CN103559971A - Nanometer rare earth permanent magnetic material with high-temperature stability and preparation method thereof - Google Patents
Nanometer rare earth permanent magnetic material with high-temperature stability and preparation method thereof Download PDFInfo
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- CN103559971A CN103559971A CN201310499302.3A CN201310499302A CN103559971A CN 103559971 A CN103559971 A CN 103559971A CN 201310499302 A CN201310499302 A CN 201310499302A CN 103559971 A CN103559971 A CN 103559971A
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Abstract
A nanometer rare earth permanent magnetic material with the high-temperature stability is characterized in that a basic expression is RxFe100-x-z-y BzNy, wherein R is one or a plurality of lanthanide series rare earth elements of neodymium, praseodymium and the like, Fe is an iron element, B is an boron element, N is one of elements of niobium, zirconium and the like, x is a number ranging from 15 to 36, z is a number ranging from 2 to 10, and y is a number ranging from 4 to 10. Preferentially, x is a number ranging from 18 to 32, z is a number ranging from 2.6 to 8.5, and y is a number ranging from 4.8 to 9. The invention further provides a preparation method of the rare earth permanent magnetic material. A Co element is not added, and the material has the advantages of being low in cost and high in working temperature and intrinsic coercivity.
Description
Technical field
The present invention relates to a kind of nano-rare earth permanent magnetic material with high-temperature stability, more specifically, relate to the Agglutinate neodymium-iron-boron nano-rare earth permanent magnetic material of a kind of low cost, elevated operating temperature, high HCJ.
Background technology
The nano-rare earth permanent magnetic material of Agglutinate neodymium-iron-boron is because of its high-performance, the advantages such as low cost, and obtain, study widely and pay attention to, but this class material Curie temperature is generally on the low side, under hot environment, apply and be very restricted, such as various motors and transducer, require its working temperature 130～150 ℃ of left and right, and at auto industry field, require its working temperature at 150～180 ℃, for improving the high-temperature stability of the nano-rare earth permanent magnetic material of Agglutinate neodymium-iron-boron, expand its range of application, much research is compound interpolation Co～Dy on NdFeB basis, Co～Ga forms a kind of NEW TYPE OF COMPOSITE permanent magnetic material, as at a patent < < nano-composite NdFeB permanent magnetic alloy with higher temperature stability and preparation method thereof > > (number of patent application: described a kind of nano combined NdFeB permanent-magnet alloy with higher temperature stability 201010215804.5), this permanent-magnet alloy composition is counted with atomic percent: Fe70～80%, Nd7～12%, Co3～8%, Ga0.1～4%, Zr0.2～5%, B4～10%.But this patent has been used too much strategic resource Co, this will make cost improve and be unfavorable for applying.
The shortcoming of the nd-fe-b permanent magnetic alloy of prior art is that magnetic property is lower, poor heat stability, serviceability temperature is low, under hot environment, be unfavorable for using, such as motor, sensor parts, the magnetic property of magnet can, because of heating or ambient temperature raising reduction greatly, even cause component failure, thereby limit the scope of application of magnet.
Summary of the invention
The nano-rare earth permanent magnetic material that the object of this invention is to provide a kind of Agglutinate neodymium-iron-boron, it does not add Co element, has advantages of low cost, elevated operating temperature, high HCJ.
For this reason, the invention provides a kind of Nd-Fe-B nano rare earth permanent-magnetic material, by adding wherein one or more such as lanthanide series rare-earth elements neodymium, praseodymium, and compoundly having added the binding Nd-Fe-B permanent magnetic material that other transition metal such as Nb, Zr obtain high HCJ, elevated operating temperature, basic representation is R
xfe
100～x～z～yb
zn
y, wherein, R is wherein one or more such as lanthanide series rare-earth elements neodymium, praseodymium, and Fe is ferro element, and B is boron element, and N is a kind of in the elements such as Nb, Zr; X is 15～36 any number, any number that z is 2～10, any number that y is 4～10.
Preferably, any number that described x is 18～32, any number that z is 2.6～8.5, any number that y is 4.8～9, more preferably, any number that described x is 20～29.5, any number that z is 3～7.9, any number that y is 5.5～7.6.Comparing with a patent < < nano-composite NdFeB permanent magnetic alloy with higher temperature stability and preparation method thereof > >, is obviously distinguishing.
The present invention improves the micro-structural of permanent-magnet alloy by adding the transition metals such as Nb, Zr, the transition metal such as Nb, Zr forms ultra-fine α-Fe phase in rapid solidification, having suppressed the forming core of Nd-Fe-B crystal grain grows up, refinement crystal grain, strengthen the exchange-coupling interaction of soft magnetism phase and Hard Magnetic phase, improved the performance of product.
The present invention also provides the preparation method of this nano-rare earth permanent magnetic material.Concrete preparation method is as follows: by technical pure metallic element Fe, Nd, B, Nb, Zr etc. prepare burden by above-mentioned atomic percent, put into vacuum melting furnace melting, obtain alloy pig, again alloy pig is put into spun furnace processing and got rid of band, by temperature, air pressure, vacuum degree, roll surface linear speeds etc. are controlled within the specific limits, by getting rid of with afterproduct, carry out crystallization processing and annealing heat treatment process is prepared a kind of rare earth permanent-magnetic material with high HCJ again, wherein, thermal anneal process is preferably the temperature range of 400 ℃～800 ℃, the thermal annealing time is preferably at 2～35 minutes.
The invention solves in prior art nd-fe-b permanent magnetic alloy magnetic property lower, poor heat stability, serviceability temperature is low, is unfavorable for obtaining the shortcoming used and have high HCJ, High Operating Temperature magnetic under hot environment in the situation that not adding Co element.Rare earth permanent-magnetic material of the present invention shows the approximately HCJ of 955～995kA/m (Hci), the high remanent magnetism (Br) of 820～840mT, 114Kj/m
3the maximum operating temperature of above maximum magnetic energy product (BHmax) and 150-180 ℃, has significantly expanded the range of application of Related product, has reduced the irreversible magnetic flux of magnetic, and more than 150 ℃ high-temperature process 1 hour, irreversible loss was below 2%.
Nano-rare earth permanent magnetic material of the present invention is applicable to the parts that motor, sensor needs use under elevated operating temperature, and magnet performance can not reduce because of the heating of device or the raising of ambient temperature.
Accompanying drawing explanation
Fig. 1 is the micro-structure diagram of like product under SEM Electronic Speculum.
Fig. 2 is the micro-structure diagram of product of the present invention under SEM Electronic Speculum.
Fig. 3 is the demagnetize amount of product of the present invention under different temperatures and the comparison diagram of like product.
Fig. 4 is according to the structure chart of the preparation system of the nano-rare earth permanent magnetic material of invention.
Embodiment
Below in conjunction with accompanying drawing 1-4 and specific embodiment, the present invention is further described, but the invention is not restricted to these embodiment, following examples only for the purpose of illustration, should not be used to limit the scope of the present invention and claim.
As shown in Figure 4, a kind of preparation system of nano-rare earth permanent magnetic material comprises that proportioner 1, smelting apparatus 2, alloy get rid of belting 3 and crystallization is processed and annealing heat treatment device 4 successively; Proportioner 1, smelting apparatus 2, alloy get rid of belting 3 and crystallization is processed and annealing heat treatment device 4 is arranged in order from process upstream to process downstream; Proportioner 1 comprise the loader of technical pure metallic element Fe, the loader of the loader of technical pure metallic element Nd, technical pure metallic element B, the atomic percent batching controller of the loader of the loader of technical pure metallic element Nb, technical pure metallic element Zr and technical pure metallic element Fe, Nd, B, Nb, Zr; Described smelting apparatus 2 obtains alloy solution and gets rid of belting 3 with alloy and be communicated with; Alloy gets rid of the band afterproduct that gets rid of that belting 3 obtains and is communicated with crystallization processing and annealing heat treatment device 4.
embodiment 1:
According to following formula, the Nd that purity is 99.9%, atomic percent is 29%, Fe-B alloy (wherein B content is 19%), the atomic percent that the atomic percent of B is 2.8%, Nb is 4.2%, remains the content into Fe.Under the protection of inert gas argon gas; putting into vacuum melting furnace smelts; obtain 50 kilograms of uniform alloy pigs of composition; again the alloy pig obtaining is carried out to rapid quenching (seeing Fig. 3); wheel speed is about 20～39m/s, obtains broken 40 eye mesh screens of crossing after metal sheet band, and at 500 ℃～700 ℃ temperature, crystallization is 10 minutes; the vibrating specimen magnetometer for sample (VSM) of preparation is measured to its magnetic property, and performance is as shown in table 1:
Table 1
By chart 1 data, can be found out, in rare earth permanent-magnetic material, in the situation that magnetic energy product BH (max) keeps performance good, can obtain the product that high-coercive force and maximum operating temperature can reach 150～180 ℃.
embodiment 2:
According to following formula, the Nd that purity is 99.9%, atomic percent is 24%, Fe-B alloy (wherein B content is 19%), the atomic percent that the atomic percent of B is 3.5%, Nb is 4.8, remains the content into Fe.The preparation process of repeat samples 1, measures its magnetic property by the vibrating specimen magnetometer for sample (VSM) of preparing, and performance is as shown in table 2:
Table 2
By chart 2 data, can be found out, in rare earth permanent-magnetic material, in the situation that magnetic energy product BH (max) keeps performance good, can obtain the product that high-coercive force and maximum operating temperature can reach 150～180 ℃.
embodiment 3:
According to following formula, the Nd that purity is 99.9%, atomic percent is 22.6%, Fe-B alloy (wherein B content is 19%), the atomic percent that the atomic percent of B is 3.8%, Nb is 5.2%, remains the content into Fe.The preparation process of repeat samples 1, measures its magnetic property by the vibrating specimen magnetometer for sample (VSM) of preparing, and performance is as shown in table 3:
Table 3
By chart 3 data, can be found out, in rare earth permanent-magnetic material, in the situation that magnetic energy product BH (max) keeps performance good, can obtain the product that high-coercive force and maximum operating temperature can reach 150～180 ℃.
embodiment 4:
This sample 1-3 is prepared into
after the magnet of 10*10mm magnetizes, put into respectively the baking oven 1 hour of 100 ℃, the baking oven of 120 ℃ 1 hour, the baking oven of 150 ℃, after 1 hour, takes out and measures its flux loss % with SF-6 type flux meter (1 grade), as shown in table 4
Table 4:
By above test data, reached a conclusion, NdFeB magnetic powder is made bonded permanent magnet under high-temperature operation, flux loss < 6%, and temperature is higher, and flux loss more tends towards stability, and shows excellent serviceability.
From above several groups of data, can find out, in NdFeB magnetic powder, by adding the transition metal such as Nb, Zr, significantly improved HCJ and the maximum operating temperature of magnetic, most importantly this product is applicable to the parts that the needs such as motor are worked under elevated operating temperature.
According to various embodiments of the present invention;
X can be 15,16,17,18,19,20,21,22,23,24,25,26,27,28,29,30,31,32,33,34,35 or 36 natural number, or be the arbitrary small number between 15～36, for example, 15.1,15.4,15.6,15.8 etc.,, 35.1,35.4,35.6,35.8 etc., for simplicity, list no longer one by one, in a word, the arbitrary small number between 15～36 and integer can become the value embodiment of x.
Similarly, z can be 2～10 any number, and the arbitrary small number between 2～10 and integer can become the value embodiment of z.Similarly, any number that y is 4～10, the arbitrary small number between 4～10 and integer can become the value embodiment of y.
The preparation system that the invention provides a kind of nano-rare earth permanent magnetic material, is characterized in that, comprises that successively proportioner, smelting apparatus, alloy get rid of belting and crystallization is processed and annealing heat treatment device; Proportioner, smelting apparatus, alloy get rid of belting and crystallization is processed and annealing heat treatment device is arranged in order from process upstream to process downstream; Proportioner comprise the loader of technical pure metallic element Fe, the loader of the loader of technical pure metallic element Nd, technical pure metallic element B, the atomic percent batching controller of the loader of the loader of technical pure metallic element Nb, technical pure metallic element Zr and technical pure metallic element Fe, Nd, B, Nb, Zr; Described smelting apparatus obtains alloy solution and gets rid of belting with alloy and be communicated with; Alloy gets rid of the band afterproduct that gets rid of that belting obtains and is communicated with crystallization processing and annealing heat treatment device.
Preferably, described atomic percent batching controller is the first proportional controller.
Preferably, described atomic percent batching controller is the second proportional controller.
Preferably, described atomic percent batching controller is the 3rd proportional controller.
Preferably, described smelting apparatus is vacuum melting furnace.
Preferably, at described smelting apparatus and described alloy, get rid of and between belting, be also provided with alloy treatment device.Preferably, described alloy gets rid of the control device that belting has temperature, air pressure, vacuum degree and/or roll surface linear speed.
Preferably, described crystallization processing and annealing heat treatment device are provided with the heat treatment that makes to anneal at 400～800 ℃ of temperature controllers that carry out.
Preferably, described crystallization process and annealing heat treatment device to be provided with the heat treatment time that makes to anneal be the time controller of 2～35 minutes.
In the present invention, term " the first proportional controller " refers to that it is R that described atomic percent batching controller has basic representation
xfe
100～x～z～yb
zn
y, wherein, R is neodymium and/or praseodymium; Fe is ferro element, and B is boron element; N is niobium or zirconium; X is 15～36 any number, any number that z is 2～10, any number that y is 4～10.
In the present invention, term " the second proportional controller " refers to that it is R that described atomic percent batching controller has basic representation
xfe
100～x～z～yb
zn
y, wherein, R is neodymium and/or praseodymium; Fe is ferro element, and B is boron element; N is niobium or zirconium; X is 18～32 any number, any number that z is 2.6～8.5, any number that y is 4.8～9.
In the present invention, term " the first proportional controller " refers to that it is R that described atomic percent batching controller has basic representation
xfe
100～x～z～yb
zn
y, wherein, R is neodymium and/or praseodymium; Fe is ferro element, and B is boron element; N is niobium or zirconium; X is 20～29.5 any number, any number that z is 3～7.9, any number that y is 5.5～7.6.
Product of the present invention when low temperature demagnetize amount a little less than like product, when high temperature far below like product.
So-called processing refer to polishing mechanical alloy pig surface oxidation part Daed and after Mo falls, put into spun furnace and carry out rapid quenching, then gained metal sheet band is carried out to fragmentation and crystallization is processed.
What is called refers to that by controls such as temperature, air pressure, vacuum degree, roll surface linear speeds adjusting gradually temperature is controlled between 1400-1500 ℃ within the specific limits, furnace pressure is when 15-35Torr, vacuum degree control is in 400Pa, and roll surface linear speed etc. is controlled at 30-45m/s.
Claims (10)
1. a nano-rare earth permanent magnetic material, is characterized in that, its basic representation is
R
xFe
100～x～z～yB
zN
y
Wherein, R is wherein one or more such as lanthanide series rare-earth elements neodymium, praseodymium; Fe is ferro element, and B is boron element; N is a kind of (not the adding Co element) in the elements such as niobium, zirconium; X is 15～36 any number, any number that z is 2～10, any number that y is 4～10.
2. nano-rare earth permanent magnetic material as claimed in claim 1, is characterized in that, any number that described x is 18～32, any number that z is 2.6～8.5, and/or the y any number that is 4.8～9.
3. nano-rare earth permanent magnetic material as claimed in claim 1 or 2, is characterized in that, any number that described x is 20～29.5, any number that z is 3～7.9, and/or the y any number that is 5.5～7.6.
4. as the nano-rare earth permanent magnetic material of claim 1-3 as described in one of them, it is characterized in that, R is one or both in didymum; N is a kind of in niobium and zirconium.
5. as the preparation method of the nano-rare earth permanent magnetic material of claim 1-4 as described in one of them, it is characterized in that, described preparation method comprises the following steps: technical pure metallic element Fe, Nd, B, Nb, Zr etc. are prepared burden by described atomic percent; Melting, obtains alloy; Alloy is got rid of to band; And will get rid of band afterproduct and carry out crystallization processing and annealing heat treatment.
6. preparation method as claimed in claim 5, is characterized in that, described melting is carried out in vacuum melting furnace.
7. the preparation method as described in claim 5 or 6, is characterized in that, after the alloy treatment that described melting obtains, gets rid of band, while getting rid of band, temperature, air pressure, vacuum degree, roll surface linear speed etc. is controlled within the specific limits; And/or annealing heat treatment temperature be 400～800 ℃, the time is 2～35 minutes.
8. preparation method as claimed in claim 7, is characterized in that, described processing refers to that alloy puts into spun furnace and carry out fast quenching pre-treatment.
9. preparation method as claimed in claim 7, it is characterized in that, described the controls such as temperature, air pressure, vacuum degree, roll surface linear speed are referred to adjusting gradually temperature is controlled between 1300 ℃-1600 ℃ within the specific limits, furnace pressure is when 15-35Torr, vacuum degree control is in 400Pa, and roll surface linear speed etc. is controlled at 20-55m/s.
10. preparation method as claimed in claim 5, is characterized in that, by technical pure metallic element Fe, Nd, B, Nb, Zr by described atomic percent prepare burden (not adding Co element).
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Cited By (7)
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|---|---|---|---|---|
| CN103871705A (en) * | 2014-03-04 | 2014-06-18 | 山西三益强磁业股份有限公司 | Praseodymium iron boron nitrogen phosphorus permanent magnet material and preparing method thereof |
| CN104575897A (en) * | 2014-12-04 | 2015-04-29 | 浙江东阳东磁有限公司 | High-performance rare-earth permanent magnetic material and preparation method thereof |
| CN105023685A (en) * | 2014-04-15 | 2015-11-04 | Tdk株式会社 | Magnet powder, bond magnet and motor |
| CN105280319A (en) * | 2014-07-14 | 2016-01-27 | 中国科学院物理研究所 | Rare earth iron boron material prepared from industrial pure mixed rare earth, and preparation method and application of rare earth iron boron material |
| CN105810380A (en) * | 2016-03-11 | 2016-07-27 | 江西江钨稀有金属新材料有限公司 | High-temperature resistant and high-magnetism rear earth permanent magnetic material and preparation method thereof |
| 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 |
| CN113838621A (en) * | 2020-06-24 | 2021-12-24 | Tdk株式会社 | R-T-B permanent magnet and motor |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103871705A (en) * | 2014-03-04 | 2014-06-18 | 山西三益强磁业股份有限公司 | Praseodymium iron boron nitrogen phosphorus permanent magnet material and preparing method thereof |
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| CN105023685A (en) * | 2014-04-15 | 2015-11-04 | Tdk株式会社 | Magnet powder, bond magnet and motor |
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| CN105280319A (en) * | 2014-07-14 | 2016-01-27 | 中国科学院物理研究所 | Rare earth iron boron material prepared from industrial pure mixed rare earth, and preparation method and application of rare earth iron boron material |
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| CN104575897B (en) * | 2014-12-04 | 2016-10-05 | 赣州市东磁稀土有限公司 | A kind of high-performance rare-earth permanent magnet material and preparation method thereof |
| 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 |
| CN105810380A (en) * | 2016-03-11 | 2016-07-27 | 江西江钨稀有金属新材料有限公司 | High-temperature resistant and high-magnetism rear earth permanent magnetic material and preparation method thereof |
| CN113838621A (en) * | 2020-06-24 | 2021-12-24 | Tdk株式会社 | R-T-B permanent magnet and motor |
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Application publication date: 20140205 |