CN105206417B - The preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force - Google Patents
The preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force Download PDFInfo
- Publication number
- CN105206417B CN105206417B CN201510755614.5A CN201510755614A CN105206417B CN 105206417 B CN105206417 B CN 105206417B CN 201510755614 A CN201510755614 A CN 201510755614A CN 105206417 B CN105206417 B CN 105206417B
- Authority
- CN
- China
- Prior art keywords
- powder
- rare earth
- magnetic
- force
- main phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention belongs to field of rare-earth permanent magnetic, the preparation method for removing magnetic coupling sintered NdFeB between a kind of main phase grain by force is specifically provided.It is characterized in that adding appropriate sulphur powder in neodymium iron boron alloy powder and low melting point rare earth-copper-aluminium alloy powder is well mixed, by magnetic field die mould and sintering densification, then product is after heat treatment obtained.It is 2 that the present invention, which is applied to any composition principal crystalline phase,:14:1 neodymium iron boron magnetic body, its advantage are that sulphur is isolated by thermal evaporation realization to magnetic powder particle with the gas phase of crystal grain in sintering process, while low melting point rare earth-albronze and 2:14:1 phase has good wetability, and the Sintered NdFeB magnet main phase grain of preparation is completely separated, so as to obtain high-coercive force.
Description
Technical field
The invention belongs to field of rare-earth permanent magnetic, magnetic coupling sintered NdFeB is removed by force between more particularly to a kind of main phase grain
Preparation method.
Background technology
Be described as the Sintered NdFeB magnet of " magnetic king " turns into electric power, telecommunication, automobile, computer, biomedicine and family
The Core Feature material in the fields such as electrical appliance, it is applied to the generating of electronic (or hybrid electrically) automobile of hundreds of kilowatts of manufacture
Mechanical, electrical motivation, and the wind-power electricity generation magneto of manufacture megawatt magnitude.
The coercivity of sintered NdFeB is an important parameter, and the coercivity of one side sintered NdFeB is improved and can driven
The raising of other combination properties, the coercivity of another aspect sintered NdFeB also have very big room for promotion, and still deficiency is managed at present
By the 30% of value.It is that coercivity is that an institutional framework is quick that Sintered NdFeB magnet coercivity, which is far below the main reason for theoretical value,
Feel parameter, and actual tissue structure and desired tissue structure have a larger gap, for example crystallite dimension is not tiny enough and 2:14:
The crystal anisotropy constant K 1 of 1 main phase grain superficial layer is relatively low, while crystal boundary rich-Nd phase can not be 2:14:1 phase intercrystalline is in
Lamelliform is continuously distributed, realizes fully effective earth magnetism isolation, and one it is particularly significant the reason for.Therefore, high rectify is obtained
The Sintered NdFeB magnet of stupid power, except refining grain size and reinforcing 2:14:Outside the anisotropy of 1 grain surface layer, it is necessary to
Ensure that rich-Nd phase is uniformly distributed in around all Nd2Fe14B crystal grain in lamelliform.
The rare earth (La, Ce, Pr, Nd, Tb, Dy, Ho, Gd, Y) of certain ingredients scope-albronze (content of rare earth 50-
90% atomic percentage) fusing point it is relatively low (400-800 DEG C or so), with 2:14:1 phase has good wetability, and this is in correlation
(application number 201510029340.1,201510335273.6 and 201510335165.9) is had been reported in patent.Simple substance simultaneously
112 DEG C of the fusing point of sulphur, 444.6 DEG C of boiling point, that is, the steams of tool S2 compositions are boiled into 444.6 DEG C, therefore can realize pair
The gas phase isolation of magnetic powder particle, so that 2:14:Preferably separated between 1 main phase grain.
The content of the invention
The invention provides the preparation method for removing magnetic coupling sintered NdFeB between a kind of main phase grain by force.It is characterized in that
Appropriate sulphur powder is added in neodymium iron boron alloy powder and low melting point rare earth-copper-aluminium alloy powder is well mixed, by magnetic field die mould and is burnt
Knot densification, then after tempered heat treatment, obtain 2:14:1 main phase grain removes magnetic coupling high-coercive force neodymium by force by completely separated
Iron boron magnet.
It is of the invention that mainly magnetic powder particle and the isolation of the gas phase of crystal grain and rare earth-copper aluminium are closed by thermal evaporation realize using sulphur
Gold and 2:14:The good wettability of 1 phase, prepare 2:14:1 main phase grain is by completely separated high-coercive force sintered NdFeB magnetic
Body, it is based primarily upon at 2 points：1. elemental sulfur is gasified at 444.6 DEG C, therefore can realize to magnetic powder particle and sinter the gas of crystal grain
It is isolated；2. the rare earth of certain ingredients-albronze fusing point is relatively low (400-800 DEG C or so), with 2:14:1 phase has good
Wetability, it is possible to achieve each 2:14:There is Grain-Boundary Phase separation around 1 main phase grain, prevent 2:14:1 intercrystalline magnetic is handed over
Change coupling.
The preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force, it is characterized in that in neodymium iron boron alloy powder
Add appropriate sulphur powder and low melting point rare earth-copper-aluminium alloy powder is well mixed, by magnetic field die mould and sintering densification, then pass through
After heat treatment, 2 are obtained:14:1 main phase grain removes magnetic coupling high-coercive force neodymium iron boron magnetic body by force by completely separated；
Concrete technology step is：
1. Nd Fe B alloys ingot casting is broken into 3-5 μm of powder particle；
2. rare earth-albronze ingot casting is broken into 0.1-3 μm of powder particle；
3. weight fraction 0.1-2% sulphur powder (particle size 20-500nm) and weight is added in neodymium iron boron alloy powder
Fraction 2-8% rare earth-copper-aluminum alloy powder, it is well mixed；
4. mixed powder is orientated die mould and isostatic pressed under more than 1.8T magnetic fields；
5. by pressed compact vacuum-sintering；Sintering temperature is 850-1050 DEG C, sintering time 1-4h, vacuum 10-3Pa。
6. temper obtains product.Temper temperature is respectively 600-800 DEG C and 350-550 DEG C, at tempering
The reason time is 1-4h, vacuum 10-3Pa。
Nd Fe B alloys composition described in step 1 both can be 2:14:1 alloy just divided, can be 2 again:14:1+ richness neodymiums
The alloy of phase.
The invention has the advantages that：
1. sulphur is isolated by the thermal evaporation gas phase to magnetic powder particle, finally realize rare earth-albronze to 2:14:1 phase crystal grain
It is completely isolated；
2. the metal sulfide of the chemical combination such as sulphur and neodymium, iron generation suppresses grain growth, crystal grain thinning, and to magnetic domain in crystal boundary
Play pinning effect；
3. realizing low-temperature sintering, temperature is reduced, has saved the energy；
4. realizing intercrystalline removes by force magnetic coupling high-coercive force Sintered NdFeB magnet；
5. the present invention has 2 suitable for any composition:14:The neodymium iron boron product of 1 main phase grain.
Embodiment
Embodiment one：2:14:1 just dividing in master alloying powder add Pr68Cu32 alloyed powders and S powder prepare it is strong between main phase grain
Remove magnetic coupling Sintered NdFeB magnet
Nd11.76Fe82.36B5.88 (atomic percentage) master alloyings are prepared respectively and Pr68Cu32 (atomic percentage) is auxiliary
Alloy, it is respectively 300 μm and 150 μm of master alloying and auxiliary alloy sheet to prepare thickness with strip casting technique, and aerating is broken with hydrogen
It is respectively 3.5 μm and 1.5 μm of master alloying powder and auxiliary alloyed powder that stream mill, which prepares average particle size particle size, and weight is added in master alloying powder
It is that 4% auxiliary alloyed powder and weight fraction are the sulphur powder that 0.5% particle is 50nm to measure fraction, by three kinds of powder in batch mixer
It is well mixed, die mould is orientated in 1.8T magnetic field and through 200MPa isostatic presseds by uniform mixed powder, by what is obtained
Pressed compact is inserted in vacuum sintering furnace, is sintered 3h at 1000 DEG C, afterwards in 800 DEG C and 400 DEG C of difference tempering heat treatment 3h, is led
The high-coercive force neodymium iron boron magnetic body that phase crystal boundary continuously separates.
Embodiment two：(2:14:1+ richness RE phases) Pr50Nd20Cu30 alloyed powders are added in master alloying powder and S powder prepares principal phase
Intercrystalline removes by force magnetic coupling Sintered NdFeB magnet
Prepare respectively Nd8.82Pr3.94Fe79.00Co1.86Zr0.5B5.88 (atomic percentage) master alloyings and
Pr50Nd20Cu30 (atomic percentage) auxiliary alloy, the master alloying thin slice that thickness is respectively 300 μm is prepared with strip casting technique,
The auxiliary alloy thin band that thickness is 50 μm is prepared with m elt-spun overqu- enching, it is 3.0 μ to break aerating stream mill to prepare average particle size particle size with hydrogen
M master alloying powder, the auxiliary alloyed powder that average particle size particle size is 1.2 μm is prepared with the method for ball milling, weight is added in master alloying powder
It is that 5% auxiliary alloyed powder and weight fraction are the sulphur powder that 1.0% particle is 100nm to measure fraction, by three kinds of powder in batch mixer
End is well mixed, die mould is orientated in 1.8T magnetic field and through 200MPa isostatic presseds by uniform mixed powder, will obtained
Pressed compact insert in vacuum sintering furnace, 980 DEG C sinter 3h, afterwards in 820 DEG C and 420 DEG C of difference tempering heat treatment 3h, obtain
The high-coercive force neodymium iron boron magnetic body that principal phase crystal boundary continuously separates.
Claims (1)
1. the preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force, it is characterized in that adding in neodymium iron boron alloy powder
Appropriate sulphur powder and low melting point rare earth-copper-aluminium alloy powder is added to be well mixed, by magnetic field die mould and sintering densification, then through heat
After processing, 2 are obtained:14:1 main phase grain removes magnetic coupling high-coercive force neodymium iron boron magnetic body by force by completely separated；
Concrete technology step is：
1) Nd Fe B alloys ingot casting is broken into 3-5 μm of powder particle；
2) rare earth-albronze ingot casting is broken into 0.1-3 μm of powder particle；
3) sulphur powder and rare earth-copper-aluminum alloy powder are added in neodymium iron boron alloy powder, is well mixed；
4) mixed powder is orientated die mould and isostatic pressed under more than 1.8T magnetic fields；
5) by pressed compact vacuum-sintering；
6) temper obtains product：
Wherein：Nd Fe B alloys composition described in step 1) is 2:14:1 alloy just divided, or be 2:14:The conjunction of 1+ richness neodymium phases
Gold；
Wherein：The rare earth in rare earth-albronze described in step 2) is La, Ce, Pr, Nd, Tb, Dy, Ho, one in Gd, Y
Kind of principal phase or several, the copper aluminium in rare earth-albronze are a kind of principal phase or two kinds in Cu, Al, content of rare earth 50-90%
Atomic percentage；
Wherein：The percetage by weight difference 0.1-2% and 2-8% of sulphur powder and rare earth-copper-aluminium alloy powder described in step 3), sulphur
Powder particles size 20-500nm；
Wherein：Sintering temperature described in step 5) is 850-1050 DEG C, sintering time 1-4h, vacuum 10-3Pa；
Wherein：Temper temperature described in step 6) is respectively 600-800 DEG C and 350-550 DEG C, the temper time
It is 1-4h, vacuum 10-3Pa。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510755614.5A CN105206417B (en) | 2015-11-09 | 2015-11-09 | The preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510755614.5A CN105206417B (en) | 2015-11-09 | 2015-11-09 | The preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105206417A CN105206417A (en) | 2015-12-30 |
| CN105206417B true CN105206417B (en) | 2018-02-23 |
Family
ID=54954032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510755614.5A Active CN105206417B (en) | 2015-11-09 | 2015-11-09 | The preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105206417B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108155004A (en) * | 2016-12-02 | 2018-06-12 | 天津三环乐喜新材料有限公司 | A kind of performance Nd Fe B sintered magnet and preparation method thereof |
| CN106783131B (en) * | 2016-12-23 | 2019-03-26 | 宁波韵升股份有限公司 | A kind of preparation method of sintered NdFeB thin slice magnet |
| CN108389711A (en) * | 2018-01-05 | 2018-08-10 | 宁波招宝磁业有限公司 | A kind of preparation method of the Sintered NdFeB magnet with high-coercive force |
| CN112133552B (en) | 2020-09-29 | 2022-05-24 | 烟台首钢磁性材料股份有限公司 | Preparation method of neodymium iron boron magnet with adjustable crystal boundary |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5930582A (en) * | 1997-12-22 | 1999-07-27 | Shin-Etsu Chemical Co., Ltd. | Rare earth-iron-boron permanent magnet and method for the preparation thereof |
| CN101105997A (en) * | 2007-06-07 | 2008-01-16 | 浙江大学 | Method for preparing high coercive force rare earth permanent magnet by modifying nano titanium powder enriched with rare earth phase |
| CN103646742A (en) * | 2013-12-23 | 2014-03-19 | 湖南航天磁电有限责任公司 | Neodymium-iron-boron magnet and preparation method thereof |
| CN104681268A (en) * | 2013-11-28 | 2015-06-03 | 湖南稀土金属材料研究院 | Processing method for improving coercive force of sintered neodymium-iron-boron magnet |
| CN104952607A (en) * | 2015-06-16 | 2015-09-30 | 北京科技大学 | Manufacturing method of light rare earth-copper alloy NdFeB magnet with grain boundary being low melting point |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103310971A (en) * | 2012-10-09 | 2013-09-18 | 中磁科技股份有限公司 | Preparation method for obtaining high-performance sintered Nd-Fe-B magnet |
-
2015
- 2015-11-09 CN CN201510755614.5A patent/CN105206417B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5930582A (en) * | 1997-12-22 | 1999-07-27 | Shin-Etsu Chemical Co., Ltd. | Rare earth-iron-boron permanent magnet and method for the preparation thereof |
| CN101105997A (en) * | 2007-06-07 | 2008-01-16 | 浙江大学 | Method for preparing high coercive force rare earth permanent magnet by modifying nano titanium powder enriched with rare earth phase |
| CN104681268A (en) * | 2013-11-28 | 2015-06-03 | 湖南稀土金属材料研究院 | Processing method for improving coercive force of sintered neodymium-iron-boron magnet |
| CN103646742A (en) * | 2013-12-23 | 2014-03-19 | 湖南航天磁电有限责任公司 | Neodymium-iron-boron magnet and preparation method thereof |
| CN104952607A (en) * | 2015-06-16 | 2015-09-30 | 北京科技大学 | Manufacturing method of light rare earth-copper alloy NdFeB magnet with grain boundary being low melting point |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105206417A (en) | 2015-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105741995B (en) | A kind of high performance sintered neodymium-iron-boron permanent magnet and preparation method thereof | |
| CN102959648B (en) | R-T-B based rare earth element permanent magnet, motor, automobile, generator, wind power generation plant | |
| CN102959647B (en) | R-T-B based rare earth element permanent magnet, motor, automobile, generator, wind power generation plant | |
| CN104952607A (en) | Manufacturing method of light rare earth-copper alloy NdFeB magnet with grain boundary being low melting point | |
| CN104112581B (en) | R T B system's rare earths sintered magnets and its manufacture method | |
| CN105206417B (en) | The preparation method of magnetic coupling sintered NdFeB is gone between a kind of main phase grain by force | |
| CN103779064B (en) | Amorphous state prepares the method for Nd-Fe-B magnet steel | |
| CN103903824B (en) | A kind of rare earth permanent-magnetic material and preparation method thereof | |
| WO2012048654A1 (en) | High-corrosion resistant sintered ndfeb magnet and preparation method therefor | |
| CN103680919B (en) | A kind of preparation method of the high anti-corrosion sintered Nd-Fe-B permanent magnet of tough height of high-coercive force | |
| CN105170976A (en) | Method for preparing high-coercivity neodymium iron boron by means of low-temperature sintering after blank compacting permeation | |
| KR102287740B1 (en) | Rare earth permanent magnet material and manufacturing method thereof | |
| CN105304249B (en) | A kind of preparation method of samarium-cobalt permanent-magnetic material | |
| CN110047636A (en) | A kind of preparation method of high-coercive force richness La/Ce sintered magnet | |
| CN107689279A (en) | One kind improves the coercitive method of sintered NdFeB built-up magnet | |
| CN104681268A (en) | Processing method for improving coercive force of sintered neodymium-iron-boron magnet | |
| CN108389711A (en) | A kind of preparation method of the Sintered NdFeB magnet with high-coercive force | |
| CN110534280A (en) | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition | |
| CN104575902A (en) | Neodymium iron boron magnet added with cerium and preparation method thereof | |
| CN100595303C (en) | Method of manufacturing single-phase Sm2Co17 nanocrystalline block body material | |
| CN107564651A (en) | A kind of high remanent magnetism material and preparation method thereof | |
| CN103000324B (en) | A kind of sintered rare-earth permanent magnetic material and preparation method thereof | |
| CN106920615B (en) | A kind of sintered neodymium iron boron material and preparation method | |
| CN107799256A (en) | A kind of permanent-magnetic composite materials and preparation method | |
| CN113593882A (en) | 2-17 type samarium-cobalt permanent magnet material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |