CN103325513A - Samarium cobalt permanent magnetic material and preparation method thereof - Google Patents

Samarium cobalt permanent magnetic material and preparation method thereof Download PDF

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Publication number
CN103325513A
CN103325513A CN2013103027853A CN201310302785A CN103325513A CN 103325513 A CN103325513 A CN 103325513A CN 2013103027853 A CN2013103027853 A CN 2013103027853A CN 201310302785 A CN201310302785 A CN 201310302785A CN 103325513 A CN103325513 A CN 103325513A
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samarium
magnetic material
cobalt
permanent magnetic
copper
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罗明
谭春林
李彬
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HUNAN AEROSPACE INDUSTRY GENERAL Corp
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HUNAN AEROSPACE INDUSTRY GENERAL Corp
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Abstract

The invention discloses a samarium cobalt permanent magnetic material and a preparation method thereof. The samarium cobalt permanent magnetic material is prepared from the following chemical ingredients by mass percent: 24.5-26% of samarium, 52-56% of cobalt, 7.5-12% of iron, 6.5-8% of copper, and 2-4% of zirconium. The samarium cobalt permanent magnet disclosed by the invention has high coercivity and low temperature coefficient; the magnetic performance at the temperature of 400-450 DEG C is that the residual magnetism Br is 0.783-0.907 T; the intrinsic coercivity Hcj is 704-1092.5 kA/m; the maximal magnetic level (BH)max is 108.5-164 kJ/m<3>; the temperature coefficient alpha of the residual magnetism is -0.0368%/DEG C to -0.054%/DEG C; and the temperature coefficient beta of the intrinsic coercivity is -0.132%/DEG C to -0.198%/DEG C. Thus, the samarium cobalt permanent magnetic material is simple in process and low in manufacturing cost.

Description

A kind of samarium-cobalt permanent-magnetic material and preparation method thereof
Technical field
The invention belongs to rare-earth permanent-magnet material technical field, be specifically related to a kind ofly have high-coercive force low-temperature coefficient, working temperature at samarium-cobalt permanent-magnetic material of 400 ℃~450 ℃ and preparation method thereof.
Background technology
Development along with science and technology, proposed to require working temperature at 400 ℃~500 ℃ high temperature magnet and the magnet of low-temperature coefficient in national defence and military industry field, such as the engine system at aircraft of new generation, need working temperature greater than 400 ℃ high temperature magnet, and the electronic devices and components that substitute original Hydraulic Power Transmission System, with the reliability that improves aircraft and the maintenance difficulties that reduces aircraft.In the magnetic property and temperature feature of existing permanent magnetic material, the serviceability temperature of AlNiCo permanent magnetic material can reach 520 ℃, but at very low (the HCJ H of high-coercive force trade mark magnet of the coercive force of this temperature lower magnet CjOnly be about 120kA/m), maximum magnetic energy product only is 80kJ/m 3About, therefore, can not for the manufacture of small and light unit, device, be difficult to satisfy actual application requirements; NdFeB with high energy product is agglomeration permanent magnetic material, because Curie temperature is low, maximum operation (service) temperature only is 100 ℃, and by the adjustment of composition and the improvement of manufacturing process, its maximum operation (service) temperature also is no more than 250 ℃, can not satisfy instructions for use; And Sm 2Co L7Permanent magnet is because magnetic property is high, Curie temperature reaches more than 820 ℃, residual magnetism temperature coefficient is low, so Sm 2Co L7Permanent magnet becomes the first-selection of high temperature magnet.Sm 2Co L7High-fire resistance can greatly improve the ability that permanent magnetic material adapts to operational environment, at high-temperature field and require the low-temperature coefficient field to have a wide range of applications, especially more and more wider in the application in Aeronautics and Astronautics and national defence field.But, common Sm 2Co L7The maximum operation (service) temperature of permanent magnet only is about 300 ℃, surpasses 330 ℃ demagnetization curve no longer linearly, and at high temperature, all should be linearly more than the working point of permanent magnet demagnetization curve in generator and the motor.
Summary of the invention
Technical problem to be solved by this invention is to overcome current common Sm 2Co L7Temperature coefficient is high, maximum operation (service) temperature only is the shortcoming about 300 ℃, and a kind of high-coercive force low-temperature coefficient, the samarium-cobalt permanent-magnetic material of working temperature about 400~450 ℃ are provided.
In order to achieve the above object, technical scheme provided by the invention is:
Described samarium-cobalt permanent-magnetic material is comprised of the component of following mass percent: samarium 24.5%~26%, cobalt 52%~56%, iron 7.5%~12%, copper 6.5%~8%, zirconium 2%~4%.
Preferably, described permanent magnetic material is comprised of the component of following mass percent: samarium 24.5%~25.5%, cobalt 52%~54%, iron 10%~11%, copper 7.5%~8%, zirconium 3.5%~4%.
Preferably, described permanent magnetic material is comprised of the component of following mass percent: samarium 24.5%~25.5%, cobalt 54%~55%, iron 11%~12%, copper 6.5%~7%, zirconium 2%~3%.
Preferably, described permanent magnetic material is comprised of the component of following mass percent: samarium 25%~26%, cobalt 55%~56%, iron 7.5%~8.5%, copper 7%~8%, zirconium 3%~4%.
The above-mentioned permanent magnetic material of stating has higher coercivity and has low-temperature coefficient, its specific performance parameter is as follows: 400 ℃~450 ℃ temperature magnetics can be remanent magnetism Br=0.783T~0.907T, HCJ Hcj=704kA/m~1092.5kA/m, maximum magnetic flux energy level (BH) max=108.5kJ/m 3~164kJ/m 3, residual magnetism temperature coefficient α=-0.0368~-0.054%/℃, HCJ temperature coefficient β=-0.132~-0.198%/℃.
The present invention also provides the preparation method of above-mentioned samarium-cobalt permanent-magnetic material, samarium-cobalt permanent-magnetic material with the method preparation has higher coercivity and low-temperature coefficient, and under 400 ℃~450 ℃ working temperature, the permanent magnet demagnetization curve is straight line more than the working point.
Described method comprises the steps:
(1) preparation raw material: samarium, cobalt, iron, copper and zirconium are prepared by described mass percent;
(2) raw material for preparing is carried out melting in intermediate frequency furnace, be incubated refining 10min~15min again under 1400 ℃~1500 ℃ temperature, then the samarium-cobalt alloy liquid with molten condition pours into chilling in the water cooled copper mould, obtains the samarium-cobalt alloy ingot casting;
(3) magnetic preparation: the samarium-cobalt alloy ingot casting is become the coarse granule of 100 μ m~150 μ m with the vibrating ball-mill coarse crushing, with planetary ball mill coarse granule is ground into again the magnetic of 3 μ m~5 μ m;
(4) oriented moulding: magnetic is orientated under the magnetic field of 1.5T~2.0T and compressing, then under 200Mpa~300Mpa pressure, carries out isostatic cool pressing, obtain the SmCo molded blank;
(5) sintering and solid solution: with the SmCo molded blank in tube furnace, in 1000 ℃~1190 ℃ vacuum pre-burning 30min, applying argon gas is in 1200 ℃~1220 ℃ sintering 90min~120min again, then be cooled to 1160 ℃~1180 ℃ solid solution 90min~120min, last air-cooled to 25 ℃~30 ℃ of room temperatures, obtain the sintering blank;
(6) temper: the blank behind the sintering is incubated 10h~20h at 800 ℃~830 ℃, then the speed with 0.3 ℃/min~1.4 ℃/min is cooled to 400 ℃, insulation 10h~15h, be cooled to 25 ℃~30 ℃ of room temperatures (namely with the speed of 25 ℃/min~30 ℃/min at last, adopt and repeatedly fill the cooling mode of taking out argon gas and quick cold wind), obtain samarium cobalt permanent magnet.
Compared with prior art, beneficial effect of the present invention is:
1) on composition of raw materials, samarium-cobalt permanent-magnetic material of the present invention only uses the conventional elements such as samarium, cobalt, iron, copper and zirconium, does not add the elements such as heavy rare earth dysprosium.Adding heavy rare earth element can make 2:17 type samarium-cobalt permanent-magnetic material residual magnetism temperature coefficient reduce, but the magnetic property of permanent magnetic material is declined to a great extent, and rare earth element is expensive, in batch production process, can greatly improve preparation cost, therefore adopt conventional element, saved greatly the cost of raw material, and magnetic property is high.
2) by rational formula Design, and the optimal control of melting, powder process, sintering and tempering process, make samarium cobalt permanent magnet body of the present invention obtain higher magnetic property and lower temperature coefficient, and reduced production cost.Aspect smelting technology, by the control smelting time, reduce the volatilization of element, simultaneously so that in the ingot casting alloying elements distribution evenly, do not produce component segregation.Adopt vibration coarse crushing and planetary ball mill further to pulverize, reasonably control the granularity of SmCo powder at 3 μ m~5 μ m, and particle size distribution concentrates, so that the grain structure size to fit of samarium-cobalt permanent-magnetic material, be evenly distributed, be conducive to coercitive raising.Sintering and temperature precisely be controlled at ± and 2 ℃; When the hot stage of tempering is cooled to low thermophase, adopt lower cooldown rate, be conducive to cell wall phase element and spread fully with the interior mutually element of born of the same parents, reasonably control phase constituent and ratio in cell wall phase and the born of the same parents, obtain higher coercive force and low temperature coefficient.
3) samarium-cobalt permanent-magnetic material of the present invention 400 ℃~450 ℃ temperature magnetics can be Br=0.783T~0.907T, Hcj=704kA/m~1092.5kA/m, (BH) max=108.5kJ/m 3~164kJ/m 3, satisfy client's instructions for use.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail, but is not limited in following examples.
Embodiment 1
(1) takes by weighing raw material: raw material is prepared burden by mass percentage: samarium 25.5%, cobalt 52%, iron 10.5%, copper 8%, zirconium 4%;
(2) alloy melting: the raw material for preparing is carried out melting in intermediate frequency furnace, under 1400 ℃~1500 ℃ temperature, be incubated again concise 10min~15min, then the samarium-cobalt alloy liquid with molten condition pours into chilling in the water cooled copper mould, obtains the samarium-cobalt alloy ingot casting;
(3) magnetic preparation: alloy cast ingot is become the coarse granule of 100 μ m with the vibrating ball-mill coarse crushing, adopt planetary ball mill further to be crushed to 3 μ m~5 μ m the magnetic after the coarse crushing;
(4) oriented moulding: magnetic is orientated under the magnetic field of 1.5T~2.0T and compressing, and then under 200Mpa~300Mpa pressure, carries out isostatic cool pressing, obtain samarium cobalt blank;
(5) sintering and solid solution: in tube furnace, at 1000 ℃~1190 ℃ vacuum presintering 30min, applying argon gas is at 1200 ℃~1220 ℃ sintering 90min~120min again, then be cooled to 1160 ℃~1180 ℃ solid solution 90min~120min, last air-cooled to 25 ℃~30 ℃ of room temperatures, obtain the sintering blank;
(6) temper: the blank behind the sintering is at 800 ℃~830 ℃ insulation 10h~20h, speed with 0.3 ℃/min~1.4 ℃/min is cooled to 400 ℃ subsequently, insulation 10h~15h, last chilling adopt repeatedly fill take out argon gas and fast air-cooled speed with 25 ℃/min~30 ℃/min be cooled to 25 ℃~30 ℃ of room temperatures, obtain the samarium cobalt permanent magnet body.
The samarium cobalt permanent magnet body sample test magnetic property of the present embodiment preparation, as shown in table 1:
Table 1
Figure BDA00003531251700041
Embodiment 2
Raw material: samarium, cobalt, iron, copper, zirconium;
Above-mentioned raw materials is prepared burden by mass percentage: samarium 24.5%, cobalt 54.5%, iron 12%, copper 6.5%, zirconium 2.5%;
The preparation method of samarium-cobalt permanent-magnetic material of the present invention is with embodiment 1.
The magnetic property of the samarium cobalt permanent magnet body sample test of the present embodiment preparation, as shown in table 2:
Table 2
Embodiment 3
Raw material: samarium, cobalt, iron, copper, zirconium;
Above-mentioned raw materials is prepared burden by mass percentage: samarium 25%, cobalt 56%, iron 7.5%, copper 8%, zirconium 3.5%;
The preparation method of samarium-cobalt permanent-magnetic material of the present invention is with embodiment 1.
The magnetic property of the samarium cobalt permanent magnet body sample test of the present embodiment preparation, as shown in table 3:
Table 3
Figure BDA00003531251700051
From the sample of above-described embodiment preparation as can be known, samarium-cobalt permanent-magnetic material of the present invention has high coercive force and lower temperature coefficient when reducing production costs, at 400 ℃~450 ℃ demagnetization curves linearly, satisfy the applied at elevated temperature requirement.
The above embodiment of the present invention is to explanation of the present invention, can not be used for restriction the present invention, and the implication suitable with claims of the present invention and any change in the scope all will be understood that it is to be included in the scope of claims.

Claims (6)

1. a samarium-cobalt permanent-magnetic material is characterized in that, described permanent magnetic material is comprised of the component of following mass percent: samarium 24.5%~26%, cobalt 52%~56%, iron 7.5%~12%, copper 6.5%~8%, zirconium 2%~4%.
2. permanent magnetic material as claimed in claim 1 is characterized in that, described permanent magnetic material is comprised of the component of following mass percent: samarium 24.5%~25.5%, cobalt 52%~54%, iron 10%~11%, copper 7.5%~8%, zirconium 3.5%~4%.
3. permanent magnetic material as claimed in claim 1 is characterized in that, described permanent magnetic material is comprised of the component of following mass percent: samarium 24.5%~25.5%, cobalt 54%~55%, iron 11%~12%, copper 6.5%~7%, zirconium 2%~3%.
4. permanent magnetic material as claimed in claim 1 is characterized in that, described permanent magnetic material is comprised of the component of following mass percent: samarium 25%~26%, cobalt 55%~56%, iron 7.5%~8.5%, copper 7%~8%, zirconium 3%~4%.
5. such as each described permanent magnetic material of claim 1 to 4, it is characterized in that, described permanent magnetic material performance parameter is as follows: 400 ℃~450 ℃ temperature magnetics can be remanent magnetism Br=0.783T~0.907T, HCJ Hcj=704kA/m~1092.5kA/m, maximum magnetic flux energy level (BH) max=108.5kJ/m 3~164kJ/m 3, residual magnetism temperature coefficient α=-0.0368~-0.054%/℃, HCJ temperature coefficient β=-0.132~-0.198%/℃.
6. a method for preparing each described permanent magnetic material of claim 1 to 4 is characterized in that, described method comprises the steps:
(1) preparation raw material: samarium, cobalt, iron, copper and zirconium are prepared by described mass percent;
(2) raw material for preparing is carried out melting in intermediate frequency furnace, be incubated refining 10min~15min again under 1400 ℃~1500 ℃ temperature, then the samarium-cobalt alloy liquid with molten condition pours into chilling in the water cooled copper mould, obtains the samarium-cobalt alloy ingot casting;
(3) magnetic preparation: the samarium-cobalt alloy ingot casting is broken into the coarse granule of 100 μ m~150 μ m, again coarse granule is ground into the magnetic of 3 μ m~5 μ m;
(4) oriented moulding: magnetic is orientated under the magnetic field of 1.5T~2.0T and compressing, then under 200Mpa~300Mpa pressure, carries out isostatic cool pressing, obtain the SmCo molded blank;
(5) sintering and solid solution: with the SmCo molded blank in tube furnace, in 1000 ℃~1190 ℃ vacuum pre-burning 30min, applying argon gas is in 1200 ℃~1220 ℃ sintering 90min~120min again, then be cooled to 1160 ℃~1180 ℃ solid solution 90min~120min, last air-cooled to 25 ℃~30 ℃, obtain the sintering blank;
(6) temper: the blank behind the sintering is incubated 10h~20h at 800 ℃~830 ℃, then the speed with 0.3 ℃/min~1.4 ℃/min is cooled to 400 ℃, insulation 10h~15h, the speed with 25 ℃/min~30 ℃/min is cooled to 25 ℃~30 ℃ at last, obtains samarium cobalt permanent magnet.
CN2013103027853A 2013-07-18 2013-07-18 Samarium cobalt permanent magnetic material and preparation method thereof Pending CN103325513A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103537684A (en) * 2013-11-07 2014-01-29 湖南航天工业总公司 Production method for samarium cobalt alloy powder
CN103632787A (en) * 2013-12-11 2014-03-12 湖南航天工业总公司 Method for sintering and tempering rare-earth cobalt permanent magnetic material
CN104609845A (en) * 2014-12-15 2015-05-13 横店集团东磁股份有限公司 Preparation method of injection molding bonded magnetic powder
CN105345008A (en) * 2015-11-13 2016-02-24 绵阳德华磁材有限公司 Method for manufacturing large-mass samarium cobalt permanent magnet blank
CN108129729A (en) * 2017-12-20 2018-06-08 宁波市鄞州智伴信息科技有限公司 A kind of preparation process of the novel plastic type magnetron based on permanent-magnet material
CN108281245A (en) * 2018-01-24 2018-07-13 绵阳德华磁材有限公司 A kind of preparation method of samarium cobalt permanent magnet body
CN109448983A (en) * 2018-12-21 2019-03-08 中国计量大学 A kind of preparation method of high-coercive force anisotropy sheet SmCo nanocrystalline 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
CN111210960A (en) * 2020-01-20 2020-05-29 北京航大新磁科技有限公司 High-squareness-degree high-magnetic-energy-product samarium cobalt permanent magnet material and preparation method thereof
EP3686301A1 (en) 2019-01-28 2020-07-29 Baotou Tianhe Magnetics Technology Co., Ltd. Samarium-cobalt magnets and method for preparing the same

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JPH1070023A (en) * 1996-08-28 1998-03-10 Tokin Corp Permanent magnet and manufacture thereof
CN1494092A (en) * 2002-10-29 2004-05-05 中南大学 High temperature rare earth permanent magnetic material and its preparation method

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JPH1070023A (en) * 1996-08-28 1998-03-10 Tokin Corp Permanent magnet and manufacture thereof
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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103537684A (en) * 2013-11-07 2014-01-29 湖南航天工业总公司 Production method for samarium cobalt alloy powder
CN103632787A (en) * 2013-12-11 2014-03-12 湖南航天工业总公司 Method for sintering and tempering rare-earth cobalt permanent magnetic material
CN103632787B (en) * 2013-12-11 2015-11-25 湖南航天磁电有限责任公司 A kind of sintering of rare earth cobalt permanent magnets and tempering method
CN104609845A (en) * 2014-12-15 2015-05-13 横店集团东磁股份有限公司 Preparation method of injection molding bonded magnetic powder
CN105345008A (en) * 2015-11-13 2016-02-24 绵阳德华磁材有限公司 Method for manufacturing large-mass samarium cobalt permanent magnet blank
CN108129729A (en) * 2017-12-20 2018-06-08 宁波市鄞州智伴信息科技有限公司 A kind of preparation process of the novel plastic type magnetron based on permanent-magnet material
CN108281245A (en) * 2018-01-24 2018-07-13 绵阳德华磁材有限公司 A kind of preparation method of samarium cobalt permanent magnet body
CN109448983A (en) * 2018-12-21 2019-03-08 中国计量大学 A kind of preparation method of high-coercive force anisotropy sheet SmCo nanocrystalline magnet
EP3686301A1 (en) 2019-01-28 2020-07-29 Baotou Tianhe Magnetics Technology Co., Ltd. Samarium-cobalt magnets and method for preparing the same
US11532412B2 (en) 2019-01-28 2022-12-20 Baotou Tianhe Magnetics Technology Co., Ltd. Samarium-cobalt magnets and method for preparing the same
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
CN111210960A (en) * 2020-01-20 2020-05-29 北京航大新磁科技有限公司 High-squareness-degree high-magnetic-energy-product samarium cobalt permanent magnet material and preparation method thereof
CN111210960B (en) * 2020-01-20 2022-05-31 苏州航大新材料科技有限公司 High-squareness-degree high-magnetic-energy-product samarium cobalt permanent magnet material and preparation method thereof

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Application publication date: 20130925