation Treatment, fully mixes with 2% silicones, and be pressed into powder core under 1.9GPa pressure;
(4) by the powder core suppressing at N
2the lower heat treatment of protection, nitrogen flow is 200mL/min, and heating rate is 30 ℃/min, and heat treatment temperature is 690 ℃, and heat treatment time is 60min.The soft-magnetic composite material effective permeability obtaining is 134, and loss is 227KW/m
3.
Embodiment 7
(1) choose composition Fe
84.5si
12p
1.5al
2, Armco iron, polysilicon, ferrorphosphorus and alloy M are dropped in vaccum sensitive stove and smelted, obtain alloy cast ingot;
(2) alloy cast ingot Mechanical Crushing is become to alloy powder, in nitrogen or argon shield atmosphere, after 600 ℃ of high-temperature heat treatment, sieve, make the mass percentage content of alloy powder granularmetric composition be :+100 orders account for 5% ,-100 ~+200 orders account for 50%,-200 ~+300 orders account for 30%, and-300 orders account for 15%;
(3) above-mentioned alloy powder, with after 0.6wt% phosphoric acid solution Passivation Treatment, fully mixes with the silicones of 2wt%, and be pressed into powder core under 1.9GPa pressure;
(4) by the powder core suppressing at N
2the lower heat treatment of protection, nitrogen flow is 200mL/min, and heating rate is 30 ℃/min, and heat treatment temperature is 720 ℃, and heat treatment time is 60min.The soft-magnetic composite material effective permeability obtaining is 136, and loss is 245KW/m
3.
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Cited By (9)
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| CN104962821A (en) * | 2015-05-26 | 2015-10-07 | 北京科技大学 | Wire printer yoke iron seat material and yoke iron seat part processing method |
| CN106024258A (en) * | 2016-06-29 | 2016-10-12 | 无锡康柏斯机械科技有限公司 | Penholder-like iron core for automobile ignition coil |
| JP2017008376A (en) * | 2015-06-23 | 2017-01-12 | 大同特殊鋼株式会社 | Fe-based alloy composition, soft magnetic powder, composite magnetic body, and method for producing soft magnetic powder |
| CN107142414A (en) * | 2017-04-17 | 2017-09-08 | 上海兴罗特种密封件有限公司 | A kind of magnetic conductor powdered metallurgical material and its application |
| CN107578872A (en) * | 2017-08-10 | 2018-01-12 | 深圳市铂科新材料股份有限公司 | A kind of preparation method of the metal soft magnetic powder core of high temperature heat-resistant processing |
| CN108538533A (en) * | 2018-06-11 | 2018-09-14 | 彭晓领 | A kind of interface scattering preparation of soft-magnetic composite material |
| CN108538568A (en) * | 2018-06-11 | 2018-09-14 | 彭晓领 | A kind of thermal deformation interface scattering preparation of soft-magnetic composite material |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
| CN109979700A (en) * | 2017-12-27 | 2019-07-05 | Tdk株式会社 | Superimposed line ring electronic component |
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| CN107578872B (en) * | 2017-08-10 | 2019-10-22 | 深圳市铂科新材料股份有限公司 | A kind of preparation method of the metal soft magnetic powder core of high temperature heat-resistant processing |
| CN109979700A (en) * | 2017-12-27 | 2019-07-05 | Tdk株式会社 | Superimposed line ring electronic component |
| CN108538533A (en) * | 2018-06-11 | 2018-09-14 | 彭晓领 | A kind of interface scattering preparation of soft-magnetic composite material |
| CN108538568A (en) * | 2018-06-11 | 2018-09-14 | 彭晓领 | A kind of thermal deformation interface scattering preparation of soft-magnetic composite material |
| CN108538568B (en) * | 2018-06-11 | 2020-07-31 | 中国计量大学 | Thermal deformation interface diffusion preparation method of soft magnetic composite material |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
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