CN100435244C - Nano crystal soft magnetic alloy superthin belt and mfg method thereof - Google Patents
Nano crystal soft magnetic alloy superthin belt and mfg method thereof Download PDFInfo
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- CN100435244C CN100435244C CNB031162797A CN03116279A CN100435244C CN 100435244 C CN100435244 C CN 100435244C CN B031162797 A CNB031162797 A CN B031162797A CN 03116279 A CN03116279 A CN 03116279A CN 100435244 C CN100435244 C CN 100435244C
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Abstract
The present invention relates to a novel nanometer crystal Fe-Zr-Nb-Si-Al-Cu, namely a soft magnetic alloy superthin belt and a preparation process thereof. Mother alloy is smelted by a vacuum medium frequency induction furnace, an amorphous belt is made by using a single roll cold emergency device, and finally, magnetic heat treatment is carried out to the amorphous belt, so that a needed product is made. The alloy superthin belt of the present invention has good soft magnetic property, and the production cost is also lower. An iron core made by the superthin belt of the present invention has greatly improved magnetic performance, and has wide application in national defence and civil industry.
Description
Technical field
The invention belongs to the metal material technical field, brilliant ultra-thin band of Fe-Zr-Nb-Si-Al-Cu magnetically soft alloy of particularly a kind of novel nano and preparation technology thereof.
Background technology
Its typical composition of traditional nano-crystal soft magnetic alloy is Fe
73.5Cu
1Nb
3Si
13.5B
9, the trade mark is Finemet.Though the Finemet alloy has good soft magnet performance, owing to contain expensive Nb in the alloy, increased the cost of material, and the viscosity of molten steel is big, Nb content is high more, and the flowability of molten alloy is poor more, and original amorphous ribbon is difficult for preparation.
Summary of the invention
The object of the present invention is to provide a kind of ultra-thin band of nano-crystal soft magnetic alloy and preparation technology thereof with good soft magnet performance and lower production cost.
The ultra-thin band of nano-crystal soft magnetic alloy that the present invention proposes makes amorphous ribbon by foundry alloy through pocket builder, again through magnetic-field heat treatment, carries out nanocrystalline crystallization and obtains, and wherein, the alloy composition mixture ratio by weight percent is:
Si 0.1----0.2％
Zr 6.0----8.0％
Nb 4.0----6.0％，
Al 0.1----1％
Cu 1.0----1.5％
All the other are Fe.
According to alloy composition and proterties, claim that alloy band of the present invention is nano-crystalline Fe-ultra-thin band of Zr-Nb-Si-Al-Cu magnetically soft alloy.Its thickness is generally 10-30 μ m.
Among the present invention, the adding of Zr element can increase crystallized temperature, but too much can make amorphous master alloy be easy to oxidation.The adding of aluminium element can make the resistivity of alloy rise the saturation magnetic field intensity decreases.The increase of Nb composition, can suppress grain growth, the average grain size D of bcc Fe-Si phase is reduced, Cu and Nb to unite increase very effective for obtaining uniform and hyperfine crystal grain, increased crystallized temperature, so the variation of crystallite dimension changes with crystallization temperature relevant.The minimizing of crystallite dimension is extremely important for the increase of the magnetic permeability of nanocrystalline material.The increase of Cu composition reduces the average grain size D of bcc Fe-Si phase, and Cu is during greater than 1at%, and little tissue is tending towards homogenizing, and average-size 10nm, Cu have increased the one-tenth nuclearity of bccFe-Si phase crystal grain.
Ultra-thin band preparation technology of the present invention comprises master alloy melting, sprays amorphous ribbon, isothermal heat treatment, and concrete steps are as follows:
Master alloy melting: the weight proportion by the alloy band takes by weighing each component, Fe, Zr, Nb ingot is put into intermediate frequency furnace smelt, and is melted to 900--1200 ℃, adds all the other intensified elements, stirs, and is generally 20-40 minute, and natural cooling makes foundry alloy then;
Spray amorphous ribbon: utilize the cold quenching apparatus fusion of single roller foundry alloy, the Ar gas shiled, pressure is 450-600Pa, copper roller linear velocity is 40-70m/s, and the quartz nozzle width is 25-40mm, is injected into amorphous ribbon, amorphous ribbon thickness is generally 10-20 μ m, and width is 15-30mm;
Isothermal heat treatment: under vacuum condition, carry out magnetic-field heat treatment,, promptly get required nano-crystalline Fe-ultra-thin band of Zr-Nb-Si-Al-Cu magnetically soft alloy 400-600 ℃ of insulation 30-60 minute.
The present invention has adopted single roller chilling technique.Single roller chilling technique is that molten metal liquid is injected on the good roll surface of heat conduction, forms liquid thin layer, dispels the heat rapidly by the heat conduction of roll surface and this thin layer, can produce near 10
6K/S or higher cooling rate.High like this cooling rate, it mainly acts on is motion and the diffusion that suppresses atom in the material, makes atom can not occupy the balance lattice point, and melt obtained bigger degree of subcooling (a few Baidu) before forming a large amount of solid phase particles, and then the institutional framework of change material, form non-equilibrium crystal.Fig. 1 has provided and has utilized single roller chilling technique to prepare the indication device of the ultra-thin band of amorphous state.The alloy material that is used for preparing the ultra-thin band of amorphous state is placed on crucible, is air inlet on the crucible, after alloy melting is good, protective gas is pressed into crucible, makes alloy liquid be ejected into the surface of roller.Because the roller high speed rotating, high temperature melt alloy is run into to solidify immediately on the roll surface and be attached to the surface and is gone up rotation, outwards flies to because centrifugal action makes the strip that has solidified break away from roll surface.Can regulate the width and the thickness of strip by the rotating speed of control injection liquid alloy speed and roller.
Nano-crystalline Fe of the present invention-ultra-thin band of Zr-Nb-Si-Al-Cu magnetically soft alloy has been broken through the restriction of original nano-crystal soft magnetic alloy band on alloying component, developed new alloy system, reduced the viscosity of molten steel, increase the flowability of molten alloy, and reduced the production cost of material to a great extent.Because the variation of composition causes the preparation technology of material and the performance of material softer magnetic alloy band that variation has taken place.For range of application and the replacement Finemet magnetically soft alloy that enlarges nano-crystalline Fe-Zr-Nb-Si-Al-Cu magnetically soft alloy lays a solid foundation.
The nanocrystalline ultra-thin band that is made by the present invention has good physical property, by the iron core that it is made, and its saturation flux density height (Bs is 1.6-1.7T), initial permeability height (μ
i＞3 * 10
4), iron loss is lower, can be widely used in national defense industry and civilian product, as: high accuracy inductor, high frequency switch power magnetic core, power transformer, pulse transformer, stored-program control exchange power supply, communication (ISDN, ADSL), inverter type welder, electron rectifier, various power transformer, pulse transformer or the like.Preparation technology of the present invention can be used for developing Fe-M (Zr, Nb, V, Mo, W)-Cu-(B, Si, Al) magnetically soft alloy, thereby has wide research and market application foreground.
Description of drawings
Fig. 1 is single roller quenching apparatus schematic diagram.
Number in the figure: 1 is crucible, and 2 is motlten metal, and 3 is nozzle, and 4 are liquid stream, and 5 is strip, and 6 is chill roll.
Embodiment
Embodiment: the preparation of nano-crystalline Fe-ultra-thin band of Zr-Nb-Si-Al-Cu magnetically soft alloy.The weight proportion of each component takes off states group:
| Si | Zr | Nb | Al | B | Cu | Fe | |
| No. 1 | 0.15 | 6.0 | 6.0 | 0.6 | 1.5 | 1.0 | 84.75 |
| No. 2 | 2.0 | 7.5 | 4.0 | 0.1 | 1.8 | 1.2 | 83.4 |
| No. 3 | 0.1 | 6.0 | 5.0 | 1 | 1 | 1.5 | 85.4 |
The preparation technology of the ultra-thin band of magnetically soft alloy as previously mentioned.During vacuum metling, vacuum degree is 6 * 10
-3Pa, smelting temperature is 1000 ℃, is prepared into foundry alloy.In the amorphous ribbon preparation, adopt single roller quenching apparatus, as shown in Figure 1.Protective gas is Ar, and pressure is 500Pa, and the roller linear velocity is 40～70m/s, and the nanocrystalline ultra-thin tape thickness that obtains is 14 microns, and is wide 20 millimeters.When annealing temperature was 540 ℃, nanocrystalline content was 63.2% in the ultra-thin band, and annealing temperature is in the time of 600 ℃, and nanocrystalline content is 73.9%.Its magnetic property is as follows:
Saturation flux density: B
30=1.4T; B
10=1.3T, B
sCan reach 1.7T
Magnetic permeability: μ
i=3.8 * 10
4
Coercive force: H
c=0.12Oe=9.6A/m
Iron loss: P
10/400=1.9097w/kg; P
2/100K=169.97w/kg
Claims (2)
1, the ultra-thin band of a kind of nano-crystal soft magnetic alloy makes amorphous ribbon by foundry alloy through pocket builder, carries out nanocrystalline crystallization and obtains, and it is characterized in that the alloy composition mixture ratio by weight percent is:
Si 0.1----0.2％
Zr 6.0----8.0％
Nb 4.0----6.0％，
Al 0.1----1％
B 1----2％
Cu 1.0----1.5％
All the other are Fe.
2, the preparation method of the ultra-thin band of a kind of nano-crystal soft magnetic alloy as claimed in claim 1 is characterized in that comprising master alloy melting, sprays amorphous ribbon, isothermal heat treatment, and concrete steps are as follows:
Master alloy melting: the weight proportion by the alloy band takes by weighing each component, Fe, Zr, Nb ingot is put into intermediate frequency furnace smelt, and is melted to 900--1200 ℃, adds all the other intensified elements, stirs 20-40 minute, and natural cooling makes foundry alloy then;
Spray amorphous ribbon: utilize single cold roller quenching apparatus fusion foundry alloy, the Ar gas shiled, pressure is 450-600Pa, and copper roller linear velocity is 40-70m/s, and the quartz nozzle width is 25-40mm, is injected into amorphous ribbon;
Isothermal heat treatment: under vacuum condition, carry out magnetic-field heat treatment,, promptly get required nano-crystalline Fe-ultra-thin band of Zr-Nb-Si-Al-Cu magnetically soft alloy in 400-600 ℃ of insulation 30-60 minute.
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| CN100435244C true CN100435244C (en) | 2008-11-19 |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365746C (en) * | 2004-07-29 | 2008-01-30 | 同济大学 | Block non crystal nano crystal double phase composite soft magnetic alloy |
| CN100348769C (en) * | 2004-09-23 | 2007-11-14 | 同济大学 | Preparation for block amorphous nanometer crystal double-phase composite soft magnetic alloy |
| JP5445888B2 (en) * | 2005-09-16 | 2014-03-19 | 日立金属株式会社 | Soft magnetic alloy, method for producing the same, and magnetic component |
| CN100445410C (en) * | 2005-09-27 | 2008-12-24 | 同济大学 | Nano-crystal soft magnetic alloy material and its production |
| CN100502633C (en) * | 2006-05-26 | 2009-06-17 | 安泰科技股份有限公司 | Composite electromagnetic shielding material and making method |
| CN101717901B (en) * | 2009-12-22 | 2011-07-20 | 上海大学 | Process and device for amorphous thin ribbon heat treatment under the action of pulsed magnetic field |
| CN101853726A (en) * | 2010-05-17 | 2010-10-06 | 南京新康达磁业有限公司 | Soft magnetic material and preparation method thereof |
| CN102129907B (en) * | 2010-12-30 | 2012-05-30 | 上海世路特种金属材料有限公司 | Nanocrystalline soft magnetic alloy iron core with high initial permeability and low remanence and preparation method thereof |
| CN102699335A (en) * | 2012-06-19 | 2012-10-03 | 浙江科达磁电有限公司 | Preparation method of metal powder for nanocrystalline magnetic core |
| CN102689010A (en) * | 2012-06-19 | 2012-09-26 | 浙江科达磁电有限公司 | Metal powder used for preparing nanometer crystal magnetic core |
| CN102728840A (en) * | 2012-06-20 | 2012-10-17 | 浙江科达磁电有限公司 | Method for preparing metal powder of nanocrystalline magnetic cores with magnetic permeability mu of 60 |
| CN102699336B (en) * | 2012-06-20 | 2014-09-03 | 浙江科达磁电有限公司 | Preparation method of metal powder for nanocrystalline magnetic core |
| CN102699320A (en) * | 2012-06-20 | 2012-10-03 | 浙江科达磁电有限公司 | Metal powder for preparing nanocrystalline magnetic core |
| CN109252128A (en) * | 2018-08-23 | 2019-01-22 | 广东思泉新材料股份有限公司 | A kind of nanocrystalline and synthetic graphite adhesion without adhesiver composite material and preparation method |
| CN110125353A (en) * | 2019-05-17 | 2019-08-16 | 山东电亮亮信息科技有限公司 | Large capacity nano-crystalline thin ribbon production system |
| CN112008053B (en) * | 2020-08-27 | 2021-09-17 | 燕山大学 | Preparation device of alloy and current application method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4985089A (en) * | 1987-07-23 | 1991-01-15 | Hitachi Metals, Ltd. | Fe-base soft magnetic alloy powder and magnetic core thereof and method of producing same |
| JPH07278764A (en) * | 1994-04-15 | 1995-10-24 | Hitachi Metals Ltd | Nano-crystal alloy and its production and magnetic core using the same |
| JP2001089833A (en) * | 1999-09-20 | 2001-04-03 | Alps Electric Co Ltd | Soft magnetic alloy for acceleration cavity, method of manufacturing the same, high frequency acceleration cavity and particle accelerator using this cavity |
-
2003
- 2003-04-10 CN CNB031162797A patent/CN100435244C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4985089A (en) * | 1987-07-23 | 1991-01-15 | Hitachi Metals, Ltd. | Fe-base soft magnetic alloy powder and magnetic core thereof and method of producing same |
| JPH07278764A (en) * | 1994-04-15 | 1995-10-24 | Hitachi Metals Ltd | Nano-crystal alloy and its production and magnetic core using the same |
| JP2001089833A (en) * | 1999-09-20 | 2001-04-03 | Alps Electric Co Ltd | Soft magnetic alloy for acceleration cavity, method of manufacturing the same, high frequency acceleration cavity and particle accelerator using this cavity |
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