CN108511178B - A kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion - Google Patents
A kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000009792 diffusion process Methods 0.000 title claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 39
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005864 Sulphur Substances 0.000 claims abstract description 18
- 239000003708 ampul Substances 0.000 claims abstract description 16
- 239000010453 quartz Substances 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 9
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 9
- 239000011574 phosphorus Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 5
- 239000006247 magnetic powder Substances 0.000 claims abstract description 5
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 16
- 230000005389 magnetism Effects 0.000 abstract description 7
- 238000002844 melting Methods 0.000 abstract description 7
- 230000008018 melting Effects 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000005457 optimization Methods 0.000 abstract description 6
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 238000009835 boiling Methods 0.000 abstract description 3
- 238000000280 densification Methods 0.000 abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
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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
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- 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
- H01F41/0266—Moulding; Pressing
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Hard Magnetic Materials (AREA)
Abstract
A kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion, belongs to rareearth magnetic material technical field.Sintered NdFeB magnetic powder is carried out half densification sintering by the present invention, half fine and close neodymium iron boron magnetic body is placed in quartz ampoule, and a certain amount of sulphur, phosphorus simple substance are added in quartz ampoule, vitreosil tube sealing is carried out again, finally 2-6h is kept the temperature at 1000-1080 DEG C in sintering furnace, it is tempered 2-4h and 480-550 DEG C of second annealing 3-6h using 800-900 DEG C of level-one, the sintered neodymium iron boron material of high magnetism is prepared.During the sintering process, the sulphur of low melting point, P elements enter in crystal boundary rich-Nd phase along magnet grain boundary decision, reduce the liquidus temperature of rich-Nd phase the present invention, to refine crystal grain, optimization boundary, improve coercivity.Meanwhile low boiling point sulphur, phosphorus simple substance become gaseous state, spread in half fine and close magnet crystal boundary, spread sulphur, P elements uniformly and be distributed in magnet.The invention has the advantages that raw material is easy to get, is cheap, preparation process is simple and convenient to operate.
Description
Technical field
The invention belongs to rareearth magnetic material technical fields, provide a kind of standby high magnetic sintered NdFeB of atmosphere diffusion
Method.
Background technique
Sintered Nd-Fe-B permanent magnetic material is third generation permanent magnet, is invented in nineteen eighty-three Japanese scholars.Since it is with pole
High coercivity and magnetic energy product and be referred to as " magnetic king ".It is widely used in aerospace, auto industry, electronic apparatus, Medical treatment device
Tool, energy-saving electric machine, new energy, field of wind power generation are with fastest developing speed, permanent magnetism materials that market prospects are best in the world today
Material.With advances in technology with the adjustment of Industry Model, sends out energetically and application sintered Nd-Fe-B magnet is with wide long-range
Prospect.
Sintered nd-fe-b magnet mainly includes Nd2Fe14B phase and rich-Nd phase.Wherein, main phase Nd2Fe14B is sintered NdFeB
Unique ferromagnetism phase in magnet, crystal grain are in irregular polygon, have been largely fixed the remanent magnetism and maximum magnetic energy of magnet
Product.Rich-Nd phase is non-magnetic phase important in magnet, and ingredient, structure and distributional pattern drastically influence the performance of magnet, mesh
Before, the remanent magnetism B of Sintered Nd-Fe-B MagnetrWith maximum magnetic energy product (BH)maxActual value have been approached its theoretical value.So
And the coercivity H of magnetcjIt is relatively low, the 10~20% of theoretical value are only reached, Sintered Nd-Fe-B Magnet is seriously limited
Further development.Therefore, the coercivity of magnet how is improved into the major issue of rareearth magnetic material industry.
Research shows that: the coercivity of Sintered NdFeB magnet is very sensitive to microstructure, and grain boundary structure lacks
It is to influence an important factor for magnet coercivity is far below theoretical value that sunken and crystal grain, which is grown up,.Pass through optimization border structure and refinement crystal grain
The coercivity of magnet can be effectively improved.Optimization border structure and control crystallite dimension are mainly started in terms of two, on the one hand
Regulate and control border structure, including improves rich-Nd phase and main phase Nd2Fe14The intergranular wetability of B reduces the fusing point of rich-Nd phase, improves
Its mobility；On the other hand the crystallite dimension of main phase particle is controlled, at present since strip casting, hydrogen break going out for gentle flowing mill technology
It is existing, the size of raw material powder is preferably controlled, therefore how to control the crystal grain behavior of growing up in sintering process is refinement crystal grain
Key link.
Has the characteristics that low melting point between nonmetallic sulphur, phosphorus simple substance, and the serious crystal boundary segregation element in steel, Zhi Nengxiang
The positions such as crystal boundary, phase boundary segregation.If introducing sulphur, the P elements of low melting point in magnet, rich-Nd phase perhaps can be effectively reduced
Fusing point, optimize border structure, refine crystal grain.But sulphur, phosphorus have the characteristics that low-boiling again, easily wave during the sintering process
Hair.Therefore, how to guarantee that sulphur, P elements can be present in magnet during the sintering process and be uniformly distributed is particularly important.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of the standby high magnetic sintered NdFeB of atmosphere diffusion, are reducing liquid phase
Line temperature, refinement crystal grain, optimization boundary and raising coercivity etc. have all reached satisfactory effect, Nd2Fe14B phase is brilliant
Grain distribution uniform, crystallite dimension are smaller.
In order to obtain above-mentioned Sintered NdFeB magnet, specific step is as follows by the present invention:
(1) NdFeB magnetic powder is subjected to orientation die mould under the magnetic field of 1.2~2.0T；
(2) green compact that step (1) medium-pressure type is completed is put into vacuum sintering furnace, carries out half dense sintering of vacuum, it is fine and close
Degree is 90%~95%, and sintering temperature is 900~950 DEG C, and soaking time is 1~3h, obtains half fine and close sintered NdFeB examination
Sample；
(3) in step (2) half fine and close sintered NdFeB is placed in quartz ampoule, and be put into quartz ampoule a certain amount of
Low melting point simple substance, then vacuum sealing tube is carried out to quartz ampoule, vacuum degree is up to 10-2~10-3Pa obtains the sample of vitreosil tube sealing；
(4) sample of vitreosil tube sealing in step (3) is placed in sintering furnace and is sintered under certain sintering condition,
2-6h is kept the temperature at 1000-1080 DEG C, is tempered 2-4h and 480-550 DEG C of second annealing 3-6h, preparation using 800-900 DEG C of level-one
Obtain the sintered neodymium iron boron material of high magnetism.
Further, the consistency of half fine and close sintered NdFeB sample described in step (2) is 90%~95%.
Further, quartz ampoule described in step (3) requires softening temperature to be higher than 1200 DEG C.
Further, low melting point simple substance described in step (3) is sulphur or phosphorus simple substance, the wherein additive amount of low melting point simple substance
Account for the 0.01-0.5wt.% of ndfeb magnets.
Further, sintering condition described in step (4) can be vacuum-sintering, be also possible to N2Or Ar atmosphere is burnt
Knot.Advantages of the present invention:
1, raw material is easy to get, is cheap, preparation process is simple and convenient to operate.
2, during the sintering process, the sulphur, P elements of low melting point enter in crystal boundary rich-Nd phase along magnet grain boundary decision, drop
The liquidus temperature of low rich-Nd phase, to refine crystal grain, optimization boundary, improve coercivity.
3, during the sintering process, the low boiling point sulphur of vitreosil tube sealing, phosphorus simple substance become gaseous state, along half fine and close magnet
Diffusion, spreads sulphur, P elements uniformly and is distributed in magnet in crystal boundary, further strengthens the beneficial effect of sulphur, P elements.
4, atmosphere diffusion is carried out using half fine and close Sintered NdFeB magnet, is conducive to the diffusion speed for accelerating sulphur, P elements
Rate improves diffusion uniformity.
5, the adjustment and optimization by sulphur, P elements to material composition, form be uniformly distributed, size it is lesser
Nd2Fe14The magnetic sintered neodymium iron boron material of the height of B phase crystal grain sum.
Specific embodiment
Embodiment 1:
A kind of preparation process of the magnetic sintered NdFeB of the standby height of atmosphere diffusion is as follows:
Step 1: NdFeB magnetic powder is subjected to oriented moulding under the magnetic field of 1.2T；
Step 2: green compact is subjected to half densification sintering in vacuum sintering furnace, sintering temperature is 950 DEG C, 1.5h is kept the temperature,
Consistency is 90%；
Step 3: the sintered NdFeB (40g) of consistency 90% being placed in quartz ampoule, is added 0.1g's in quartz ampoule
Sulphur powder, then vacuum sealing tube is carried out to quartz ampoule, vacuum degree is up to 10-2Pa or more；
Step 4: the sample of vitreosil tube sealing is placed in sintering furnace and carries out vacuum-sintering, sintering temperature is 1040 DEG C,
3h is kept the temperature, is tempered 3h and 550 DEG C of second annealing 5h using 850 DEG C of level-ones；
Step 5: the neodymium iron boron magnetic body prepared progress VSM magnetism being capable of measuring, see Table 1 for details for result.
Comparative example 1:
The sintered NdFeB of consistency 90% in embodiment 1 is subjected to vacuum-sintering, sintering process is the same as embodiment 1.Finally
See Table 1 for details for the magnetic property for the neodymium iron boron magnetic body being prepared.
Influence of 1. Different Preparation of table to sintered NdFeB sample magnetic property
Embodiment 2:
A kind of preparation process of the magnetic sintered NdFeB of the standby height of atmosphere diffusion is as follows:
Step 1: NdFeB magnetic powder is subjected to oriented moulding under the magnetic field of 2.0T；
Step 2: green compact being subjected to half densification sintering in vacuum sintering furnace, sintering temperature is 950 DEG C, keeps the temperature 3h, causes
Density is 95%；
Step 3: the sintered NdFeB (35g) of consistency 95% being placed in quartz ampoule, is added 0.03g's in quartz ampoule
Phosphorus powder, then vacuum sealing tube is carried out to quartz ampoule, vacuum degree is up to 10-2Pa or more；
Step 4: the sample of vitreosil tube sealing is placed in sintering furnace and carries out vacuum-sintering, sintering temperature is 1050 DEG C,
5h is kept the temperature, is tempered 2h and 500 DEG C of second annealing 6h using 885 DEG C of level-ones；
Step 5: the neodymium iron boron magnetic body prepared progress VSM magnetism being capable of measuring, see Table 2 for details for result.
Comparative example 1:
The sintered NdFeB of consistency 95% in embodiment 2 is subjected to vacuum-sintering, sintering process is the same as embodiment 2.Finally
See Table 2 for details for the magnetic property for the neodymium iron boron magnetic body being prepared.
The magnetic property of the sintered NdFeB sample of 2. Different Preparation of table compares
Claims (4)
1. a kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion, which comprises the following steps:
(1) NdFeB magnetic powder is subjected to orientation die mould under the magnetic field of 1.2 ~ 2.0T；
(2) green compact that step (1) medium-pressure type is completed is put into vacuum sintering furnace, carries out half dense sintering of vacuum, consistency is
90% ~ 95%, sintering temperature is 900 ~ 950 DEG C, and soaking time is 1 ~ 3h, obtains half fine and close sintered NdFeB sample；
(3) half fine and close sintered NdFeB in step (2) is placed in quartz ampoule, and is put into sulphur or phosphorus simple substance in quartz ampoule,
Vacuum sealing tube is carried out to quartz ampoule again, vacuum degree is up to 10-2~10-3Pa obtains the sample of vitreosil tube sealing；
(4) sample of vitreosil tube sealing in step (3) is placed in sintering furnace and is sintered under certain sintering condition, 1000-
2-6h is kept the temperature at 1080 DEG C, 2-4h and 480-550 DEG C of second annealing 3-6h is tempered using 800-900 DEG C of level-one, is prepared
High magnetic sintered neodymium iron boron material；
Quartz ampoule described in step (3) requires softening temperature to be higher than 1200 DEG C.
2. a kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion according to claim 1, it is characterised in that: step
Suddenly the consistency of half fine and close sintered NdFeB sample described in (2) is 90% ~ 95%.
3. a kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion according to claim 1, it is characterised in that: step
Suddenly the additive amount of sulphur described in (3) or phosphorus simple substance accounts for the 0.01-0.5wt.% of ndfeb magnets.
4. a kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion according to claim 1, it is characterised in that: step
Suddenly sintering condition described in (4) is vacuum-sintering, or is N2Or Ar atmosphere sintering.
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| CN201810179183.6A CN108511178B (en) | 2018-03-05 | 2018-03-05 | A kind of method of the standby high magnetic sintered NdFeB of atmosphere diffusion |
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| JP2013225533A (en) * | 2012-03-19 | 2013-10-31 | Hitachi Metals Ltd | Method of manufacturing r-t-b-based sintered magnet |
| CN103366944B (en) * | 2013-07-17 | 2016-08-10 | 宁波韵升股份有限公司 | A kind of method improving Sintered NdFeB magnet performance |
| CN104425092B (en) * | 2013-08-26 | 2018-02-09 | 比亚迪股份有限公司 | A kind of neodymium-iron-boron magnetic material and preparation method thereof |
| CN105185501B (en) * | 2015-08-28 | 2017-08-11 | 包头天和磁材技术有限责任公司 | The manufacture method of rare earth permanent-magnetic material |
| CN105355412A (en) * | 2015-12-07 | 2016-02-24 | 北京科技大学 | Method for obtaining high-magnetism sintered NdFeB through sulfidizing |
| CN105355413B (en) * | 2015-12-07 | 2017-06-16 | 北京科技大学 | It is a kind of to reduce the method that sintering temperature prepares magnetic sintered NdFeB high |
| CN105489334B (en) * | 2016-01-14 | 2017-06-13 | 北京科技大学 | A kind of method that grain boundary decision obtains magnetic sintered NdFeB high |
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