CN105206417A - Preparation method of strong-demagnetizing coupling sintered NdFeB with spaced main-phase crystal particles - Google Patents
Preparation method of strong-demagnetizing coupling sintered NdFeB with spaced main-phase crystal particles Download PDFInfo
- Publication number
- CN105206417A CN105206417A CN201510755614.5A CN201510755614A CN105206417A CN 105206417 A CN105206417 A CN 105206417A CN 201510755614 A CN201510755614 A CN 201510755614A CN 105206417 A CN105206417 A CN 105206417A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- powder
- strong
- sintered ndfeb
- preparation
- 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.)
- Granted
Links
Abstract
The invention belongs to the field of rare earth permanent magnetic materials and particularly relates to a preparation method of strong-demagnetizing coupling sintered NdFeB with spaced main-phase crystal particles. The preparation method is characterized by adding a proper amount of powdered sulfur and rare earth-copper aluminum alloy powder with low melting point into NdFeB alloy powder, mixing uniformly, carrying out compression in a magnetic field and sintering for compaction, and carrying out heat treatment to obtain a product. The sintered NdFeB is suitable for any NdFeB magnets with the main-phase crystal particles being 2 to 14 to 1, and has the advantages that in the sintering process, sulfur is heated to be gasified to realize the gas phase separation of magnetic powder particles and crystal particles, meanwhile, the rare earth-copper aluminum alloy and the phase being 2 to 14 to 1 have good wettability, the main-phase crystal particles of the sintered NdFeB magnet are spaced completely, so that the high coercivity is obtained.
Description
Technical field
The invention belongs to field of rare-earth permanent magnetic, particularly the preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain.
Background technology
The Sintered NdFeB magnet being described as " magnetic king " has become the Core Feature material in the fields such as electric power, telecommunication, automobile, computer, biomedicine and household electrical appliance, be applied to generator, the motor of electronic (or hybrid electrically) automobile manufacturing hundreds of kilowatt, and manufacture the wind power generation magneto of megawatt magnitude.
The coercive force of sintered NdFeB is an important parameter, and the coercive force raising of sintered NdFeB can drive the raising of other combination property on the one hand, and the coercive force of sintered NdFeB also has very large room for promotion on the other hand, at present still not enough theoretical value 30%.Sintered NdFeB magnet coercive force is coercive force far below the main cause of theoretical value is an institutional framework sensitive parameter, and there is larger gap in actual tissue structure and desired tissue structure, such as crystallite dimension crystal anisotropy constant K 1 that is tiny not and 2:14:1 main phase grain superficial layer is lower, simultaneously crystal boundary rich-Nd phase can not be that lamelliform distributes continuously, realizes fully effective earth magnetism and completely cut off at 2:14:1 phase intercrystalline, is also a very important reason.Therefore, the Sintered NdFeB magnet of high-coercive force be obtained, except refining grain size is with except the anisotropy of strengthening 2:14:1 grain surface layer, must ensure that rich-Nd phase is that lamelliform is distributed to around all Nd2Fe14B crystal grain equably.
Rare earth (the La of certain ingredients scope, Ce, Pr, Nd, Tb, Dy, Ho, Gd, the fusing point lower (about 400-800 DEG C) of Y)-albronze (content of rare earth 50-90% atomic percentage), have good wetability with 2:14:1 phase, this has been reported in Patents (application number 201510029340.1,201510335273.6 and 201510335165.9).The fusing point 112 DEG C of elemental sulfur simultaneously, boiling point 444.6 DEG C, namely to 444.6 DEG C is boiled into the steam that tool S2 forms, and therefore can realize isolating the gas phase of magnetic powder particle, thus make to separate better between 2:14:1 main phase grain.
Summary of the invention
The invention provides the preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain.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 mixes, through magnetic field die mould and sintering densification, again after tempered heat treatment, obtain 2:14:1 main phase grain by the strong degaussing coupling high-coercive force neodymium iron boron magnetic body separated completely.
The present invention mainly utilizes sulphur to be subject to thermal evaporation realization to the gas phase isolation of magnetic powder particle and crystal grain and the rare earth-albronze good wettability with 2:14:1 phase, preparation 2:14:1 main phase grain is by the high-coercive force Sintered NdFeB magnet separated completely, mainly based on 2 points: 1. elemental sulfur is vaporized at 444.6 DEG C, the gas phase isolation to magnetic powder particle and sintering crystal grain therefore can be realized; 2. rare earth-albronze the fusing point of certain ingredients lower (about 400-800 DEG C), with 2:14:1 phase, there is good wetability, can be implemented in around each 2:14:1 main phase grain all has Grain-Boundary Phase to separate, and stops the intercrystalline magnetic exchange coupling of 2:14:1.
The preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain, 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 mixes, through magnetic field die mould and sintering densification, again after heat treatment, 2:14:1 main phase grain is obtained by the strong degaussing coupling high-coercive force neodymium iron boron magnetic body separated completely;
Concrete technology step is:
1. Nd Fe B alloys ingot casting is broken into the powder particle of 3-5 μm;
2. rare earth-albronze ingot casting is broken into the powder particle of 0.1-3 μm;
3. in neodymium iron boron alloy powder, add the sulphur powder (particle size 20-500nm) of weight fraction 0.1-2% and the rare earth-copper-aluminum alloy powder of weight fraction 2-8%, mix;
4. mixed powder is being greater than orientation die mould and isostatic pressed under 1.8T magnetic field;
5. by pressed compact vacuum-sintering; Sintering temperature is 850-1050 DEG C, and sintering time is 1-4h, vacuum degree 10
-3pa.
6. temper obtains product.Temper temperature is for being respectively 600-800 DEG C and 350-550 DEG C, and the temper time is 1-4h, vacuum degree 10
-3pa.
The alloy that Nd Fe B alloys composition described in step 1 both just can divide for 2:14:1 can be again the alloy of the rich neodymium phase of 2:14:1+.
The invention has the advantages that:
1. sulphur is isolated by the thermal evaporation gas phase to magnetic powder particle, finally realizes completely isolated to 2:14:1 phase crystal grain of rare earth-albronze;
2. the metal sulfide that sulphur and the chemical combination such as neodymium, iron generate suppresses grain growth at crystal boundary, crystal grain thinning, and plays pinning effect to magnetic domain;
3. realize low-temperature sintering, reduce temperature, saved the energy;
4. achieve intercrystalline strong degaussing coupling high-coercive force Sintered NdFeB magnet;
5. the present invention is applicable to the neodymium iron boron product with 2:14:1 main phase grain of any composition.
Embodiment
Embodiment one: 2:14:1 is just being divided in master alloying powder and is added Pr68Cu32 alloyed powder and S powder and prepare strong degaussing coupling Sintered NdFeB magnet between main phase grain
Prepare Nd11.76Fe82.36B5.88 (atomic percentage) master alloying and Pr68Cu32 (atomic percentage) auxiliary alloy respectively, prepare thickness by strip casting technique and be respectively the master alloying of 300 μm and 150 μm and auxiliary alloy sheet, break with hydrogen and add air-flow and grind standby average particle size particle size and be respectively the master alloying powder of 3.5 μm and 1.5 μm and auxiliary alloyed powder, in master alloying powder, add weight fraction is the auxiliary alloyed powder of 4% and the sulphur powder of weight fraction to be 0.5% particle be 50nm, in batch mixer, three kinds of powder are mixed, powder after Homogeneous phase mixing orientation die mould through 200MPa isostatic pressed in the magnetic field of 1.8T, the pressed compact obtained is inserted in vacuum sintering furnace, at 1000 DEG C of sintering 3h, afterwards at 800 DEG C and 400 DEG C of difference tempering heat treatment 3h, obtain the high-coercive force neodymium iron boron magnetic body that principal phase crystal boundary is separated continuously.
Embodiment two: add Pr50Nd20Cu30 alloyed powder and S powder in (2:14:1+ rich RE phase) master alloying powder and prepare strong degaussing between main phase grain and to be coupled Sintered NdFeB magnet
Prepare Nd8.82Pr3.94Fe79.00Co1.86Zr0.5B5.88 (atomic percentage) master alloying and Pr50Nd20Cu30 (atomic percentage) auxiliary alloy respectively, the master alloying thin slice that thickness is respectively 300 μm is prepared by strip casting technique, the auxiliary alloy thin band that thickness is 50 μm is prepared with m elt-spun overqu-enching, break with hydrogen and add air-flow and grind the master alloying powder that standby average particle size particle size is 3.0 μm, the auxiliary alloyed powder that average particle size particle size is 1.2 μm is prepared by the method for ball milling, in master alloying powder, add weight fraction is the auxiliary alloyed powder of 5% and the sulphur powder of weight fraction to be 1.0% particle be 100nm, in batch mixer, three kinds of powder are mixed, powder after Homogeneous phase mixing orientation die mould through 200MPa isostatic pressed in the magnetic field of 1.8T, the pressed compact obtained is inserted in vacuum sintering furnace, at 980 DEG C of sintering 3h, afterwards at 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 is separated continuously.
Claims (6)
1. the preparation method of strong degaussing coupling sintered NdFeB between a main phase grain, 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 mixes, through magnetic field die mould and sintering densification, again after heat treatment, 2:14:1 main phase grain is obtained by the strong degaussing coupling high-coercive force neodymium iron boron magnetic body separated completely;
Concrete technology step is:
1). Nd Fe B alloys ingot casting is broken into the powder particle of 3-5 μm;
2). rare earth-albronze ingot casting is broken into the powder particle of 0.1-3 μm;
3). in neodymium iron boron alloy powder, add sulphur powder and rare earth-copper-aluminum alloy powder, mix;
4). mixed powder is being greater than orientation die mould and isostatic pressed under 1.8T magnetic field;
5). by pressed compact vacuum-sintering;
6). temper obtains product.
2. the preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain as claimed in claim 1, is characterized in that: step 1) described in Nd Fe B alloys composition be the alloy that 2:14:1 is just dividing, or be the alloy of 2:14:1+ richness neodymium phase.
3. the preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain as claimed in claim 1, it is characterized in that: step 2) described in rare earth-albronze in rare earth be La, Ce, Pr, Nd, Tb, Dy, Ho, Gd, a kind of principal phase or several in Y, the copper aluminium in rare earth-albronze is a kind of principal phase in Cu, Al or two kinds, content of rare earth 50-90% atomic percentage.
4. the preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain as claimed in claim 1, it is characterized in that: step 3) described in sulphur powder and percetage by weight respectively 0.1-2% and 2-8%, the sulphur powder particles size 20-500nm of rare earth-copper-aluminium alloy powder.
5. the preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain as claimed in claim 1, is characterized in that: step 5) described in sintering temperature be 850-1050 DEG C, sintering time is 1-4h, vacuum degree 10
-3pa.
6. the preparation method of strong degaussing coupling sintered NdFeB between a kind of main phase grain as claimed in claim 1, it is characterized in that: step 6) described in temper temperature for being respectively 600-800 DEG C and 350-550 DEG C, the temper time is 1-4h, vacuum degree 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 true CN105206417A (en) | 2015-12-30 |
| CN105206417B 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) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106783131A (en) * | 2016-12-23 | 2017-05-31 | 宁波韵升股份有限公司 | A kind of preparation method of sintered NdFeB thin slice magnet |
| 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 |
| 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 |
| EP3975212A1 (en) | 2020-09-29 | 2022-03-30 | Yantai Shougang Magnetic Materials Inc. | A method for preparation of a sintered type ndfeb permanent magnet with an adjusted grain boundary |
Citations (6)
| 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 |
| 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 |
| 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 |
-
2015
- 2015-11-09 CN CN201510755614.5A patent/CN105206417B/en active Active
Patent Citations (6)
| 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 |
| 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 |
| 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 |
Cited By (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 |
| CN106783131A (en) * | 2016-12-23 | 2017-05-31 | 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 |
| EP3975212A1 (en) | 2020-09-29 | 2022-03-30 | Yantai Shougang Magnetic Materials Inc. | A method for preparation of a sintered type ndfeb permanent magnet with an adjusted grain boundary |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105206417B (en) | 2018-02-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104952607A (en) | Manufacturing method of light rare earth-copper alloy NdFeB magnet with grain boundary being low melting point | |
| CN102959648B (en) | R-T-B based rare earth element permanent magnet, motor, automobile, generator, wind power generation plant | |
| CN103280290B (en) | Containing cerium low melting point rare earth permanent magnetic liquid phase alloy and permanent magnet preparation method thereof | |
| CN106601407B (en) | Improve the coercitive method of neodymium iron boron magnetic body | |
| CN105170976A (en) | Method for preparing high-coercivity neodymium iron boron by means of low-temperature sintering after blank compacting permeation | |
| CN103426624B (en) | The preparation method of Nd-Fe-B permanent magnet | |
| CN106128673A (en) | A kind of Sintered NdFeB magnet and preparation method thereof | |
| 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 | |
| US9818516B2 (en) | High temperature hybrid permanent magnet | |
| CN103903823A (en) | Rare earth permanent magnetic material and preparation method thereof | |
| CN110047636A (en) | A kind of preparation method of high-coercive force richness La/Ce sintered magnet | |
| CN104841927A (en) | Preparation method of high corrosion resistance and high weather resistance rare earth permanent magnetic material | |
| CN110911077B (en) | Preparation method of high-coercivity neodymium cerium iron boron magnet | |
| CN104681268A (en) | Processing method for improving coercive force of sintered neodymium-iron-boron magnet | |
| CN106710765A (en) | High-coercivity sintered-neodymium-iron-boron magnetic body and preparing method thereof | |
| CN103187133A (en) | Rare earth permanent magnetic alloy and magnetic phase composite preparation method thereof | |
| CN105206417A (en) | Preparation method of strong-demagnetizing coupling sintered NdFeB with spaced main-phase crystal particles | |
| CN107742564A (en) | A kind of method that auxiliary alloy addition of high dysprosium prepares low-cost neodymium iron boron magnet | |
| CN108389711A (en) | A kind of preparation method of the Sintered NdFeB magnet with high-coercive force | |
| CN106782978B (en) | A kind of preparation method of high-coercive force sintered NdFeB rare-earth permanent magnet material | |
| CN110534280A (en) | A kind of preparation method of the performance Nd Fe B sintered magnet based on crystal boundary addition | |
| CN106298134B (en) | A kind of double main phase agglomeration permanent magnetic materials and preparation method and application | |
| CN107799256A (en) | A kind of permanent-magnetic composite materials and preparation method | |
| CN113838622A (en) | High-coercivity sintered neodymium-iron-boron magnet and preparation method thereof | |
| CN103495733A (en) | Method for preparing sintered Nd-Fe-B permanent magnet material with intergranular Nd-rich phase replaced |
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 |