CN109273240A - A kind of preparation method of samarium cobalt permanent magnet body - Google Patents
A kind of preparation method of samarium cobalt permanent magnet body Download PDFInfo
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- CN109273240A CN109273240A CN201811251319.6A CN201811251319A CN109273240A CN 109273240 A CN109273240 A CN 109273240A CN 201811251319 A CN201811251319 A CN 201811251319A CN 109273240 A CN109273240 A CN 109273240A
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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
- H01F41/0266—Moulding; Pressing
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- 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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0556—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together pressed
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- 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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
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- Powder Metallurgy (AREA)
Abstract
A kind of preparation method of samarium cobalt permanent magnet body, comprising the following steps: (1) raw material containing samarium, cobalt, iron, copper, zirconium prepared in advance is subjected to melting, frequency reducing heat preservation refining, chilling obtains samarium-cobalt alloy ingot casting；(2) coarse granule for being 20 ~ 100 microns at partial size by the coarse crushing of samarium-cobalt alloy ingot casting；(3) samarium-cobalt alloy coarse granule is further crushed using airflow milling；(4) airflow milling powder is orientated under magnetic field and compression moulding, progress isostatic cool pressing obtains SmCo green compact；(5) by samarium cobalt blank, successively vacuum is pre-sintered, filling with inert gas sintering, cooling solid solution, air-cooled to room temperature, obtains sintering blank；(6) ageing treatment is carried out, samarium cobalt permanent magnet body is obtained.The shortcomings that present invention is adjusted by formula and sintering process, and samarium cobalt permanent magnet body high comprehensive magnetic properties and elevated operating temperature can be overcome to cannot be considered in terms of obtains while having Good All-around Property and the samarium cobalt permanent magnet body compared with elevated operating temperature.
Description
Technical field
The present invention relates to rare-earth permanent-magnet material technical fields, are specifically related to a kind of preparation method of samarium cobalt permanent magnet body.
Background technique
In recent years, sintered samarium cobalt permanent-magnet material is fast-developing due to its high temperature resistance is good, is widely used in motor, instrument
Table, sensor, detector, engine, radar and other high-tech areas.The method of industrially prepared samarium-cobalt permanent-magnetic material is mainly
Powder metallurgic method, the process flow generally produced are as follows: ingredient → melting → powder → molding → sintering → timeliness → magnetic detection processed
→ post-processing → surface treatment → inspection → finished product.
The maximum operating temperature of samarium-cobalt permanent-magnetic material can achieve 300 ~ 500 DEG C, but samarium-cobalt permanent-magnetic material have remanent magnetism and
The lower disadvantage of maximum magnetic energy product, the especially samarium-cobalt permanent-magnetic material of low-temperature coefficient series, remanent magnetism Br be 0.9 ~ 1.02T(9 ~
10.2kGs), maximum magnetic energy product (BH) max sacrifices comprehensive magnetic energy, nothing although operating temperature is higher for 20 ~ 25MGOe
Method takes into account operating temperature and comprehensive magnetic energy.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a kind of preparation of samarium cobalt permanent magnet body
Method, gained samarium cobalt permanent magnet body have compared with high comprehensive magnetic properties, can work compared with elevated operating temperature.
The technical solution used to solve the technical problems of the present invention is that a kind of preparation method of samarium cobalt permanent magnet body, including with
Lower step:
(1) raw material containing samarium, cobalt, iron, copper, zirconium prepared in advance is subjected to melting, then frequency reducing heat preservation refining, then chilling, obtains
To samarium-cobalt alloy ingot casting；
(2) coarse granule for being 20 ~ 100 microns (μm) at partial size by samarium-cobalt alloy ingot casting coarse crushing obtained by step (1) obtains SmCo conjunction
Golden coarse granule；
(3) samarium-cobalt alloy coarse granule obtained by step (2) is further crushed using airflow milling, obtains airflow milling powder；
(4) airflow milling powder obtained by step (3) is orientated under magnetic field and compression moulding, progress isostatic cool pressing obtains SmCo pressure
Base；
(5) by samarium cobalt blank obtained by step (4), successively vacuum is pre-sintered, filling with inert gas sintering, and cooling solid solution is air-cooled to room
Temperature obtains sintering blank；
(6) ageing treatment is carried out, samarium cobalt permanent magnet body is obtained.
Further, in step (1), containing samarium, cobalt, iron, copper, zirconium raw material in, samarium, cobalt, iron, copper, zirconium are according to following quality
Percentage ingredient: samarium 26 ~ 28%, cobalt 45.8~51%, iron 14.5 ~ 18%, copper 5~7%, zirconium 1.5~3%, the sum of each Material Percentage
It is 100%.Samarium, cobalt are the collection element of volume of magnet, form the anisotropic structure with easy magnetizing axis, and the increase of samarium content can mention
The remanent magnetism Br of high magnet；Iron may replace the Sm in samarium-cobalt magnet in cell structure2Co17The part Co of phase forms the Sm of richness Fe2
(CoFe)2Phase improves its maximum magnetic energy product, Cu and Zr by cell wall invigoration effect and second-phase strength mechanism intracellular, improves samarium
The intrinsic coercivity and maximum operation (service) temperature of cobalt magnet.These are added to together, synergistic effect can be generated, improves the property of material
Energy.
Further, in step (1), melting frequency is 40 ~ 60Hz.
Further, in step (1), the refining temperature is 1400 ~ 1600 DEG C, and the time is 5 ~ 15min.
Further, in step (1), refining frequency is reduced to 5 ~ 20Hz.
Further, successively broken using jaw crusher, intermediate crusher in step (2).
Further, in step (3), the partial size of the airflow milling powder is 3~5 μm.
Further, in step (4), the magnetic field is 1.5 ~ 2T, and typed pressure is 1 ~ 20MPa, and isostatic cool pressing pressure is 170
~220MPa。
Further, in step (5), vacuum degree≤2.0 × 10 of vacuum pre-sintering-1Pa, the temperature of pre-sintering is 1180 ~
1195 DEG C, keep the temperature 30min or more；Inert gas is the argon gas of percent by volume purity >=99.99%；Sintering temperature be 1220 ~
1250 DEG C, 100 ~ 180min of soaking time；Solid solubility temperature is 1150 ~ 1180 DEG C, 100 ~ 180min of soaking time.Sintering temperature
It improves, the density of magnet can be improved and then promotes the maximum magnetic energy product of magnet, suitable solid solubility temperature and rapid cooling can be protected
Stay high-temperature-phase, prepare optimum condition for ageing treatment and uniform sufficient dislocation source be provided, can in ag(e)ing process the company of being formed
Continuous phase transition.
Further, in step (6), time-triggered protocol are as follows: be first warming up to 800 ~ 830 DEG C, 10 ~ 20h of soaking time；Again with 0.3 ~
The speed of 0.7 DEG C/min is cooled to 350 ~ 450 DEG C, 10 ~ 15h of soaking time.Suitable aging treatment process, can be improved magnet
Intrinsic coercivity, mainly pass through timeliness and promote to form uniform cell wall phase Sm(Co, Cu in samarium-cobalt magnet in cellular structure)5,
Magnet is made to obtain higher coercivity and elevated operating temperature by cell wall phase pinning domain wall.
The present invention can overcome samarium cobalt permanent magnet body high comprehensive magnetic properties and elevated operating temperature by formula and sintering process adjustment
The shortcomings that cannot be considered in terms of obtains while having Good All-around Property and the samarium cobalt permanent magnet body compared with elevated operating temperature.
Specific embodiment
Present invention is further described in detail combined with specific embodiments below.
Comparative example 1
This comparative example the following steps are included:
(1) raw material samarium, cobalt, iron, copper, zirconium ingredient: are weighed；By raw material press following mass percent ingredient: samarium 25.5%, cobalt 52%,
Iron 10.5%, copper 8%, zirconium 4%；
(2) alloy melting: carrying out melting for prepared raw material in intermediate frequency furnace, then refining is kept the temperature at a temperature of 1450 DEG C
Then 10min pours into chilling in condensation mould, obtains samarium-cobalt alloy ingot casting；
(3) samarium-cobalt alloy ingot casting jaw crusher and intermediate crusher alloy cast ingot coarse crushing: are broken into partial size at 20 ~ 100 μm
Coarse granule；
(4) airflow milling powder: coarse granule is further crushed to 3~5 μm using airflow milling, obtains airflow milling magnetic powder；
(5) oriented moulding: airflow milling magnetic powder is orientated under the magnetic field of 1.8T and compression moulding, then again under 200Mpa pressure
Isostatic cool pressing is carried out, samarium cobalt blank is obtained；
(6) be sintered and be dissolved: in vertical sintering furnace, by samarium cobalt blank, vacuum is pre-sintered 30min at 1185 DEG C, and vacuum degree is
0.2Pa, then applying argon gas are sintered 90min at 1200 DEG C, are then cooled to 1175 DEG C of solid solution 120min, last air-cooled to room temperature,
Obtain sintering blank；
(7) ageing treatment: keeping the temperature 20h for sintering blank at 800 DEG C, be then cooled to 400 DEG C with the speed of 0.5 DEG C/min,
10h is kept the temperature, room temperature is finally chilled to and obtains samarium cobalt permanent magnet body.
The samarium cobalt permanent magnet body sample test magnetic property of this comparative example preparation, test result are as shown in table 1.
Comparative example 2
This comparative example the following steps are included:
(1) raw material samarium, cobalt, iron, copper, zirconium ingredient: are weighed；By raw material press following mass percent ingredient: samarium 25.5%, cobalt 52%,
Iron 10.5%, copper 8%, zirconium 4%；
(2) alloy melting: carrying out melting for prepared raw material in intermediate frequency furnace, then reduces frequency to 15Hz, 1520
Then heat preservation refining 5min at a temperature of DEG C pours into chilling in condensation mould and obtains samarium-cobalt alloy ingot casting；
(3) samarium-cobalt alloy ingot casting jaw crusher and intermediate crusher alloy cast ingot coarse crushing: are broken into partial size at 20 ~ 100 μm
Coarse granule；
(4) airflow milling powder: coarse granule is further crushed to 3~5 μm using airflow milling, obtains airflow milling magnetic powder；
(5) oriented moulding: airflow milling magnetic powder is orientated under the magnetic field of 1.9T and compression moulding, then again under 190Mpa pressure
Isostatic cool pressing is carried out, samarium cobalt blank is obtained；
(6) be sintered and be dissolved: in vertical sintering furnace, by samarium cobalt blank, vacuum is pre-sintered 30min at 1185 DEG C, and vacuum degree is
0.2Pa, then applying argon gas are sintered 150min at 1210 DEG C, are then cooled to 1175 DEG C of solid solution 150min, last air-cooled to room temperature,
Obtain sintering blank；
(7) ageing treatment: keeping the temperature 20h for sintering blank at 800 DEG C, be then cooled to 400 DEG C with the speed of 0.5 DEG C/min,
10h is kept the temperature, room temperature is finally chilled to and obtains samarium cobalt permanent magnet body.
The samarium cobalt permanent magnet body sample test magnetic property of this comparative example preparation, test result are as shown in table 1.
Comparative example 3
Comparative example 3 is commercially available common elevated operating temperature (low-temperature coefficient) samarium-cobalt permanent-magnetic material.
Embodiment 1
The present embodiment the following steps are included:
(1) raw material samarium, cobalt, iron, copper, zirconium ingredient: are weighed；Raw material is pressed into following mass percent ingredient: samarium 26.5%, cobalt
49.2%, iron 14.6%, copper 6.8%, zirconium 2.9%；Prepared raw material is subjected to melting in intermediate frequency furnace, melting frequency is
40Hz；Frequency is reduced again to 15Hz, and heat preservation refining 5min, then pours into and condense chilling in mould, obtain samarium at a temperature of 1520 DEG C
Cobalt alloy ingot casting；
(2) alloy cast ingot coarse crushing: successively use jaw crusher, intermediate crusher broken on samarium-cobalt alloy ingot casting obtained by step (1)
The coarse granule that coarse crushing is 20 ~ 100 microns (μm) at partial size, obtains samarium-cobalt alloy coarse granule；
(3) airflow milling powder: coarse granule is further crushed to 3~5 μm using airflow milling, obtains airflow milling magnetic powder；
(4) airflow milling powder obtained by step (3) oriented moulding: is orientated simultaneously compression moulding, typed pressure under the magnetic field of 1.9T
For 10MPa, isostatic cool pressing is then carried out under 190Mpa pressure again, obtains samarium cobalt blank；
(5) be sintered and be dissolved: in vertical sintering furnace, by samarium cobalt blank obtained by step (4), vacuum is pre-sintered at 1185 DEG C
30min, vacuum degree are 2.0 × 10-1Pa；The argon gas for filling percent by volume purity >=99.99% again is sintered at 1220 DEG C
Then 150min is cooled to 1175 DEG C of solid solution 150min, last air-cooled to room temperature, obtains sintering blank；
(6) ageing treatment: keeping the temperature 10h for sintering blank at 820 DEG C, be then cooled to 400 DEG C with the speed of 0.5 DEG C/min,
10h is kept the temperature, room temperature is finally chilled to and obtains samarium cobalt permanent magnet body.
Samarium cobalt permanent magnet body sample test magnetic property manufactured in the present embodiment, test result are as shown in table 1.
Embodiment 2
The present embodiment and the difference of embodiment 1 are only that: in step (5), sintering temperature is 1230 DEG C.Remaining is the same as embodiment 1.
Samarium cobalt permanent magnet body sample test magnetic property manufactured in the present embodiment, test result are as shown in table 1.
Embodiment 3
The present embodiment and the difference of embodiment 1 are only that: in step (5), sintering temperature is 1240 DEG C.Remaining is the same as embodiment 1.
Samarium cobalt permanent magnet body sample test magnetic property manufactured in the present embodiment, test result are as shown in table 1.
Table 1
From properties of sample prepared in the above embodiments it is found that samarium-cobalt permanent-magnetic material prepared by the present invention has both compared with comparative example
Higher comprehensive magnetic energy and elevated operating temperature, are applicable to 400 DEG C of hot environment.
Those skilled in the art can carry out various modifications to the present invention and modification, if these modifications and variations are at this
Within the scope of invention claim and its equivalent technologies, then these modifications and variations are also within protection scope of the present invention.
The prior art that the content being not described in detail in specification is known to the skilled person.
Claims (10)
1. a kind of preparation method of samarium cobalt permanent magnet body, which comprises the following steps:
(1) raw material containing samarium, cobalt, iron, copper, zirconium prepared in advance is subjected to melting, then frequency reducing heat preservation refining, then chilling, obtains
To samarium-cobalt alloy ingot casting；
(2) coarse granule for being 20 ~ 100 microns at partial size by samarium-cobalt alloy ingot casting coarse crushing obtained by step (1), it is thick to obtain samarium-cobalt alloy
Particle；
(3) samarium-cobalt alloy coarse granule obtained by step (2) is further crushed using airflow milling, obtains airflow milling powder；
(4) airflow milling powder obtained by step (3) is orientated under magnetic field and compression moulding, progress isostatic cool pressing obtains SmCo pressure
Base；
(5) by samarium cobalt blank obtained by step (4), successively vacuum is pre-sintered, filling with inert gas sintering, and cooling solid solution is air-cooled to room
Temperature obtains sintering blank；
(6) ageing treatment is carried out, samarium cobalt permanent magnet body is obtained.
2. the preparation method of samarium cobalt permanent magnet body according to claim 1, which is characterized in that in step (1), containing samarium, cobalt,
Iron, copper, zirconium raw material in, samarium, cobalt, iron, copper, zirconium are according to following mass percent ingredient: samarium 26 ~ 28%, cobalt 45.8~51%, iron
14.5 ~ 18%, copper 5~7%, zirconium 1.5~3%, the sum of each Material Percentage are 100%.
3. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (1), melting frequency
Rate is 40 ~ 60Hz.
4. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (1), the essence
Refining temperature is 1400 ~ 1600 DEG C, and the time is 5 ~ 15min.
5. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (1), refining frequency
Rate is reduced to 5 ~ 20Hz.
6. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (2), successively adopt
It is broken with jaw crusher, intermediate crusher.
7. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (3), the gas
The partial size at stream milling end is 3~5 μm.
8. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (4), the magnetic
Field is 1.5 ~ 2T, and typed pressure is 1 ~ 20MPa, and isostatic cool pressing pressure is 170 ~ 220MPa.
9. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (5), vacuum is pre-
Vacuum degree≤2.0 × 10 of sintering-1Pa, the temperature of pre-sintering are 1180 ~ 1195 DEG C, keep the temperature 30min or more；Inert gas is body
The argon gas of product percent purity >=99.99%；Sintering temperature is 1220 ~ 1250 DEG C, 100 ~ 180min of soaking time；Solid solubility temperature
It is 1150 ~ 1180 DEG C, 100 ~ 180min of soaking time.
10. the preparation method of samarium cobalt permanent magnet body according to claim 1 or 2, which is characterized in that in step (6), at the time
Reason are as follows: be first warming up to 800 ~ 830 DEG C, 10 ~ 20h of soaking time；350 ~ 450 DEG C are cooled to the speed of 0.3 ~ 0.7 DEG C/min again,
10 ~ 15h of soaking time.
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| CN109859945A (en) * | 2019-03-01 | 2019-06-07 | 杭州科德磁业有限公司 | A kind of preparation method of high temperature samarium-cobalt permanent-magnetic material |
| CN111128502A (en) * | 2019-12-04 | 2020-05-08 | 湖南航天磁电有限责任公司 | Preparation method of super-corrosion-resistant high-performance sintered samarium-cobalt magnet |
| CN111161933A (en) * | 2019-12-23 | 2020-05-15 | 湖南航天磁电有限责任公司 | Preparation method of high-coercivity low-temperature-coefficient sintered samarium-cobalt permanent magnet |
| CN111180157A (en) * | 2019-12-24 | 2020-05-19 | 中国计量大学 | A method of manufacturing a semiconductor device, comprises the following steps: 17-type SmCoCuFeZrB sintered permanent magnet and preparation method thereof |
| CN112017831A (en) * | 2020-08-20 | 2020-12-01 | 合肥工业大学 | Preparation method of high-toughness samarium-cobalt magnet |
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| CN113903587B (en) * | 2021-09-15 | 2023-07-07 | 太原科技大学 | Preparation method of high-temperature 2:17 sintered samarium cobalt magnet |
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