CN106782974A - A kind of preparation method of neodymium iron boron magnetic body - Google Patents
A kind of preparation method of neodymium iron boron magnetic body Download PDFInfo
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- 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
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- 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
- H01F1/0576—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 pressed, e.g. hot working
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- 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
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Abstract
A kind of preparation method of neodymium iron boron magnetic body of the present invention is related to neodymium iron boron magnetic body production field, by optimization of C/C composites, oriented moulding controls the techniques such as magnet oxygen content, a kind of preparation method of performance Nd Fe B sintered magnet is provided, the problem of the batch production of high performance sintered neodymium-iron-boron product is solved.Praseodymium neodymium 30.0% 31.5%, boron 0.9% 1.0%, terbium 0 2.0%, aluminium 0.03% 0.60%, copper 0.05% 0.25%, cobalt 0.3% 1.5%, zirconium 0 0.2%, niobium 0 0.3%, gallium 0.05 0.3% and iron 62.35% 68.67% being weighed by element weight percent and carrying out fusing casting obtain slab；Slab is put into processing in rotary hydrogen crushing furnace and obtains meal；Be milled obtaining fine powder to lubricant is added in meal；To lubricant and antioxidant is added in fine powder, powder is obtained with the bipyramid mixed powder of mixed powder machine；Model is made, raw embryo product is obtained, acquisition product is sintered and cool down.
Description
Technical field
In particular it is a kind of preparation method of neodymium iron boron magnetic body the present invention relates to neodymium iron boron magnetic body production field.
Background technology
Neodymium iron boron magnetic body has excellent magnetic performance, and usual its Making programme is dispensing, melting, broken hydrogen, powder processed, orientation
Compacting, isostatic pressed, sintering, tempering, post-processing, surface treatment etc..
The theoretical magnetic energy product of sintered NdFeB magnet is 64MGOe, but principal phase ratio by actual magnet, relative density, is taken
To the limitation of the factors such as degree, the magnetic energy product limit in experiment is 59MGOe or so, is said in a sense, high energy product NdFeB
The development potentiality of permanent-magnet material is extremely limited.But from for the angle for producing and applying, high magnetic energy in current permanent magnetism market
Product NdFeB permanent-magnet materials N54,52M, 50H etc., can stablize the enterprise for producing in enormous quantities simultaneously seldom, main reason is that high-performance
Equipment of the production of sintered NdFeB to producing, technique and management requirement are higher, and low oxygen process system is generally used in current industry
Standby performance Nd Fe B sintered magnet.
The remanent magnetism high energy product trades mark high such as the production such as N54,52M, 50H of current high performance sintered neodymium-iron-boron, in order to improve
Magnet Br, it is necessary to as far as possible increase principal phase volume fraction, therefore formula middle rare earth total amount it is relatively low, if production process control not
If good, magnet oxygen content can be caused higher, magnet magnetic property declines rapidly.Therefore, it is necessary to strengthen to material in production process
Protection, the oxygen content of strict control magnet, it is to avoid magnet is aoxidized.
The content of the invention
The present invention solves the technical problem of a kind of preparation method of neodymium iron boron magnetic body is provided, by optimization of C/C composites,
A kind of techniques such as oriented moulding, the distribution of control powder particles, magnet oxygen content, there is provided preparation of performance Nd Fe B sintered magnet
Method, solves the problem of the batch production of high performance sintered neodymium-iron-boron product.
In order to solve the above technical problems, being in particular a kind of neodymium iron the present invention relates to neodymium iron boron magnetic body production field
The preparation method of boron magnet, comprises the following steps：
(1) praseodymium neodymium 30.0%-31.5%, boron 0.9%-1.05%, terbium 0-2.0%, aluminium are weighed by element weight percent
0.03%-0.60%, copper 0.05%-0.25%, cobalt 0.3%-1.5%, zirconium 0-0.2%, niobium 0-0.3%, gallium 0.05-0.3%
With iron 62.35%-68.67%；
(2) material that step (1) is weighed is fitted into crucible, crucible is evacuated to below 10Pa, dried with 50kw power
Stove, when vacuum is less than 5Pa, then applying argon gas to 26.8kPa increase power to 550kw meltings, and 7- is refined again after iron fusing
12 minutes start casting when being 1440-1500 DEG C to temperature, obtain slab and cool down；
(3) slab that step (2) is obtained is put into rotary hydrogen crushing furnace, is evacuated to below 1Pa, be passed through 0.066-
The hydrogen of 0.098MPa, after saturation inhales hydrogen, is heated to 540-600 DEG C, dehydrogenase 34-8 hours, and discharging obtains thick after being cooled to normal temperature
Powder；
(4) lubricant and 0.01-0.2% of meal weight 0.01%-0.15% are added in the meal for obtaining to step (3)
Antioxidant it is well mixed after add three-dimensional mixed powder machine mixed powder 0.5-4 hour, then will be ground in powder addition airflow milling
Powder, not oxygenating in milling process, it is SMD 2.7-3.4 microns, D90/D10 to obtain powder particles<5.2 fine powder；
(5) lubricant and 0.01%- of fine powder weight 0.01%-0.15% are added in the fine powder for obtaining to step (4)
0.2% antioxidant, powder is obtained in 0.5-4 hours with bipyramid mixed powder machine mixed powder；
(6) powder for obtaining step (5) is according to the big little makings model of product size, and in press system oxygen content<
0.05%, mold center's magnetic field intensity>Orientation compacting is carried out under conditions of 1.8T, green density is reached 3.6-4.3g/cm3,
Then green density is made to bring up to 4.4-4.7g/cm using isostatic pressed compacting3, obtain raw embryo product；
(7) the raw embryo product that step (6) is obtained is removed into vacuum packaging bag under airbreak environment, is then placed in nitrogen filled protection
Glove box in, the Control for Oxygen Content in glove box within 0.2%, in glove box by raw embryo product removal film swing in stone
In print cartridge, sintering furnace is then sent through, sintering furnace is evacuated to below 1Pa, sintering furnace temperature keeps 1020-1100 DEG C, insulation
3-12 hours, terminate rear applying argon gas be cooled to less than 90 DEG C be warming up to again 870-930 DEG C or directly stove be cooled to 870-930
DEG C, 2-5 hour is incubated, then applying argon gas are cooled to less than 90 DEG C, then are warmed up to 460-600 DEG C of insulation 2-7 hours, and insulation terminates
After be cooled to less than 80 DEG C and come out of the stove.
As the further optimization of the technical program, the lubricant described in a kind of preparation method of neodymium iron boron magnetic body of the invention
For the YSH-06 neodymium iron boron lubricant agent specials that Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd. produces.
As the further optimization of the technical program, a kind of preparation method of neodymium iron boron magnetic body of the invention, it is characterised in that：
Described antioxidant is the YSH-01 neodymium iron boron special antioxidants of Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd..
A kind of of the invention preparation method of neodymium iron boron magnetic body has the beneficial effect that：
By optimization of C/C composites, oriented moulding controls the techniques such as powder particles distribution, magnet oxygen content, there is provided a kind of property high
The preparation method of energy Sintered NdFeB magnet, solves the problem of the batch production of high performance sintered neodymium-iron-boron product.
Specific embodiment
Specific embodiment one：
In particular it is a kind of preparation method of neodymium iron boron magnetic body the present invention relates to neodymium iron boron magnetic body production field, bag
Include following steps：
(1) praseodymium neodymium 30.0%-31.5%, boron 0.9%-1.05%, terbium 0-2.0%, aluminium are weighed by element weight percent
0.03%-0.60%, copper 0.05%-0.25%, cobalt 0.3%-1.5%, zirconium 0-0.2%, niobium 0-0.3%, gallium 0.05-0.3%
With iron 62.35%-68.67%；
(2) material that step (1) is weighed is fitted into crucible, crucible is evacuated to below 10Pa, dried with 50kw power
Stove, when vacuum is less than 5Pa, then applying argon gas to 26.8kPa increase power to 550kw meltings, and 7- is refined again after iron fusing
12 minutes start casting when being 1440-1500 DEG C to temperature, obtain slab and cool down；
(3) slab that step (2) is obtained is put into rotary hydrogen crushing furnace, is evacuated to below 1Pa, be passed through 0.066-
The hydrogen of 0.098MPa, after saturation inhales hydrogen, is heated to 540-600 DEG C, dehydrogenase 34-8 hours, and discharging obtains thick after being cooled to normal temperature
Powder；
(4) lubricant and 0.01-0.2% of meal weight 0.01%-0.15% are added in the meal for obtaining to step (3)
Antioxidant it is well mixed after add three-dimensional mixed powder machine mixed powder 0.5-4 hour, then will be ground in powder addition airflow milling
Powder, not oxygenating in milling process, it is SMD 2.7-3.4 microns, D90/D10 to obtain powder particles<5.2 fine powder；
(5) lubricant and 0.01%- of fine powder weight 0.01%-0.15% are added in the fine powder for obtaining to step (4)
0.2% antioxidant, powder is obtained in 0.5-4 hours with bipyramid mixed powder machine mixed powder；Lubricant is properly added, is conducive to powder to take
To shaping, the degree of orientation is improved, so that increase remanent magnetism, but lubricant addition can excessively reduce coercivity.
(6) powder for obtaining step (5) is according to the big little makings model of product size, and in press system oxygen content<
0.05%, mold center's magnetic field intensity>Orientation compacting is carried out under conditions of 1.8T, green density is reached 3.6-4.3g/cm3,
Then green density is made to bring up to 4.4-4.7g/cm using isostatic pressed compacting3, obtain raw embryo product；Press system oxygen content mistake
Height, can cause product to aoxidize deformation, and hydraulic performance decline, and green density is too high in addition, and orientation resistance is increased, and is unfavorable for remanent magnetism
Lifting.
(7) the raw embryo product that step (6) is obtained is removed into vacuum packaging bag under airbreak environment, is then placed in nitrogen filled protection
Glove box in, the Control for Oxygen Content in glove box within 0.2%, in glove box by raw embryo product removal film swing in stone
In print cartridge, sintering furnace is then sent through, sintering furnace is evacuated to below 1Pa, sintering furnace temperature keeps 1020-1100 DEG C, insulation
3-12 hours, terminate rear applying argon gas be cooled to less than 90 DEG C be warming up to again 870-930 DEG C or directly stove be cooled to 870-930
DEG C, 2-5 hour is incubated, then applying argon gas are cooled to less than 90 DEG C, then are warmed up to 460-600 DEG C of insulation 2-7 hours, and insulation terminates
After be cooled to less than 80 DEG C and come out of the stove.Sintering temperature is too high, and overlong time all may result in product burning, crystal grain occurs extremely long
Greatly, coercivity declines；And sintering temperature is relatively low, time length partially can then cause product underburnt, and product density is too low, under remanent magnetism etc.
Drop.
Described lubricant is the YSH-06 neodymium iron boron lubricant agent specials that Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd. produces, and is one
Macromolecule esters polymer is planted, there is preferable lubricity, dispersiveness, oxygen-proof property to sintered NdFeB product and product is improved
The effect of performance.
Described antioxidant is the YSH-01 neodymium iron boron special antioxidants of Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd., is
A kind of low molecule alkane polymer, has preferable oxygen-proof property, lubricity to sintered NdFeB product and enhances product performance
Effect.
Concrete case one：A kind of N54 Sintered NdFeB magnets.
1. dispensing.Formula is as follows：Praseodymium neodymium 30.1%, boron 0.94%, aluminium 0.05%, copper are weighed by element weight percent
0.09%th, cobalt 0.7%, zirconium 0.06%, niobium 0.1%, gallium 0.1% and iron 67.86%.
2. melting.Above-mentioned dispensing is fitted into crucible, the vacuum of stove is evacuated to below 10Pa, with 50kw power bakers,
When vacuum is less than 5Pa, then applying argon gas to 26.8kPa increase power to 550kw meltings, and 7 minutes are refined after iron fusing extremely
Temperature starts casting when being 1440 DEG C, obtain slab and cool down, after blow-on discharging after slab cooling.
3. hydrogen is broken.Above-mentioned slab is put into rotary hydrogen crushing furnace, below 1Pa is evacuated to, the hydrogen of 0.066MPa is passed through
Gas, after saturation inhales hydrogen, is heated to 540 DEG C of dehydrogenase 34s hour, and discharging obtains meal after being cooled to normal temperature.
4. powder processed.After being well mixed to the lubricant and 0.01% antioxidant of meal plus addition meal weight 0.01%
Add the three-dimensional mixed mixed powder of powder machine 3 hours, be milled during powder then is added into airflow milling, not oxygenating in milling process is obtained
Powder particles are SMD 2.7-3.4 microns, D90/D10<5.2 fine powder.To addition fine powder weight 0.01% in the fine powder for obtaining
Lubricant and 0.01% antioxidant, obtain powder within 2 hours with the bipyramid mixed powder of mixed powder machine；Lubricant is properly added, favorably
In powder oriented moulding, the degree of orientation is improved, so that increase remanent magnetism, but lubricant addition can excessively reduce coercivity.
5. suppress.During orientation compacting, press system oxygen content<0.05%, to substantially ensure that powder is not oxidized, in mould
Core field intensity>To improve the degree of orientation of magnet, green density is 3.6-4.3g/cm to 1.8T3.Hydrostatic pressure is used
160MPa, green density brings up to 4.4-4.7g/cm after isostatic pressed3.Press system too high oxygen level, can cause product to aoxidize and become
Shape, and hydraulic performance decline, green density is too high in addition, and orientation resistance is increased, and is unfavorable for the lifting of remanent magnetism.
6. sinter.The raw embryo product that step (6) is obtained is removed into vacuum packaging bag under airbreak environment, nitrogen charging is then placed in
In the glove box of protection, the Control for Oxygen Content in glove box puts raw embryo product removal film in glove box within 0.2%
Enter in graphite, be then sent through sintering furnace, sintering furnace is evacuated to below 1Pa, sintering furnace temperature is kept for 1020-1100 DEG C,
Insulation 7 hours, terminates rear applying argon gas and is cooled to less than 90 DEG C to be warming up to 870-930 DEG C again or direct stove is cooled to 870-
930 DEG C, 3 hours are incubated, then applying argon gas are cooled to less than 90 DEG C, then are warmed up to 460-600 DEG C and be incubated 5 hours, insulation terminates
After be cooled to less than 80 DEG C and come out of the stove.It is above-mentioned to be warming up to 870-930 DEG C or directly stove is cooled to 870-930 DEG C of temperature model and select
Take 900 DEG C, 905 DEG C, 910 DEG C, 915 DEG C, 925 DEG C of equitemperatures, be warmed up to 460-600 DEG C of temperature model can choose 470 DEG C,
485 DEG C, 500 DEG C, 520 DEG C, 550 DEG C, 580 DEG C of equitemperatures.Sintering temperature is too high, and overlong time all may result in product mistake
Burn, abnormal grain growth occur, coercivity declines；And sintering temperature is relatively low, time length partially can then cause product underburnt, and product is close
Spend low, the decline such as remanent magnetism.
The neodymium iron boron magnetic body magnet oxygen content of acquisition is less than 800ppm, and remaining performance test is as shown in the table.
| Br | Hcb | Hcj | (BH)max | Hk/Hcj |
| 14.76 | 11.41 | 11.86 | 53.08 | 0.97 |
| 14.81 | 11.36 | 11.74 | 52.97 | 0.98 |
Concrete case two：A kind of 52M Sintered NdFeB magnets.
1. dispensing.Formula is as follows：Praseodymium neodymium 30.08%, boron 0.94%, terbium 0.12%, aluminium are weighed by element weight percent
0.09%th, copper 0.11%, cobalt 0.9%, zirconium 0.06%, niobium 0.1%, gallium 0.18%, remaining be iron.
2. melting.Above-mentioned dispensing is fitted into crucible, the vacuum of stove is evacuated to below 10Pa, with 50kw power bakers,
When vacuum is less than 5Pa, then applying argon gas to 26.8kPa increase power to 550kw meltings, and 8 minutes are refined after iron fusing extremely
Temperature starts casting when being 1445 DEG C, obtain slab and cool down, after blow-on discharging after slab cooling.
3. hydrogen is broken.Above-mentioned slab is put into rotary hydrogen crushing furnace, below 1Pa is evacuated to, the hydrogen of 0.07MPa is passed through
Gas, after saturation inhales hydrogen, is heated to 570 DEG C of dehydrogenase 35s hour, and discharging obtains meal after being cooled to normal temperature.
4. powder processed.After being well mixed to the lubricant and 0.12% antioxidant of meal plus addition meal weight 0.12%
Add the three-dimensional mixed mixed powder of powder machine 3 hours, be milled during powder then is added into airflow milling, not oxygenating in milling process is obtained
Powder particles are SMD 2.7-3.4 microns, D90/D10<5.2 fine powder.To addition fine powder weight 0.1% in the fine powder for obtaining
Lubricant and 0.1% antioxidant, powder is obtained in 2 hours with the bipyramid mixed powder of mixed powder machine；Lubricant is properly added, is conducive to powder
Material oriented moulding, improves the degree of orientation, so that increase remanent magnetism, but lubricant addition can excessively reduce coercivity.
5. suppress.During orientation compacting, press system oxygen content<0.05%, to substantially ensure that powder is not oxidized, in mould
Core field intensity>To improve the degree of orientation of magnet, green density is 3.6-4.3g/cm to 1.8T3.Hydrostatic pressure uses 160-
240MPa, green density brings up to 4.4-4.7g/cm after isostatic pressed3.Press system too high oxygen level, can cause product to aoxidize and become
Shape, and hydraulic performance decline, green density is too high in addition, and orientation resistance is increased, and is unfavorable for the lifting of remanent magnetism.
6. sinter.The raw embryo product that step (6) is obtained is removed into vacuum packaging bag under airbreak environment, nitrogen charging is then placed in
In the glove box of protection, the Control for Oxygen Content in glove box puts raw embryo product removal film in glove box within 0.2%
Enter in graphite, be then sent through sintering furnace, sintering furnace is evacuated to below 1Pa, sintering furnace temperature is kept for 1020-1100 DEG C,
Insulation 7 hours, terminates rear applying argon gas and is cooled to less than 90 DEG C to be warming up to 870-930 DEG C again or direct stove is cooled to 870-
930 DEG C, 3 hours are incubated, then applying argon gas are cooled to less than 90 DEG C, then are warmed up to 460-600 DEG C and be incubated 5 hours, insulation terminates
After be cooled to less than 80 DEG C and come out of the stove.It is above-mentioned to be warming up to 870-930 DEG C or directly stove is cooled to 870-930 DEG C of temperature model and select
Take 900 DEG C, 905 DEG C, 910 DEG C, 915 DEG C, 925 DEG C of equitemperatures, be warmed up to 460-600 DEG C of temperature model can choose 470 DEG C,
485 DEG C, 500 DEG C, 520 DEG C, 550 DEG C, 580 DEG C of equitemperatures.Sintering temperature is too high, and overlong time all may result in product mistake
Burn, abnormal grain growth occur, coercivity declines；And sintering temperature is relatively low, time length partially can then cause product underburnt, and product is close
Spend low, the decline such as remanent magnetism.
The neodymium iron boron magnetic body magnet oxygen content of acquisition is less than 1000ppm, and remaining performance test is as shown in the table.
| Br | Hcb | Hcj | (BH)max | Hk/Hcj |
| 14.48 | 13.68 | 14.14 | 51.86 | 0.97 |
| 14.42 | 13.67 | 14.27 | 51.35 | 0.98 |
Concrete case three：A kind of 50H Sintered NdFeB magnets.
1. dispensing.Formula is as follows：Praseodymium neodymium 30.5%, boron 0.95%, terbium 1.4%, aluminium are weighed by element weight percent
0.18%th, copper 0.11%, cobalt 0.9%, zirconium 0.06%, niobium 0.12%, gallium 0.25%, remaining be iron.
2. melting.Above-mentioned dispensing is fitted into crucible, the vacuum of stove is evacuated to below 10Pa, with 50kw power bakers,
When vacuum is less than 5Pa, then applying argon gas to 26.8kPa increase power to 550kw meltings, are refined 12 minutes after iron fusing
To temperature be 1500 DEG C when start casting, obtain slab simultaneously cool down, after slab cooling after blow-on discharging.
3. hydrogen is broken.Above-mentioned slab is put into rotary hydrogen crushing furnace, below 1Pa is evacuated to, the hydrogen of 0.098MPa is passed through
Gas, after saturation inhales hydrogen, is heated to 600 DEG C of dehydrogenations 8 hours, and discharging obtains meal after being cooled to normal temperature.
4. powder processed.After being well mixed to the lubricant and 0.15% antioxidant of meal plus addition meal weight 0.15%
Add the three-dimensional mixed mixed powder of powder machine 3 hours, be milled during powder then is added into airflow milling, not oxygenating in milling process is obtained
Powder particles are SMD 2.7-3.4 microns, D90/D10<5.2 fine powder.To addition fine powder weight 0.15% in the fine powder for obtaining
Lubricant and 0.15% antioxidant, obtain powder within 4 hours with the bipyramid mixed powder of mixed powder machine；Lubricant is properly added, favorably
In powder oriented moulding, the degree of orientation is improved, so that increase remanent magnetism, but lubricant addition can excessively reduce coercivity.
5. suppress.During orientation compacting, press system oxygen content<0.05%, to substantially ensure that powder is not oxidized, in mould
Core field intensity>To improve the degree of orientation of magnet, green density is 3.6-4.3g/cm to 1.8T3.Hydrostatic pressure is used
240MPa, green density brings up to 4.4-4.7g/cm after isostatic pressed3.Press system too high oxygen level, can cause product to aoxidize and become
Shape, and hydraulic performance decline, green density is too high in addition, and orientation resistance is increased, and is unfavorable for the lifting of remanent magnetism.
6. sinter.The raw embryo product that step (6) is obtained is removed into vacuum packaging bag under airbreak environment, nitrogen charging is then placed in
In the glove box of protection, the Control for Oxygen Content in glove box puts raw embryo product removal film in glove box within 0.2%
Enter in graphite, be then sent through sintering furnace, sintering furnace is evacuated to below 1Pa, sintering furnace temperature is kept for 1020-1100 DEG C,
Insulation 7 hours, terminates rear applying argon gas and is cooled to less than 90 DEG C to be warming up to 870-930 DEG C again or direct stove is cooled to 870-
930 DEG C, 3 hours are incubated, then applying argon gas are cooled to less than 90 DEG C, then are warmed up to 460-600 DEG C and be incubated 5 hours, insulation terminates
After be cooled to less than 80 DEG C and come out of the stove.It is above-mentioned to be warming up to 870-930 DEG C or directly stove is cooled to 870-930 DEG C of temperature model and select
Take 900 DEG C, 905 DEG C, 910 DEG C, 915 DEG C, 925 DEG C of equitemperatures, be warmed up to 460-600 DEG C of temperature model can choose 470 DEG C,
485 DEG C, 500 DEG C, 520 DEG C, 550 DEG C, 580 DEG C of equitemperatures.Sintering temperature is too high, and overlong time all may result in product mistake
Burn, abnormal grain growth occur, coercivity declines；And sintering temperature is relatively low, time length partially can then cause product underburnt, and product is close
Spend low, the decline such as remanent magnetism.
The neodymium iron boron magnetic body magnet oxygen content of acquisition is less than 1000ppm, and remaining performance test is as shown in the table.
| Br | Hcb | Hcj | (BH)max | Hk/Hcj |
| 14.07 | 13.96 | 18.48 | 49.84 | 0.99 |
| 14.11 | 13.99 | 18.19 | 49.95 | 0.98 |
Certainly, described above not limitation of the present invention, the present invention is also not limited to the example above, the art
Change, remodeling, addition or replacement that those of ordinary skill is made in essential scope of the invention, fall within guarantor of the invention
Shield scope.
Claims (3)
1. a kind of preparation method of neodymium iron boron magnetic body, it is characterised in that：
(1) praseodymium neodymium 30.0%-31.5%, boron 0.9%-1.05%, terbium 0-2.0%, aluminium are weighed by element weight percent
0.03%-0.60%, copper 0.05%-0.25%, cobalt 0.3%-1.5%, zirconium 0-0.2%, niobium 0-0.3%, gallium 0.05-0.3%
With iron 62.35%-68.67%；
(2) material that step (1) is weighed is fitted into crucible, crucible is evacuated to below 10Pa, with 50kw power bakers, directly
When being less than 5Pa to vacuum, then applying argon gas to 26.8kPa increase power to 550kw meltings, and 7-12 points is refined again after iron fusing
Clock starts casting when being 1440-1500 DEG C to temperature, obtains slab and cools down；
(3) slab that step (2) is obtained is put into rotary hydrogen crushing furnace, is evacuated to below 1Pa, be passed through 0.066-
The hydrogen of 0.098MPa, after saturation inhales hydrogen, is heated to 540-600 DEG C, dehydrogenase 34-8 hours, and discharging obtains thick after being cooled to normal temperature
Powder；
(4) added in the meal for obtaining to step (3) meal weight 0.01%-0.15% lubricant and 0.01-0.2% it is anti-
The three-dimensional mixed mixed powder of powder machine is added after oxidant is well mixed 0.5-4 hours, be milled during powder then is added into airflow milling, ground
Not oxygenating during powder, it is SMD 2.7-3.4 microns, D90/D10 to obtain powder particles<5.2 fine powder；
(5) lubricant and 0.01%-0.2% of fine powder weight 0.01%-0.15% are added in the fine powder for obtaining to step (4)
Antioxidant, powder is obtained in 0.5-4 hours with bipyramid mixed powder machine mixed powder；
(6) powder for obtaining step (5) is according to the big little makings model of product size, and in press system oxygen content<0.05%,
Mold center's magnetic field intensity>Orientation compacting is carried out under conditions of 1.8T, green density is reached 3.6-4.3g/cm3, then use
Isostatic pressed compacting makes green density bring up to 4.4-4.7g/cm3, obtain raw embryo product；
(7) the raw embryo product that step (6) is obtained is removed into vacuum packaging bag under airbreak environment, is then placed in the hand of nitrogen filled protection
In casing, raw embryo product removal film is swung in graphite by the Control for Oxygen Content in glove box within 0.2% in glove box
It is interior, sintering furnace is then sent through, sintering furnace is evacuated to below 1Pa, sintering furnace temperature is kept for 1020-1100 DEG C, is incubated 3-12
Hour, terminate rear applying argon gas and be cooled to less than 90 DEG C to be warming up to 870-930 DEG C again or direct stove is cooled to 870-930 DEG C,
2-5 hours is incubated, then applying argon gas are cooled to less than 90 DEG C, then is warmed up to 460-600 DEG C and be incubated 2-7 hours, after insulation terminates
Less than 80 DEG C are cooled to come out of the stove.
2. the preparation method of a kind of neodymium iron boron magnetic body according to claim 1, it is characterised in that：Described lubricant is day
The YSH-06 neodymium iron boron lubricant agent specials that Jin Yuesheng magnetoelectricities Technology Co., Ltd. produces.
3. the preparation method of a kind of neodymium iron boron magnetic body according to claim 1, it is characterised in that：Described antioxidant is
The YSH-01 neodymium iron boron special antioxidants of Tianjin Yue Sheng magnetoelectricities Technology Co., Ltd..
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| CN107240470A (en) * | 2017-07-12 | 2017-10-10 | 浙江中科磁业有限公司 | A kind of low weightless Sintered NdFeB magnet and preparation method |
| CN107919200A (en) * | 2017-11-03 | 2018-04-17 | 赵宇靖 | A kind of method for preparing sintering RETMB systems permanent magnetic powder |
| CN108417376A (en) * | 2018-02-05 | 2018-08-17 | 宁波松科磁材有限公司 | A kind of Sintered NdFeB magnet preparation method without heavy rare earth |
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