CN102737799A - Preparation method of nanometer crystal magnetic powder core with magnetic conductivity mum of 60 - Google Patents
Preparation method of nanometer crystal magnetic powder core with magnetic conductivity mum of 60 Download PDFInfo
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Abstract
The invention discloses a preparation method of a nanometer crystal magnetic powder core with a magnetic conductivity mumof 60. The method comprises the following steps: thermally treating an iron-based amorphous thin ribbon prepared by a rapid cooling method into a nano-crystalline ribbon, wherein the iron-based amorphous thin ribbon has the following components by weight: 3-15% of Ni, 1-10% of Si, 1-4% of B, 1-9% of Al and the balance of Fe; crushing the nano-crystalline ribbon to obtain nano-crystalline metal powders; conducting ball-milling and shaping the nano-crystalline metal powders; screening the nano-crystalline metal powders, and mixing the nano-crystalline metal powders into powder particle consisting of 90%-98% of first powder screened by a -200-mesh sieve and 2%-10% of second powder screened by a (-150)-(+200)-mesh sieve for distribution; mixing the mixed nano-crystalline metal powders with a bonding agent, and pressing to form the magnetic core; and annealing the formed magnetic core, and then, coating the magnetic core with insulating resin. According to the technical scheme, the magnetic powder core has stable magnetic conductivity, a loss value and direct-current bias ability.
Description
The application is
The applying date is: on June 20th, 2012
Application number is: 201210208100.4
The application name is called: the preparation method of high performance nano-crystal magnetic core
The dividing an application of patent application.
Technical field
The present invention relates to the preparation method of the nanocrystalline magnetic core of a kind of magnetic permeability μ=60.
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 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 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 the nanocrystalline magnetic core of a kind of magnetic permeability μ=60, its magnetic core has stable magnetic permeability, loss value and direct current biasing ability.
In order to reach above-mentioned purpose, the technical scheme below the present invention has adopted:
The preparation method of the nanocrystalline magnetic core of magnetic permeability μ=60 comprises the steps:
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.
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.
As preferably, the bonding agent in the said step 5) is a sodium metasilicate, and adding concentration is 3～8wt ‰.
As preferably, the magnetic core heat treatment in the said step 5) was being carried out 1～3 hour under 500～700 ℃, in the mist of hydrogen and nitrogen.Further preferred, the mist mass ratio of said hydrogen and nitrogen is: hydrogen 5～15%, surplus are nitrogen.
The present invention can be used for preparing the nanocrystalline magnetic core of magnetic permeability μ=60 owing to adopted above technical scheme, and the magnetic core has stable magnetic permeability, 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.
Embodiment
Following specific embodiments of the invention is done a detailed explanation.
The preparation method of the nanocrystalline magnetic core of magnetic permeability μ=60 comprises the steps:
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 loss 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 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, 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 loss 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 permeability μ=60 nanocrystalline magnetic cores, when having more stable magnetic permeability, 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 loss 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 permeability (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 permeability μ=60 nanocrystalline magnetic cores, when having more stable magnetic permeability, 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 permeability.
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 permeability, 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 permeability 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 permeability μ=60 nanocrystalline magnetic cores; When having more stable magnetic permeability, 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 permeability 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 (5)
1. the preparation method of the nanocrystalline magnetic core of magnetic permeability μ=60 comprises the steps:
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.
2. the preparation method of the nanocrystalline magnetic core of magnetic permeability μ according to claim 1=60 is characterized in that, 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.
3. the preparation method of the nanocrystalline magnetic core of magnetic permeability μ according to claim 1=60 is characterized in that, the bonding agent in the said step 5) is a sodium metasilicate, and adding concentration is 3～8wt ‰.
4. the preparation method of the nanocrystalline magnetic core of magnetic permeability μ according to claim 1=60 is characterized in that, the magnetic core heat treatment in the said step 5) was being carried out 1～3 hour under 500～700 ℃, in the mist of hydrogen and nitrogen.
5. the preparation method of the nanocrystalline magnetic core of magnetic permeability μ according to claim 4=60 is characterized in that, the mist mass ratio of said hydrogen and nitrogen is: hydrogen 5～15%, surplus are nitrogen.
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| CN113572319A (en) * | 2021-07-08 | 2021-10-29 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Radial amorphous iron core and preparation method thereof |
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