CN106898486A - A kind of preparation method of high-performance Ne-Fe-B permanent magnet - Google Patents
A kind of preparation method of high-performance Ne-Fe-B permanent magnet Download PDFInfo
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- CN106898486A CN106898486A CN201510958714.8A CN201510958714A CN106898486A CN 106898486 A CN106898486 A CN 106898486A CN 201510958714 A CN201510958714 A CN 201510958714A CN 106898486 A CN106898486 A CN 106898486A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The present invention provides a kind of preparation method of high-performance Ne-Fe-B permanent magnet, and the preparation method comprises the following steps：1) rare earth metal powder and organic solvent are first compared 1 according to weight：5 are mixed, rod milling, filtering, with the rare earth metal powder after being filtered；Wherein, the organic solvent is the monohydric alcohol and/or resin of C1~C4, and the rare earth metal powder is more than 80% with the percentage by weight of the organic solvent；2) after filtering, Nd-Fe-B permanent magnet sample is sprayed using spraying equipment under pressure 0.15-0.4MPA air pressure, is dried naturally, to obtain the Nd-Fe-B permanent magnet with rare earth metal.
Description
Technical field
The present invention relates to a kind of new coating technology for improving coating binding force, and the preparation method of the performance of Nd-Fe-B permanent magnet is directly improved using rare earth metal.
Background technology
The application of neodymium iron boron (NdFeB) permanent-magnet material in recent years and development are very rapid, and the protection success or not of Nd-Fe-B permanent magnet material be related to material can popularization and application one of key technology.The material is mainly and is prepared from by powder metallurgical technique by elements such as rare earth metal neodymium Nd, iron and boron.As magnetic material most strong at present, all fields such as electroplating device, machinery, medical treatment, automobile are had been widely used for, application prospect is very wide.But with the further rise of heavy rare earth dysprosium terbium price, external neodymium iron boron enterprise especially Japanese enterprises using being deposited with (CN103597108), the method for coating (CN201210410546) improves the magnetic property of neodymium iron boron by the way of neodymium iron boron is heat-treated.
But it is poor by ethanol solution formation coating binding force that above-mentioned technology is difficult to solution, easy to fall off, and introduces other metal impurities.It uses fluoride or oxide in addition, the poor-performing in material preparation.
The content of the invention
In order to solve above-mentioned the deficiencies in the prior art part, the present invention provides a kind of preparation method of high-performance Ne-Fe-B permanent magnet, and the preparation method comprises the following steps：The preparation method comprises the following steps：1) rare earth metal or rare earth alloy powder and organic solvent are first compared 1 according to weight：4-10 is mixed, rod milling, filtering, with the flaky rare earth metal dust after being filtered；Wherein, the organic solvent is the monohydric alcohol and/or resin of C1~C4, and the rare earth metal powder or rare earth alloy powder are more than 80% with the percentage by weight of the organic solvent；2) after filtering, Nd-Fe-B permanent magnet sample is sprayed using spraying equipment under pressure 0.15-0.4MPA air pressure, is dried naturally, to obtain the Nd-Fe-B permanent magnet with rare earth metal.
Further illustrated as to the preparation method of the invention, preferably, be additionally included in step 1) in mixed before, in the organic solvent add anti-settling agent or dispersant, the content of the anti-settling agent or dispersant in the organic solvent be 0.8-1.5wt.%.
Further illustrated as to the preparation method of the invention, preferably, the rare earth metal powder is dysprosium powder, terbium powder or dysprosium powder and terbium powder mixed-powder, the rare earth alloy powder is the rare earth alloy powder containing any element in dysprosium or terbium, and the D50 of the flaky rare earth metal dust after the filtering is 1-15 microns.D50 tests use the wet method testing graininess of Malvern 2000.
Further illustrated as to the preparation method of the invention, it is preferable that the monohydric alcohol of the C1~C4 is methyl alcohol, ethanol, propyl alcohol or butanol；Preferably, the monohydric alcohol of the C1~C4 is anhydrous.The resin is epoxy resin or acrylic resin.
Further illustrated as to the preparation method of the invention, it is preferable that the anti-settling agent is glycerine or hydroxyl first class cellulose, the dispersant is polyethylene glycol, citric acid or Si Mahuagong CE64.
Further illustrated as to the preparation method of the invention, it is preferable that 300-1000 revs/min of the rotating speed during rod milling.
Further illustrated as to the preparation method of the invention, it is preferable that once filtered using screen cloth more than 100-300 mesh, the pressure of the filtering is less than 0.2MPA.
Further illustrated as to the preparation method of the invention, it is preferable that carry out secondary filter using 5~20 microns of screen clothes, the pressure of the filtering is less than 0.2MPA..
Further illustrated as to the preparation method of the invention, it is preferable that the thickness of sprayed coating is at 5-20 microns.
Further illustrated as to the preparation method of the invention, it is preferable that before the spraying of Nd-Fe-B permanent magnet sample, conventional chemical oil removing and acid pickling and rust removing are carried out to Nd-Fe-B permanent magnet sample.
Product after the method for the present invention is sprayed is heat-treated, by the way that after vacuum heat, magnet performance is improved.
Brief description of the drawings
Fig. 1 is product of the rare earth metal flakelike powder size less than 30 microns after filtering of the invention；
Fig. 2 is the product after the Mm filter of rare earth metal flakelike powder size 15 sieve after filtering of the invention.
Specific embodiment
In order that auditor can further appreciate that structure of the invention, feature and other purposes, it is accompanied by accompanying drawing in conjunction with appended preferred embodiment and describes in detail as follows, this accompanying drawing embodiment described is merely to illustrate technical scheme, and the non-limiting present invention.
Embodiment 1
900 μm of terbium powder of D50 and absolute ethyl alcohol are first compared 1 according to weight：5 are mixed, are carried out rod milling according to conventional rod milling technique, 300-1000 revs/min of rotating speed during rod milling, then the screen cloth of 400 mesh is crossed, filtered again, filtering uses 15 microns of screen cloth, filter pressure is less than 0.2MPA. and then tests granularity, the wet method testing graininess of testing graininess equipment choosing Malvern 2000.Its D50 is 2.12 microns, sees Fig. 2, and its microstructure to see Fig. 1, and powder is distributed in the form of sheets.Take 1wt.% dispersant Sima chemical industry CE64, it is added thereto to 1wt.% acrylic resins and absolute ethyl alcohol is mixed, the D50 for being subsequently adding above-mentioned preparation is 2.12 microns of terbium powder, by after 2000 revs/min of mixing of dispersing speed, it is the sample of 35*5.2*2 that specification is sprayed under pressure 0.15-0.4MPA air pressure, naturally dry, spray layer thickness is at 10 microns.Then one side in addition is sprayed.Wherein, conventional chemical oil removing and acid pickling and rust removing are carried out before sample spraying, spraying equipment is conventional spray gun and spraying equipment.
580 degree of specification 35*5.2*2 raw materials heat treatment temperature, 10 hours time.Wherein raw material carries out magnetism testing with treatment sample, is specifically shown in Table 1.
Table 1
As can be seen from Table 1, after heat treatment, magnetic property is improved largely magnet, especially HCJ coercivities.
Embodiment 2
D50 is first compared 1 in 1000 microns of dysprosium powder and absolute methanol according to weight：10 are mixed, are carried out rod milling according to conventional rod milling technique, 300 revs/min of rotating speed during rod milling, then the screen cloth of 100 mesh is crossed, filtered again, filtering uses 20 microns of screen cloth, filter pressure is less than 0.2MPA. and then tests granularity, the wet method testing graininess of testing graininess equipment choosing Malvern 2000.Its D50 is 5.12 microns, and it is that sheet takes 15wt.% dispersants citric acid and anti-settling agent glycerine, it is added thereto to 1wt.% epoxy resin and absolute methanol is mixed, D50 is subsequently adding for 6.2 microns of terbium powder, by the way that after 2000 revs/min of mixing of dispersing speed, it is the sample of 35*5.2*2 that specification is sprayed under pressure 0.15-0.4MPA air pressure, naturally dry, spray layer thickness is at 10 microns.Then one side in addition is sprayed.Wherein, conventional chemical oil removing and acid pickling and rust removing are carried out before sample spraying, spraying equipment is conventional spray gun and spraying equipment.
520 degree of specification 35*5.2*2 raw materials heat treatment temperature, 20 hours time.Wherein raw material carries out magnetism testing with treatment sample, is specifically shown in Table 2.
Table 2
As can be seen from Table 2, after heat treatment, magnetic property is improved largely magnet, especially HCJ coercivities.
Embodiment 3
It is first that 900 microns of dysprosium powder and anhydrous isopropyl alcohol compare 1 according to weight by D50：8 are mixed, are carried out rod milling according to conventional rod milling technique, 300 revs/min of rotating speed during rod milling, then the screen cloth of 300 mesh is crossed, filtered again, filtering uses 5 microns of screen cloth, filter pressure is less than 0.2MPA. and then tests granularity, the wet method testing graininess of testing graininess equipment choosing Malvern 2000.Its D50 is 1.3 microns, and it is that sheet takes 0.8wt.% dispersants polyethylene glycol and anti-settling agent hydroxyl first class cellulose, it is added thereto to 0.8wt.% epoxy resin and absolute methanol is mixed, D50 is subsequently adding for 6.2 microns of terbium powder, by the way that after 2000 revs/min of mixing of dispersing speed, it is the sample of 35*5.2*2 that specification is sprayed under pressure 0.15-0.4MPA air pressure, naturally dry, spray layer thickness is at 20 microns.Then one side in addition is sprayed.Wherein, conventional chemical oil removing and acid pickling and rust removing are carried out before sample spraying, spraying equipment is conventional spray gun and spraying equipment.
720 degree of specification 35*5.2*2 raw materials heat treatment temperature, 12 hours time.Wherein raw material carries out magnetism testing with treatment sample, is specifically shown in Table 3.
Table 3
As can be seen from Table 3, after heat treatment, magnetic property is improved largely magnet, especially HCJ coercivities.
Embodiment 4
First compare 1 according to weight in 1000 microns of terbium powder and anhydrous butanol by 50：5 are mixed, are carried out rod milling according to conventional rod milling technique, 300 revs/min of rotating speed during rod milling, then the screen cloth of 200 mesh is crossed, filtered again, filtering uses 5 microns of screen cloth, filter pressure is less than 0.2MPA. and then tests granularity, the wet method testing graininess of testing graininess equipment choosing Malvern 2000.Its D50 is 0.99 micron, and it is sheet by Si Mahuagong dispersing agent Cs E64, it is added thereto to 1wt.% epoxy resin and anhydrous butanol is mixed, D50 is subsequently adding for 0.99 micron of terbium powder, by the way that after 2000 revs/min of mixing of dispersing speed, it is the sample of 35*5.2*2 that specification is sprayed under pressure 0.15-0.4MPA air pressure, naturally dry, spray layer thickness is at 15 microns.Then one side in addition is sprayed.Wherein, conventional chemical oil removing and acid pickling and rust removing are carried out before sample spraying, spraying equipment is conventional spray gun and spraying equipment.
520 degree of specification 35*5.2*2 raw materials heat treatment temperature, 20 hours time.Wherein raw material carries out magnetism testing with treatment sample, is specifically shown in Table 4.
Table 4
As can be seen from Table 4, after heat treatment, magnetic property is improved largely magnet, especially HCJ coercivities.
It is to be understood that, foregoing invention content and specific embodiment are intended to prove the practical application of technical scheme provided by the present invention, should not be construed as limiting the scope of the present invention.Those skilled in the art in spirit and principles of the present invention, when can various modifications may be made, equivalent or improvement.Protection scope of the present invention is defined by appended claims.
Claims (10)
1. a kind of preparation method of high-performance Ne-Fe-B permanent magnet, it is characterised in that the preparation
Method comprises the following steps：
1) rare earth metal or rare earth alloy powder and organic solvent are first compared 1 according to weight：4-10
Mixed, rod milling, filtering, with the flaky rare earth metal dust after being filtered；Wherein,
The organic solvent for C1~C4 monohydric alcohol and/or resin, the rare earth metal powder with it is described
The percentage by weight of organic solvent is more than 80%；
2) filter after, under pressure 0.15-0.4MPA air pressure using spraying equipment to neodymium iron boron forever
Magnet sample is sprayed, dried naturally, to obtain the Nd-Fe-B permanent magnet with rare earth metal.
2. preparation method as claimed in claim 1, it is characterised in that be additionally included in step 1)
In mixed before, in the organic solvent add anti-settling agent or dispersant, the anti-settling agent
Or content of the dispersant in the organic solvent is 0.8-1.5wt.%.
3. preparation method as claimed in claim 1 or 2, it is characterised in that the rare earth metal
Powder be dysprosium powder, terbium powder or dysprosium powder and terbium powder mixed-powder, the rare earth alloy powder be containing
There is the rare earth alloy powder of any element in dysprosium or terbium, the flaky rare earth gold after the filtering
The D50 for belonging to powder is 1-15 micron, the monohydric alcohol of the C1~C4 be methyl alcohol, ethanol, propyl alcohol or
Butanol；The resin is epoxy resin or acrylic resin.
4. preparation method as claimed in claim 1 or 2, it is characterised in that the C1~C4's
Monohydric alcohol is anhydrous.
5. preparation method as claimed in claim 1 or 2, it is characterised in that the anti-settling agent is
Glycerine or hydroxyl first class cellulose, the dispersant are polyethylene glycol, citric acid or Si Mahuagong
CE64。
6. preparation method as claimed in claim 1 or 2, it is characterised in that during rod milling
300-1000 revs/min of rotating speed.
7. preparation method as claimed in claim 1 or 2, it is characterised in that use 100-300
Screen cloth more than mesh is once filtered, and the pressure of the filtering is less than 0.2MPA.
8. preparation method as claimed in claim 7, it is characterised in that using 5~20 microns
Screen cloth carries out secondary filter, and the pressure of the filtering is less than 0.2MPA.
9. preparation method as claimed in claim 1, it is characterised in that the thickness of sprayed coating exists
5-20 microns.
10. preparation method as claimed in claim 1, it is characterised in that in Nd-Fe-B permanent magnet
Before sample spraying, conventional chemical oil removing and acid pickling and rust removing are carried out to Nd-Fe-B permanent magnet sample.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510958714.8A CN106898486B (en) | 2015-12-18 | 2015-12-18 | Preparation method of high-performance neodymium iron boron permanent magnet |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510958714.8A CN106898486B (en) | 2015-12-18 | 2015-12-18 | Preparation method of high-performance neodymium iron boron permanent magnet |
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| CN106898486A true CN106898486A (en) | 2017-06-27 |
| CN106898486B CN106898486B (en) | 2021-05-25 |
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| CN201510958714.8A Active CN106898486B (en) | 2015-12-18 | 2015-12-18 | Preparation method of high-performance neodymium iron boron permanent magnet |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107516595A (en) * | 2017-09-19 | 2017-12-26 | 江苏晨朗电子集团有限公司 | Ooze dysprosium, terbium technique and agitating device in a kind of surface for sintered NdFeB product |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002220675A (en) * | 2001-01-23 | 2002-08-09 | Sumitomo Special Metals Co Ltd | Method for forming metal oxide film by sol-gel process |
| WO2013176096A1 (en) * | 2012-05-21 | 2013-11-28 | 日本発條株式会社 | Laminated body and method for manufacturing same |
| CN103915230A (en) * | 2014-04-11 | 2014-07-09 | 合肥工业大学 | Preparation method of corrosion resistant sintered Nd-Fe-B magnet |
| CN104134528A (en) * | 2014-07-04 | 2014-11-05 | 宁波韵升股份有限公司 | Method for improving the magnetic property of sintered NdFeB flaky magnets |
-
2015
- 2015-12-18 CN CN201510958714.8A patent/CN106898486B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002220675A (en) * | 2001-01-23 | 2002-08-09 | Sumitomo Special Metals Co Ltd | Method for forming metal oxide film by sol-gel process |
| WO2013176096A1 (en) * | 2012-05-21 | 2013-11-28 | 日本発條株式会社 | Laminated body and method for manufacturing same |
| CN103915230A (en) * | 2014-04-11 | 2014-07-09 | 合肥工业大学 | Preparation method of corrosion resistant sintered Nd-Fe-B magnet |
| CN104134528A (en) * | 2014-07-04 | 2014-11-05 | 宁波韵升股份有限公司 | Method for improving the magnetic property of sintered NdFeB flaky magnets |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107516595A (en) * | 2017-09-19 | 2017-12-26 | 江苏晨朗电子集团有限公司 | Ooze dysprosium, terbium technique and agitating device in a kind of surface for sintered NdFeB product |
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