CN109859945B - Preparation method of high-temperature samarium cobalt permanent magnet material - Google Patents
Preparation method of high-temperature samarium cobalt permanent magnet material Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-temperature samarium cobalt permanent magnet material, which comprises the following steps: samarium cobalt permanent magnet material headFirstly according to Sm (Co)1‑u‑v‑wCuuFevZrw)zDosing with u =0.082-0.088, v =0.093-0.143, w =0.027-0.028 and z = 6.2-6.5; then, putting the prepared raw materials into a vacuum induction smelting furnace for smelting to obtain alloy ingots with uniform components; then, grinding the alloy ingot by airflow to obtain alloy powder with the granularity SDM =3.2-3.8 μm; then, the powder is subjected to magnetic field orientation pressing and isostatic pressing to obtain a green body; and finally, carrying out multi-section sintering, solid solution and aging treatment on the green body. The invention solves the problem of high temperature resistance of the 2:17 type samarium cobalt permanent magnet at 500 ℃ by the combination of five metals of metal samarium, metal cobalt, metal copper, metal iron and metal zirconium on the premise of not adding trace elements (Mn, Er and the like).
Description
Technical Field
The invention belongs to the technical field of preparation of samarium cobalt permanent magnet materials, and particularly relates to a preparation method of a high-temperature samarium cobalt permanent magnet material.
Background
Samarium cobalt permanent magnet material is widely used in high-tech fields such as motor, sensor, detector, engine and radar with advantages such as high temperature resistance, corrosion resistance and higher magnetic property, but aims at some special use environment (ultra-high temperature condition in aerospace field) and still has the problem that magnetic property is lower and the highest working temperature is lower under high temperature.
Disclosure of Invention
Aiming at the problems of the background technology, the invention aims to provide a preparation method of a high-temperature samarium cobalt permanent magnet material.
Therefore, the invention adopts the following technical scheme: a method for preparing high-temperature samarium cobalt permanent magnet material comprises
Firstly, samarium cobalt permanent magnet material is firstly prepared according to Sm (Co)1-u-v-wCuuFevZrw)zDosing with u =0.082-0.088, v =0.093-0.143, w =0.027-0.028 and z = 6.2-6.5;
step two, putting the prepared raw materials into a vacuum induction smelting furnace for smelting to obtain alloy ingots with uniform components;
crushing the alloy ingot through an airflow mill to obtain alloy powder with the granularity SDM =3.2-3.8 μm;
fourthly, performing magnetic field orientation pressing and isostatic pressing on the powder to obtain a green body;
and step five, carrying out multi-section sintering, solid solution and aging treatment on the green body.
In addition to the above technical solutions, the present invention also includes the following technical features.
And in the second step, the prepared raw materials are sequentially placed into a vacuum induction melting furnace according to the sequence of Fe-Zr-Fe-Co-Cu-Sm, a furnace cover of the vacuum induction melting furnace is closed to carry out vacuum pumping treatment after the charging is finished, low-power heating is started when the vacuum degree in the furnace is less than or equal to 7Pa, moisture and adsorbed gas of the crucible, the hearth and the raw materials are removed, the vacuum pumping is stopped when the vacuum degree in the furnace is less than or equal to 5Pa, Ar gas charging is stopped to open an Ar gas charging valve to charge Ar gas into the hearth, the charging is stopped when the gas pressure reaches-0.06 +/-0.03 MPa, high-power (65 +/-5 KW) heating melting is started for 15 +/-5 min, and the raw materials are directly cast into a water-: 7-phase alloy ingot.
And in the third step, the alloy ingot is subjected to coarse crushing and then to airflow milling to prepare powder.
And step four, specifically, the method comprises two aspects of magnetic field orientation compression and isostatic pressing, wherein the intensity of the orientation magnetic field in the process of the magnetic field orientation compression is not less than 1.8T, and the oxygen content in the pressing space is not more than 5000 PPM.
In the fifth step, the sintering specifically comprises the following steps: placing the green body subjected to isostatic pressing into a vacuum sintering furnace, closing a furnace door, vacuumizing, starting heating when the vacuum degree is less than or equal to 5Pa, keeping the temperature for 10 +/-5 min when the sintering temperature rises to 900 +/-10 ℃, then starting inflating (inert gas) until the air pressure in the furnace body reaches-0.05 +/-0.01 MPa, stopping inflating, then continuing heating and sintering, keeping the temperature for 60 +/-30 min at 1205 +/-5 ℃ for carrying out highest temperature sintering, then keeping the temperature for 120 +/-30 min at 1185 +/-10 ℃ for carrying out pretreatment, and immediately air-cooling to prepare the room temperature after the pretreatment is finished;
the solid solution comprises the following specific steps: placing the sintered blank into a vacuum furnace, closing a furnace door, vacuumizing, starting to fill inert gas and heating when the vacuum degree is less than or equal to 5Pa, firstly heating to 1160 +/-5 ℃ at the speed of 4 +/-1 ℃/min, preserving the heat for 10 +/-5 min, then heating to 1165 +/-5 ℃ at the speed of 2 ℃/min, preserving the heat for 180 +/-5 min at the temperature, and then immediately cooling by air, wherein the inert gas is filled in the process to effectively prevent the volatilization of the metal samarium;
the aging method comprises the following specific steps: putting the blank after solid solution into a vacuum furnace, closing a furnace door, vacuumizing, filling inert gas and heating when the vacuum degree is less than or equal to 5Pa, wherein the aging process adopted by the invention is multistage aging, firstly heating to 840 +/-5 ℃ at the heating rate of 4 ℃/min, then preserving heat for 600 +/-30 min, then cooling to 600 +/-5 ℃ at the cooling rate of 0.8 +/-0.2 ℃/min, then cooling to 400 +/-5 ℃ at the cooling rate of 1.5 +/-0.5 ℃/min, then preserving heat for 120 +/-30 min, and then cooling to room temperature.
The invention can achieve the following beneficial effects: the invention solves the problem of high temperature resistance of the 2:17 type samarium cobalt permanent magnet at 500 ℃ by the combination of five metals of metal samarium, metal cobalt, metal copper, metal iron and metal zirconium on the premise of not adding trace elements (Mn, Er and the like).
Detailed Description
With Sm (Co)0.791Cu0.087Fe0.093Zr0.027)6.298The embodiments of the present invention are further illustrated by way of examples:
1, preparing materials: selecting high-purity raw materials (Sm/RE is more than or equal to 99.7%, Co is more than or equal to 99.6%, Cu + Ag is more than or equal to 99.95%, Zr + Hf is more than or equal to 99.3%, and Fe is more than or equal to 99.75%) according to Sm (Co)0.791Cu0.087Fe0.093Zr0.027)6.298、Sm(Co0.745Cu0.084Fe0.142Zr0.027)6.497And Sm (Co)0.768Cu0.082Fe0.121Zr0.027)6.399The ingredients are mixed according to the atomic ratio;
2, smelting: putting the prepared raw materials into a smelting crucible in sequence according to the sequence of Fe-Zr-Fe-Co-Cu-Sm, closing a furnace cover of a vacuum induction smelting furnace for vacuumizing treatment after the charging is finished, starting low-power heating when the vacuum degree in the furnace is less than or equal to 7Pa, removing water and adsorbed gas of the crucible, a hearth and the raw materials, stopping vacuumizing when the vacuum degree in the furnace is less than or equal to 5Pa, opening an Ar gas charging valve to charge Ar gas into the hearth, stopping charging when the gas pressure reaches-0.06 +/-0.03 MPa, starting high-power (65 +/-5 KW) heating and smelting for 15 +/-5 min, directly casting to a water-cooled ingot casting copper mold after the smelting is finished, and quickly cooling to form a single 1: a 7-phase alloy ingot;
3, pulverizing: the alloy ingot is coarsely crushed and then is subjected to airflow milling to prepare powder, wherein the powder is protected by inert gas (nitrogen or argon) in the airflow milling process to prevent oxidation of the powder, in addition, the particle size range SMD =3.2-3.8 μm of the powder is controlled by the rotation speed of the airflow mill, the fine particle size of the powder can cause the oxidation degree to rise and further cause the reduction of magnetic performance parameters such as remanence and intrinsic coercive force, and the single-particle powder polycrystal proportion to rise and further cause the reduction of remanence if the particle size is higher, so the oxygen content of a milling chamber and the particle size of the powder need to be strictly controlled in the whole powder preparation process.
4, profiling: the compression mainly refers to two aspects of magnetic field orientation compression and isostatic pressing, wherein the intensity of the oriented magnetic field in the process of the magnetic field orientation compression is required to be more than or equal to 1.8T, and the oxygen content in a pressing space is required to be less than or equal to 5000 PPM.
5, sintering: placing the green body after isostatic pressing into a vacuum sintering furnace, closing a furnace door, vacuumizing, starting heating when the vacuum degree is less than or equal to 5Pa, keeping the temperature for 10 +/-5 min when the sintering temperature rises to 900 +/-10 ℃, then starting inflating (inert gas) until the air pressure in the furnace body reaches-0.05 +/-0.01 MPa, stopping inflating, then continuing heating and sintering, keeping the temperature for 60 +/-30 min at 1205 +/-5 ℃ for carrying out highest temperature sintering, then keeping the temperature for 120 +/-30 min at 1185 +/-10 ℃ for carrying out pretreatment, and immediately air-cooling to prepare the room temperature after the pretreatment is finished. Compared with the traditional vacuum sintering, the sintering process adopting the inert gas sintering can effectively prevent the volatilization of the metal samarium, and in addition, compared with the traditional single-stage sintering, the multi-stage sintering adopted by the invention can further improve the blank density, and simultaneously can obtain a larger cell structure to promote the Fe element to enter 2: 17R phase, and further improving various magnetic performance parameters (remanence, squareness and the like).
6, solid solution: placing the sintered blank into a vacuum furnace, closing a furnace door, vacuumizing, starting to fill inert gas and heating when the vacuum degree is less than or equal to 5Pa, firstly heating to 1160 +/-5 ℃ at the speed of 4 +/-1 ℃/min, preserving the heat for 10 +/-5 min, then heating to 1165 +/-5 ℃ at the speed of 2 ℃/min, preserving the heat for 180 +/-5 min at the temperature, and then immediately cooling by air, wherein the inert gas is filled in the process, so that the volatilization of metal samarium can be effectively prevented, and the intrinsic coercive force temperature coefficient is further reduced.
7, aging: putting the blank after solid solution into a vacuum furnace, closing a furnace door, vacuumizing, filling inert gas and heating when the vacuum degree is less than or equal to 5Pa, wherein the aging process adopted by the invention is multistage aging, firstly heating to 840 +/-5 ℃ at the heating rate of 4 ℃/min, then preserving heat for 600 +/-30 min, then cooling to 600 +/-5 ℃ at the cooling rate of 0.8 +/-0.2 ℃/min, then cooling to 400 +/-5 ℃ at the cooling rate of 1.5 +/-0.5 ℃/min, then preserving heat for 120 +/-30 min, and then cooling to room temperature.
8, detection of magnetic properties:
Claims (4)
1. a preparation method of a high-temperature samarium cobalt permanent magnet material is characterized by comprising the following steps:
firstly, samarium cobalt permanent magnet material is firstly prepared according to Sm (Co)1-u-v-wCuuFevZrw)zDosing with u =0.082-0.088, v =0.093-0.143, w =0.027-0.028 and z = 6.2-6.5;
step two, putting the prepared raw materials into a vacuum induction smelting furnace for smelting to obtain alloy ingots with uniform components;
crushing the alloy ingot through an airflow mill to obtain alloy powder with the granularity SDM =3.2-3.8 μm;
fourthly, performing magnetic field orientation pressing and isostatic pressing on the powder to obtain a green body;
step five, carrying out multi-section sintering, solid solution and aging treatment on the green body;
the sintering method comprises the following specific steps: placing the green body subjected to isostatic pressing into a vacuum sintering furnace, closing a furnace door, vacuumizing, starting heating when the vacuum degree is less than or equal to 5Pa, keeping the temperature for 10 +/-5 min when the sintering temperature rises to 900 +/-10 ℃, then starting filling inert gas until the air pressure in the furnace body reaches-0.05 +/-0.01 MPa, stopping filling gas, then continuing heating and sintering, keeping the temperature for 60 +/-30 min at 1205 +/-5 ℃ for carrying out maximum temperature sintering, then keeping the temperature for 120 +/-30 min at 1185 +/-10 ℃ for carrying out pretreatment, and immediately cooling to room temperature by air after the pretreatment is finished;
the solid solution comprises the following specific steps: placing the sintered blank into a vacuum furnace, closing a furnace door, vacuumizing, starting to fill inert gas and heating when the vacuum degree is less than or equal to 5Pa, firstly heating to 1160 +/-5 ℃ at the speed of 4 +/-1 ℃/min, preserving the heat for 10 +/-5 min, then heating to 1165 +/-5 ℃ at the speed of 2 ℃/min, preserving the heat for 180 +/-5 min at the temperature, and then immediately cooling by air, wherein the inert gas is filled in the process to effectively prevent the volatilization of the metal samarium;
the aging method comprises the following specific steps: putting the blank after solid solution into a vacuum furnace, closing a furnace door, vacuumizing, filling inert gas and heating when the vacuum degree is less than or equal to 5Pa, wherein the aging process adopted by the invention is multistage aging, firstly heating to 840 +/-5 ℃ at the heating rate of 4 ℃/min, then preserving heat for 600 +/-30 min, then cooling to 600 +/-5 ℃ at the cooling rate of 0.8 +/-0.2 ℃/min, then cooling to 400 +/-5 ℃ at the cooling rate of 1.5 +/-0.5 ℃/min, then preserving heat for 120 +/-30 min, and then cooling to room temperature.
2. The method of making a high temperature samarium cobalt permanent magnet material of claim 1, comprising: and in the second step, the prepared raw materials are sequentially placed into a vacuum induction melting furnace according to the sequence of Fe-Zr-Fe-Co-Cu-Sm, a furnace cover of the vacuum induction melting furnace is closed to carry out vacuum pumping treatment after the charging is finished, low-power heating is started when the vacuum degree in the furnace is less than or equal to 7Pa, moisture and adsorbed gas of the crucible, the hearth and the raw materials are removed, the vacuum pumping is stopped when the vacuum degree in the furnace is less than or equal to 5Pa, Ar gas charging is stopped to open an Ar gas charging valve to charge Ar gas into the hearth, the charging is stopped when the gas pressure reaches-0.06 +/-0.03 MPa, high-power (65 +/-5 KW) heating melting is started for 15 +/-5 min, and the raw materials are directly cast into a water-: 7-phase alloy ingot.
3. The method of making a high temperature samarium cobalt permanent magnet material of claim 1, comprising: and in the third step, the alloy ingot is subjected to coarse crushing and then to airflow milling to prepare powder.
4. The method of making a high temperature samarium cobalt permanent magnet material of claim 1, comprising: and step four, specifically, the method comprises two aspects of magnetic field orientation compression and isostatic pressing, wherein the intensity of the orientation magnetic field in the process of the magnetic field orientation compression is not less than 1.8T, and the oxygen content in the pressing space is not more than 5000 PPM.
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| CN110957089A (en) * | 2019-11-21 | 2020-04-03 | 杭州科德磁业有限公司 | Preparation method of samarium cobalt permanent magnet material |
| CN111243804B (en) * | 2019-11-29 | 2023-10-17 | 南京安德海睿智能科技有限公司 | Rare earth permanent magnet with hydrogen resistance and preparation method thereof |
| CN111370191B (en) * | 2020-03-20 | 2022-05-31 | 杭州永磁集团有限公司 | Heavy rare earth element-free samarium-cobalt permanent magnet material with low coercive force temperature coefficient and high temperature and preparation method thereof |
| CN113388757B (en) * | 2021-04-29 | 2022-04-29 | 福建省长汀卓尔科技股份有限公司 | Samarium cobalt rare earth magnet and preparation method thereof |
| CN113436874B (en) * | 2021-05-27 | 2023-04-18 | 北矿科技股份有限公司 | Sm 2 Co 17 Molded high-temperature magnet and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102543340A (en) * | 2011-12-30 | 2012-07-04 | 北矿磁材科技股份有限公司 | High-performance samarium-cobalt magnetic powder and preparation method thereof |
| CN104637642A (en) * | 2015-02-13 | 2015-05-20 | 宁波宁港永磁材料有限公司 | Samarium and cobalt sintered permanent magnet material and preparation method thereof |
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| CN106782977B (en) * | 2017-01-24 | 2019-08-09 | 湖南航天磁电有限责任公司 | A kind of preparation method of large scale sintered samarium cobalt permanent magnet |
| CN109216007B (en) * | 2018-09-07 | 2020-04-17 | 杭州永磁集团有限公司 | Preparation process of samarium cobalt magnet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104637642A (en) * | 2015-02-13 | 2015-05-20 | 宁波宁港永磁材料有限公司 | Samarium and cobalt sintered permanent magnet material and preparation method thereof |
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