CN101255506B - Method for manufacturing super-magnetic conducting nanocrystalline alloy and nanocrystalline alloy - Google Patents
Method for manufacturing super-magnetic conducting nanocrystalline alloy and nanocrystalline alloy Download PDFInfo
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- CN101255506B CN101255506B CN2008100850157A CN200810085015A CN101255506B CN 101255506 B CN101255506 B CN 101255506B CN 2008100850157 A CN2008100850157 A CN 2008100850157A CN 200810085015 A CN200810085015 A CN 200810085015A CN 101255506 B CN101255506 B CN 101255506B
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Abstract
The invention relates to a manufacture method for super magnetic conductive nanocrystal alloy, wherein a master alloy includes 72.5 to 74.5 at% of Fe, 0.5 to 1.5 at% of Cu, 2.5 to 3.5 at% of Nb, 12.5 to 14.5 at% of Si and 8 to 10 at% of B. The method comprises the following steps: the master alloy is prepared by vacuum furnace smelting, the vacuum degree is less than 0.026*10<-6>MPa; when the temperature reaches to 1400 DEG C to 1450 DEG C, C is added to the vacuum furnace for deoxidation and refined, the temperature is lowered to deflate, and an ingot is cast; under argon protection, quenched amorphous nanocrystal alloy is formed by single roller fast cooling through a nozzle packet; the nozzle packet is provided with 25-30PPI Al2O3 ceramic filter to filter steel liquid, making SiO2 less than 0.026% (wt%) and B2O3 less than 0.019% (wt%). The magnetic conductivity mu of the iron core of the super magnetic conductive nanocrystal alloy manufactured by the method satisfies the followingconditions: mu50Hz (H=5mOe) >=60*10<4>, and mu1kHz (H=5mOe)>=20*10<4>.
Description
Technical field
The present invention relates to a kind of manufacture method and nanometer crystal alloy of super-magnetic conducting nanocrystalline alloy.
Background technology
High magnetic conducting nanocrystalline alloy is the patent (clear 64-31922) of inventions such as the De Ji of Hitachi Metal Co., Ltd. swamp gram benevolence in 1989, this patent disclosure add the nanometer crystal alloy of various elements, wherein optimal components is Fe73.5Cu1Nb3Si13.5B9 (at%), and μ 1kHz (H=5mOe) reaches 101000 after optimised process thermal treatment.This alloy has formed industrialization at home and abroad, but the oxide content in the not mentioned alloy of this patent content is to its Effect on Performance.In the research of permalloy, lay special stress on inclusion (impurity) content is to the influence of its permeability.The size of alloy coercivity H is the important parameter of sign alloy soft magnetic performance.Coercivity H indicates the obstacle that domain wall moves.The internal stress that inclusion causes is to influence the important factor that domain wall moves, and will reduce the coercivity H of alloy effectively so reduce alloy inclusions content, thereby effectively improve the permeability of alloy.
Nanometer crystal alloy is because of its good cost performance, and progressively substituted for silicon steel disc, permalloy are widely used in aspects such as power current transformer, instrument precision current/voltage transformer, zero sequence current mutual inductor, common mode inductance in field of power electronics.
The permeability that improves nanometer crystal alloy helps improving the angular difference of measuring the level mutual inductor, improves the mutual inductor service precision.In addition, compare, when making the mutual inductor of same precision, can effectively reduce production volume and weight unshakable in one's determination, complied with the needs of power electronic equipment to the miniaturization development with siliconized plate.The high permeability nanometer crystal alloy is used for zero sequence current mutual inductor, has improved the reaction sensitivity of earth leakage circuit-breaker, and when reaching protective current, protection switch moves rapidly, cuts off the electricity supply.
The amorphous nano peritectic alloy that general industrialization is produced, the starting material of use are ferro-niobium (NbFe), and the content of Nb is 65～66%; Ferro-boron (BFe), the content of B are 17～19% and technically pure iron, electrolytic copper, industrial silicon, adopt the method for vacuum metling to prepare mother alloy.Owing to contain a large amount of oxygen and oxide compound thereof in ferro-niobium (NbFe), ferro-boron (BFe) and the technically pure iron, if the way that in smelting process, does not adopt effective deoxidation measure and necessary deoxidation thing to be mingled with, these inclusiones are present in the alloy with dissolved state or non-dissolved state, they have destroyed non-crystal structure and stoped moving freely of domain wall in the subsequent crystallization processes, will affect greatly the nanometer crystal alloy soft magnetic performance.
Summary of the invention
The objective of the invention is to overcome the weak point of existing amorphous nano-crystalline manufacturing technology, a kind of reduction alloy inclusions content is provided, particularly reduce oxygen or oxide content, improve the manufacture method and the nanometer crystal alloy of amorphous nano peritectic alloy permeability effectively.
Technical scheme of the present invention is: a kind of manufacture method of super-magnetic conducting nanocrystalline alloy, mother alloy Chemical Composition are Fe72.5～74.5, Cu0.5～1.5, Nb2.5～3.5, Si12.5～14.5, B8～10 (at%); The method that at first adopts vacuum oven to smelt prepares mother alloy, and vacuum degree control is＜0.026 * 10
-6MPa; In the mother alloy smelting process, when temperature reaches 1400～1450 ℃, in vacuum oven, add C and carry out deoxidation, cooling venting after the refining, ingot casting; Secondly mother alloy remelting under the protection of perlite covering slag adds the deoxidation once more of silicon calcium powder reductor simultaneously, skims before the tapping; At last, under argon shield, use single roller chilling to make to quench attitude amorphous nano peritectic alloy band through the nozzle bag; Supporting 25-30PPI Al in the nozzle bag
2O
3Porcelain filter filters molten steel, finally makes SiO
2＜0.026%, B
2O
3＜0.019% (wt%).
A kind of super-magnetic conducting nanocrystalline alloy, the composition of this alloy are Fe72.5～74.5, Cu0.5～1.5, Nb2.5～3.5, Si12.5～14.5, B8～10 (at%); Foreign matter content is SiO
2＜0.026%, B
2O
3＜0.019% (wt%), the magnetic permeability mu of alloy
50Hz(H=5mOe) 〉=60 * 10
4, μ
1kHz(H=5mOe) 〉=20 * 10
4
Adopt nanocrystalline its magnetic permeability mu of the Fe73.5Cu1Nb3Si13.5B9 of general technology production
50Hz(H=5mOe) be 20～40 * 10
4The optimum treatment process of the super-magnetic conducting rate nanometer crystal alloy of manufacturing of the present invention is 545～550 ℃ * 1h under the vacuum state, and it is cold to handle the back stove, and until the air cooling of coming out of the stove below 300 ℃, the iron core permeability is brought up to μ
50Hz(H=5mOe) 〉=60 * 10
4, μ
1kHz(H=5mOe) 〉=20 * 10
4, be higher than the performance of Finemet serial nano peritectic alloy, be a kind of super-magnetic conducting nanocrystalline alloy.
Embodiment
The manufacture method of a kind of super-magnetic conducting nanocrystalline alloy provided by the invention, mother alloy Chemical Composition are Fe72.5～74.5, Cu0.5～1.5, Nb2.5～3.5, Si12.5～14.5, B8～10 (at%).The method that at first adopts vacuum oven to smelt prepares mother alloy, and vacuum degree control is＜0.026 * 10
-6MPa.In the mother alloy smelting process, when temperature reaches 1400～1450 ℃, in vacuum oven, add C and carry out deoxidation, cooling venting after the refining, ingot casting; Secondly mother alloy remelting under the protection of perlite covering slag adds the deoxidation once more of silicon calcium powder reductor simultaneously, prevents to increase oxygen or oxide content in the alloy material, skims before the tapping; At last, under argon shield, use single roller chilling to make to quench attitude amorphous nano peritectic alloy band through the nozzle bag; For impurity thing content, particularly oxygen or the oxide content in the strictness control alloy, supporting 25-30PPI Al in the nozzle bag
2O
3Porcelain filter filters molten steel, finally makes SiO
2＜0.026%, B
2O
3＜0.019% (wt%).
Embodiment 1
The chemical ingredients of mother alloy is Fe73.1Cu1.0Nb3.1Si13.6B9.2 (at%); The method that at first adopts vacuum oven to smelt prepares mother alloy, vacuum tightness 0.020 * 10
-6MPa when temperature reaches 1400 ℃, adds the C deoxidation of 0.1% (wt%), cooling venting after the refining, ingot casting.Secondly mother alloy remelting under the protection of perlite covering slag adds reductor deoxidations once more such as silicon calcium powder simultaneously, skims before the tapping.At last, under argon shield, through 25-30PPI Al
2O
3Porcelain filter filters molten steel, uses single roller chilling to make to quench attitude amorphous nano peritectic alloy band.System bandwidth 40mm, thickness 30 μ m, coiling magnetic core specification 25/30 * 40mm.545～550 ℃ * 1h handles under the employing optimum treatment process vacuum state, and it is cold until the air cooling of coming out of the stove below 300 ℃ to handle the back stove, and the obtained magnetic core permeability is μ
50Hz(H=5mOe)=64 * 10
4, μ
1kHz(H=5mOe)=24.5 * 10
4Analysis obtains SiO
2=0.021%, B
2O
3=0.015% (wt%).
Embodiment 2
The chemical ingredients of mother alloy is Fe73.3Cu0.9Nb3.2Si13.7B8.9 (at%); Vacuum oven, vacuum tightness 0.018 * 10 are adopted in the smelting of mother alloy
-6MPa when temperature reaches 1430 ℃, adds the C deoxidation of 0.1% (wt%), and ingot is cast in the cooling venting after the refining.Secondly mother alloy remelting under the protection of perlite covering slag adds reductor deoxidations once more such as silicon calcium powder simultaneously, skims before the tapping.At last, under argon shield, through 25-30PPI Al
2O
3Porcelain filter filters molten steel, uses single roller chilling to make to quench attitude amorphous nano peritectic alloy band.System bandwidth 25mm, thickness 30 μ m, coiling magnetic core specification 25/30 * 25mm, 545～550 ℃ * 1h handles under the employing optimum treatment process vacuum state, and it is cold until the air cooling of coming out of the stove below 300 ℃ to handle the back stove, and recording the obtained magnetic core permeability is μ
50Hz(H=5mOe)=62 * 10
4, μ
1kHz(H=5mOe)=22 * 10
4SiO after testing
2=0.024%, B
2O
3=0.018% (wt%).
Embodiment 3
The chemical ingredients of mother alloy is Fe73.4Cu1.2Nb3.0Si13.4B9.0, (at%); Vacuum oven, vacuum tightness 0.011 * 10 are adopted in the smelting of mother alloy
-6MPa when temperature reaches 1430 ℃, adds the C deoxidation of 0.1% (wt%), cooling venting after the refining, ingot casting.Remelting under the protection of perlite covering slag adds the silicon calcium powder reductor simultaneously and carries out the secondary deoxidation, skims before the tapping.At last, under argon shield, through 25-30PPI Al
2O
3Porcelain filter filters molten steel, uses single roller chilling to make to quench attitude amorphous nano peritectic alloy band.System bandwidth 10mm, thickness 30 μ m, volume core specification 16/21 * 10mm, 545～550 ℃ * 1h handles under the employing optimum treatment process vacuum state, and it is cold until the air cooling of coming out of the stove below 300 ℃ to handle the back stove, and recording the obtained magnetic core permeability is μ
50Hz(H=5mOe)=65 * 10
4, μ
1kHz(H=5mOe)=27 * 10
4SiO after testing
2=0.022%, B
2O
3=0.017% (wt%).
Example 4
The chemical ingredients of mother alloy is Fe73.2Cu0.95Nb3.15Si13.6B9.1; Vacuum oven, vacuum tightness 0.011 * 10 are adopted in the smelting of mother alloy
-6MPa when temperature reaches 1450 ℃, adds the C deoxidation of 0.1% (wt%), cooling venting after the refining, ingot casting.Remelting adds the silicon calcium powder reductor simultaneously and carries out the secondary deoxidation under perlite covering slag protection, skims before the tapping.At last, under argon shield, through 25-30PPI Al
2O
3Porcelain filter filters molten steel, uses single roller chilling to make to quench attitude amorphous nano peritectic alloy band.System bandwidth 15mm, the amorphous ribbon of thickness 31 μ m, volume core specification 25/30 * 15mm, 545～550 ℃ * 1h handles under the employing optimum treatment process vacuum state, and it is cold until the air cooling of coming out of the stove below 300 ℃ to handle the back stove, and recording the obtained magnetic core permeability is μ
50Hz(H=5mOe)=60.15 * 10
4, μ
1kHz(H=5mOe)=20.4 * 10
4Analysis records SiO
2=0.020%, B
2O
3=0.016% (wt%).
Example 5
The chemical ingredients of mother alloy is Fe73.18Cu0.92Nb3.2Si13.7B9; Vacuum oven, vacuum tightness 0.011 * 10 are adopted in the smelting of mother alloy
-6MPa when temperature reaches 1450 ℃, adds the C deoxidation of 0.1% (wt%), cooling venting after the refining, ingot casting.Add the deoxidation of silicon calcium powder reductor in the mother alloy reflow process, and, prevent to increase oxygen or oxide content, skim before the tapping at the surface coverage perlite.At last, under argon shield, through 25-30PPI Al
2O
3Porcelain filter filters molten steel, uses single roller chilling to make to quench attitude amorphous nano peritectic alloy band.System bandwidth 8mm, the amorphous ribbon of thickness 32 μ m, volume core specification 14/19 * 8mm, 545～550 ℃ * 1h handles under the employing optimum treatment process vacuum state, and it is cold until the air cooling of coming out of the stove below 300 ℃ to handle the back stove, and recording the obtained magnetic core permeability is μ
50Hz(H=5mOe)=62.02 * 10
4, μ
1kHz(H=5mOe)=22.9 * 10
4Record SiO
2=0.019%, B
2O
3=0.015% (wt%).
Comparative example
Fe73.69Cu0.91Nb3.0Si13.2B9.2 prepares the amorphous nano-crystalline alloy strip steel rolled stock according to general technology, wherein analyzes SiO
2=0.0506%, B
2O
3=0.030% (wt%), system bandwidth 10mm, the amorphous ribbon of thickness 32 μ m, volume core specification 16/21 * 10mm, after the thermal treatment identical with embodiment 5, its permeability is μ
50Hz(H=5mOe)=24.8 * 10
4, μ
1kHz(H=5mOe)=7 * 10
4
Claims (2)
1. the manufacture method of a super-magnetic conducting amorphous nano peritectic alloy band is characterized in that the mother alloy Chemical Composition is Fe72.5～74.5, Cu0.5～1.5, Nb2.5～3.5, Si12.5～14.5, B8～10 (at%); The method that at first adopts vacuum oven to smelt prepares mother alloy, and vacuum degree control is＜0.026 * 10
-6MPa; In the mother alloy smelting process, when temperature reaches 1400～1450 ℃, in vacuum oven, add C and carry out deoxidation, cooling venting after the refining, ingot casting; Secondly mother alloy remelting under the protection of perlite covering slag adds the deoxidation once more of silicon calcium powder reductor simultaneously, skims before the tapping; At last, under argon shield, use single roller chilling to make to quench attitude amorphous nano peritectic alloy band through the nozzle bag; Supporting 25-30PPI Al in the nozzle bag
2O
3Porcelain filter filters molten steel, finally makes SiO
2＜0.026%, B
2O
3＜0.019% (wt%).
2. the super-magnetic conducting amorphous nano peritectic alloy band of the described method preparation of a claim 1, the composition that it is characterized in that this alloy band is Fe72.5～74.5, Cu0.5～1.5, Nb2.5～3.5, Si12.5～14.5, B8～10 (at%); Foreign matter content is SiO
2＜0.026%, B
2O
3＜0.019% (wt%); When H=5mOe, the magnetic permeability mu of alloy
50Hz〉=60 * 10
4, μ
1kHz〉=20 * 10
4
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| CN102080165B (en) * | 2009-11-30 | 2013-04-10 | 比亚迪股份有限公司 | Method for preparing zirconium-based amorphous alloy |
| CN102181808B (en) * | 2011-04-08 | 2013-01-02 | 郭莉 | Method for producing high-permeability amorphous nanocrystalline alloy |
| CN103060691A (en) * | 2013-01-14 | 2013-04-24 | 青岛云路新能源科技有限公司 | Iron-based nanocrystalline ribbon and preparation method thereof |
| CN103526104B (en) * | 2013-10-12 | 2015-06-24 | 太原钢铁(集团)有限公司 | Special intermediate alloy for iron base amorphous nanocrystalline alloy and smelting method thereof |
| CN104878326A (en) * | 2015-06-03 | 2015-09-02 | 上海理工大学 | Soft-magnet-based amorphous alloy product and preparation method thereof |
| CN105047348B (en) * | 2015-08-03 | 2017-08-25 | 江苏奥玛德新材料科技有限公司 | A kind of current transformer core of amorphous and nanocrystalline soft magnetic alloy and preparation method thereof |
| CN109628696B (en) * | 2019-01-31 | 2021-04-27 | 武汉钢铁有限公司 | Vacuum melting process of aluminum-free low-oxygen steel |
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