CN112435846A - Manufacturing method of 550-DEG C-resistant samarium-cobalt permanent magnet material - Google Patents
Manufacturing method of 550-DEG C-resistant samarium-cobalt permanent magnet material Download PDFInfo
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- CN112435846A CN112435846A CN202011170702.6A CN202011170702A CN112435846A CN 112435846 A CN112435846 A CN 112435846A CN 202011170702 A CN202011170702 A CN 202011170702A CN 112435846 A CN112435846 A CN 112435846A
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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
- H01F1/10—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 non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
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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
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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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Abstract
The invention discloses a method for manufacturing a 550-DEG C-resistant samarium cobalt permanent magnet material, which combines powder metallurgy with a low-oxygen process, and finally forms the high-temperature samarium cobalt permanent magnet material by six links of material preparation, vacuum melting, powder making, magnetic field forming, isostatic pressing, sintering and heat treatment on five metal elements of samarium, cobalt, copper, iron and zirconium, wherein the density of the high-temperature samarium cobalt permanent magnet material is 8.30g/cm3‑8.50g/cm3The intrinsic coercivity is larger than 7kOe between the maximum magnetic energy product of 16MGOe and 20MGOe at normal temperature and between the maximum magnetic energy product of 8MGOe and 12MGOe at the high temperature of 550 ℃, and the magnetic coercivity is a straight line on a demagnetization curve of 550 ℃.
Description
Technical Field
The invention relates to the field of preparation of high-temperature type samarium cobalt permanent magnet materials, in particular to a method for preparing a 550-DEG C-resistant type samarium cobalt permanent magnet material.
Background
The 2:17 type samarium cobalt permanent magnet material has excellent temperature characteristic and higher magnetic property, is widely applied to the fields of aviation, aerospace, national defense and military industry, petroleum, special motors and the like, and 2: the production of the 17-type sintered samarium cobalt magnetic material is divided into five processes of smelting, powder making, molding, sintering and heat treatment, and 2: the 17-type samarium cobalt permanent magnetic material has a subdivision field called as a high-temperature-resistant samarium cobalt permanent magnetic material, still has higher coercive force and magnetic performance at the high temperature of 500 ℃, particularly has linear magnetic induction coercive force at the temperature of 500 ℃, and really has the service capability at the temperature of 500 ℃. The samarium cobalt permanent magnet material has important application in the fields of electric propulsion systems of aircrafts, turbofan engines with high thrust-weight ratio and the like, so that the development of the samarium cobalt permanent magnet material has important significance and value.
At present, the ordinary samarium cobalt permanent magnet material is called to be used at 350 ℃, the actual maximum use temperature is only about 300 ℃, the magnetic induction coercive force is nonlinear at 350 ℃, secondary use conditions are not provided, the content of iron is reduced by increasing the content of copper and samarium, the use temperature of the samarium cobalt permanent magnet material can be increased to a certain degree, but the samarium cobalt permanent magnet material can be only increased to about 450 ℃. The use temperature of the samarium cobalt permanent magnet material cannot be effectively improved by simply changing the components and adjusting the subsequent process unsuitably, so the suitable components and the matched process are key factors for improving the use temperature of the samarium cobalt permanent magnet material and are also a difficulty.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a method for manufacturing a 550-DEG C-resistant samarium-cobalt permanent magnet material.
In order to solve the problems, the technical scheme of the invention is as follows: A550-DEG C-resistant samarium cobalt permanent magnet material comprises 26.5% of samarium, 50.8% of cobalt, 9.5% of copper, 10% of iron and 3.2% of zirconium, and the preparation process comprises the following steps:
(1) 26.5 percent of samarium, 50.8 percent of cobalt, 9.5 percent of copper, 10 percent of iron and 3.2 percent of zirconium are mixed according to the weight ratio, from bottom to top, the raw materials are placed in a crucible in an induction furnace according to the sequence of half of cobalt-iron and zirconium-the other half of cobalt-copper-samarium, the vacuum environment is adjusted, and when the vacuum is lower than 1.5pa, the induction heating is started;
(2) when the temperature of the alloy liquid reaches 1650 ℃, casting the alloy liquid into a water-cooling copper mould for rapid cooling, and coarsely crushing and crushing the alloy cast ingot;
(3) after the alloy is crushed, adding two parts per million of lubricant aluminum stearate and five parts per million of antioxidant, mixing for 2 hours, jet milling, and mixing for 4 hours for passivation for 12 hours to grind the alloy into 3-5um alloy powder;
(4) placing the powder in a mold, pressing the powder to a mill-pressed density of 4.2g/cm under an orientation field of greater than 1.5 Tesla3-4.3g/cm3The green compact of (a);
(5) and (2) carrying out vacuum packaging on the green body, placing the green body into a 270MPA water isostatic pressing for pressure maintaining for 30s, then placing the green body into a sintering furnace, carrying out heat preservation for 150min at 1230 ℃ of 1200-type sand-baked materials, then carrying out heat preservation for 4h at 1215 ℃ of 1185-type sand-baked materials, finally carrying out heat preservation for 2h at 1200 ℃ of 1170-type sand-baked materials, then carrying out rapid cooling, carrying out heat treatment for 12h at 820 ℃ of 800-type sand-baked materials, reducing the temperature to 600 ℃ at 0.5 ℃/min, carrying out heat preservation for 12h, and then reducing the temperature to 400 ℃ at 0.5 ℃/min.
Furthermore, the samarium, cobalt, copper, iron and zirconium have requirements of 084040, Co9998, A-grade cathode electrolytic copper, YT01 raw material pure iron and Hzr-01 industrial grade sponge zirconium.
Further, the steps (1) to (5) all adopt a low-oxygen process, and the steps (1) to (5) are completely realized under the protection of nitrogen.
Compared with the prior art, the invention has the advantages that: through tests of Beijing aerospace university, the density of the samarium cobalt permanent magnet material developed by the process is 8.30g/cm3-8.50g/cm3The intrinsic coercivity is larger than 7kOe between the maximum magnetic energy product of 16MGOe and 20MGOe at normal temperature and between the maximum magnetic energy product of 8MGOe and 12MGOe at the high temperature of 550 ℃, and the magnetic coercivity is a straight line on a demagnetization curve of 550 ℃.
Drawings
FIG. 1 is the metallographic phase of the alloy of the invention after melting.
FIG. 2 is an EDS spectrum of an alloy of the present invention after melting.
FIG. 3 is a laser particle size distribution plot of jet milled alloy powder of the present invention.
Fig. 4 is a graph of 550 degree demagnetization of a samarium cobalt permanent magnet material prepared by the present invention.
Fig. 5 is a measurement diagram of the high-temperature demagnetization curve according to the first embodiment of the invention.
Fig. 6 is a measurement diagram of the high-temperature demagnetization curve of the second embodiment of the present invention.
Fig. 7 is a measurement diagram of the high-temperature demagnetization curve of the third embodiment of the invention.
Detailed Description
The present invention is further described below by way of specific examples, but the present invention is not limited to only the following examples. Variations, combinations, or substitutions of the invention, which are within the scope of the invention or the spirit, scope of the invention, will be apparent to those of skill in the art and are within the scope of the invention.
Example one
Preparation of high-temperature samarium cobalt permanent magnet material
A550-DEG C-resistant samarium cobalt permanent magnet material comprises 26.5% of samarium, 50.8% of cobalt, 9.5% of copper, 10% of iron and 3.2% of zirconium, and the preparation process comprises the following steps:
(1) (1) mixing 26.5% of samarium, 50.8% of cobalt, 9.5% of copper, 10% of iron and 3.2% of zirconium in percentage by weight from bottom to top, placing the raw materials in a crucible in an induction furnace according to the sequence of half of cobalt-iron and zirconium-the other half of cobalt-copper-samarium, and adjusting the vacuum environment to enable the vacuum to be lower than 1.5pa, and starting induction heating;
(2) when the temperature of the alloy liquid reaches 1650 ℃, casting the alloy liquid into a water-cooling copper mould for rapid cooling, and coarsely crushing and crushing the alloy cast ingot;
(3) after the alloy is crushed, adding two parts per million of lubricant aluminum stearate and five parts per million of antioxidant, mixing for 2 hours, jet milling, and mixing for 4 hours for passivation for 12 hours to grind the alloy into 3-5um alloy powder;
(4) placing the powder in a mold, pressing the powder to a mill-pressed density of 4.2g/cm under an orientation field of greater than 1.5 Tesla3-4.3g/cm3The green compact of (a);
(5) and (2) carrying out vacuum packaging on the green body, placing the green body into a 270MPA water isostatic pressing for pressure maintaining for 30s, then placing the green body into a sintering furnace, carrying out heat preservation for 150min at 1230 ℃ of 1200-type sand-baked materials, then carrying out heat preservation for 4h at 1215 ℃ of 1185-type sand-baked materials, finally carrying out heat preservation for 2h at 1200 ℃ of 1170-type sand-baked materials, then carrying out rapid cooling, carrying out heat preservation for 12h at 850 ℃ of 800-type sand-baked materials during heat treatment, reducing the temperature to 600 ℃ at 0.5 ℃/min, carrying out heat preservation for 12h, and then reducing the temperature to 400 ℃ at 0..
The samarium, cobalt, copper, iron and zirconium requirements are 084040, Co9998, A-grade cathode electrolytic copper, YT01 raw material pure iron and Hzr-01 industrial grade sponge zirconium.
And (3) adopting a low-oxygen process from the step (1) to the step (5), and completely realizing the step (1) to the step (5) under the protection of nitrogen.
(II) high-temperature demagnetization curve measurement
The demagnetization curve at the high temperature of 450 ℃ is tested by using an NIM-500C permanent magnet high-temperature measurement system produced by China measurement institute, if the intrinsic coercivity of the material at 450 ℃ is greater than 12kOe, the demagnetization curve of the material at 550 ℃ is further measured, the size of a test sample column is phi 10 x 10 mm, and through the test, the intrinsic coercivity of the material at 450 ℃ is 10.6kOe, which is shown in figure 5.
Example two
Preparation of high-temperature samarium cobalt permanent magnet material
A550-DEG C-resistant samarium-cobalt permanent magnet material comprises 26.5% of samarium, 50.8% of cobalt, 9.5% of copper, 10% of iron and 3.2% of zirconium, and the preparation process is the same as that of the first embodiment.
(II) high-temperature demagnetization curve measurement
The test method is the same as that in the first embodiment, and the test result shows that the intrinsic coercivity of the material is 6.68kOe at 550 ℃, which is shown in fig. 6.
EXAMPLE III
Preparation of high-temperature samarium cobalt permanent magnet material
A550-DEG C-resistant samarium cobalt permanent magnet material comprises 26.5% of samarium, 50.8% of cobalt, 9.5% of copper, 10% of iron and 3.2% of zirconium, the preparation process is the same as that of the first embodiment, and the only difference is that the heat treatment temperature in the step (5) for preparing the high-temperature samarium cobalt permanent magnet material is changed from 800-850 ℃ to 800-820 ℃ and the heat preservation is carried out at 600 ℃ for 12 hours.
(II) high-temperature demagnetization curve measurement
The test method is the same as that in the first embodiment, and the test result shows that the intrinsic coercivity of the material is 6.98kOe at 550 ℃, which is shown in fig. 7.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. The utility model provides a 550 degrees high temperature resistant type samarium cobalt permanent magnet material which characterized in that: comprises 26.5 percent of samarium, 50.8 percent of cobalt, 9.5 percent of copper, 10 percent of iron and 3.2 percent of zirconium, and the preparation process comprises the following steps:
(1) 26.5 percent of samarium, 50.8 percent of cobalt, 9.5 percent of copper, 10 percent of iron and 3.2 percent of zirconium are mixed according to the weight ratio, from bottom to top, the raw materials are placed in a crucible in an induction furnace according to the sequence of half of cobalt-iron and zirconium-the other half of cobalt-copper-samarium, the vacuum environment is adjusted, and when the vacuum is lower than 1.5pa, the induction heating is started;
(2) when the temperature of the alloy liquid reaches 1650 ℃, casting the alloy liquid into a water-cooling copper mould for rapid cooling, and coarsely crushing and crushing the alloy cast ingot;
(3) after the alloy is crushed, adding two parts per million of lubricant aluminum stearate and five parts per million of antioxidant, mixing for 2 hours, jet milling, and mixing for 4 hours for passivation for 12 hours to grind the alloy into 3-5um alloy powder;
(4) placing the powder in a mold, pressing the powder to a mill-pressed density of 4.2g/cm under an orientation field of greater than 1.5 Tesla3-4.3g/cm3The green compact of (a);
(5) and (2) carrying out vacuum packaging on the green body, placing the green body into a 270MPA water isostatic pressing for pressure maintaining for 30s, then placing the green body into a sintering furnace, carrying out heat preservation for 150min at 1230 ℃ of 1200-type sand-baked materials, then carrying out heat preservation for 4h at 1215 ℃ of 1185-type sand-baked materials, finally carrying out heat preservation for 2h at 1200 ℃ of 1170-type sand-baked materials, then carrying out rapid cooling, carrying out heat treatment for 12h at 820 ℃ of 800-type sand-baked materials, reducing the temperature to 600 ℃ at 0.5 ℃/min, carrying out heat preservation for 12h, and then reducing the temperature to 400 ℃ at 0.5 ℃/min.
2. The samarium cobalt permanent magnet material resistant to the high temperature of 550 ℃ prepared by the method of claim 1, is characterized in that: the samarium, cobalt, copper, iron and zirconium requirements are 084040, Co9998, A-grade cathode electrolytic copper, YT01 raw material pure iron and Hzr-01 industrial grade sponge zirconium.
3. The samarium cobalt permanent magnet material resistant to the high temperature of 550 ℃ prepared by the method of claim 1, is characterized in that: and (3) adopting a low-oxygen process from the step (1) to the step (5), and completely realizing the step (1) to the step (5) under the protection of nitrogen.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0331517A2 (en) * | 1988-03-04 | 1989-09-06 | Shin-Etsu Chemical Co., Ltd. | Method for manufacture of rare earth permanent magnet |
| JP2005136356A (en) * | 2003-10-31 | 2005-05-26 | Tdk Corp | Method of manufacturing sintered rare-earth magnet |
| CN104233138A (en) * | 2014-09-29 | 2014-12-24 | 中南大学 | Microwave aging treatment method for cobalt-based rare earth permanent magnetic materials |
| CN107895620A (en) * | 2017-11-30 | 2018-04-10 | 北京航空航天大学 | A kind of high Fe content samarium-cobalt permanent-magnetic material and preparation method |
| CN108039258A (en) * | 2017-12-01 | 2018-05-15 | 北京航空航天大学 | A kind of high temperature high-coercive force samarium-cobalt permanent-magnetic material and preparation method |
| CN109706338A (en) * | 2019-01-23 | 2019-05-03 | 成都银河磁体股份有限公司 | A kind of sintered samarium cobalt magnet preparation method |
-
2020
- 2020-10-28 CN CN202011170702.6A patent/CN112435846A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0331517A2 (en) * | 1988-03-04 | 1989-09-06 | Shin-Etsu Chemical Co., Ltd. | Method for manufacture of rare earth permanent magnet |
| JP2005136356A (en) * | 2003-10-31 | 2005-05-26 | Tdk Corp | Method of manufacturing sintered rare-earth magnet |
| CN104233138A (en) * | 2014-09-29 | 2014-12-24 | 中南大学 | Microwave aging treatment method for cobalt-based rare earth permanent magnetic materials |
| CN107895620A (en) * | 2017-11-30 | 2018-04-10 | 北京航空航天大学 | A kind of high Fe content samarium-cobalt permanent-magnetic material and preparation method |
| CN108039258A (en) * | 2017-12-01 | 2018-05-15 | 北京航空航天大学 | A kind of high temperature high-coercive force samarium-cobalt permanent-magnetic material and preparation method |
| CN109706338A (en) * | 2019-01-23 | 2019-05-03 | 成都银河磁体股份有限公司 | A kind of sintered samarium cobalt magnet preparation method |
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Application publication date: 20210302 |