CN108746640A - It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab - Google Patents
It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab Download PDFInfo
- Publication number
- CN108746640A CN108746640A CN201810495229.5A CN201810495229A CN108746640A CN 108746640 A CN108746640 A CN 108746640A CN 201810495229 A CN201810495229 A CN 201810495229A CN 108746640 A CN108746640 A CN 108746640A
- Authority
- CN
- China
- Prior art keywords
- slab
- hydrogen
- heat treatment
- sintered ndfeb
- broken
- 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.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
Abstract
It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab, hydrogen crushing furnace is added in slab and is evacuated down to 5.0X10‑1Hereinafter, being warming up to 800-1000 degree by 3-10 degree per minute keeps the temperature 2-8h, the heat treatment to slab is completed.The present invention is not in the case where increasing new process and equipment, also slab is heat-treated while hydrogen is broken, α iron a small amount of in slab is not only further obviated, the ultra-fine grain in slab tissue can also reduced, microstructure and tissue consistency obtain optimization and improve；The sintered NdFeB produced using above-mentioned new process can improve remanent magnetism 0.5-1.5%, while material processability improves obviously, and finishing qualification rate improves, and especially the larger thin-wall product of difficulty of processing, passing rate of processing can improve 10% or more.
Description
One, technical field：
Patent of the present invention carries out sintered NdFeB slab using the broken equipment of existing hydrogen to be heat-treated the+broken technique of hydrogen, is not increasing
In the case of new process and equipment, also slab is heat-treated while hydrogen is broken, belongs to sintered NdFeB production technology
Innovation
Two, background technology
HDDR techniques are a kind of technological means of very effective production Anisotropy NdFeB Powder.HDDR processes include inhaling
Hydrogen-disproportionation-dehydrogenation-is compound again（hydrogenation –disproportionation – desorption –
Recombination, abbreviation HDDR）Four-stage.The essence of HDDR processes is that rare earth intermetallic compound is inhaled hydrogen and is disproportionated
It decomposes, then disproportionation products are combined into the tiny former compound phase of crystal grain in subsequent pressure certain embodiments, to realize to material
Expect the refinement of crystal grain（Average grain size is 300nm）, and the crystal structure along main phase C axis directions is produced, to prepare
It can be with the magnetic powder of magnetic anisotropy with excellent magnetic.The conventional broken technique of hydrogen is that slab is added after hydrogen crushing furnace vacuumizes in room temperature
Hydrogen is inhaled between to 300, fragmentation after disproportionated reaction can occur for neodymium iron boron slab, be then warming up between 500-650 degree vacuumize it is de-
Hydrogen is cooled to 40 degree or less after the completion of dehydrogenation and comes out of the stove.
Sintered NdFeB industry melting process has generally used can be with crystal grain thinning and the rapid hardening slab for essentially eliminating α iron
Furnace apparatus, but rapid hardening slab stove, during rapid condensation forms slab, slab contacts the local portion on chilling roller surface
It can be because supercooling causes the crystallite less than 1.5 microns, these a small amount of crystallites can be to sintered neodymium iron after powder process processed
Boron material performance and processability generate totally unfavorable influence.
Three, invention content：
In order to overcome disadvantages described above to improve the magnetic property of sintered NdFeB, 800- is carried out again to the slab of rapid hardening slab stove production
1000 degree of heat treatment, so that it may so that this part crystallite is grown up to 2-4 microns satisfactory, while can further eliminate still
So a small amount of existing α iron.
The technical scheme is that：It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab,
It is characterized in that：Hydrogen crushing furnace is added in slab and is evacuated down to 5.0X10-1Hereinafter, being warming up to 800-1000 degree by 3-10 degree per minute
2-8h is kept the temperature, the heat treatment to slab is completed.
The difference of heavy rare earth content, can select rapid cooling or slow cooling during the present invention is formulated after being heat-treated according to slab
To improve the coercivity of product or improve material processability.
It is a kind of rotary hydrogen crushing furnace that this process exploitation, which is tested used in process, and it includes both ends to be supported on support element
Rotatable flue, the electric furnace positioned at flue outer layer, flue rotary drive mechanism and for vacuumizing, being flushed with hydrogen in flue
Vacuum extractor, air distributing device, one end of flue is into and out of material mouth, and the other end is sealed with vacuum extractor and air distributing device
Communicate, electric furnace by can the left and right furnace bodies of opening and closing constitute, left and right furnace body is respectively placed in the supporting rack that lower part is equipped with idler wheel
On, it is equipped with flight in flue and ensures that inhaling hydrogen process and cooling procedure uniformly overturns material.
Invention of the present invention has also carried out hot place while hydrogen is broken in the case where not increasing new process and equipment to slab
Reason, not only further obviate α iron a small amount of in slab, the ultra-fine grain in slab tissue can also reduced, microstructure with
Tissue consistency, which obtains optimization, to be improved.The sintered NdFeB produced using above-mentioned new process can improve remanent magnetism 0.5-1.5%, together
When material processability improve apparent, finishing qualification rate improves, especially the larger thin-wall product of difficulty of processing, and passing rate of processing can
To improve 10% or more.
Four, specific implementation mode
The primary operational process of the technique of the broken heat treatment of hydrogen of the present invention is as follows：
(1) slab that weight has accurately been checked is got according to dispatch command, be added to hydrogen crushing furnace be evacuated down to 5.0X10-1Pa with
Under（Notice that carrying out pressurize picks up vaccum leakage rate）.
(2) it heats to 800-1000 degree and keeps 2-8h（According to furnace entering volume difference and formula components adjustment）, in hydrogen
Heating process parameter auto-controll operation is set on broken stove controller.
(3) cooling：After pumped vacuum systems is closed, argon gas is filled in displacement pressure value, self cooling 3-6 minutes of elder generation（Furnace pressure
When insufficient, it is automatically replenished argon gas）After start water cooling 2-4 hours and be less than 300 degree to temperature of charge.
(4) hydrogen is broken：1. hunting leak：It presses " automatic running ", argon gas imports furnace body, and equipment proceeds by positive pressure leak detection, hunts leak
Rear furnace body is vented to atmospheric pressure, carries out vacuumizing negative pressure leakage detection.After meeting technique card request, equipment alarm prompt is pressed at this time
Lower H2Valve is opened, and hydrogen is broken to enter the automatic running stage, imports hydrogen.
2. leading hydrogen：When furnace pressure reaches H when hydrogen pressure maximum value is inhaled in setting2Valve is automatically closed, and material inhales stove internal pressure after hydrogen
Power declines（Start barrel rotation at this time）；System automatically turns on H again2Valve imports hydrogen, repeatedly this process to quantitative hydrogen
Automatically argon gas is filled into when gas is not supplied, unsaturation is inhaled hydrogen process and completed.
3. replacing:System automatically opens air bleeding valve, is closed when being vented to atmospheric pressure, and argon gas imports valve and successively opens.Pressure
When reaching displacement pressure, one of argon gas imports valve and closes, other two are normally opened, and air bleeding valve automatically opens exhaust, so
Setting time is arrived repeatedly.Air bleeding valve is opened, and atmospheric pressure is vented to, and displacement is completed.
4. dehydrogenation：Extract system starts automatically, when being first pumped to 40mba or less, the auto-power on heating of system, in heating
It vacuumizes, general heating 40 minutes.When temperature reaches operation card set temperature, heat preservation vacuumizes 3-6 hours.Vacuum degree reaches work
When skill card request, dehydrogenation is completed.It will continue to vacuumize dehydrogenation if not reaching requirement, until reaching requirement, dehydrogenation is completed, vacuum system
System is automatically closed.
5. cooling down：After pumped vacuum systems is closed, argon gas is filled in displacement pressure value, self cooling 3-6 minutes of elder generation（Furnace pressure is not
When sufficient, it is automatically replenished argon gas）After start water cooling 2-4 hours to 40 degree or less and come out of the stove charging.
The present invention is a kind of to be carried out at the same time the broken technique of heat treatment+hydrogen using the broken equipment of existing hydrogen to sintered NdFeB slab,
In the case where not increasing new process and equipment, also slab is heat-treated while hydrogen is broken.
Slab is added hydrogen crushing furnace and is evacuated down to 5.0X10-1 hereinafter, being warming up to 800- by 3-10 degree per minute by the present invention
1000 degree of heat preservation 2-8h, complete the heat treatment to slab.This heat treatment process further obviates α iron a small amount of in slab,
The ultra-fine grain in slab tissue can be made to reduce.
The difference of heavy rare earth content, can select rapid cooling or slow cooling during the present invention is formulated after being heat-treated according to slab
To improve the coercivity of product or improve material processability.
Claims (2)
1. a kind of being carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab, it is characterised in that：Slab is added
Hydrogen crushing furnace is evacuated down to 5.0X10-1Hereinafter, being warming up to 800-1000 degree by 3-10 degree per minute keeps the temperature 2-8h, complete to slab
Heat treatment.
2. it is according to claim 1 it is a kind of being carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab,
It is characterized in that：The difference of heavy rare earth content in being formulated according to slab after heat treatment, can select rapid cooling or slow cooling to carry
The coercivity of high product improves material processability.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810495229.5A CN108746640A (en) | 2018-05-22 | 2018-05-22 | It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810495229.5A CN108746640A (en) | 2018-05-22 | 2018-05-22 | It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108746640A true CN108746640A (en) | 2018-11-06 |
Family
ID=64008457
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810495229.5A Pending CN108746640A (en) | 2018-05-22 | 2018-05-22 | It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108746640A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220538A (en) * | 2011-05-17 | 2011-10-19 | 南京理工大学 | Sintered neodymium-iron-boron preparation method capable of improving intrinsic coercivity and anticorrosive performance |
| CN102360910A (en) * | 2011-06-30 | 2012-02-22 | 安徽大地熊新材料股份有限公司 | Method for processing neodymium iron boron magnet |
| WO2014017249A1 (en) * | 2012-07-24 | 2014-01-30 | インターメタリックス株式会社 | PROCESS FOR PRODUCING NdFeB-BASED SINTERED MAGNET |
| CN103769593A (en) * | 2013-12-30 | 2014-05-07 | 安徽万磁电子有限公司 | Sintered Ne-Fe-B hydrogen decrepitation method capable of lowering cost and improving efficiency |
| CN104164636A (en) * | 2014-06-30 | 2014-11-26 | 中磁科技股份有限公司 | Thermal processing method of neodymium-iron-boron casting strip and thermal processing device |
| CN106782969A (en) * | 2016-12-21 | 2017-05-31 | 宁波科田磁业有限公司 | Cerium mischmetal permanent-magnet material and preparation method thereof |
-
2018
- 2018-05-22 CN CN201810495229.5A patent/CN108746640A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220538A (en) * | 2011-05-17 | 2011-10-19 | 南京理工大学 | Sintered neodymium-iron-boron preparation method capable of improving intrinsic coercivity and anticorrosive performance |
| CN102360910A (en) * | 2011-06-30 | 2012-02-22 | 安徽大地熊新材料股份有限公司 | Method for processing neodymium iron boron magnet |
| WO2014017249A1 (en) * | 2012-07-24 | 2014-01-30 | インターメタリックス株式会社 | PROCESS FOR PRODUCING NdFeB-BASED SINTERED MAGNET |
| CN103769593A (en) * | 2013-12-30 | 2014-05-07 | 安徽万磁电子有限公司 | Sintered Ne-Fe-B hydrogen decrepitation method capable of lowering cost and improving efficiency |
| CN104164636A (en) * | 2014-06-30 | 2014-11-26 | 中磁科技股份有限公司 | Thermal processing method of neodymium-iron-boron casting strip and thermal processing device |
| CN106782969A (en) * | 2016-12-21 | 2017-05-31 | 宁波科田磁业有限公司 | Cerium mischmetal permanent-magnet material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘海洲: "烧结钕铁硼永磁材料制备工艺的研究进展", 《稀有金属与硬质合金》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI427648B (en) | Production method of permanent magnet and permanent magnet | |
| TWI469161B (en) | Method for manufacturing permanent magnets and permanent magnets | |
| EP2808877A1 (en) | Method for preparing R-Fe-B based sintered magnet | |
| CN107326155B (en) | A kind of rare earth permanent magnet vacuum-sintering heat treatment method and vacuum heat treatment equipment | |
| US11920236B2 (en) | Coating machine and coating method | |
| TWI755152B (en) | NdFeB MAGNET MATERIAL, RAW MATERIAL COMPOSITION, PREPARATION METHOD AND APPLICATION | |
| CN106601459B (en) | Reduce the sintering method of neodymium iron boron magnetic body carbon content | |
| KR20210151940A (en) | R-T-B type rare earth permanent magnet material, manufacturing method and application | |
| CN109097540A (en) | A kind of parallel vacuum Equipment for Heating Processing and vacuum heat-treating method | |
| WO2008032666A1 (en) | Vacuum evaporation processing equipment | |
| CN105513733B (en) | A kind of preparation method of sintering type Nd iron boron permanent magnetic material | |
| CN107321977A (en) | A kind of rare earth permanent magnet vacuum sintering method and vacuum-sintering Equipment for Heating Processing | |
| US9543063B2 (en) | Continuous hydrogen pulverization method and production device of rare earth permanent magnetic alloy | |
| CN106591555B (en) | A kind of annealing process after non-directional cold-rolling silicon steel disc cold rolling | |
| CN107326156B (en) | A kind of Nd-Fe-B permanent magnetic vacuum-sintering heat treatment method and vacuum heat treatment equipment | |
| CN103219146A (en) | Method for enhancing magnet performance through reducing-dispersing method | |
| CN108746640A (en) | It is a kind of to be carried out at the same time heat treatment and the broken technique of hydrogen using sintered NdFeB slab | |
| CN111761158A (en) | Vacuum chamber for continuously vacuumizing vacuum cup and continuous vacuumizing process | |
| CN103617856A (en) | Neodymium iron boron magnetic material strong in corrosion resistance | |
| US5851312A (en) | Production method, production apparatus and heat treatment apparatus for anisotropic magnet powder | |
| CN109014191A (en) | A kind of rare earth permanent magnet vacuum heat treatment furnace and rare earth permanent magnet heat treatment method | |
| CN103317135B (en) | High-temperature sintering process for neodymium iron boron | |
| JP2859704B2 (en) | Vacuum heat treatment furnace | |
| CN109473247A (en) | A kind of preparation method of neodymium iron boron crystal boundary infiltration alloy casting piece | |
| CN110106334A (en) | One kind being carried out continuously grain boundary decision and heat-treating apparatus and method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181106 |