CN102728840A - Method for preparing metal powder of nanocrystalline magnetic cores with magnetic permeability mu of 60 - Google Patents
Method for preparing metal powder of nanocrystalline magnetic cores with magnetic permeability mu of 60 Download PDFInfo
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Abstract
The invention discloses a method for preparing metal powder of nanocrystalline magnetic cores with magnetic permeability mu of 60. The method comprises the steps that: heat treatment for iron-based amorphous ribbons is carried out to produce nanocrystalline ribbons, wherein the iron-based amorphous ribbons are prepared with a rapid cooling method; the iron-based amorphous ribbons consist of, on a mass basis, 3-15% of Ni, 1-10% of Si, 1-4% of B, 1-9% of Al, and the balance being of Fe; the nanocrystalline ribbons are broken to obtain nanocrystalline metal powder; ball milling shaping of the nanocrystalline metal powder is carried out; the nanocrystalline metal powder is screened; and powder particle composition comprises 90%-98% of the first powder which is screened by using a sieve with a size of -200 meshes and 2%-10% of second powder is screened by using a sieve with a size of -150-+200 meshes. According to the technical scheme, nanocrystalline magnetic cores with magnetic permeability mu of 60 are prepared; magnetic permeability, loss value and direct current bias capability of the magnetic cores are stable.
Description
The application is
The applying date is: on June 20th, 2012
Application number is: 201210208100.4
Application name is called: the dividing an application of the preparation method's of high performance nano-crystal magnetic core patent application.
Technical field
The present invention relates to the preparation method of a kind of magnetic conductivity μ=60 nanocrystalline magnet cores with metal dust.
Background technology
In power electronic equipment, noise is main circuit interference source, so must use various filtering devices to be used for reducing noise.And the magnetic core plays key effect as the main element of differential mode inductance in wave filter.Magnetic core product mainly contains ferrocart core, Fe-Si-Al magnetic core, iron nickel magnetic core, MPP magnetic core etc. at present.Conventional ferrocart core is inexpensive, but high frequency characteristics is bad.When the choke coil of design and preparing various kinds Switching Power Supply and inductance, all select Fe-Si-Al magnetic core, iron nickel magnetic core and MPP magnetic core basically for use now.
Compare with ferrocart core; Fe-Si-Al magnetic core has low-down core loss; Simultaneously its frequency characteristic is better, but the direct current biasing ability of Fe-Si-Al magnetic core under big electric current is relatively poor, so that the use of Fe-Si-Al magnetic core under unfavorable conditions is restricted.
And iron nickel magnetic 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 50% nickel in the iron nickel magnetic core, expensive, production cost is high.
In like manner MPP magnetic core has splendid frequency characteristic equally in the frequency range of 1MHz, and core loss is minimum in various metal magnetic powder cores.But the direct current biasing ability of MPP magnetic core is general, and MPP magnetic core also has precious metals such as nickel, molybdenum simultaneously, and expensive makes it be difficult to be used widely.
Summary of the invention
In order to solve above-mentioned technical problem; The purpose of this invention is to provide the preparation method of a kind of magnetic conductivity μ=60 nanocrystalline magnet cores with metal dust; Be used to prepare the nanocrystalline magnetic core of magnetic conductivity μ=60, this magnetic core has stable magnetic conductivity, loss value and direct current biasing ability.
In order to reach above-mentioned purpose, the technical scheme below the present invention has adopted:
Magnetic conductivity μ=60 nanocrystalline magnet cores comprise the steps: with the preparation method of metal dust
1) iron-based amorphous thin ribbon that utilizes method for rapid cooling to make is heat-treated, be converted into nano-crystalline thin ribbon; Wherein, the iron-based amorphous thin ribbon mass percent is: 3～15%Ni, and 1～10%Si, 1～4%B, 1～9% Al, surplus is Fe;
2) said nano-crystalline thin ribbon is carried out fragmentation and obtain the nanocrystalline metal powder;
3) said nanocrystalline metal powder is carried out the ball milling shaping;
4) said nanocrystalline metal powder is screened, the powder particle that is mixed into then by second powder constituent that passes through-150～+ 200 sieve meshes of 90%～98% first powder that passes through-200 sieve meshes and 2%～10% distributes.
As preferably, the iron-based amorphous thin ribbon heat treatment in the said step 1) was carried out under 500～700 ℃, in inert gas 1～3 hour.
The present invention can be used for preparing the nanocrystalline magnetic core of magnetic conductivity μ=60 owing to adopted above technical scheme, and this magnetic core has stable magnetic conductivity, loss value and direct current biasing ability.Have the following advantages: 1, manufacture craft is simple, and use equipment is simple, and production cost is low; 2, the magnetic core product with specific magnetic conductance that adopts the inventive method to make when keeping good inductance value, higher quality factor, has reduced the loss value of product, has improved the direct current biasing ability.Nanocrystalline magnetic core of the present invention mainly is applicable to the Active PFC of Switching Power Supply and the output filtering of Switching Power Supply; Improve the efficient of exchange power with this, and can be at certain occasion replacement Fe-Si-Al magnetic core, iron nickel magnetic core and MPP magnetic core.
The specific embodiment
Following specific embodiments of the invention is done a detailed explanation.
Magnetic conductivity μ=60 nanocrystalline magnet cores comprise the steps: with the preparation method of metal dust
1) iron-based amorphous thin ribbon that utilizes method for rapid cooling to make is heat-treated, be converted into nano-crystalline thin ribbon; Wherein, the iron-based amorphous thin ribbon mass percent is: 3～15%Ni, and 1～10%Si, 1～4%B, 1～9% Al, surplus is Fe;
2) said nano-crystalline thin ribbon is carried out fragmentation and obtain the nanocrystalline metal powder;
3) said nanocrystalline metal powder is carried out the ball milling shaping;
4) said nanocrystalline metal powder is screened, the powder particle that is mixed into then by second powder constituent that passes through-150～+ 200 sieve meshes of 90%～98% first powder that passes through-200 sieve meshes and 2%～10% distributes;
5) the nanocrystalline metal powder that mixes is mixed with bonding agent again, through the compression moulding magnetic core; And the magnetic core of said moulding annealed, be coated with said magnetic core with insulating resin then.
The present invention mainly studies the performance impact of preparation technology to the magnetic core of identical component proportioning.Below through aspects such as powder particle distribution, iron-based amorphous thin ribbon heat treatment temperature, magnetic core heat treatment protective gas, bonding agent ratio are described the present invention program.
Instance 1:
With the iron-based amorphous thin ribbon that utilizes method for rapid cooling to make heat treatment 1 hour in 580 ℃ inert gas, obtain nano-crystalline thin ribbon; And with its fragmentation, shaping; Choose first powder of 90%-200 sieve meshes and second powder of 10%-150～+ 200 sieve meshes; Mix with the sodium metasilicate of 5wt ‰,, choose magnetic core annealing through compression moulding; Feed nitrogen in the heat treated stove simultaneously; 500 ℃ of temperature, adopt epoxy resin paint to be coated in the surface of magnetic core at last at 2 hours time.Obtain the nanocrystalline magnetic core product 1 of Φ 26.9/ Φ 14.7 * 11.2 (being that external diameter is that 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) specification.
Instance 2:
With the iron-based amorphous thin ribbon that utilizes method for rapid cooling to make heat treatment 1 hour in 620 ℃ inert gas, obtain nano-crystalline thin ribbon; And with its fragmentation, shaping; Choose first powder of 90%-200 sieve meshes and second powder of 10%-150～+ 200 sieve meshes; Mix with the sodium metasilicate of 5wt ‰,, choose magnetic core annealing through compression moulding; Feed nitrogen in the heat treated stove simultaneously; 500 ℃ of temperature, adopt epoxy resin paint to be coated in the surface of magnetic core at last at 2 hours time.Obtain the nanocrystalline magnetic core product 2 of Φ 26.9/ Φ 14.7 * 11.2 (being that external diameter is that 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) specification.
Instance 3:
With the iron-based amorphous thin ribbon that utilizes method for rapid cooling to make heat treatment 1 hour in 620 ℃ inert gas, obtain nano-crystalline thin ribbon; And with its fragmentation, shaping; Choose first powder of 95%-200 sieve meshes and second powder of 5%-150～+ 200 sieve meshes; Mix with the sodium metasilicate of 5wt ‰,, choose magnetic core annealing through compression moulding; Feed nitrogen in the heat treated stove simultaneously; 500 ℃ of temperature, adopt epoxy resin paint to be coated in the surface of magnetic core at last at 2 hours time.Obtain the nanocrystalline magnetic core product 3 of Φ 26.9/ Φ 14.7 * 11.2 (being that external diameter is that 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) specification.
Instance 4:
With the iron-based amorphous thin ribbon that utilizes method for rapid cooling to make heat treatment 1 hour in 620 ℃ inert gas, obtain nano-crystalline thin ribbon; And with its fragmentation, shaping; Choose first powder of 95%-200 sieve meshes and second powder of 5%-100～+ 200 sieve meshes; Mix with the sodium metasilicate of 5wt ‰,, choose magnetic core annealing through compression moulding; Feed nitrogen in the heat treated stove simultaneously; 500 ℃ of temperature, adopt epoxy resin paint to be coated in the surface of magnetic core at last at 2 hours time.Obtain the nanocrystalline magnetic core product 4 of Φ 26.9/ Φ 14.7 * 11.2 (being that external diameter is that 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) specification.
Instance 5:
With the iron-based amorphous thin ribbon that utilizes method for rapid cooling to make heat treatment 1 hour in 620 ℃ inert gas, obtain nano-crystalline thin ribbon; And with its fragmentation, shaping; Choose first powder of 95%-200 sieve meshes and second powder of 5%-150～+ 200 sieve meshes; Mix with the sodium metasilicate of 5wt ‰,, choose magnetic core annealing through compression moulding; Feed hydrogen in the heat treated stove simultaneously; 500 ℃ of temperature, adopt epoxy resin paint to be coated in the surface of magnetic core at last at 2 hours time.Obtain the nanocrystalline magnetic core product 5 of Φ 26.9/ Φ 14.7 * 11.2 (being that external diameter is that 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) specification.
Instance 6:
With the iron-based amorphous thin ribbon that utilizes method for rapid cooling to make heat treatment 1 hour in 620 ℃ inert gas, obtain nano-crystalline thin ribbon; And with its fragmentation, shaping; Choose first powder of 95%-200 sieve meshes and second powder of 5%-150～+ 200 sieve meshes; Mix with the sodium metasilicate of 5wt ‰,, choose magnetic core annealing through compression moulding; Feed the mist (hydrogen 5～15wt%) of hydrogen and nitrogen simultaneously in the heat treated stove; 500 ℃ of temperature, adopt epoxy resin paint to be coated in the surface of magnetic core at last at 2 hours time.Obtain the nanocrystalline magnetic core product 6 of Φ 26.9/ Φ 14.7 * 11.2 (being that external diameter is that 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) specification.
Above-mentioned instance product is tested and is explained as follows:
(1) f ﹑ L ﹑ Q test
Copper wire adopts Φ 0.5mm, and coil turn is 26 circles, the magnetic parameter such as the following table 1 of the said goods 1 to 6 test:
(2) power attenuation test
Copper wire adopts Φ 0.8mm, and coil turn is 34 circles, the magnetic parameter such as the following table 2 of the said goods 1 to 6 test:
| Product | Frequency f (kHz) | Magnetic flux density B pk(Gauss) | Power attenuation (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, the magnetic parameter such as the following table 3 of the said goods 1 to 6 test:
(4) saturation induction density
The elementary employing Φ of copper wire 0.5mm, coil turn is 200 circles, secondary employing Φ 0.29mm, coil turn is 50 circles, through the BH loop tester, the magnetic parameter such as the following table 4 of the said goods 1 to 6 test:
| Product | Saturation induction density (Gauss) |
| Product 1 | 11000 |
| Product 2 | 12000 |
| Product 3 | 12000 |
| Product 4 | 11500 |
| Product 5 | 12500 |
| Product 6 | 13000 |
Distribute to the magnetic core Effect on Performance about metal powder granulates.Can know from the data comparison of product 3 and product 4; With respect to product 3; Along with powder particle increases (second powder of product 3 is-150～+ 200 sieve meshes, and second powder of product 4 is-100～+ 200 sieve meshes), the quality factor q of product 4 significantly reduces; Power attenuation significantly increases, and the direct current biasing ability significantly reduces.And; Through the more evidence of inventor; The powder particle of first powder that passes through-200 sieve meshes by 90%～98% and 2%～10% second powder constituent that passes through-150～+ 200 sieve meshes " distribute " is the optimal selection of preparation magnetic conductivity μ=60 nanocrystalline magnetic cores, when having more stable magnetic conductivity, possesses less consumption value and direct current biasing ability preferably.Can cause the magnetic core air gap too small when first powder through-200 sieve meshes surpasses 98%, the direct current biasing ability significantly reduces; Can cause the magnetic core air gap too much when first powder through-200 sieve meshes is less than 90%, power attenuation significantly increases.
About the iron-based amorphous thin ribbon heat treatment temperature to the magnetic core Effect on Performance.Can know that from the data comparison of product 1 and product 2 both each item performance datas are slightly variant, but all meet design requirement.In addition; Through the more evidence of inventor; When heat treatment temperature below 500 ℃ or more than 700 ℃ the time, the remarkable off-design characteristic value of magnetic conductivity (surpassing 5%), therefore; " iron-based amorphous thin ribbon heat treatment was carried out under 500～700 ℃, in inert gas 1～3 hour " is the optimal selection of preparation magnetic conductivity μ=60 nanocrystalline magnetic cores, when having more stable magnetic conductivity, possesses less consumption value and direct current biasing ability preferably.
About magnetic core heat treatment protective gas to the magnetic core Effect on Performance.Can know from the data comparison of product 3, product 5 and product 6; Product 3 (nitrogen protection), product 6 (nitrogen, hydrogen combine) have preferable performance with respect to product 5 (hydrogen shield); And further, product 6 (nitrogen, hydrogen combine) slightly promotes with respect to the aspects such as stability, loss value and saturation induction density of product 3 (nitrogen protection) at magnetic conductivity.
About the adding proportion of bonding agent, explain referring to following instance:
Instance 7:
With the iron-based amorphous thin ribbon that utilizes method for rapid cooling to make heat treatment 1 hour in 580 ℃ inert gas, obtain nano-crystalline thin ribbon; And with its fragmentation, shaping; Choose first powder of 90%-200 sieve meshes and second powder of 10%-150～+ 200 sieve meshes, select for use sodium metasilicate as bonding agent, respectively according to 1wt ‰; 3wt ‰, and 5wt ‰, and 8wt ‰, 10wt ‰ add mixing; Through compression moulding, choose magnetic core annealing, feed the mist (hydrogen 5～15wt%) of hydrogen and nitrogen simultaneously in the heat treated stove; 500 ℃ of temperature, adopt epoxy resin paint to be coated in the surface of magnetic core at last at 2 hours time.Obtain nanocrystalline magnetic core product 7, product 8, product 9, product 10, the product 11 of Φ 26.9/ Φ 14.7 * 11.2 (being that external diameter is that 26.9mm ﹑ internal diameter is 14.7mm ﹑ height 11.2mm) specification.
The said goods 7, product 8, product 9, product 10, product 11 are tested under the same conditions, and the correction data aspect magnetic conductivity, core loss (50kHz/1000Gs), direct current biasing (100Oe) is as shown in the table:
Can know that by table the addition of bonding agent has bigger influence to performance of products, when bonding agent addition too high (surpassing 8wt ‰), the magnetic conductivity of magnetic core can reduce, and core loss can increase, and the direct current biasing ability can reduce; When bonding agent addition very few (being lower than 3wt ‰), can cause properties of product to worsen, even product can not moulding.Therefore; " bonding agent is a sodium metasilicate; adding concentration is 3～8wt ‰ " is the optimal selection of preparation magnetic conductivity μ=60 nanocrystalline magnetic cores; When having more stable magnetic conductivity, possess less consumption value and direct current biasing ability preferably, and further, it is that 5wt ‰ is optimal selection that sodium metasilicate adds concentration.
Provided magnetic conductivity in the following table and be the soft magnet performance result of 60 various magnetic cores, shown that the present invention has excellent soft magnet performance.
It is emphasized that: above only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction; Every foundation technical spirit of the present invention all still belongs in protection scope of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (2)
1. magnetic conductivity μ=60 nanocrystalline magnet cores comprise the steps: with the preparation method of metal dust
1) iron-based amorphous thin ribbon that utilizes method for rapid cooling to make is heat-treated, be converted into nano-crystalline thin ribbon; Wherein, the iron-based amorphous thin ribbon mass percent is: 3～15%Ni, and 1～10%Si, 1～4%B, 1～9%Al, surplus is Fe;
2) said nano-crystalline thin ribbon is carried out fragmentation and obtain the nanocrystalline metal powder;
3) said nanocrystalline metal powder is carried out the ball milling shaping;
4) said nanocrystalline metal powder is screened, the powder particle that is mixed into then by second powder constituent that passes through-150～+ 200 sieve meshes of 90%～98% first powder that passes through-200 sieve meshes and 2%～10% distributes.
2. magnetic conductivity μ according to claim 1=60 nanocrystalline magnet cores is characterized in that with the preparation method of metal dust the iron-based amorphous thin ribbon heat treatment in the said step 1) was carried out 1～3 hour under 500～700 ℃, in inert gas.
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