CN101892376A - Thermal treatment process for crystallizing nano-composite NdFeB permanent magnetic alloy - Google Patents
Thermal treatment process for crystallizing nano-composite NdFeB permanent magnetic alloy Download PDFInfo
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- CN101892376A CN101892376A CN 201010215783 CN201010215783A CN101892376A CN 101892376 A CN101892376 A CN 101892376A CN 201010215783 CN201010215783 CN 201010215783 CN 201010215783 A CN201010215783 A CN 201010215783A CN 101892376 A CN101892376 A CN 101892376A
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Abstract
The invention relates to a thermal treatment process for crystallizing nano-composite NdFeB permanent magnetic alloy, belonging to the technical field of thermal treatment process for magnetic material preparation. The process is characterized in that: the NdFeB permanent magnetic amorphous alloy is subjected to vacuum annealing thermal treatment at the crystallizing temperature in a magnetic field with pulse magnetic field strength of between 2 and 8T; and a mode that pulse magnetic field and annealing are applied asynchronously is adopted, namely magnet charging is started when annealing insulation is performed in the halfway, and is stopped until air is cooled for 5 to 10 minutes. By adopting the process, the magnetic performance of the nano-composite NdFeB permanent magnetic alloy can be remarkably improved, wherein the coercive force and remanence are improved by 9.38 percent and 14.7 percent respectively. The process provides a novel scheme for preparing the nano-composite NdFeB permanent magnetic alloy with excellent magnetic performance.
Description
Technical field
The present invention relates to a kind of thermal treatment process of crystallizing nano-composite NdFeB permanent magnetic alloy, belong to the thermal treatment process technology field of preparation magneticsubstance.
Background technology
Nano-crystal composite permanent magnetic alloy is by soft magnetism and Hard Magnetic compound permanent magnet material of forming in nano-scale, and it is characterized by: matrix can be the Hard Magnetic phase mutually, also can be the soft magnetism phase, and the equal highly dispersed of two-phase ground uniform distribution is compound at nano-scale each other; For obtaining high permanent magnetism performance, require Hard Magnetic that high as far as possible magnetocrystalline anisotropy is arranged mutually, and soft magnetism have high as far as possible saturation magnetization mutually; Two-phase (or second phase) grain-size reaches nano level size, and there is the magnetic exchange coupling in the two-phase interface place.The appearance of nanocrystalline composite permanent-magnet material has caused countries in the world material supplier authors' great attention, with experimentally, has all carried out deep research from theoretical.
The nanocrystalline composite permanent-magnet material alloy preparation method mainly contains melt-quenching method, machine-alloying (MA), hydride process (HDDR), magnetron sputtering method, gas atomization (GA) etc.Because melt-quenching method, easy to operate, technology is simple, helps suitability for industrialized production, thereby becomes most important a kind of preparation method.
For obtaining optimum magnetic property, in fact many employing melt-spuns add amorphous crystallization method.Earlier the mother alloy fast quenching is become amorphous thin ribbon, then carry out crystallization and handle.For the performance that obtains, can also adopt some non-traditional annealing processs as high pressure annealing, flash annealing, laser annealing, pulse annealing and magnetic-field annealing etc.People such as Wang utilize the high pressure annealing crystallization to obtain high performance Pr
2(Fe, Co)
14B/ α-(Fe, Co) nanocrystalline composite permanent-magnet material.Human amorphous crystallization methods such as Gao have been studied rate of heating to Nd
7Fe
86Nb
1B
6The phase transition process of nanocrystalline composite permanent-magnet material crystallization, weave construction and Effect on Performance found that flash annealing can obtain the higher magnetic property of conventional annealing.People such as Zhang utilize laser beam with the rate of heating of 200 ℃/sec with Nd
15Fe
78.5C
5.5The alloy amorphous strip of B is heated to 800 ℃～900 ℃ rapidly, compare with conventional annealing, the Hard Magnetic of flash annealing mutually with soft magnetism mutually forming core and grow up rapidly limited, thereby organize tiny and even, the permanent magnetism excellent performance.Magnetic-field annealing is a kind of novel crystallization method that occurs in recent years, and it not only can crystal grain thinning, also can make crystal grain that certain directional profile is arranged.People such as Yang are Nd to composition
4Fe
73.5Co
3(Hf
1-xGa
x) B
18.5Alloy handled 5 minutes with strip crystallization under 650～710 ℃ of conditions of 40m/s fast quenching speed preparation, when thermal treatment, apply the magnetic field of 398kA/m (5KOe) along the belt length direction, found that: with conventional heat treatment phase ratio, the magnetic field crystallization and thermal treatment can suppress grain growing, make soft magnetism phase grain refining about 20%, and uniform distribution makes remanent magnetism and magnetic energy product increase about 30%.Magnetic field treatment at the existing literature report adopts constant magnetic field more, and expense is expensive, the cost height.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 crystallization and thermal treatment technology that improves the comprehensive magnetic property of nano-composite NdFeB permanent magnetic alloy.
The objective of the invention is to realize by following technique means.
A. the fast quenching thin strap with Nd-Fe-B alloys carries out conventional subsequent annealing in heat treatment furnace, in 640 ℃～750 ℃ temperature range, with 640 ℃ be starting temperature, every increase is selected a temperature for 30 ℃, selects 4 temperature altogether.By to sample measurement magnetic property and X-ray diffraction analysis behind each annealing temperature, determine the crystallization temperature of Nd-Fe-B alloys fast quenching thin strap.
B. the fast quenching thin strap of Nd-Fe-B alloys is put into vacuum heat treatment furnace and carry out the pulsed magnetic field anneal, vacuum annealing furnace is that the parallel magnetic field direction is put into pulsed magnetic field coil (wherein strip roll surface direction is parallel with field direction), extracts furnace air and reaches 3 * 10 up to vacuum tightness
-3～5 * 10
-3Begin during Pa to heat up, insulation after being warming up to 640～750 ℃, the annealing soaking time is 20～40min, a half that is incubated the annealing soaking time begins to carry out pulsed magnetic field and magnetizes and stop behind cooling air-cooling 5～10min, the pulsed magnetic field frequency that magnetizes is 0.01～0.10Hz, the time of magnetizing is 15～35min, and magneticstrength is 2～8T.
Characteristics of the present invention are:
(1) adopted the method for when the annealing crystallization is handled the fast quenching thin strap of nanocrystal composite NdFeB alloy, introducing pulsed magnetic field, purpose is that the assurance alloy is separated out in the process of soft or hard magnetic phase in crystallization, the applying pulse magnetic field energy plays crystal grain thinning, promotes the effect that soft or hard magnetic forms mutually and magnetic domain is rotated; (2) adopt pulsed magnetic field and the asynchronous mode of annealing of applying, a half that promptly is incubated the annealing soaking time begins to magnetize again and stops behind cooling air-cooling 5～10min, purpose is to impel in the alloy soft or hard magnetic to separate out mutually, and magnetic domain is deflected, promote exchange-coupling interaction, thereby improve the remanent magnetism and the coercive force of alloy, improve the magnetic property of alloy.
The present invention is the applying pulse thermomagnetic treatment technology that nano-composite NdFeB permanent magnetic alloy is carried out, and adopts the magnetic property of the nano-composite NdFeB permanent magnetic alloy after this technology crystallization to improve a lot.Fig. 1 is nano-crystal composite permanent magnetic alloy 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, the coercive force that alloy has behind the conventional annealing is 586kA/m, and remanent magnetism is 68Am
2/ kg, and the coercive force of the nano-crystal composite permanent magnetic alloy by the applying pulse magnetic-field annealing is 641kA/m, remanent magnetism is 78Am
2/ kg.Coercive force and remanent magnetism improve 9.38% and 14.7% respectively.
Technology of the present invention provides a kind of new departure for the nano-composite NdFeB permanent magnetic alloy that preparation has the excellent magnetic energy.
Description of drawings
Fig. 1 is nano-crystal composite permanent magnetic alloy demagnetizing curve figure at room temperature.
Embodiment
After now example of the present invention specifically being described in.
Embodiment 1
(1). the composition (atomic percent) of preparation nano-crystal composite permanent magnetic alloy is Fe75.5%, Nd10%, Co5%, Zr3% and B6.5%.Technical pure raw metal Fe, Nd, Co, Zr 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 180A/cm
2, alloy is stood up melting 4 times; Alloy pig is broken into the fritter of 3～5g, in the silica tube of packing into, makes the fast quenching alloy thin band in the electro-induction vacuum quick quenching furnace, the silica tube 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, prepares the fast quenching thin strap of nanocrystal composite NdFeB alloy.
(2). the fast quenching thin strap of NdFeB alloy is carried out conventional subsequent annealing in heat treatment furnace, select temperature to be respectively 640 ℃, 670 ℃, 700 ℃, 730 ℃, by the sample after the annealing of each annealing temperature point is surveyed magnetic property and X-ray diffraction analysis, the crystallization temperature of determining NdFeB alloy fast quenching thin strap is 730 ℃.
(3). the fast quenching thin strap of NdFeB alloy is put into vacuum heat treatment furnace carry out the pulsed magnetic field anneal, vacuum annealing furnace is that the parallel magnetic field direction is put into pulsed magnetic field coil (wherein strip roll surface direction is parallel with field direction), extracts furnace air and reaches 4 * 10 until vacuum
-3Heat up behind the Pa, be warming up to 730 ℃ after the insulation, the annealing soaking time is 30min, beginning to carry out pulsed magnetic field when being incubated to 15min again magnetizes and stops behind cooling air-cooling 5～10min, the pulsed magnetic field frequency that is applied is 0.05Hz, and magneticstrength is 5T, and the time of magnetizing is 20min.
Prepared nanocrystal composite NdFeB alloy in the present embodiment is through conventional annealing and two kinds of processing schemes of applying pulse magnetic-field annealing.At room temperature, the nanocrystal composite NdFeB alloy of two kinds of treatment process is carried out magnetic property measure, see accompanying drawing 1.The curve that with dashed lines is drawn among the figure is meant the magnetic hysteresis loop of nanocrystal composite NdFeB alloy behind conventional annealing, and is meant the magnetic hysteresis loop of nanocrystal composite NdFeB alloy after adding pulsed magnetic field annealing with the curve that solid line is drawn.After can finding out that from accompanying drawing the nanocrystal composite NdFeB alloy crystallization of using technology of the present invention is handled, its magnetic property is significantly improved.The coercive force of alloy is by 586kAm
-1Bring up to 641kAm
-1, increase rate is 9.38%; The remanent magnetism of alloy is by 68Am
2Kg
-1Bring up to 78Am
2Kg
-1, increase rate is 14.7%.
Claims (1)
1. the thermal treatment process of a crystallizing nano-composite NdFeB permanent magnetic alloy is characterized in that having following processing step:
(1) fast quenching thin strap with Nd-Fe-B alloys carries out conventional subsequent annealing in heat treatment furnace, in 640～750 ℃ temperature range, with 640 ℃ be starting temperature, every increase is selected a temperature for 30 ℃, selects 4 temperature altogether; By to sample measurement magnetic property and X-ray diffraction analysis behind each annealing temperature, determine the crystallization temperature of Nd-Fe-B alloys fast quenching thin strap;
(2) fast quenching thin strap of Nd-Fe-B alloys is put into vacuum heat treatment furnace and carry out the pulsed magnetic field anneal, vacuum annealing furnace is that the parallel magnetic field direction is put into the pulsed magnetic field coil, wherein strip roll surface direction is parallel with field direction, extracts furnace air and reaches 3 * 10 up to vacuum tightness
-3～5 * 10
-3Begin during Pa to heat up, insulation after being warming up to 640～750 ℃, the annealing soaking time is 20～40min, a half that is incubated the annealing soaking time begins to carry out pulsed magnetic field and magnetizes and stop behind cooling air-cooling 5～10min, the pulsed magnetic field frequency that magnetizes is 0.01～0.10Hz, the time of magnetizing is 15～35min, and magneticstrength is 2～8T.
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Cited By (3)
| 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 |
| CN107377907A (en) * | 2017-08-04 | 2017-11-24 | 芜湖君华材料有限公司 | A kind of ultra-thin Fe-based amorphous alloy magnetic band preparation method |
| CN117305573A (en) * | 2023-11-30 | 2023-12-29 | 太原科技大学 | Capsule type tension-magnetic field coupling annealing furnace based on Helmholtz coil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182594A (en) * | 2007-12-06 | 2008-05-21 | 上海大学 | Heat treating process for Fe-based big block amorphous alloy crystallization |
| CN101521069A (en) * | 2008-11-28 | 2009-09-02 | 北京工业大学 | Method for preparing heavy rare earth hydride nano-particle doped sintered NdFeB permanent magnet |
-
2010
- 2010-06-29 CN CN 201010215783 patent/CN101892376A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182594A (en) * | 2007-12-06 | 2008-05-21 | 上海大学 | Heat treating process for Fe-based big block amorphous alloy crystallization |
| CN101521069A (en) * | 2008-11-28 | 2009-09-02 | 北京工业大学 | Method for preparing heavy rare earth hydride nano-particle doped sintered NdFeB permanent magnet |
Cited By (5)
| 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 |
| CN107377907A (en) * | 2017-08-04 | 2017-11-24 | 芜湖君华材料有限公司 | A kind of ultra-thin Fe-based amorphous alloy magnetic band preparation method |
| CN117305573A (en) * | 2023-11-30 | 2023-12-29 | 太原科技大学 | Capsule type tension-magnetic field coupling annealing furnace based on Helmholtz coil |
| CN117305573B (en) * | 2023-11-30 | 2024-02-02 | 太原科技大学 | Capsule type tension-magnetic field coupling annealing furnace based on Helmholtz coil |
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Open date: 20101124 |