CN102969108B - A kind of metal dust for the preparation of magnetic permeability μ=60 nanocrystalline magnet core - Google Patents
A kind of metal dust for the preparation of magnetic permeability μ=60 nanocrystalline magnet core Download PDFInfo
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Abstract
The invention discloses a kind of metal dust for the preparation of magnetic permeability μ=60 nanocrystalline magnet core, adopt following steps preparation: to utilizing the obtained iron-based amorphous thin ribbon of method for rapid cooling to heat-treat, being converted into nano-crystalline thin ribbon; Fragmentation is carried out to described nano-crystalline thin ribbon and obtains nanocrystalline metal powder; Ball milling shaping is carried out to described nanocrystalline metal powder; Described nanocrystalline metal powder is screened, is then mixed into and is distributed by the powder particle passing through the second powder constituent of-150 ~+200 sieve meshes of first powder passing through-200 sieve meshes of 90% ~ 98% and 2% ~ 10%.The technical program magnetic core has stable magnetic permeability, loss value and direct current biasing ability.
Description
The application is
The applying date is: on June 19th, 2012
Application number is: 201210206560.3
Application name is called: the divisional application of the patent application of a kind of preparation method of high-performance nano-crystal magnetic powder core.
Technical field
The present invention relates to a kind of metal dust for the preparation of magnetic permeability μ=60 nanocrystalline magnet core.
Background technology
In power electronic equipment, noise is main circuit interference source, so various filtering device must be used to be used for reducing noise.And powder core is as the main element of differential mode inductance, in filter, play key effect.Current powder core product mainly contains ferrocart core, Fe-Si-Al magnetic core, iron nickel powder core, MPP powder core etc.Conventional ferrocart core is inexpensive, but high frequency characteristics is bad.Now when choke and the inductance of all kinds of Switching Power Supply of designing and making, substantially all select Fe-Si-Al magnetic core, iron nickel powder core and MPP powder core.
Compared with ferrocart core, Fe-Si-Al magnetic core has low-down core loss, its frequency characteristic is better simultaneously, but the direct current biasing ability of Fe-Si-Al magnetic core under larger current is poor, so make Fe-Si-Al magnetic core use in adverse conditions be restricted.
And iron nickel powder core has splendid frequency characteristic in the frequency range of 1MHz, and loss is lower.And in metal magnetic powder core, iron nickel magnetic core has the highest direct current biasing ability, good product performance.But also have the nickel of 50% in iron nickel powder core, price is high, and production cost is high.
In like manner MPP powder core has splendid frequency characteristic equally in the frequency range of 1MHz, and core loss is minimum in various metal magnetic powder core.But the direct current biasing ability of MPP powder core is general, MPP powder core also has the precious metal such as nickel, molybdenum simultaneously, and price is high, makes it be difficult to be used widely.
Summary of the invention
In order to solve above-mentioned technical problem, the object of this invention is to provide a kind of metal dust for the preparation of magnetic permeability μ=60 nanocrystalline magnet core, this magnetic core has stable magnetic permeability, loss value and direct current biasing ability.
To achieve the above object, present invention employs following technical scheme:
For the preparation of a metal dust for magnetic permeability μ=60 nanocrystalline magnet core, adopt following steps preparation:
1) to utilizing the obtained iron-based amorphous thin ribbon of method for rapid cooling to heat-treat, nano-crystalline thin ribbon is converted into;
2) fragmentation is carried out to described nano-crystalline thin ribbon and obtain nanocrystalline metal powder;
3) ball milling shaping is carried out to described nanocrystalline metal powder;
4) described nanocrystalline metal powder is screened, be then mixed into and distributed by the powder particle passing through the second powder constituent of-150 ~+200 sieve meshes of first powder passing through-200 sieve meshes of 90% ~ 98% and 2% ~ 10%.
Above-mentioned steps 1) in iron-based amorphous thin ribbon mass percent be: 3 ~ 15%Ni, 1 ~ 30% at least one is selected from the element of Si, B, Al, P, Nb, Cu and Zr, and surplus is Fe.
As preferably, the iron-based amorphous thin ribbon heat treatment in described step 1) carries out 1 ~ 3 hour at 500 ~ 700 DEG C, in inert gas.
The present invention is owing to have employed above technical scheme, and magnetic core has stable magnetic permeability, loss value and direct current biasing ability.Have the following advantages: 1, manufacture craft is simple, use equipment simple, production cost is low;
2, the magnetic core product with specific magnetic conductance adopting the present invention to make, while keeping good inductance value, higher quality factor, reduces the loss value of product, improves direct current biasing ability.Nanocrystalline magnetic core of the present invention is mainly applicable to the Active PFC of Switching Power Supply and the output filtering of Switching Power Supply, improve with this efficiency exchanging power, and Fe-Si-Al magnetic core, iron nickel powder core and MPP powder core can be replaced in certain occasion.
Embodiment
The following specific embodiments of the present invention is to make a detailed explanation.
A kind of magnetic permeability μ=60 nanocrystalline magnet core, adopts following steps preparation:
1) to utilizing the obtained iron-based amorphous thin ribbon of method for rapid cooling to heat-treat, nano-crystalline thin ribbon is converted into;
2) fragmentation is carried out to described nano-crystalline thin ribbon and obtain nanocrystalline metal powder;
3) ball milling shaping is carried out to described nanocrystalline metal powder;
4) described nanocrystalline metal powder is screened, be then mixed into and distributed by the powder particle passing through the second powder constituent of-150 ~+200 sieve meshes of first powder passing through-200 sieve meshes of 90% ~ 98% and 2% ~ 10%;
5) the nanocrystalline metal powder of mixing is mixed with bonding agent, by compressing magnetic core again; And described shaping magnetic core is annealed, be then coated with described magnetic core with insulating resin.
In such scheme, iron-based amorphous thin ribbon mass percent is: 3 ~ 15%Ni, and 1 ~ 30% at least one is selected from the element of Si, B, Al, P, Nb, Cu and Zr, and surplus is Fe.The present invention mainly studies the performance impact of preparation technology to the powder core of identical component proportioning.From the aspect such as powder particle distribution, iron-based amorphous thin ribbon heat treatment temperature, powder core heat treating atmosphere gas, bonding agent ratio, the present invention program is described below.
Example 1:
The iron-based amorphous thin ribbon obtained utilizing method for rapid cooling heat treatment 1 hour in the inert gas of 580 DEG C, obtains nano-crystalline thin ribbon; And it is broken, shaping; Choose the second powder of the first powder of-200 sieve meshes of 90% and-150 ~+200 sieve meshes of 10%, mix with the sodium metasilicate of 5wt ‰, by compressing, choose magnetic core annealing, pass into nitrogen in heat treated stove simultaneously, temperature 500 DEG C, time 2 h, finally adopts epoxy resin paint to be coated in the surface of powder core.To obtain Φ 26.9/ Φ 14.7 × 11.2(and external diameter be 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) the nanocrystalline magnetic core product 1 of specification.
Example 2:
The iron-based amorphous thin ribbon obtained utilizing method for rapid cooling heat treatment 1 hour in the inert gas of 620 DEG C, obtains nano-crystalline thin ribbon; And it is broken, shaping; Choose the second powder of the first powder of-200 sieve meshes of 90% and-150 ~+200 sieve meshes of 10%, mix with the sodium metasilicate of 5wt ‰, by compressing, choose magnetic core annealing, pass into nitrogen in heat treated stove simultaneously, temperature 500 DEG C, time 2 h, finally adopts epoxy resin paint to be coated in the surface of powder core.To obtain Φ 26.9/ Φ 14.7 × 11.2(and external diameter be 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) the nanocrystalline magnetic core product 2 of specification.
Example 3:
The iron-based amorphous thin ribbon obtained utilizing method for rapid cooling heat treatment 1 hour in the inert gas of 620 DEG C, obtains nano-crystalline thin ribbon; And it is broken, shaping; Choose the second powder of the first powder of-200 sieve meshes of 95% and-150 ~+200 sieve meshes of 5%, mix with the sodium metasilicate of 5wt ‰, by compressing, choose magnetic core annealing, pass into nitrogen in heat treated stove simultaneously, temperature 500 DEG C, time 2 h, finally adopts epoxy resin paint to be coated in the surface of powder core.To obtain Φ 26.9/ Φ 14.7 × 11.2(and external diameter be 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) the nanocrystalline magnetic core product 3 of specification.
Example 4:
The iron-based amorphous thin ribbon obtained utilizing method for rapid cooling heat treatment 1 hour in the inert gas of 620 DEG C, obtains nano-crystalline thin ribbon; And it is broken, shaping; Choose the second powder of the first powder of-200 sieve meshes of 95% and-100 ~+200 sieve meshes of 5%, mix with the sodium metasilicate of 5wt ‰, by compressing, choose magnetic core annealing, pass into nitrogen in heat treated stove simultaneously, temperature 500 DEG C, time 2 h, finally adopts epoxy resin paint to be coated in the surface of powder core.To obtain Φ 26.9/ Φ 14.7 × 11.2(and external diameter be 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) the nanocrystalline magnetic core product 4 of specification.
Example 5:
The iron-based amorphous thin ribbon obtained utilizing method for rapid cooling heat treatment 1 hour in the inert gas of 620 DEG C, obtains nano-crystalline thin ribbon; And it is broken, shaping; Choose the second powder of the first powder of-200 sieve meshes of 95% and-150 ~+200 sieve meshes of 5%, mix with the sodium metasilicate of 5wt ‰, by compressing, choose magnetic core annealing, pass into hydrogen in heat treated stove simultaneously, temperature 500 DEG C, time 2 h, finally adopts epoxy resin paint to be coated in the surface of powder core.To obtain Φ 26.9/ Φ 14.7 × 11.2(and external diameter be 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) the nanocrystalline magnetic core product 5 of specification.
Example 6:
The iron-based amorphous thin ribbon obtained utilizing method for rapid cooling heat treatment 1 hour in the inert gas of 620 DEG C, obtains nano-crystalline thin ribbon; And it is broken, shaping; Choose the second powder of the first powder of-200 sieve meshes of 95% and-150 ~+200 sieve meshes of 5%, mix with the sodium metasilicate of 5wt ‰, by compressing, choose magnetic core annealing, pass into the mist (hydrogen 5 ~ 15wt%) of hydrogen and nitrogen in heat treated stove simultaneously, temperature 500 DEG C, time 2 h, finally adopts epoxy resin paint to be coated in the surface of powder core.To obtain Φ 26.9/ Φ 14.7 × 11.2(and external diameter be 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) the nanocrystalline magnetic core product 6 of specification.
Above-mentioned example product is tested and is described as follows:
(1) f ﹑ L ﹑ Q test
Copper wire adopts Φ 0.5mm, and coil turn is 26 circles, and the magnetic parameter that the said goods 1 to 6 is tested is as following table 1:
(2) power loss test
Copper wire adopts Φ 0.8mm, and coil turn is 34 circles, and the magnetic parameter that the said goods 1 to 6 is tested is as following table 2:
| Product | Frequency f (kHz) | Magnetic flux density Bpk (Gauss) | Power loss (mW/cm3) |
| Product 1 | 50 | 1000 | 292 |
| Product 2 | 50 | 1000 | 278 |
| Product 3 | 50 | 1000 | 271 |
| Product 4 | 50 | 1000 | 305 |
| Product 5 | 50 | 1000 | 283 |
| Product 6 | 50 | 1000 | 259 |
(3) magnetism testing
Copper wire adopts Φ 0.8mm, and coil turn is 34 circles, and frequency is 100kHz, and the magnetic parameter that the said goods 1 to 6 is tested is as following table 3:
(4) saturation induction density
Copper wire elementary employing Φ 0.5mm, coil turn is 200 circles, secondary employing Φ 0.29mm, and coil turn is 50 circles, and through BH loop tester, the magnetic parameter that the said goods 1 to 6 is tested is as following table 4:
| Product | Saturation induction density (Gauss) |
| Product 1 | 11000 |
| Product 2 | 12000 |
| Product 3 | 12000 |
| Product 4 | 11500 |
| Product 5 | 12500 |
| Product 6 | 13000 |
About the impact of metal powder granulates distribution on magnetic core performance.From the data of product 3 and product 4 relatively, relative to product 3, along with powder particle increases, (the second powder of product 3 is-150 ~+200 sieve meshes, second powder of product 4 is-100 ~+200 sieve meshes), the quality factor q of product 4 significantly reduces, power loss significantly increases, and direct current biasing ability significantly reduces.And, more proof is tested through inventor, " the first powder passing through-200 sieve meshes by 90% ~ 98% and 2% ~ 10% pass through the second powder constituent of-150 ~+200 sieve meshes powder particle distribution " be the optimal selection preparing magnetic permeability μ=60 nanocrystalline magnetic core, while there is more stable magnetic permeability, possess less loss value and good direct current biasing ability.When the first powder by-200 sieve meshes can cause magnetic core air gap too small more than 98%, direct current biasing ability significantly reduces; Magnetic core air gap can be caused too much when the first powder by-200 sieve meshes is less than 90%, power loss significantly increases.
About the impact of iron-based amorphous thin ribbon heat treatment temperature on magnetic core performance.From the data of product 1 and product 2 relatively, both properties data slightly difference, but all meet design requirement.In addition, more proof is tested through inventor, when heat treatment temperature below 500 DEG C or more than 700 DEG C time, the remarkable off-design characteristic value (more than 5%) of magnetic permeability, therefore, " iron-based amorphous thin ribbon heat treatment carries out 1 ~ 3 hour at 500 ~ 700 DEG C, in inert gas " is the optimal selection preparing magnetic permeability μ=60 nanocrystalline magnetic core, possesses less loss value and good direct current biasing ability while having more stable magnetic permeability.
About the impact of powder core heat treating atmosphere gas on magnetic core performance.From the data of product 3, product 5 and product 6 relatively; product 3(nitrogen protection), product 6(nitrogen, hydrogen combine) relative to product 5(hydrogen shield) there is good performance; and further, product 6(nitrogen, hydrogen combine) relative to product 3(nitrogen protection) slightly promote in the stability of magnetic permeability, loss value and saturation induction density etc.
About the adding proportion of bonding agent, illustrate see following example:
Example 7:
The iron-based amorphous thin ribbon obtained utilizing method for rapid cooling heat treatment 1 hour in the inert gas of 580 DEG C, obtains nano-crystalline thin ribbon; And it is broken, shaping; Choose the second powder of the first powder of-200 sieve meshes of 90% and-150 ~+200 sieve meshes of 10%, select sodium metasilicate as bonding agent, respectively according to 1wt ‰, 3wt ‰, 5wt ‰, 8wt ‰, 10wt ‰ carry out interpolation mixing, by compressing, choose magnetic core annealing, pass into the mist (hydrogen 5 ~ 15wt%) of hydrogen and nitrogen in heat treated stove simultaneously, temperature 500 DEG C, time 2 h, finally adopts epoxy resin paint to be coated in the surface of powder core.To obtain Φ 26.9/ Φ 14.7 × 11.2(and external diameter be 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) nanocrystalline magnetic core product 7, product 8, product 9, product 10, the product 11 of specification.
Test under the same conditions the said goods 7, product 8, product 9, product 10, product 11, the correction data in magnetic permeability, core loss (50kHz/1000Gs), direct current biasing (100Oe) is as shown in the table:
As seen from table, the performance of addition on product of bonding agent has larger impact, and as bonding agent addition too high (more than 8wt ‰), the magnetic permeability of powder core can reduce, and core loss can increase, and direct current biasing ability can reduce; As bonding agent addition very few (lower than 3wt ‰), properties of product can be caused to worsen, and even product can not be shaping.Therefore, " bonding agent is sodium metasilicate; adding concentration is 3 ~ 8wt ‰ " is the optimal selection preparing magnetic permeability μ=60 nanocrystalline magnetic core, less loss value and good direct current biasing ability is possessed while there is more stable magnetic permeability, and further, sodium metasilicate interpolation concentration is 5wt ‰ is optimal selection.
Give the soft magnet performance result that magnetic permeability is the various powder cores of 60 in following table, display the present invention has excellent soft magnet performance.
It is emphasized that: be only preferred embodiment of the present invention above; not any pro forma restriction is done to the present invention; every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong in protection scope of the present invention.
Claims (1)
1., for the preparation of a metal dust for magnetic permeability μ=60 nanocrystalline magnet core, adopt following steps preparation:
1) to utilizing the obtained iron-based amorphous thin ribbon of method for rapid cooling to heat-treat, nano-crystalline thin ribbon is converted into; Wherein, iron-based amorphous thin ribbon mass percent is: 3 ~ 15%Ni, and 1 ~ 30% at least one is selected from the element of Si, B, Al, P, Nb, Cu and Zr, and surplus is Fe; Iron-based amorphous thin ribbon heat treatment carries out 1 ~ 3 hour at 500 ~ 700 DEG C, in inert gas;
2) fragmentation is carried out to described nano-crystalline thin ribbon and obtain nanocrystalline metal powder;
3) ball milling shaping is carried out to described nanocrystalline metal powder;
4) described nanocrystalline metal powder is screened, be then mixed into and distributed by the powder particle passing through the second powder constituent of-150 ~+200 sieve meshes of first powder passing through-200 sieve meshes of 90% ~ 98% and 2% ~ 10%.
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| KR101385756B1 (en) * | 2013-01-24 | 2014-04-21 | 주식회사 아모그린텍 | Manufacturing methods of fe-based amorphous metallic powders and soft magnetic cores |
| CN103273068A (en) * | 2013-05-22 | 2013-09-04 | 安泰科技股份有限公司 | Iron-based amorphous powder and method for preparing coil-embedded integral-forming inductor |
| KR101470513B1 (en) * | 2013-07-17 | 2014-12-08 | 주식회사 아모그린텍 | Soft Magnetic Cores Having Excellent DC Biased Characteristics in High Current and Core Loss Characteristics, and Manufacturing Methods thereof |
| CN105671461B (en) * | 2016-04-05 | 2018-05-15 | 广州齐达材料科技有限公司 | A kind of non-crystalline material and its preparation method and application |
| CN107578877B (en) * | 2017-06-29 | 2020-02-18 | 安泰科技股份有限公司 | Iron-based nanocrystalline magnetic powder core with magnetic conductivity mu-90 and preparation method thereof |
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| CN1579682A (en) * | 2003-08-14 | 2005-02-16 | 阿莫先思电子电器有限公司 | Method for making nano-scale metal powder and method for making high-frequency soft magnetic core using same |
| CN101501932A (en) * | 2006-08-11 | 2009-08-05 | 三井化学株式会社 | Antenna core and antenna |
| CN102360671A (en) * | 2011-08-12 | 2012-02-22 | 天通控股股份有限公司 | Preparation method for mu75 magnetic powder core of ferrosilicon aluminum |
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| CN1967736A (en) * | 2006-10-20 | 2007-05-23 | 南昌大学 | A method for preparing iron-base amorphous and nanocrystalline magnetic core |
| CN102208237A (en) * | 2010-03-29 | 2011-10-05 | 深圳市铂科磁材有限公司 | Nano ferrosilicon soft magnetic material |
| CN102382958A (en) * | 2011-11-08 | 2012-03-21 | 佛山市中研非晶科技股份有限公司 | Heat treatment method for improving magnetic conductivity of nanocrystalline magnetic core |
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| CN1579682A (en) * | 2003-08-14 | 2005-02-16 | 阿莫先思电子电器有限公司 | Method for making nano-scale metal powder and method for making high-frequency soft magnetic core using same |
| CN101501932A (en) * | 2006-08-11 | 2009-08-05 | 三井化学株式会社 | Antenna core and antenna |
| CN102360671A (en) * | 2011-08-12 | 2012-02-22 | 天通控股股份有限公司 | Preparation method for mu75 magnetic powder core of ferrosilicon aluminum |
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Address after: 313200 Zhejiang city of Huzhou province Deqing County Wukang Qu Yuan Road No. 525 Patentee after: Zhejiang east east Keda magnetoelectric Co., Ltd. Address before: 313200 Zhejiang city of Huzhou province Deqing County Wukang Qu Yuan Road No. 525 Patentee before: Zhejiang Keda Magnetoelectricity Co., Ltd. |