CN100465323C - Nano crystal composite permanent-magnet alloy and its preparation method - Google Patents
Nano crystal composite permanent-magnet alloy and its preparation method Download PDFInfo
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- CN100465323C CN100465323C CNB2007100437761A CN200710043776A CN100465323C CN 100465323 C CN100465323 C CN 100465323C CN B2007100437761 A CNB2007100437761 A CN B2007100437761A CN 200710043776 A CN200710043776 A CN 200710043776A CN 100465323 C CN100465323 C CN 100465323C
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Abstract
The invention relates to a nano-crystal composite permanent magnetic alloys and the method for preparing the same. The nano-crystal composite permanent magnetic alloys comprise( atom percent ): Nd7-11%, Fe70-82%, Co2-8%, Zr1-4%, Ga0.1- 1.5%, B4-8%. The method comprises following steps: (1) batching according to alloy formulation above, fusing by using vacuum non-consumable electrode arc furnace under argon gas protection, fusing the master alloy turnover and repeatedly; (2) getting the melt-spun ribbons of nano-crystal composite permanent magnetic alloys in vacuum induction extracting cage; (3) placing the alloy ribbons in a external pulsed magnetic field with frequency being 0.02-0.05Hz, magnetic field 1-6T, vacuum annealing at 200-400 Deg. C. The invention is characterized in that the coercivity and remanence of nano-crystal composite permanent magnetic alloys are increased after annealing in external pulsed magnetic field, and the maximum magnetic energy product of alloy is increased by 24.8% compared to that of in conventional process.
Description
Technical field
The present invention relates to a kind of nano-crystal composite permanent magnetic alloy and preparation method thereof, belong to magneticsubstance and technology field.
Background technology
Nano-crystal composite permanent magnetic alloy is a kind of novel permanent magnet material, and it is by soft magnetism and Hard Magnetic compound permanent magnet material of forming in nanometer range.Owing to having the high and tempting commercial promise of low, the theoretical magnetic energy product of content of rare earth, this material causes numerous investigators' very big concern.
Since 1989, human melt-quenching methods such as R.Coehoon were at first developed Nd
4.5Fe
78B
18.5Since the nano composite permanent magnetic material, the investigator has been developed mechanical alloying method in succession both at home and abroad, and magnetron sputtering method and HDDR method are developed nano composite permanent magnetic material.Because melt-quenching method, easy to operate, technology is simple, helps suitability for industrialized production, thereby becomes most important a kind of preparation method.
In order to improve the comprehensive magnetic property of nanocrystalline composite permanent-magnet material, the investigator has carried out the optimization research of permanent magnet material magnetic property from elemental composition interpolation and preparation technology two aspects respectively.The do time spent of research Al such as Pan Shuming in nano composite permanent magnetic material finds that Al substitutes Fe and makes J
2The in-plane anisotropy of brilliant position reduces, and has improved the coercive force of alloy.The Kanekiyo H of Japan is at research Nd
5Fe
76.5B
18.5During alloy, unite add Co and Ga element after, make grain refining to 20～30nm, the over-all properties of alloy improves.
After utilizing melt-quenching method to obtain the fast quenching thin strap of nano composite permanent magnetic alloy, the crystallization of annealing is handled obtaining the crystal grain of nano-scale, thereby makes the soft or hard magnetic of alloy produce exchange-coupling interaction between mutually, improves the magnetic property of alloy.Except carrying out traditional conventional annealing, recent years several novel crystallization treatment process also appearred, as flash annealing, steady magnetic field annealing method.People such as Gao Yandong are at research Nd
8Fe
86B
6During the nano composite permanent magnetic alloy, find the raising along with rate of heating, the grain-size of alloy is reduced to 20nm by 50nm, thereby makes the magnetic energy product of alloy be improved.People such as the Yang Zhong cross board at the rear of an ancient carriage of Korea S are to Nd
4Fe
73.5Co
3(Hf
1-xGa
x) B
18.5In the crystallization process of fast quenched alloy, apply the steady magnetic field that adds of 0.5T, made grain refining 20%, remanence ratic has improved 30%, but because the strength ratio of steady magnetic field is lower, manufacturing cost and maintenance cost are very high, thereby the investigator fails to study under higher magneticstrength.In addition, methods such as high pressure annealing and laser annealing have also been developed.
By above introduction, can find, utilize conventional annealing process to be difficult to continue to improve the magnetic property of alloy, some other novel annealing process of while, because the cost height, complex process also is difficult to promote the use of in the suitability for industrialized production, so it is low to press for a kind of cost now, method for annealing simple to operate.For this reason, after we utilize melt-quenching method to make the fast quenching thin strap of alloy, developed utilize high strength, the pulsed magnetic field method is annealed cheaply, has further improved the comprehensive magnetic property of alloy.
Summary of the invention
The purpose of this invention is to provide a kind of nano-crystal composite permanent magnetic alloy and preparation method thereof.
The objective of the invention is to realize by following technique means.
A kind of nano-crystal composite permanent magnetic alloy is characterized in that the composition of this alloy, counts with atomic percentage conc:
Nd 7～11％
Fe 70～82％
Co 2～8％
Zr 1～4％
Ga 0.1～1.5％
B 4～8％。
The preparation method of above-mentioned nano-crystal composite permanent magnetic alloy is characterized in that this method has following processing step:
A. with technical pure raw metal Nd, Fe, Co, Zr, Ga and FeB alloy; count with atomic percentage conc by the nano-crystal composite permanent magnetic alloy composition: Nd7～11%, Fe70～82%, Co2～8%, Zr1～4%, Ga0.1～1.5%, B4～8% are prepared burden; carry out melting with vacuum non-consumable arc furnace under argon shield then, the melting current density is 150～250A/cm
2, alloy is stood up melting 4～7 times, obtain alloy button ingot;
B. melted button ingot is broken for the dead small of 3～6g, in the quartz crucible of packing into, the nozzle diameter of quartz crucible is 0.7～1mm, gets rid of at vacuum induction and makes the fast quenching alloy thin band in the band machine, and the linear velocity of its running roller is 10～18m/s;
C. with above-mentioned fast quenching alloy thin band at 200～400 ℃, vacuum tightness is 3～5 * 10
-3Under the Pa condition, carry out the applying pulse magnetic-field annealing, annealing time is 10～30min, and the applying pulse field frequency is 0.02～0.05Hz, and magneticstrength is 1～6T.
Used raw material is pure metal Nd, Fe, Co, Zr, Ga and FeB master alloy among the present invention.
Alloy of the present invention has the microstructure (about 20～50nm) and the excellent comprehensive magnetic property of nanoscale.The present invention carries out pulsed magnetic field annealing to nano-crystal composite permanent magnetic alloy, thereby the coercive force of nano-crystal composite permanent magnetic alloy and remanent magnetism are improved, and finally makes the maximum magnetic energy product of alloy be improved significantly.Fig. 1 is nano-crystal composite permanent magnetic alloy of the present invention demagnetizing curve figure at room temperature, has compared conventional annealing and pulsed magnetic field annealed alloy magnetic property among the figure.As can be seen, alloy of the present invention is 531kA/m through the coercive force that has behind the conventional annealing, and remanent magnetism is 0.92T, and maximum magnetic energy product is 105kJ/m
3, and the coercive force of the nano-crystal composite permanent magnetic alloy by the applying pulse magnetic-field annealing is 582kA/m, and remanent magnetism is 0.98T, maximum magnetic energy product is 131kJ/m
3, remanent magnetism and coercive force all are improved significantly, and the maximum magnetic energy product increase rate of alloy reaches 24.8%.
Characteristics of the present invention are: 1) special alloy formula; 2) adopt technology with low cost, easy to operate, that pulsed magnetic field that intensity is high carries out annealed, obtain having the nano-crystal composite permanent magnetic alloy of excellent comprehensive magnetic property; 3) by nano-crystal composite permanent magnetic alloy being heated near the alloy Curie temperature, applying pulsed magnetic field simultaneously anneals, the soft magnetism of alloy is arranged in parallel with the magnetic moment of Hard Magnetic phase is consistent mutually, improve the coercive force and the remanent magnetism of alloy, thereby further improved the maximum magnetic energy product of nano-crystal composite permanent magnetic alloy.Have the nano-crystal composite permanent magnetic alloy of excellent comprehensive magnetic property, can extensively get rid of in the magnetic device in fields such as automobile, communication, medical facilities, Micro Electro Mechanical System, computer equipment.This nano-crystal composite permanent magnetic alloy is because low cost of manufacture, and comprehensive magnetic property height will quicken its industrialized production and applied.
Description of drawings
Fig. 1 is nano-crystal composite permanent magnetic alloy of the present invention demagnetizing curve figure at room temperature.
Embodiment
After now embodiments of the invention specifically being described in.
Embodiment 1
The composition of the nano-crystal composite permanent magnetic alloy of present embodiment (atomic percentage conc) is: Nd 8.5%, Fe 77%, Co 5%, Zr 2.7%, Ga 0.6%, B 6.2%.Preparation process is as follows with step: technical pure raw metal Nd, Fe, Co, Zr, Ga and FeB alloy are become assignment system 15 grams by the nano-crystal composite permanent magnetic alloy of present embodiment; carry out melting with vacuum non-consumable arc furnace under argon shield then, the melting current density is 200A/cm
2, molten alloy is stood up melting 5 times; Adopt melt-quenching method to make the fast quenching thin strap of alloy, the running roller linear velocity is 15m/s; At 300 ℃, vacuum tightness is 3 * 10 with above-mentioned fast quenching thin strap
-3Under the Pa condition, carry out pulsed magnetic field annealing, annealing time is 18min, and the applying pulse field frequency is 0.05Hz, and magneticstrength is 5T, makes nano-crystal composite permanent magnetic alloy of the present invention at last.
Prepared nano-crystal composite permanent magnetic alloy in the present embodiment is through conventional annealing and two kinds of treatment process of applying pulse magnetic-field annealing.At room temperature, the nano-crystal composite permanent magnetic alloy that two kinds of methods are prepared carries out the magnetic property measurement, and its demagnetizing curve is seen accompanying drawing 1.After can finding out that from accompanying drawing nano-crystal composite permanent magnetic alloy of the present invention is through the applying pulse magnetic-field annealing, its coercive force and remanent magnetism 531kA/m and the 0.92T during from conventional annealing brings up to 582kA/m and 0.98T, thereby makes the 105kJ/m of the maximum magnetic energy product of alloy by conventional annealing
3131kJ/m when bringing up to pulsed magnetic field annealing
3, increase rate is up to 24.8%.
Embodiment 2
The composition of the nano-crystal composite permanent magnetic alloy of present embodiment (atomic percentage conc) is: Nd 9.5%, Fe 75.8%, Co 5%, Zr 3%, Ga 0.2%, B 6.5%.Preparation process is as follows with step: technical pure raw metal Nd, Fe, Co, Zr, Ga and FeB alloy are become assignment system 20 grams by the nano-crystal composite permanent magnetic alloy of present embodiment; carry out melting with vacuum non-consumable arc furnace under argon shield then, the melting current density is 220A/cm
2, molten alloy is stood up melting 4 times; Adopt melt-quenching method to make the fast quenching thin strap of alloy, the running roller linear velocity is 12m/s; At 320 ℃, vacuum tightness is 5 * 10 with above-mentioned fast quenching thin strap
-3Under the Pa condition, carry out pulsed magnetic field annealing, annealing time is 23 minutes, and the applying pulse field frequency is 0.05Hz, and magneticstrength is 3T, makes nano-crystal composite permanent magnetic alloy of the present invention at last.
Prepared nano-crystal composite permanent magnetic alloy in the present embodiment is through conventional annealing and two kinds of treatment process of applying pulse magnetic-field annealing.At room temperature, nano-crystal composite permanent magnetic alloy to two kinds of method preparations carries out the magnetic property measurement, after can learning that nano-crystal composite permanent magnetic alloy of the present invention is through the applying pulse magnetic-field annealing, its coercive force and remanent magnetism 625kA/m and the 0.87T during from conventional annealing brings up to 669kA/m and 0.92T, thereby makes the 116kJ/m of the maximum magnetic energy product of alloy by conventional annealing
3134kJ/m when bringing up to pulsed magnetic field annealing
3, increase rate is up to 15.5%.
Claims (1)
1. the preparation method of a nano-crystal composite permanent magnetic alloy is characterized in that this method has following processing step:
A. with technical pure raw metal Nd, Fe, Co, Zr, Ga and FeB alloy; count with atomic percentage conc by the nano-crystal composite permanent magnetic alloy composition: Nd7～11%, Fe70～82%, Co2～8%, Zr1～4%, Ga0.1～1.5%, B4～8% are prepared burden; carry out melting with vacuum non-consumable arc furnace under argon shield then, the melting current density is 150～250A/cm
2, alloy is stood up melting 4～7 times, obtain alloy button ingot;
B. melted button ingot is broken for the dead small of 3～6g, in the quartz crucible of packing into, the nozzle diameter of quartz crucible is 0.7～1mm, gets rid of at vacuum induction and makes the fast quenching alloy thin band in the band machine, and the linear velocity of its running roller is 10～18m/s;
C. with above-mentioned fast quenching alloy thin band at 200～400 ℃, vacuum tightness is 3～5 * 10
-3Under the pa condition, carry out the applying pulse magnetic-field annealing, annealing time is 10～30min, and the applying pulse field frequency is 0.02～0.05Hz, and magneticstrength is 1～6T.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101908396A (en) * | 2010-06-29 | 2010-12-08 | 上海大学 | Nanocrystal composite NdFeB permanent magnet alloy with higher temperature stability and preparation method thereof |
| CN101894644A (en) * | 2010-06-29 | 2010-11-24 | 上海大学 | Anisotropic nanocrystalline compound NdFeB permanent magnet alloy and preparation method thereof |
| CN101894645A (en) * | 2010-06-29 | 2010-11-24 | 上海大学 | Nano-crystal composite NdFeB permanent magnet alloy and heating processing technology for improving magnetic performance thereof |
| CN102568729B (en) * | 2012-01-10 | 2015-04-15 | 福州大学 | Method for preparing bulk composite nanocrystalline rare earth permanent magnetic material |
| CN102703794B (en) * | 2012-06-20 | 2014-04-30 | 江苏美特林科特殊合金有限公司 | Method of vacuum induction argon bottom blowing for smelting high-performance magnetic material |
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| CN1376301A (en) * | 1999-02-01 | 2002-10-23 | 马格内昆茨国际公司 | Rare earth permanent magnet and method for making same |
| CN1411006A (en) * | 1996-08-07 | 2003-04-16 | 户田工业株式会社 | Rare earth bonded magnet and rare earth iron boron type magnet alloy |
| CN1440317A (en) * | 2000-10-06 | 2003-09-03 | 株式会社三德 | Process for producing, through strip casting, raw alloy for nanocomposite type permanent magnet |
| JP2005290398A (en) * | 2004-03-31 | 2005-10-20 | Neomax Co Ltd | Rare-earth magnet powder, compound using it, and bond magnet using it |
| JP2007005786A (en) * | 2006-05-31 | 2007-01-11 | Aichi Steel Works Ltd | Rare-earth magnet powder and method for manufacturing same |
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2007
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1411006A (en) * | 1996-08-07 | 2003-04-16 | 户田工业株式会社 | Rare earth bonded magnet and rare earth iron boron type magnet alloy |
| CN1376301A (en) * | 1999-02-01 | 2002-10-23 | 马格内昆茨国际公司 | Rare earth permanent magnet and method for making same |
| CN1440317A (en) * | 2000-10-06 | 2003-09-03 | 株式会社三德 | Process for producing, through strip casting, raw alloy for nanocomposite type permanent magnet |
| JP2005290398A (en) * | 2004-03-31 | 2005-10-20 | Neomax Co Ltd | Rare-earth magnet powder, compound using it, and bond magnet using it |
| JP2007005786A (en) * | 2006-05-31 | 2007-01-11 | Aichi Steel Works Ltd | Rare-earth magnet powder and method for manufacturing same |
Non-Patent Citations (2)
| Title |
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| 纳米晶双相Nd10.5Fe78-xCo5ZrxB6.5合金磁性能与结构的研究. 谭晓华，徐晖，戚楠楠，倪建森，候雪玲，董远达.稀有金属材料与工程，第34卷第12期. 2005 |
| 纳米晶双相Nd10.5Fe78-xCo5ZrxB6.5合金磁性能与结构的研究. 谭晓华，徐晖，戚楠楠，倪建森，候雪玲，董远达.稀有金属材料与工程，第34卷第12期. 2005 * |
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