CN101894644A - Anisotropic nanocrystalline compound NdFeB permanent magnet alloy and preparation method thereof - Google Patents
Anisotropic nanocrystalline compound NdFeB permanent magnet alloy and preparation method thereof Download PDFInfo
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- CN101894644A CN101894644A CN 201010215766 CN201010215766A CN101894644A CN 101894644 A CN101894644 A CN 101894644A CN 201010215766 CN201010215766 CN 201010215766 CN 201010215766 A CN201010215766 A CN 201010215766A CN 101894644 A CN101894644 A CN 101894644A
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Abstract
The invention relates to an anisotropic nanocrystalline compound NdFeB permanent magnet alloy and a preparation method thereof, belonging to the technical field of magnetic materials. The alloy comprises the following components by weight percent: 70-80% of Fe, 7-15% of Nd, 3-8% of Co, 1-5% of Zr and 3-9% of B. The preparation method comprises the following steps: mixing materials according to a proportion, then smelting under the protection of argon, and turning over for 3-6 times during smelting to obtain an alloy fastener ingot; crushing the fastener ingot into small pieces of materials to put in a quartz pipe, and preparing the small pieces of materials into an alloy thin strip in an electric induction vacuum melt spinning furnace; under a constant magnetic field of 8-10T, annealing the roll surface of the thin belt along a direction parallel or vertical to the direction of the magnetic field, heating to 650-800 DEG C under a vacuum condition, preserving the heat for 20-40 min, and then cooling for 30-60 min along with the vacuum melt spinning furnace; and after the constant magnetic field annealing, the magnetic field enables grains to carry out preferred orient along the direction of the additional magnetic field so that the magnetic property of Nd10Fe76Co5Zr3B6 thin strip presents discrepancy in different directions.
Description
Technical field
The present invention relates to a kind of anisotropic nano-composite NdFeB permanent magnetic alloy and preparation method thereof, belong to technical field of magnetic materials.
Background technology
Nanocrystalline composite permanent-magnet material is one of the focus in investigation of materials field in recent years, this permanent magnetic material by soft, Hard Magnetic mutually between by strong exchange-coupling interaction, making its general performance is permanent magnetism.This material has characteristics such as high theoretical maximum magnetic energy product, cost are low, therefore has very big development prospect.
After biphase nanocrystalline composite permanent-magnet material was found, people expected naturally, prepare anisotropic biphase nanocrystalline composite permanent-magnet material and can obtain more excellent magnetism energy undoubtedly.People such as D.Dadon obtained having anisotropic Nd at the direct fast quenching of low roller speed in 1987
2Fe
14The B strip, Nd
2Fe
14It is vertical strip direction that B crystal grain c axle gauge then is orientated, and this is because the directional solidification under thermal gradient.Though can form anisotropy Nd-Fe-B biphase permanent magnetic material in low roller speed, crystal grain is thick to make that the magnetic property of material is very low owing to low roller speed causes.People such as calendar year 2001 Zhang X Y are Nd to composition
3.6Pr
5.4Fe
83Co
3B
5In fast quenching speed is under the 20m/s, directly obtains having anisotropic Nd
2Fe
14B/ α-Fe two-phase strip.J wherein
r=0.74J
s, (BH)
Max=194kJ/m
3Magnetic field treated can significantly improve the magnetic property of material.Simultaneously, magnetic field can also make crystal grain along the growth of externally-applied magnetic field direction preferred orientation, forms texture, and this just provides technical support for preparation Nd-Fe-B biphase nanocrystalline composite anisotropic permanent magnetic material.Ji.Q.G. wait people heat treatment Nd under magnetic field
10Fe
84-xB
6In
x(x=0,1), annealing temperature near Curie point 300 ℃～400 ℃.Magnetic field makes the micro-structural of magnet inside that certain preferred orientation take place, and comprises that crystal grain grows up in a certain direction or rotate.We utilize strong permanent magnetic field to change the crystal grain forming core in the amorphous state permanent-magnet alloy crystallization process and grow up, form and arrangement, obtained the anisotropy composite permanent-magnetic material of grain orientation growth, function admirable, effectively improved the magnetic property of material.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with anisotropic nano-composite NdFeB permanent magnetic alloy of excellent magnetic energy.
The objective of the invention is to realize by following technological means.
A kind of nano-composite NdFeB permanent magnetic alloy is characterized in that the composition of this alloy, counts with atomic percent:
Nd 7～15％
Co 3～8％
Zr 1～5％
B 3～9％
The preparation method of above-mentioned nano-composite NdFeB permanent magnetic alloy is characterized in that this method has following processing step:
A. with technical pure raw metal Fe, Nd, Co, Zr and FeB alloy; count with atomic percent by the nano-composite NdFeB permanent magnetic alloy composition: Fe 70～80%, Nd 7～15%, Co 3～8%, Zr 1～5% and B 3～9% prepare burden; carry out melting with vacuum non-consumable arc furnace under argon shield then, the melting current density is 100～250A/cm
2, molten alloy is stood up melting 3～6 times, obtain alloy button ingot;
B. the button ingot is broken into the cobbing of 3～6g, in the quartz ampoule of packing into, in the electric induction vacuum quick quenching furnace, makes alloy thin band; The quartz ampoule nozzle diameter is 0.6～1.2mm, and nozzle and roll surface distance are 5～10mm, and the argon pressure difference is 0.8 * 10
5～1.5 * 10
5Pa, roll surface speed are 12～22m/s;
C. under the permanent magnetic field of 10T, the roll surface direction of strip is parallel or anneal perpendicular to magnetic field orientating.Be warmed up to uniform temperature (600～800 ℃) earlier, be incubated 20～40 minutes, then with stove cooling 30～60 minutes.Utilize JDM-13 type vibrating specimen magnetometer (VSM), measure the magnetic property of parallel roll surface of strip (//) and vertical roll surface direction (⊥) respectively, its maximum field is 1.8T.
Used raw material is pure Fe, Nd, Co, Zr and FeB intermediate alloy among the present invention.
Alloy of the present invention has anisotropy and good magnetic property.
Characteristics of the present invention are: 1) new alloy formula: contain Co and Zr element in alloy simultaneously.Adding Co can replace Hard Magnetic and obtain Nd with the Fe of soft magnetism in mutually mutually
2(Fe, Co)
14B/ α-(Fe, Co) built-up magnet are improved coercive force, remanent magnetization and the maximum magnetic energy product of magnet simultaneously.The Zr element can crystal grain thinning, can make soft magnetism and Hard Magnetic mutually crystal grain reach nano-scale, further strengthened strengthening the exchange-coupling interaction between soft, the Hard Magnetic phase, thereby improved the comprehensive magnetic property of alloy.2) heating anneal under permanent magnetic field not only can crystal grain thinning, and can also make preferable grain orientation, obtains having the anisotropic nano-crystal composite permanent magnetic alloy of fine magnetic property.
The present invention has better magnetic properties, can be widely used in the magnetic device in fields such as information, communication, computer.
Description of drawings
Fig. 1 is the room temperature magnetic measurement curve of anisotropic nano-crystal composite permanent magnetic alloy conventional annealing of the present invention and permanent magnetic-field annealing.Wherein dotted line is represented is the roll surface direction of the alloy thin band magnetic hysteresis loop after perpendicular to magnetic direction annealing, is magnetic hysteresis loop after the roll surface direction of alloy thin band is parallel to magnetic direction annealing and solid line is represented.
Fig. 2 is the X ray diffracting spectrum of anisotropic nano-crystal composite permanent magnetic alloy conventional annealing of the present invention and permanent magnetic-field annealing.
Embodiment
After now example of the present invention specifically being described in.
Embodiment 1
The composition of the nano-crystal composite permanent magnetic alloy of present embodiment (atomic percent) is Fe76%, Nd10%, Co5%, Zr3.0% and B6.0%.Preparation process is as follows with step: technical pure raw metal Fe, Nd, Co, Zr and FeB alloy are become assignment system 16 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 180A/cm
2, alloy is stood up melting 4 times; Alloy pig is broken into the fritter of 3～6g, in the quartz ampoule of packing into, makes the fast quenching alloy thin band in the electric induction vacuum quick quenching furnace, the quartz ampoule nozzle diameter is 0.8mm, and nozzle and roll surface distance are 8mm, and the argon pressure difference is 1.0 * 10
5Pa, the linear velocity of running roller is 17m/s; Under the permanent magnetic field of 10T, the roll surface direction of strip is parallel or perpendicular to magnetic direction annealing, at 710 ℃, vacuum degree is 3 * 10 with above-mentioned fast quenching thin strap
-3Carry out crystallization and thermal treatment under the Pa condition, temperature retention time was 30min, with stove cooling 40 minutes.Make nano-crystal composite permanent magnetic alloy of the present invention at last.
Prepared nano-crystal composite permanent magnetic alloy in the present embodiment, through conventional annealing and permanent magnetic-field annealing treatment process, its agnetic property at room temperature m is seen accompanying drawing 1.The magnetic property of the parallel roll surface direction of alloy thin band (//) is: saturation magnetization M
s=105.46Am
2/ kg, remanent magnetism M
r=85.5Am
2/ kg, coercive force
jH
c=595kA/m.The magnetic property of the vertical roll surface direction of alloy thin band (⊥) is: saturation magnetization M
s=80.00Am
2/ kg, remanent magnetism M
r=70.4Am
2/ kg, coercive force
jH
c=593kA/m.This explanation alloy is anisotropic, is different in different direction magnetic promptly.
Prepared nano-crystal composite permanent magnetic alloy in the present embodiment, through conventional annealing and permanent magnetic-field annealing treatment process, its X ray diffracting spectrum is seen accompanying drawing 2.As can be seen, the Nd after two kinds of conditions are annealed
10Fe
76Co
5Zr
3B
6Strip all is to contain Nd
2Fe
14The B Hard Magnetic is mutually with α-the Fe soft magnetism mutually.Nd in the strip of magnetic-field annealing
2Fe
14The relative intensity of (513) of B Hard Magnetic phase and (703) crystal face diffraction maximum is obviously greater than the corresponding peak intensity of conventional annealing, and the relative intensity of (105) and (411) crystal face diffraction maximum reduces.This illustrates that further magnetic field makes crystal grain along externally-applied magnetic field direction preferred orientation, makes Nd
10Fe
76Co
5Zr
3B
6The alloy magnetic property is variant in different directions.
Claims (2)
1. anisotropic nano-composite NdFeB permanent magnetic alloy is characterized in that the composition of this alloy, with atomic percent
Count:
Fe 70～80％
Nd 7～15％
Co 3～8％
Zr 1～5％
B 3～9％
2. preparation method who is used for the described anisotropic nano-composite NdFeB permanent magnetic alloy of claim 1 is characterized in that this method has following processing step:
A. with technical pure raw metal Fe, Nd, Co, Zr and FeB alloy; count with atomic percent by the nano-composite NdFeB permanent magnetic alloy composition: Fe 70～80%, Nd 7～15%, Co 3～8%, Zr 1～5% and B 3～9% prepare burden 15～18 the gram; carry out melting with vacuum non-consumable arc furnace under argon shield then, the melting current density is 100～250A/cm
2, molten alloy is stood up melting 3～6 times, obtain alloy button ingot;
B. the button ingot is broken into the cobbing of 3～6g, in the quartz ampoule of packing into, in the electric induction vacuum quick quenching furnace, makes alloy thin band; The quartz ampoule nozzle diameter is 0.6～1.2mm, and nozzle and roll surface distance are 5～10mm, and the argon pressure difference is 0.8 * 10
5～1.5 * 10
5Pa, roll surface speed are 12～22m/s;
C. under the permanent magnetic field of 8～10T, the roll surface direction of strip is parallel or perpendicular to magnetic direction annealing, is 2 * 10 in vacuum degree
-3Pa～4 * 10
-3Be warmed up to 650～800 ℃ under the Pa condition, be incubated 20～40 minutes, then with stove cooling 30～60 minutes.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031414A (en) * | 2012-12-28 | 2013-04-10 | 哈尔滨工业大学 | Fabrication method of directional solidification neodymium ferrum boron magnetic alloy |
| CN103996476A (en) * | 2014-05-19 | 2014-08-20 | 上海大学 | Preparation method for rare-earth permanent magnet alloy quick quenching stripe |
| CN104240885A (en) * | 2014-09-09 | 2014-12-24 | 宁波韵升股份有限公司 | NdFeB double-phase composite permanent magnet nanomaterial and preparation method |
| CN105149532A (en) * | 2015-09-09 | 2015-12-16 | 上海大学 | Method for preparing rare earth permanent magnetic rapid-quenching ribbon |
| CN106057461A (en) * | 2016-05-20 | 2016-10-26 | 中国计量大学 | Anisotropic blocky nanocomposite permanent magnet and preparation method therefor |
| CN106856118A (en) * | 2015-12-08 | 2017-06-16 | 北京中科三环高技术股份有限公司 | The thinning method and bonded permanent magnet of nanocrystalline fast quenching rare-earth permanent-magnet material and its crystallite dimension |
| CN108831658A (en) * | 2018-08-28 | 2018-11-16 | 中国计量大学 | A kind of method that grain boundary decision prepares high-coercive force neodymium iron boron magnetic body under Constant charge soil |
| CN112201429A (en) * | 2020-10-14 | 2021-01-08 | 燕山大学 | Permanent magnet with nanoscale gradient structure and preparation method thereof |
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| JP2004253697A (en) * | 2003-02-21 | 2004-09-09 | Hitachi Metals Ltd | Permanent magnet and material thereof |
| CN101026034A (en) * | 2006-02-22 | 2007-08-29 | 南京理工大学 | Method for preparing corrosion resistance rare earth permanent-magnetic material |
| CN101086053A (en) * | 2007-07-13 | 2007-12-12 | 上海大学 | Nano crystal composite permanent-magnet alloy and its preparation method |
| CN101673605A (en) * | 2008-09-08 | 2010-03-17 | 南京理工大学 | Anisotropic nano/amorphous complex phase block permanent-magnetic material and preparation method thereof |
| CN101717888A (en) * | 2009-11-26 | 2010-06-02 | 上海大学 | Nano-crystalline composite NdFeB permanent magnetic alloy and method for producing same |
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| JP2004253697A (en) * | 2003-02-21 | 2004-09-09 | Hitachi Metals Ltd | Permanent magnet and material thereof |
| CN101026034A (en) * | 2006-02-22 | 2007-08-29 | 南京理工大学 | Method for preparing corrosion resistance rare earth permanent-magnetic material |
| CN101086053A (en) * | 2007-07-13 | 2007-12-12 | 上海大学 | Nano crystal composite permanent-magnet alloy and its preparation method |
| CN101673605A (en) * | 2008-09-08 | 2010-03-17 | 南京理工大学 | Anisotropic nano/amorphous complex phase block permanent-magnetic material and preparation method thereof |
| CN101717888A (en) * | 2009-11-26 | 2010-06-02 | 上海大学 | Nano-crystalline composite NdFeB permanent magnetic alloy and method for producing same |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031414A (en) * | 2012-12-28 | 2013-04-10 | 哈尔滨工业大学 | Fabrication method of directional solidification neodymium ferrum boron magnetic alloy |
| CN103031414B (en) * | 2012-12-28 | 2014-03-05 | 哈尔滨工业大学 | Fabrication method of directional solidification neodymium ferrum boron magnetic alloy |
| CN103996476A (en) * | 2014-05-19 | 2014-08-20 | 上海大学 | Preparation method for rare-earth permanent magnet alloy quick quenching stripe |
| CN104240885A (en) * | 2014-09-09 | 2014-12-24 | 宁波韵升股份有限公司 | NdFeB double-phase composite permanent magnet nanomaterial and preparation method |
| CN105149532A (en) * | 2015-09-09 | 2015-12-16 | 上海大学 | Method for preparing rare earth permanent magnetic rapid-quenching ribbon |
| CN106856118A (en) * | 2015-12-08 | 2017-06-16 | 北京中科三环高技术股份有限公司 | The thinning method and bonded permanent magnet of nanocrystalline fast quenching rare-earth permanent-magnet material and its crystallite dimension |
| CN106057461A (en) * | 2016-05-20 | 2016-10-26 | 中国计量大学 | Anisotropic blocky nanocomposite permanent magnet and preparation method therefor |
| CN108831658A (en) * | 2018-08-28 | 2018-11-16 | 中国计量大学 | A kind of method that grain boundary decision prepares high-coercive force neodymium iron boron magnetic body under Constant charge soil |
| CN112201429A (en) * | 2020-10-14 | 2021-01-08 | 燕山大学 | Permanent magnet with nanoscale gradient structure and preparation method thereof |
| CN112201429B (en) * | 2020-10-14 | 2021-12-21 | 燕山大学 | Permanent magnet with nanoscale gradient structure and preparation method thereof |
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Open date: 20101124 |