CN103310936A - Low-loss Fe-based nanocrystalline soft magnetic powder core and manufacturing method thereof - Google Patents

Low-loss Fe-based nanocrystalline soft magnetic powder core and manufacturing method thereof Download PDF

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CN103310936A
CN103310936A CN2013102807932A CN201310280793A CN103310936A CN 103310936 A CN103310936 A CN 103310936A CN 2013102807932 A CN2013102807932 A CN 2013102807932A CN 201310280793 A CN201310280793 A CN 201310280793A CN 103310936 A CN103310936 A CN 103310936A
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严密
熊亚东
张念伟
赵国梁
姜银珠
周连明
曹阳
林坤
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NANTONG WANBAO INDUSTRY Co Ltd
Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a low-loss Fe-based nanocrystalline soft magnetic powder core and a manufacturing method thereof. The ingredient of the alloy powder core forming the powder core is FeaSibBcCudMeYf, wherein M refers to C, P, Cr or Mn, the subscripts a, b, c, d, e, f represent corresponding atomic percent of alloying elements, and the following formulas are met: a is not less than 70 and not more than 90, b is not less than 2 and not more than 15, c is not less than 4 and not more than 13, d is not less than 0.4 and not more than 3, e is not less than 2 and not more than 8, f is less than 0 and not more than 5, and besides, the total percent of a, b, c, d, e and f equals to 100. The prepared magnetic powder core has smaller eddy-current loss, the preparation technology is simple, the formation is easy, the environmental protection is facilitated, and a certain cost advantage is guaranteed.

Description

A kind of low-loss Fe base nanometer crystal powder core and preparation method thereof
Technical field
The present invention relates to field of magnetic material, relate in particular to a kind of low-loss Fe base nanometer crystal powder core and preparation method thereof.
Background technology
Soft magnetic-powder core has a wide range of applications in electronic information, electrician and medium-high frequency field.Along with the development of electronics industry, more and more higher for the requirement of electronic product microminiaturization.In recent decades, in order to satisfy the development of electronics industry, the various countries researcher adopts distinct methods to prepare various soft magnetic-powder cores with different magnetic properties, and these powder cores are widely used in filter, frequency modulation choke and the Switching Power Supply.
Nineteen twenty-one, the Arnold of US Westinghouse company and G.W.Elmen etc. are pressed into electrolytic iron powder powder core first, they with this powder core mainly as the load inductance in the telephone line, after 2 years, they develop again the high magnetic permeability permalloy, and in nineteen twenty-seven it have been made powder core, because it has advantages of good, very fast by industrialization, be widely used to nineteen fifty generation.1932, the Japanese increased this amount and the grand sendust of having invented in Yamamoto, because invention ground is at celestial platform, so sendust is also referred to as Sendust.But, until at the beginning of the 1980's, industrialization is just successfully developed and realize gradually to the Sendust powder core.1940, the V.E.Legg of U.S.'s Bell Laboratory and F.J.Given developed iron nickel-molybdenum alloy powder core, and this powder core is comprised of 81% nickel, 17% iron and 2% molybdenum.Because containing molybdenum about 2%, so magnetic permeability and resistivity significantly improves, has the advantages such as good time stability, less temperature coefficient, low-loss, shown great attention to afterwards.In the time of the sixties in last century, guidance and the control section of the MK-46II torpedo of the U.S. have just used this magnetic core in a large number.
People make it have the characteristics such as high frequency, low-loss, high Q value in order to make electronic device to adapt to the operational environment of different frequency range, have done a large amount of work.At present, iron nickel-molybdenum alloy powder core has occupied main share on high-end market, but because iron nickel molybdenum powder core involves great expense, its application is restricted always.In recent years, Fe base nanometer crystal-amorphous soft magnet powder core is lower because of its cost, and preparation technology is simple, and excellent performance and receiving much concern is expected to replace the part purposes of iron nickel molybdenum powder core
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of low-loss Fe base nanometer crystal powder core and preparation method thereof is provided.
Consisting of of low-loss Fe base nanometer crystal powder core: Fe aSi bB cCu dM eY f, M is C, P, Cr or Mn in the formula, subscript a, b, c, d, e, f represent the atomic percent of respective alloy element, meet the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2≤e≤8,0＜f≤5; And a+b+c+d+e+f=100.
The preparation method's of low-loss Fe base nanometer crystal powder core step is as follows:
(1) with Fe aSi bB cCu dM eY fAmorphous thin ribbon in vacuum annealing furnace in 420 ℃ the insulation 1h after, it is carried out Mechanical Crushing, M is C, P, Cr or Mn in the formula, subscript a, b, c, d, e, f represent the atomic percent of respective alloy element, meet the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2≤e≤8,0＜f≤5; And a+b+c+d+e+f=100;
(2) Fe aSi bB cCu dM eY fAfter the amorphous thin ribbon Mechanical Crushing, place the planetary ball mill ball milling, ratio of grinding media to material is 5:1, and Ball-milling Time is 4h, and rotating speed is 260r/min, and adds the anti-oxidation of ethanol, the dry Fe that obtains the variable grain degree by screening aSi bB cCu dM eY fMagnetic;
(3) with the Fe of different meshes aSi bB cCu dM eY fMagnetic mixes, wherein-100 order～+ 200 purpose Fe aSi bB cCu dM eY fMagnetic accounts for 15% ,-200 orders of gross mass～+ 300 purpose Fe aSi bB cCu dM eY fMagnetic accounts for 70% ,-300 orders of gross mass～+ 400 purpose Fe aSi bB cCu dM eY fMagnetic accounts for 10% ,-400 purpose Fe of gross mass aSi bB cCu dM eY fMagnetic accounts for 5% of gross mass, through after the phosphate aqueous solution Passivation Treatment of 0.4wt%, fully mixes with the organic binder bond of 0.5wt%, and be pressed into powder core under 1.80GPa pressure;
(4) powder core that suppresses is placed 500 ℃ of insulations of vacuum annealing furnace 1h, obtain Fe base nanometer crystal powder core.
Described organic binder bond is epoxy resin or silicone resin.
Advantage of the present invention is: can obtain the low-loss Fe base nanometer crystal powder core of soft magnet performance excellence by this method, and technique is simple, is easy to moulding, is beneficial to environmental protection, and has certain cost advantage.
Embodiment
Consisting of of low-loss Fe base nanometer crystal powder core: Fe aSi bB cCu dM eY f, M is C, P, Cr or Mn in the formula, subscript a, b, c, d, e, f represent the atomic percent of respective alloy element, meet the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2≤e≤8,0＜f≤5; And a+b+c+d+e+f=100.
Embodiment 1
(1) with Fe 70Si 15B 4Cu 0.4M 8Y 2.6Amorphous thin ribbon behind 420 ℃ of insulation 1h, carries out Mechanical Crushing to it in vacuum annealing furnace;
(2) Fe 70Si 15B 4Cu 0.4M 8Y 2.6After the amorphous thin ribbon Mechanical Crushing, place the planetary ball mill ball milling, ratio of grinding media to material is 5:1, and Ball-milling Time is 4h, and rotating speed is 260r/min, and adds the anti-oxidation of ethanol, the dry Fe that obtains the variable grain degree by screening 70Si 15B 4Cu 0.4M 8Y 2.6Magnetic;
(3) with the Fe of different meshes 70Si 15B 4Cu 0.4M 8Y 2.6Magnetic mixes, wherein-100 order～+ 200 purpose Fe 70Si 15B 4Cu 0.4M 8Y 2.6Magnetic accounts for 15% ,-200 orders of gross mass～+ 300 purpose Fe 70Si 15B 4Cu 0.4M 8Y 2.6Magnetic accounts for 70% ,-300 orders of gross mass～+ 400 purpose Fe 70Si 15B 4Cu 0.4M 8Y 2.6Magnetic accounts for 10% ,-400 purpose Fe of gross mass 70Si 15B 4Cu 0.4M 8Y 2.6Magnetic accounts for 5% of gross mass, through after the phosphate aqueous solution Passivation Treatment of 0.4wt%, fully mixes with the epoxy adhesive of 0.5wt%, and be pressed into ring-like base sample under 1.80GPa pressure; The external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.
(4) powder core that suppresses is placed 500 ℃ of insulations of vacuum annealing furnace 1h, obtain Fe base nanometer crystal powder core.
After testing, associated electrical magnetic parameter such as the table 1 of target product:
Figure BDA00003468409600031
Embodiment 2
(1) with Fe 90Si 2B 4Cu 1P 2Y 1Amorphous thin ribbon behind 420 ℃ of insulation 1h, carries out Mechanical Crushing to it in vacuum annealing furnace;
(2) Fe 90Si 2B 4Cu 1P 2Y 1After the amorphous thin ribbon Mechanical Crushing, place the planetary ball mill ball milling, ratio of grinding media to material is 5:1, and Ball-milling Time is 4h, and rotating speed is 260r/min, and adds the anti-oxidation of ethanol, the dry Fe that obtains the variable grain degree by screening 90Si 2B 4Cu 1P 2Y 1Magnetic;
(3) with the Fe of different meshes 90Si 2B 4Cu 1P 2Y 1Magnetic mixes, wherein-100 order～+ 200 purpose Fe 90Si 2B 4Cu 1P 2Y 1Magnetic accounts for 15% ,-200 orders of gross mass～+ 300 purpose Fe 90Si 2B 4Cu 1P 2Y 1Magnetic accounts for 70% ,-300 orders of gross mass～+ 400 purpose Fe 90Si 2B 4Cu 1P 2Y 1Magnetic accounts for 10% ,-400 purpose Fe of gross mass 90Si 2B 4Cu 1P 2Y 1Magnetic accounts for 5% of gross mass, through after the phosphate aqueous solution Passivation Treatment of 0.4wt%, fully mixes with the silicone resin binding agent of 0.5wt%, and be pressed into powder core under 1.80GPa pressure;
(4) powder core that suppresses is placed 500 ℃ of insulations of vacuum annealing furnace 1h, obtain Fe base nanometer crystal powder core.
After testing, associated electrical magnetic parameter such as the table 2 of target product:
Figure BDA00003468409600041
Embodiment 3
(1) with Fe 60Si 11B 13Cu 3Cr 8Y 5Amorphous thin ribbon behind 420 ℃ of insulation 1h, carries out Mechanical Crushing to it in vacuum annealing furnace;
(2) Fe 60Si 11B 13Cu 3Cr 8Y 5After the amorphous thin ribbon Mechanical Crushing, place the planetary ball mill ball milling, ratio of grinding media to material is 5:1, and Ball-milling Time is 4h, and rotating speed is 260r/min, and adds the anti-oxidation of ethanol, the dry Fe that obtains the variable grain degree by screening 60Si 11B 13Cu 3Cr 8Y 5Magnetic;
(3) with the Fe of different meshes 60Si 11B 13Cu 3Cr 8Y 5Magnetic mixes, wherein-100 order～+ 200 purpose Fe 60Si 11B 13Cu 3Cr 8Y 5Magnetic accounts for 15% ,-200 orders of gross mass～+ 300 purpose Fe 60Si 11B 13Cu 3Cr 8Y 5Magnetic accounts for 70% ,-300 orders of gross mass～+ 400 purpose Fe 60Si 11B 13Cu 3Cr 8Y 5Magnetic accounts for 10% ,-400 purpose Fe of gross mass 60Si 11B 13Cu 3Cr 8Y 5Magnetic accounts for 5% of gross mass, through after the phosphate aqueous solution Passivation Treatment of 0.4wt%, fully mixes with the epoxy adhesive of 0.5wt%, and be pressed into powder core under 1.80GPa pressure;
(4) powder core that suppresses is placed 500 ℃ of insulations of vacuum annealing furnace 1h, obtain Fe base nanometer crystal powder core.
After testing, associated electrical magnetic parameter such as the table 3 of target product:
Figure BDA00003468409600042
Embodiment 4
(1) with Fe 74Si 6B 6Cu 3Mn 6Y 5Amorphous thin ribbon behind 420 ℃ of insulation 1h, carries out Mechanical Crushing to it in vacuum annealing furnace;
(2) Fe 74Si 6B 6Cu 3Mn 6Y 5After the amorphous thin ribbon Mechanical Crushing, place the planetary ball mill ball milling, ratio of grinding media to material is 5:1, and Ball-milling Time is 4h, and rotating speed is 260r/min, and adds the anti-oxidation of ethanol, the dry Fe that obtains the variable grain degree by screening 74Si 6B 6Cu 3Mn 6Y 5Magnetic;
(3) with the Fe of different meshes 74Si 6B 6Cu 3Mn 6Y 5Magnetic mixes, wherein-100 order～+ 200 purpose Fe 74Si 6B 6Cu 3Mn 6Y 5Magnetic accounts for 15% ,-200 orders of gross mass～+ 300 purpose Fe 74Si 6B 6Cu 3Mn 6Y 5Magnetic accounts for 70% ,-300 orders of gross mass～+ 400 purpose Fe 74Si 6B 6Cu 3Mn 6Y 5Magnetic accounts for 10% ,-400 purpose Fe of gross mass 74Si 6B 6Cu 3Mn 6Y 5Magnetic accounts for 5% of gross mass, through after the phosphate aqueous solution Passivation Treatment of 0.4wt%, fully mixes with the silicone resin binding agent of 0.5wt%, and be pressed into powder core under 1.80GPa pressure;
(4) powder core that suppresses is placed 500 ℃ of insulations of vacuum annealing furnace 1h, obtain Fe base nanometer crystal powder core.
After testing, associated electrical magnetic parameter such as the table 4 of target product:
Figure BDA00003468409600052

Claims (3)

1. a low-loss Fe base nanometer crystal powder core is characterized in that it consists of: Fe aSi bB cCu dM eY f, M is C, P, Cr or Mn in the formula, subscript a, b, c, d, e, f represent the atomic percent of respective alloy element, meet the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2≤e≤8,0＜f≤5; And a+b+c+d+e+f=100.
2. the preparation method of a low-loss Fe base nanometer crystal powder core is characterized in that its step is as follows:
(1) with Fe aSi bB cCu dM eY fAmorphous thin ribbon in vacuum annealing furnace in 420 ℃ the insulation 1h after, it is carried out Mechanical Crushing, M is C, P, Cr or Mn in the formula, subscript a, b, c, d, e, f represent the atomic percent of respective alloy element, meet the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2≤e≤8,0＜f≤5; And a+b+c+d+e+f=100;
(2) Fe aSi bB cCu dM eY fAfter the amorphous thin ribbon Mechanical Crushing, place the planetary ball mill ball milling, ratio of grinding media to material is 5:1, and Ball-milling Time is 4h, and rotating speed is 260r/min, and adds the anti-oxidation of ethanol, the dry Fe that obtains the variable grain degree by screening aSi bB cCu dM eY fMagnetic;
(3) with the Fe of different meshes aSi bB cCu dM eY fMagnetic mixes, wherein-100 order ~+200 purpose Fe aSi bB cCu dM eY fMagnetic accounts for 15% ,-200 orders of gross mass ~+300 purpose Fe aSi bB cCu dM eY fMagnetic accounts for 70% ,-300 orders of gross mass ~+400 purpose Fe aSi bB cCu dM eY fMagnetic accounts for 10% ,-400 purpose Fe of gross mass aSi bB cCu dM eY fMagnetic accounts for 5% of gross mass, through after the phosphate aqueous solution Passivation Treatment of 0.4wt%, fully mixes with the binding agent of 0.5wt%, and be pressed into powder core under 1.80GPa pressure;
(4) powder core that suppresses is placed 500 ℃ of insulations of vacuum annealing furnace 1h, obtain Fe base nanometer crystal powder core.
3. the preparation method of a kind of low-loss Fe base nanometer crystal powder core according to claim 2 is characterized in that described binding agent is epoxy resin or silicone resin.
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CN103500643A (en) * 2013-09-29 2014-01-08 青岛云路新能源科技有限公司 Method for modified silicon iron boron soft magnetic powder core with magnetic conductivity of 90
CN103500645A (en) * 2013-09-29 2014-01-08 青岛云路新能源科技有限公司 Method for manufacturing modified silicon iron boron soft magnetic powder core with magnetic conductivity of 50
CN103500646A (en) * 2013-09-29 2014-01-08 青岛云路新能源科技有限公司 Method for manufacturing modified silicon iron boron soft magnetic powder core with magnetic conductivity of 26
CN104036904A (en) * 2014-05-28 2014-09-10 浙江大学 High saturation magnetic induction intensity iron-based amorphous soft magnetic composite material and manufacturing method thereof
CN104032241A (en) * 2014-05-28 2014-09-10 浙江大学 Preparation method of amorphous soft-magnetic composite material
CN104157441A (en) * 2014-08-15 2014-11-19 无锡斯贝尔磁性材料有限公司 Technology for manufacturing finished magnetic core
CN106128681A (en) * 2016-06-08 2016-11-16 青岛云路先进材料技术有限公司 A kind of Fe-based amorphous powder core and preparation method thereof
CN106653278A (en) * 2016-12-29 2017-05-10 江西艾特磁材有限公司 Novel iron-silicon magnetic core and preparation method thereof
CN104036941B (en) * 2014-06-10 2017-06-13 毛圣华 A kind of wireless charging preparation method of amorphous metal powder antifreeze plate
CN106890999A (en) * 2015-12-21 2017-06-27 北京中科三环高技术股份有限公司 A kind of preparation method of amorphous or nano-crystal soft-magnetic powder core
CN109411176A (en) * 2017-08-18 2019-03-01 三星电机株式会社 Fe Based Nanocrystalline Alloys and the electronic building brick for using the Fe Based Nanocrystalline Alloys
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CN103500643A (en) * 2013-09-29 2014-01-08 青岛云路新能源科技有限公司 Method for modified silicon iron boron soft magnetic powder core with magnetic conductivity of 90
CN103500645A (en) * 2013-09-29 2014-01-08 青岛云路新能源科技有限公司 Method for manufacturing modified silicon iron boron soft magnetic powder core with magnetic conductivity of 50
CN103500646A (en) * 2013-09-29 2014-01-08 青岛云路新能源科技有限公司 Method for manufacturing modified silicon iron boron soft magnetic powder core with magnetic conductivity of 26
CN103500645B (en) * 2013-09-29 2016-01-20 青岛云路新能源科技有限公司 A kind of magnetic permeability is the preparation method of the Modified Iron silicon boron soft magnetic-powder core of 50
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CN103500646B (en) * 2013-09-29 2016-01-20 青岛云路新能源科技有限公司 A kind of magnetic permeability is the preparation method of the Modified Iron silicon boron soft magnetic-powder core of 26
CN104032241A (en) * 2014-05-28 2014-09-10 浙江大学 Preparation method of amorphous soft-magnetic composite material
CN104032241B (en) * 2014-05-28 2015-07-29 浙江大学 A kind of preparation method of amorphous soft magnet matrix material
CN104036904A (en) * 2014-05-28 2014-09-10 浙江大学 High saturation magnetic induction intensity iron-based amorphous soft magnetic composite material and manufacturing method thereof
CN104036941B (en) * 2014-06-10 2017-06-13 毛圣华 A kind of wireless charging preparation method of amorphous metal powder antifreeze plate
CN104157441A (en) * 2014-08-15 2014-11-19 无锡斯贝尔磁性材料有限公司 Technology for manufacturing finished magnetic core
CN106890999A (en) * 2015-12-21 2017-06-27 北京中科三环高技术股份有限公司 A kind of preparation method of amorphous or nano-crystal soft-magnetic powder core
CN106890999B (en) * 2015-12-21 2019-06-28 北京中科三环高技术股份有限公司 A kind of preparation method of amorphous or nano-crystal soft-magnetic powder core
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CN109411176A (en) * 2017-08-18 2019-03-01 三星电机株式会社 Fe Based Nanocrystalline Alloys and the electronic building brick for using the Fe Based Nanocrystalline Alloys
CN109411176B (en) * 2017-08-18 2021-02-05 三星电机株式会社 Fe-based nanocrystalline alloy and electronic component using same
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