CN101651037B - Method for preparing Nanocrystalline NdFeB high-compactness magnet - Google Patents
Method for preparing Nanocrystalline NdFeB high-compactness magnet Download PDFInfo
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- CN101651037B CN101651037B CN2009100726258A CN200910072625A CN101651037B CN 101651037 B CN101651037 B CN 101651037B CN 2009100726258 A CN2009100726258 A CN 2009100726258A CN 200910072625 A CN200910072625 A CN 200910072625A CN 101651037 B CN101651037 B CN 101651037B
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Abstract
The invention discloses a method for preparing a nanocrystalline NdFeB high-compactness magnet and relates to a method for preparing a nanocrystalline NdFeB magnet. The invention solves the problems that a bonded magnet prepared by the prior method is poor in low magnetic performance and mechanical strength and small relative density. The method comprises the following steps: breaking NdFeB casting alloy into coarse powder and carrying out the high energy ball milling of rough powder at room temperature in a hydrogen atmosphere for 10-30 hours to obtain nanocrystalline disproportionate state NdFeB alloy powder; pressing the disproportionate state NdFeB alloy powder into a high-compactness magnet blank; and then sintering under the conditions of the vacuum degree of 10<-5>-10<-2>Pa and thetemperature of 700-850 DEG C for 30 minutes to 1 hour to obtain the nanocrystalline NdFeB high-compactness magnet with the crystalline grain size of 30-80nm. The nanocrystalline NdFeB high-compactness magnet prepared by the method has the relative density of more than 0.92, the compressive strength of 212-273MPa and the magnetic energy product of 176-249k J/m<3>.
Description
Technical field
The present invention relates to a kind of preparation method of Nanocrystalline NdFeB magnet.
Background technology
The preparation method of Nanocrystalline NdFeB magnetic mainly contains quick quenching technique and mechanical ball milling method, and this class nanocrystalline magnetic is mainly used in the preparation bonded permanent magnet.At present, the fast quenching magnetic powders bonded permanent magnet that adopts Magnequench company of internationally famous magnetic material company to produce, the magnetic energy product of gained bonded permanent magnet is 85kJ/m
3About, the relative density of bonded permanent magnet is 0.64～0.85, and the compression strength of bonded permanent magnet is 130～200MPa, and its magnetic property and mechanical strength index are difficult to satisfy the needs that relevant high-end industrial technology develops.Therefore, must develop preparation and have the more method of the high density nano crystalline substance NdFeB magnet of high magnetic characteristics and mechanical strength.
Summary of the invention
Technical problem to be solved by this invention is for the bonded permanent magnet magnetic that solves existing method preparation, the problem that energy is low, relative density is little and mechanical strength is low, and a kind of new process for preparing Nanocrystalline NdFeB high-compactness magnet is provided.
The preparation method of Nanocrystalline NdFeB compactness magnet of the present invention is as follows: one, adopting Mechanical Method or the quick-fried method of hydrogen that the NdFeB cast alloy is broken into particle diameter is 0.5～1mm meal; Two, meal is carried out high-energy ball milling 10～30h under room temperature, hydrogen atmosphere, realize hydrogenation-disproportionation-, obtain by crystallite dimension all less than the disproportionation phase NdH of 10nm
2 ± χ, α-Fe and Fe
2The disproportionation attitude NdFeB alloy powder that B forms; Three, adopting the normal temperature mould pressing method, is under the condition of 1000～1500MPa disproportionation attitude NdFeB alloy powder to be pressed into the high-compactness magnet blank at pressing pressure; Four, be 10 with the high-compactness magnet blank in vacuum degree
-5～10
-2Pa, temperature are sintering 30 minutes～1 hour under 700～850 ℃ the condition, promptly obtain its main magnetic phase Nd
2Fe
14The B crystallite dimension is the Nanocrystalline NdFeB high-compactness magnet of 30～80nm.
Adopt the relative density of the Nanocrystalline NdFeB high-compactness magnet of the inventive method preparation to reach more than 0.92, compression strength is 212～273MPa, and magnetic energy product is 176～249k J/m
3The inventive method technology is simple, process is easy to control, cost is low, moulding is easy, because NdH
2 ± χ, α-Fe and Fe
2It is Nd that the suppression performance of the disproportionation attitude NdFeB alloy powder that B forms is much better than principal phase
2Fe
14The fast quenching NdFeB manocrystalline powders of B so be easy to according to user demand, is produced strip, sheet, tubulose, high-compactness magnet product circular or other complicated shapes, and is convenient to produce in batches.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the preparation method of Nanocrystalline NdFeB high-compactness magnet is as follows in the present embodiment: one, adopting Mechanical Method or the quick-fried method of hydrogen that the NdFeB cast alloy is broken into particle diameter is 0.5～1mm meal; Two, meal is carried out high-energy ball milling 10～30h under room temperature, hydrogen atmosphere, realize hydrogenation-disproportionation-, obtain by crystallite dimension all less than the disproportionation phase NdH of 10nm
2 ± χ, α-Fe and Fe
2The disproportionation attitude NdFeB alloy powder that B forms; Three, adopting the normal temperature mould pressing method, is under the condition of 1000～1500MPa disproportionation attitude NdFeB alloy powder to be pressed into the high-compactness magnet blank at pressing pressure; Four, be 10 with the high-compactness magnet blank in vacuum degree
-5～10
-2Pa, temperature are sintering 30 minutes～1 hour under 700～850 ℃ the condition, promptly obtain its main magnetic phase Nd
2Fe
14The B crystallite dimension is the Nanocrystalline NdFeB high-compactness magnet of 30～80nm.
The mass content of α-Fe is 70% in the described disproportionation attitude of the present embodiment step 2 NdFeB alloy powder; The relative density of magnet blank is more than 0.92 in the step 3.
The relative density of the Nanocrystalline NdFeB compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 212～273MPa, and magnetic energy product is 176～249k J/m
3
Embodiment two: what present embodiment and embodiment one were different is that the Nd-Fe-B cast alloy described in the step 1 is Nd
12Fe
82B
6Alloy, Nd
8Fe
86B
6Alloy, Nd
2Fe
14B alloy, Nd
16Fe
76B
8Alloy, Nd
12.2Fe
81.8B
6Alloy, Nd
12.2Fe
80.8Ga
1B
6Alloy, Nd
12.2Fe
64.3Co
17.5B
6Alloy or Nd
14Fe
66.9Co
11B
7Zr
0.1Ga
1Alloy.Other is identical with embodiment one.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 212～273MPa, and magnetic energy product is 176～249k J/m
3
Embodiment three: present embodiment is different with embodiment one or two is that the particle diameter of the disproportionation attitude alloy powder described in the step 2 is 0.5～1 μ m.Other is identical with embodiment one or two.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 220～270MPa, and magnetic energy product is 178～245k J/m
3
Embodiment four: present embodiment and embodiment three are different be in the step 2 ball milling time be 15～25h.Other is identical with embodiment three.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 218～260MPa, and magnetic energy product is 180～240k J/m
3
Embodiment five: present embodiment and embodiment three are different be in the step 2 ball milling time be 20h.Other is identical with embodiment three.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 222～263MPa, and magnetic energy product is 186～239k J/m
3
Embodiment six: present embodiment and embodiment one, two or four are different is under pressure is the condition of 1100～1400MPa disproportionation attitude NdFeB alloy powder to be pressed into the compactness magnet blank in the step 3.Other is identical with embodiment one, two or four.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 230～260MPa, and magnetic energy product is 180～230k J/m
3
Embodiment seven: present embodiment and embodiment one, two or four are different is under pressure is the condition of 1300MPa disproportionation attitude NdFeB alloy powder to be pressed into the compactness magnet blank in the step 3.Other is identical with embodiment one, two or four.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 235～255MPa, and magnetic energy product is 177～228k J/m
3
Embodiment eight: present embodiment and embodiment six are different is to be 10 in vacuum degree in the step 4
-3Under the condition of Pa the magnet blank is carried out sintering.Other is identical with embodiment six.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 240～250MPa, and magnetic energy product is 190～220k J/m
3
Embodiment nine: present embodiment and embodiment one, two, four or eight are different is under temperature is 800 ℃ condition the magnet blank to be carried out sintering in the step 4.Other is identical with embodiment one, two, four or eight.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 245～250MPa, and magnetic energy product is 200～210k J/m
3
Embodiment ten: present embodiment and embodiment nine are different is that the sintering time of densified sintering product magnet blank in the step 4 is 45 minutes.Other is identical with embodiment nine.
The relative density of the Nanocrystalline NdFeB high-compactness magnet of present embodiment preparation reaches 0.952, and compression strength is 248MPa, and magnetic energy product is 199k J/m
3
Claims (10)
1. the preparation method of Nanocrystalline NdFeB high-compactness magnet is characterized in that the preparation method of Nanocrystalline NdFeB high-compactness magnet is as follows: one, adopting Mechanical Method or the quick-fried method of hydrogen that the NdFeB cast alloy is broken into particle diameter is 0.5～1mm meal; Two, meal is carried out high-energy ball milling 10～30h under room temperature, hydrogen atmosphere, realize hydrogenation-disproportionation-, obtain by crystallite dimension all less than the disproportionation phase NdH of 10nm
2 ± χ, α-Fe and Fe
2The disproportionation attitude NdFeB alloy powder that B forms; Three, adopting the normal temperature mould pressing method, is under the condition of 1000～1500MPa disproportionation attitude NdFeB alloy powder to be pressed into the high-compactness magnet blank at pressing pressure; Four, be 10 with the high-compactness magnet blank in vacuum degree
-5～10
-2Pa, temperature are sintering 30 minutes～1 hour under 700～850 ℃ the condition, promptly obtain its main magnetic phase Nd
2Fe
14The B crystallite dimension is the Nanocrystalline NdFeB high-compactness magnet of 30～80nm.
2. the preparation method of Nanocrystalline NdFeB high-compactness magnet according to claim 1 is characterized in that the NdFeB cast alloy described in the step 1 is Nd
12Fe
82B
6Alloy, Nd
8Fe
86B
6Alloy, Nd
2Fe
14B alloy, Nd
16Fe
76B
8Alloy or Nd
12.2Fe
81.8B
6Alloy.
3. the preparation method of Nanocrystalline NdFeB high-compactness magnet according to claim 1 and 2, the particle diameter that it is characterized in that the disproportionation attitude alloy powder described in the step 2 is 0.5～1 μ m.
4. the preparation method of Nanocrystalline NdFeB high-compactness magnet according to claim 3 is characterized in that the ball milling time is 15～25h in the step 2.
5. the preparation method of Nanocrystalline NdFeB high-compactness magnet according to claim 3 is characterized in that the ball milling time is 20h in the step 2.
6. according to the preparation method of claim 1,2 or 4 described Nanocrystalline NdFeB high-compactness magnets, it is characterized in that in the step 3 under pressure is the condition of 1100～1400MPa, disproportionation attitude NdFeB alloy powder being pressed into the high-compactness magnet blank.
7. according to the preparation method of claim 1,2 or 4 described Nanocrystalline NdFeB high-compactness magnets, it is characterized in that in the step 3 under pressure is the condition of 1300MPa, disproportionation attitude NdFeB alloy powder being pressed into the compactness magnet blank.
8. the preparation method of Nanocrystalline NdFeB high-compactness magnet according to claim 6 is characterized in that in the step 4 in vacuum degree being 10
-3Under the condition of Pa the magnet blank is carried out sintering.
9. according to the preparation method of claim 1,2,4 or 8 described Nanocrystalline NdFeB high-compactness magnets, it is characterized in that in the step 4 under temperature is 800 ℃ condition, the magnet blank being carried out sintering.
10. the preparation method of Nanocrystalline NdFeB high-compactness magnet according to claim 9, the sintering time that it is characterized in that densified sintering product magnet blank in the step 4 is 45 minutes.
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| CN101651037B true CN101651037B (en) | 2011-06-22 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103123843B (en) * | 2011-11-21 | 2015-10-07 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of fine grain anisotropy densification Nd-Fe-B permanent magnet |
| CN102403118B (en) * | 2011-11-23 | 2013-05-08 | 北京航空航天大学 | Preparation method of anisotropic samarium cobalt-based nanocrystalline rare earth permanent magnet |
| CN103310972A (en) * | 2012-10-09 | 2013-09-18 | 中磁科技股份有限公司 | Method for preparing high-performance sintered Nd-Fe-B magnet |
| CN103426623B (en) * | 2013-08-05 | 2015-12-02 | 四川大学 | A kind of preparation method of anisotropy nano-crystalline neodymium-iron-boronmagnet magnet |
| CN110246644B (en) * | 2019-08-01 | 2020-08-07 | 中国计量大学 | Preparation method of high-performance multi-main-phase Ce-based nanocrystalline magnet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6444052B1 (en) * | 1999-10-13 | 2002-09-03 | Aichi Steel Corporation | Production method of anisotropic rare earth magnet powder |
| CN101090014A (en) * | 2007-04-29 | 2007-12-19 | 哈尔滨工业大学 | Method for preparing nano crystal NdFcB anisotropic magnetic powder |
| CN101379574A (en) * | 2006-11-30 | 2009-03-04 | 日立金属株式会社 | R-Fe-B microcrystalline high-density magnet and process for production thereof |
-
2009
- 2009-07-31 CN CN2009100726258A patent/CN101651037B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6444052B1 (en) * | 1999-10-13 | 2002-09-03 | Aichi Steel Corporation | Production method of anisotropic rare earth magnet powder |
| CN101379574A (en) * | 2006-11-30 | 2009-03-04 | 日立金属株式会社 | R-Fe-B microcrystalline high-density magnet and process for production thereof |
| CN101090014A (en) * | 2007-04-29 | 2007-12-19 | 哈尔滨工业大学 | Method for preparing nano crystal NdFcB anisotropic magnetic powder |
Non-Patent Citations (5)
| Title |
|---|
| JP特开2002-367819A 2002.12.20 |
| 王迎 等.纳米复相稀土永磁材料研究进展.《粉末冶金技术》.2007,第25卷(第5期), |
| 王迎等.纳米复相稀土永磁材料研究进展.《粉末冶金技术》.2007,第25卷(第5期), * |
| 石刚 等.机械球磨与HDDR结合制备纳米晶Nd12Fe82B6合金粉末及其组织特征.《稀有金属材料与工程》.2006,第35卷(第4期), |
| 石刚等.机械球磨与HDDR结合制备纳米晶Nd12Fe82B6合金粉末及其组织特征.《稀有金属材料与工程》.2006,第35卷(第4期), * |
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