CN1889201A - Method for producing Nd2Fe14B/Fe double-phase nano crystal composite permanent-magnetic materials - Google Patents
Method for producing Nd2Fe14B/Fe double-phase nano crystal composite permanent-magnetic materials Download PDFInfo
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- CN1889201A CN1889201A CN 200610089122 CN200610089122A CN1889201A CN 1889201 A CN1889201 A CN 1889201A CN 200610089122 CN200610089122 CN 200610089122 CN 200610089122 A CN200610089122 A CN 200610089122A CN 1889201 A CN1889201 A CN 1889201A
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- nd2fe14b
- pentane
- sintering
- liquid
- magnetic powder
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- 239000002131 composite material Substances 0.000 title claims abstract description 7
- 239000000696 magnetic material Substances 0.000 title abstract description 7
- 229910001172 neodymium magnet Inorganic materials 0.000 title abstract 5
- 238000004519 manufacturing process Methods 0.000 title 1
- 239000002159 nanocrystal Substances 0.000 title 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000006247 magnetic powder Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 13
- 239000002114 nanocomposite Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 230000006835 compression Effects 0.000 claims description 5
- 238000007906 compression Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000012265 solid product Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 12
- 230000005389 magnetism Effects 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 238000007578 melt-quenching technique Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- Hard Magnetic Materials (AREA)
Abstract
The preparation method of Nd2Fe14B/Fe biphase nanocrystalline composite permanent magnetic material belongs to the magnetism material field. Currently it is impossible that the ideal model of soft and hard magnetic phase is conformed at the same time that the block is densified. The specific steps are as follow. In the protection of inert gas, Nd2Fe14B hard magnetic powder below 5 mum is dispersed in decane. After adding Fe (CO) 5, the Fe weight rate of Nd2Fe14B and Fe (CO) 5 is 9:1 and cool it below 0DEG C. Open the supersonic generator, adjust the power to 100-240W and let it react for 1-3h. Centrifugate, remove the liquid and clean it with pentane. After pentane volatilizes, Nd2Fe14B/Fe coating nanometer composite magnetic powder is obtained. Put the magnetic powder into the mould and put it in the plasma fritting furnace. The pressure is 30-1000MPa. In the gas of Ar, the temperature increases in the speed of 40-100DEG C/min to 500-700DEG C. The fritting time is 2-10min. Cool down with the furnace. The invention prepares fully dense, massive, biphase, nanometer and composite magnet. The crystal grain is small and distributes uniformly.
Description
Technical field
A kind of preparation Nd
2Fe
14The method of B/Fe biphase nanocrystalline composite permanent-magnet material belongs to the magnetic material preparation
Technical field.
Background technology
Nanocrystalline diphasic magnet contain simultaneously Hard Magnetic mutually with soft magnetism mutually.Calculate according to the micromagnetics principle, if Hard Magnetic mutually and soft magnetism can produce exchange-coupling interaction fully between mutually, magnet will not only have the high-coercive force of hard magnetic body but also keep the high saturation and magnetic intensity of soft magnetic bodies, thereby had very high magnetic energy product.No matter be or produce originally that nanocrystalline two-phase magnetic material all has important application prospects from magnetic property.Nd
2Fe
14B/ α-Fe is the maximum magnetic energy product (BH) of nano double phase rare earth permanent magnetic material
MaxTheoretical value be 800kJ/m
3, but have only when two-phase crystal grain all is in nano-grade size and evenly distributes, could produce strong ferromagnetism coupling.Present preparation technology can not obtain the desirable complete nanostructure of nano composite permanent magnetic material, thereby influences the exchange-coupling interaction of soft or hard two magnetic phases.So obtain the key of high magnetic characteristics nanometer diphasic magnet is the control crystallite dimension.
At present this preparation methods mainly contains two kinds of melt-quenching method and machine-alloyings, though a lot of scientific workers have carried out continuous improvement to two kinds of methods, but still there is very big gap between the actual magnetic performance of nanometer complex phase magnetic material and the theoretical magnetic property, and research mostly concentrates on the powder body material, preparation progress for block is comparatively slow always, mainly be because crystallite dimension is faced Jie's size greater than the exchange coupling of soft or hard magnetic between mutually, and the crystal grain of soft or hard magnetic phase is in contact with one another bad, skewness, its greatest difficulty is exactly to realize the densification of block in the ideal model that satisfies soft or hard magnetic phase, thereby causes the exchange coupling between the soft or hard magnetic phase abundant inadequately.
The present invention adopts the soft magnetism/Hard Magnetic nano composite powder of SPS technology sintering cladded type, substantially improved the exchange-coupling interaction of soft magnetism, Hard Magnetic two-phase, the crystal grain of the soft or hard magnetic phase that obtains is tiny, be evenly distributed, provide a new way for realizing preparation with desirable microstructural Nanocomposite magnet.
Summary of the invention
The present invention is directed to the problem that exists in the above-mentioned technology, adopt sonochemistry nanometer cladding process, prepare the Nd that crystallite dimension is evenly distributed less than 50nm and two-phase in conjunction with discharge plasma sintering technique
2Fe
14The B/Fe magnet provides a new way for realizing the preparation with desirable microstructural Nanocomposite magnet.
This preparation method comprises following concrete steps:
1) at N
2Gas or Ar gas or both are with under any atmosphere protection than mixing, with the Nd below ball milling to the 5 μ m
2Fe
14B Hard Magnetic powder is distributed in the appropriate amount of fluid n-decane;
2) add Fe (CO)
5Liquid makes Nd
2Fe
14B and Fe (CO)
5In contain Fe weight ratio be 9: 1, the temperature with this solidliquid mixture is cooled to below 0 ℃ then;
3) ultrasonic head is stretched in the above-mentioned solidliquid mixture, open supersonic generator, power is adjusted into 100-240W, and the reaction time is 1-3 hour;
4) carry out centrifugation after reaction finishes and remove liquid, solid product is cleaned for several times with pentane, promptly obtain cladded type Nd behind the pentane of waiting to volatilize
2Fe
14The nano combined Magnaglo of B/Fe;
5) above-mentioned Magnaglo is packed in the sintered-carbide die, place the discharge plasma sintering stove, predetermined fixed pressure 30-1000MPa is warmed up to 500-700 ℃ with the speed of 40-100 ℃/min and carries out sintering, sintering time 2-10 minute in Ar compression ring border;
6) sample cooled off with stove after sintering finished, and obtained fine and close Nd
2Fe
14The B/Fe Nanocomposite magnet.
Adopt said method can prepare fully compact massive biphase built-up magnet, wherein the crystal grain of soft magnetism phase, Hard Magnetic phase is tiny, is evenly distributed, and provides a new way for realizing the preparation with desirable microstructural Nanocomposite magnet.
Description of drawings
Fig. 1 is the cladded type Nd of sonochemical method preparation among the embodiment 1
2Fe
14The scanning electron micrograph of the nano combined magnetic of B/Fe;
Fig. 2 is Nd among the embodiment 1
2Fe
14The transmission electron micrograph of B/Fe biphase built-up magnet;
Fig. 3 is Nd among the embodiment 2
2Fe
14The transmission electron micrograph of B/Fe biphase built-up magnet;
Embodiment
Embodiment 1.
At inertia N
2Under the gas shiled, with the Nd below ball milling to the 5 μ m
2Fe
14B Hard Magnetic powder is distributed in the liquid n-decane; Add Fe (CO)
5Liquid makes Nd
2Fe
14B and Fe (CO)
5The weight ratio of middle Fe is 9: 1, and the temperature with this solidliquid mixture is cooled to below 0 ℃ then, and the temperature with this solidliquid mixture is cooled to below 0 ℃ then; Ultrasonic head is stretched in the above-mentioned solidliquid mixture, open supersonic generator, power is adjusted into 100W, and the reaction time is 3 hours; Carry out centrifugation after reaction finishes and remove liquid, solid product is cleaned for several times with pentane, promptly obtain cladded type Nd behind the pentane of waiting to volatilize
2Fe
14The nano combined Magnaglo of B/Fe, as shown in Figure 1, after sonochemistry coats, Nd
2Fe
14The B particle surface has covered the superfine Fe particle of one deck, and its size is less than 100nm; Material is packed in the sintered-carbide die, place the discharge plasma sintering stove, predetermined fixed pressure 30MPa is warmed up to 500 ℃ with the speed of 40 ℃/min and carries out sintering, sintering time 2 minutes in Ar compression ring border; Sintering finishes the back sample and cools off with stove, obtains the Nd of density 98.2%
2Fe
14B/Fe Nanocomposite magnet, its microscopic structure as shown in Figure 2, white particle is a Fe crystal grain among the figure, grey and black particle are Nd
2Fe
14B crystal grain, as can be seen, Nd
2Fe
14B mutually with Fe mutually two-phase crystal grain be evenly distributed, size is all at 20-30nm.Measure Nd through the BH loop instrument
2Fe
14The magnetic property result of B/Fe Nanocomposite magnet is as follows: Br=0.92T, Hci=723.6kA/m, (BH) max=106.1kJ/m
3
Embodiment 2.
Under inertia Ar gas shiled, with the Nd below ball milling to the 5 μ m
2Fe
14B Hard Magnetic powder is distributed in the liquid n-decane; Add Fe (CO)
5Liquid makes Nd
2Fe
14B and Fe (CO)
5The weight ratio of middle Fe is 9: 1, and the temperature with this solidliquid mixture is cooled to below 0 ℃ then, and the temperature with this solidliquid mixture is cooled to below 0 ℃ then; Ultrasonic head is stretched in the above-mentioned solidliquid mixture, open supersonic generator, power is adjusted into 150W, and the reaction time is 2 hours; Carry out centrifugation after reaction finishes and remove liquid, solid product is cleaned for several times with pentane, promptly obtain cladded type Nd behind the pentane of waiting to volatilize
2Fe
14The nano combined Magnaglo of B/Fe; Material is packed in the sintered-carbide die, place the discharge plasma sintering stove, predetermined fixed pressure 500MPa is warmed up to 630 ℃ with the speed of 70 ℃/min and carries out sintering, sintering time 5 minutes in Ar compression ring border; Sintering finishes the back sample and cools off with stove, obtains the Nd of density 98.7%
2Fe
14B/Fe Nanocomposite magnet, its microscopic structure as shown in Figure 3, white particle is a Fe crystal grain among the figure, grey and black particle are Nd
2Fe
14B crystal grain, as can be seen, Nd
2Fe
14B mutually with Fe mutually two-phase crystal grain be evenly distributed, size is all at 20-30nm.Measure Nd through the BH loop instrument
2Fe
14The magnetic property result of B/Fe Nanocomposite magnet is as follows: B
r=0.94T, H
Ci=648.7kA/m, (BH)
Max=113.6kJ/m
3
Embodiment 3.
At inertia N
2, Ar gaseous mixture protection down, with the Nd below ball milling to the 5 μ m
2Fe
14B Hard Magnetic powder is distributed in the liquid n-decane; Add Fe (CO)
5Liquid makes Nd
2Fe
14B and Fe (CO)
5The weight ratio of middle Fe is 9: 1, and the temperature with this solidliquid mixture is cooled to below 0 ℃ then, and the temperature with this solidliquid mixture is cooled to below 0 ℃ then; Ultrasonic head is stretched in the above-mentioned solidliquid mixture, open supersonic generator, power is adjusted into 240W, and the reaction time is 3 hours; Carry out centrifugation after reaction finishes and remove liquid, solid product is cleaned for several times with pentane, promptly obtain cladded type Nd behind the pentane of waiting to volatilize
2Fe
14The nano combined Magnaglo of B/Fe; Material is packed in the sintered-carbide die, place discharge plasma sintering (SPS) stove, predetermined fixed pressure 1000MPa is warmed up to 700 ℃ with the speed of 100 ℃/min and carries out sintering, sintering time 10 minutes in Ar compression ring border; Sintering finishes the back sample and cools off with stove, obtains the Nd of density 98.8%
2Fe
14The B/Fe Nanocomposite magnet, Nd
2Fe
14B mutually with Fe mutually two-phase crystal grain be evenly distributed, size is all at 20-30nm.It is as follows to measure magnetic property through the BH loop instrument: B
r=0.88T, H
Ci=637.6kA/m, (BH)
Max=99.7kJ/m
3
Claims (1)
1. Nd
2Fe
14B/Fe biphase nanocrystalline composite permanent-magnet material preparation method is characterized in that, may further comprise the steps:
1) at N
2Gas or Ar gas or both are with under any atmosphere protection than mixing, with the Nd below ball milling to the 5 μ m
2Fe
14B Hard Magnetic powder is distributed in the liquid n-decane;
2) add Fe (CO)
5Liquid makes Nd
2Fe
14B and Fe (CO)
5The weight ratio of the contained Fe of liquid is 9: 1, and the temperature with this solidliquid mixture is cooled to below 0 ℃ then;
3) ultrasonic head is stretched in the above-mentioned solidliquid mixture, open supersonic generator, power is adjusted into 100-240W, and the reaction time is 1-3 hour;
4) carry out centrifugation after reaction finishes and remove liquid, solid product is cleaned with pentane, promptly obtain cladded type Nd behind the pentane of waiting to volatilize
2Fe
14The nano combined Magnaglo of B/Fe;
5) above-mentioned Magnaglo is packed in the sintered-carbide die, place the discharge plasma sintering stove, predetermined fixed pressure 30-1000MPa is warmed up to 500-700 ℃ with the speed of 40-100 ℃/min and carries out sintering, sintering time 2-10 minute in Ar compression ring border;
6) sample cooled off with stove after sintering finished, and obtained fine and close Nd
2Fe
14The B/Fe Nanocomposite magnet.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610089122 CN1889201A (en) | 2006-08-04 | 2006-08-04 | Method for producing Nd2Fe14B/Fe double-phase nano crystal composite permanent-magnetic materials |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610089122 CN1889201A (en) | 2006-08-04 | 2006-08-04 | Method for producing Nd2Fe14B/Fe double-phase nano crystal composite permanent-magnetic materials |
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| Publication Number | Publication Date |
|---|---|
| CN1889201A true CN1889201A (en) | 2007-01-03 |
Family
ID=37578468
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101425355B (en) * | 2008-07-31 | 2011-04-13 | 中国计量学院 | Pr/Nd based biphase composite permanent magnetic material and block body preparing method thereof |
| CN102114537A (en) * | 2011-03-14 | 2011-07-06 | 中国科学院宁波材料技术与工程研究所 | Method for preparing enriched rare earth nanometer crystal dual-phase composite magnetic powder |
| CN110586951A (en) * | 2018-06-13 | 2019-12-20 | 中国科学院宁波材料技术与工程研究所 | High-saturation-magnetism ultrafine-grain nano dual-phase permanent magnet material and preparation method thereof |
| CN110858508A (en) * | 2018-08-24 | 2020-03-03 | 中国科学院宁波材料技术与工程研究所 | High-performance anisotropic nanocrystalline dual-phase magnetic powder and preparation method thereof |
-
2006
- 2006-08-04 CN CN 200610089122 patent/CN1889201A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101425355B (en) * | 2008-07-31 | 2011-04-13 | 中国计量学院 | Pr/Nd based biphase composite permanent magnetic material and block body preparing method thereof |
| CN102114537A (en) * | 2011-03-14 | 2011-07-06 | 中国科学院宁波材料技术与工程研究所 | Method for preparing enriched rare earth nanometer crystal dual-phase composite magnetic powder |
| CN110586951A (en) * | 2018-06-13 | 2019-12-20 | 中国科学院宁波材料技术与工程研究所 | High-saturation-magnetism ultrafine-grain nano dual-phase permanent magnet material and preparation method thereof |
| CN110586951B (en) * | 2018-06-13 | 2022-04-12 | 中国科学院宁波材料技术与工程研究所 | High-saturation-magnetism ultrafine-grain nano dual-phase permanent magnet material and preparation method thereof |
| CN110858508A (en) * | 2018-08-24 | 2020-03-03 | 中国科学院宁波材料技术与工程研究所 | High-performance anisotropic nanocrystalline dual-phase magnetic powder and preparation method thereof |
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