CN105225780B - A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet and preparation method thereof - Google Patents
A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet and preparation method thereof Download PDFInfo
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Abstract
A kind of high temperature resistant anisotropy samarium iron nitrogen bonded permanent magnet and preparation method thereof, belongs to technical field of function materials.The present invention is using anisotropy samarium iron nitrogen magnetic as magnetisable material, using sodium metasilicate as main binder, using high-temperature-resistant epoxy resin as additional adhesive, anisotropic bond samarium iron nitrogen magnet, which is made, not only has higher magnetic property, its temperature tolerance is also largely increased, operating ambient temperature can reach 200 DEG C, and have the advantages that impermeabilisation, corrosion-resistant.A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet of the present invention and preparation method thereof, gained magnet has high magnetic performance, higher temperature in use, equipment is simple in implementation process, easy to operate, cost is relatively low, it is easy to mass produce, economic value is high, there is very big application prospect in permanent-magnet material field.
Description
Technical field
A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet of invention and preparation method thereof, belongs to functional material
Technical field.
Background technology
Nineteen ninety, Hong Sun and Coey etc. have synthesized interstitial atom intermetallic compound using gas-solid phase reaction
R2Fe17Nx, the extensive concern of magnetics circle is caused, immediately becomes the focus that domestic and international magnetics circle is studied.Applied by Peking University
The major project of country " 12 " 863 that magnetics center is undertaken, samarium iron nitrogen anisotropic magnet powder production line is successfully have developed, and
Realize product supply market.
In recent years, the high speed development of wind-power electricity generation, electric automobile and magnetic suspension train motor, magnet temperature in use is proposed
Higher requirement.The Curie temperature of samarium iron nitrogen magnetic is 470 DEG C, and higher than NdFeB magnetics (312 DEG C), therefore, samarium iron nitrogen system is forever
Magnetic material faces new opportunity to develop with its good resistance to elevated temperatures.Contrasted with existing rare-earth magnetic, anisotropy samarium
Not only magnetic energy product is high, heat-resisting quantity is good but also the cost of material is low for iron nitrogen magnetic.Prepared using anisotropy samarium iron nitrogen magnetic viscous
Knot samarium iron nitrogen magnet has not only adhered to the high energy product of magnetic, can also reduce required magnet volume, it is small to adapt to current electrical equipment
The growth requirement of type.Therefore, before the research and development of high temperature resistant bonding samarium iron nitrogen magnet are with good realistic meaning and application
Scape.
Being used primarily for the binding agent of samarium-ferronitrogen permanent magnet has rubber, nylon, epoxy resin, phenolic resin, PS, PPS, polyamides
Imines-composite epoxy resin etc., but the shortcomings that due to binding agent itself, the mechanical property of obtained magnet, heat endurance etc. is all
Having much room for improvement, (leaf inscription on ancient bronze objects, Liu Ying, Zhang Ran, Chen Mei, Zhu Guoli, promotion is lucky, applies inscription ancient type of banner hoisted on a featherdecked mast isotropism samarium iron nitrogen magnetics and its glues
Tie preparation [J] the Rare Metals Materials and engineering of magnet, 2007,36 (2):329-331.).Recent study finds low melting point
Metal Zn, Al, Pb, Sn and Pb-Sn alloy etc. can be used as binding agent, and obtained magnet can be applied to higher temperature, but magnetic
The remanent magnetism of body declines the serious (influence of Wang Min, Li Hongwei, Yu Dunbo, Li Kuoshe, Luo Yang samarium iron nitrogen bonded permanent magnet magnetic properties
Factor [J] Metallic Functional Materials, 2010,17 (2):72-76.).The high temperature resistant anisotropic bond samarium iron nitrogen magnet of the present invention
Using sodium metasilicate as main binder, using high-temperature-resistant epoxy resin as additional adhesive, samarium iron nitrogen can be not only maximally maintained
The magnetic property of magnetic, the temperature tolerance of magnet can be also effectively improved, its operating ambient temperature can reach 200 DEG C.
Using sodium metasilicate as bonded permanent magnet binding agent, Japan Patent once reported one kind and prepares sodium metasilicate to be mixed with magnetic
The method of the standby bonded permanent magnet part of rear mold compacting, obtained bonded permanent magnet part can be in the slightly higher Wen Huan such as motor, generator
Normal work in border, but magnet assembly the problem of moisture absorption is big be present, it is necessary to which carrying out necessary surface treatment could use
(Minami Tadashi,Nakamura Katsuya,Odakane Masaaki.Manufacture of bond
magnet.Japan,H01F 41/02,1997.).If sodium metasilicate and High temperature epoxy resinses are used for into bonded permanent magnet simultaneously,
Gained magnet can combine every advantage of epoxy bonded permanent magnet and sodium metasilicate bonded permanent magnet, in high temperature resistant, activeness and quietness, impermeabilisation
Moisture absorption, corrosion-resistant etc. have the advantage of uniqueness.Sodium metasilicate has good heat resistance and intensity, can make up epoxy resin not
Resistant to elevated temperatures shortcoming, and improve the strength character of magnet；Meanwhile epoxy resin penetrates into sodium metasilicate system, crosslinking with molecular scale
The inierpeneirating network structure of sodium metasilicate and epoxy resin is formed after solidification, the anti-permeability performance of magnet and corrosion-resistant will be improved well
Property, and further reduce its hygroscopicity.
The present invention is using anisotropy samarium iron nitrogen magnetic as magnetisable material, using sodium metasilicate as main binder, with fire resistant epoxy
Resin is additional adhesive, and obtained anisotropic bond samarium iron nitrogen magnet not only has higher magnetic property, its temperature tolerance
It is largely increased, operating ambient temperature can reach 200 DEG C, and have the advantages that impermeabilisation, corrosion-resistant.
The content of the invention
It is an object of the invention to provide a kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet and preparation method thereof, raw material
Easily obtain, can be mass-produced and cost is low.
A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet of the present invention is with anisotropy samarium iron nitrogen magnetic and bonding
Agent is main constitutive material, prepared by adding proper amount of surfactant and lubricant bonded permanent magnet.Each main group of magnet
Mass ratio into raw material is respectively：Anisotropy samarium iron nitrogen magnetic 90~96%, sodium silicate binder 3~6.5%, epoxy bonds
Agent 0.5~3.3%, surfactant 0.1~0.3%, lubricant 0.1~0.3%.
Described sodium silicate binder is sodium silicate aqueous solution, modulus 3.1~3.4,39~41 ° of Baume degrees.
Described surfactant preferably is selected from：KH-550, KH-560, KH-570, stearic acid, Aluminate, titanate esters.
Described lubricant preferably is selected from：Paraffin, glycerine, esters of silicon acis, silicone oil.
A kind of preparation method of high temperature resistant anisotropic bond samarium iron nitrogen magnet of the present invention is as follows：
The first step, anisotropy samarium iron nitrogen magnetic is mixed with the surfactant of certain mass, stirs, obtains bonding
Magnetic A；
Second step, the bonding magnetic A that the first step obtains is mixed with epoxy adhesive by certain mass ratio, stirred,
Until magnetic is in fluffy, cohesive magnetic B is obtained；
3rd step, the bonding magnetic B that second step obtains is mixed in mass ratio with sodium silicate binder, stirred, directly
It is in fluffy to magnetic, obtains cohesive magnetic C；
4th step, the bonding magnetic C and the mix lubricant of certain mass that the 3rd step is obtained, stirs, obtains bonding
Magnetic D；
5th step, a little organic solvent is sprayed to accelerate moisture in binding agent to wave in the bonding magnetic D obtained to the 4th step
Hair, stirs loose to magnetic, obtains cohesive magnetic E；
6th step, the appropriate magnetic E that bonds that the 5th step is obtained are placed in jolt ramming in mould, in orientating molded forming machine first
Magnetic field orientating, is then pressed into type, and the demoulding obtains initial magnet base F；
7th step, the initial magnet base F that the 6th step obtains is placed in equal pressing equipment, makes its densification, obtains densification
Change magnet base G；
8th step, the densification magnet base G that the 7th step obtains is placed in vacuum or inert gas environment and solidified, is obtained resistance to
High temperature anisotropic bond samarium iron nitrogen magnet, solidification temperature are 175~200 DEG C, 30~40min of time.
Described epoxy adhesive is first diluted with a small amount of acetone before use and dissolved, instant to use.
Described organic solvent is one or more of mixing in acetone, methanol, ethanol, ethyl acetate.
Conventional anisotropic bond samarium iron nitrogen magnet, as binding agent, is easy to batch production, chi more using epoxy resin
It is very little accurate, it is the conventional forming method of magnetic material, but the shortcomings that long-term use of temperature is relatively low be present, it is usually no more than 110
DEG C, which has limited use of the bonded permanent magnet in some fields.Therefore, resistant to elevated temperatures anisotropic bond samarium iron nitrogen magnet is developed,
Not only there is important application prospect in permanent-magnet material field, and there is very big economic value.
The present invention has the advantages that compared with prior art.
A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet of the present invention and preparation method thereof, not only with high magnetics
Performance, higher temperature in use (200 DEG C), meanwhile, equipment is simple in implementation process, easy to operate, cost is relatively low by the present invention,
It is easy to mass produce, economic value is high.Therefore, the present invention has very big application prospect in permanent-magnet material field.
Embodiment
With reference to embodiment, the present invention will be further described, but the present invention is not limited to following examples.
Embodiment 1：A kind of high temperature resistant anisotropic bond Sm2Fe17N3The preparation method of magnet, carry out according to the following steps.
The first step, by 96g anisotropy Sm2Fe17N3Magnetic mixes with 0.3gKH-550, stirs, and obtains cohesive magnetic
A1；
Second step, the bonding magnetic A1 that the first step obtains is mixed with 0.5g epoxy adhesives, stirred, until magnetic
In fluffy, cohesive magnetic B1 is obtained；
3rd step, the bonding magnetic B1 that second step is obtained are mixed with 3g sodium silicate binders (modulus 3.1,40 ° of Baume degrees)
Close, stir, until magnetic is in fluffy, obtain cohesive magnetic C1；
4th step, the bonding magnetic C1 that the 3rd step obtains is mixed with 0.2g paraffin, stirred, obtain cohesive magnetic D1；
5th step, 5ml acetone is sprayed in the bonding magnetic D1 obtained to the 4th step, stir loose to magnetic, obtain bonding magnetic
Powder E1；
6th step, the appropriate magnetic E1 that bonds that the 5th step is obtained is placed in jolt ramming in mould, in orientating molded forming machine
10T magnetic field orientatings are first used, are then pressed into type, the demoulding obtains initial magnet base F1；
7th step, the initial magnet base F1 that the 6th step obtains is placed in equal pressing equipment, makes its densification, obtains densification
Change magnet base G1；
8th step, the densification magnet base G1 that the 7th step obtains is placed in vacuum environment and solidified, obtain high temperature resistant respectively to
The opposite sex bonds Sm2Fe17N3Magnet, solidification temperature are 175 DEG C, time 40min.
Using this embodiment identical processing step instead, sodium silicate binder is used to the epoxy adhesive of phase homogenous quantities,
Anisotropic bond Sm is made2Fe17N3The # of magnet 1 ".Two kinds of anisotropic bond Sm obtained by this embodiment2Fe17N3Magnet
The # of 1# and 1 " temperature coefficient data are as shown in table 1.Anisotropic bond Sm obtained by this embodiment2Fe17N3Magnet 1# and
Magnetic property at 1 " # room temperature and 200 DEG C is as shown in table 2.
The anisotropic bond Sm of table 12Fe17N3Magnet 1# and 1 " # magnetic property temperature coefficient (easy axle)
Note：The # of bonded permanent magnet 1 " is binding agent using only epoxy resin, and its working environment is no more than 110 DEG C.
The anisotropic bond Sm of table 22Fe17N3Magnet 1# and 1 " # magnetic property (easy axle)
Note：The # of bonded permanent magnet 1 " is binding agent using only epoxy resin, fragmentation when it is tested at 200 DEG C, without data.
Embodiment 2：A kind of high temperature resistant anisotropic bond Sm2Fe17N3The preparation method of magnet, carry out according to the following steps.
The first step, by 93g anisotropy Sm2Fe17N3Magnetic mixes with 0.2gKH-560, stirs, and obtains cohesive magnetic
A2；
Second step, the bonding magnetic A2 that the first step obtains is mixed with 1.5g epoxy adhesives, stirred, until magnetic
In fluffy, cohesive magnetic B2 is obtained；
3rd step, the bonding magnetic B2 that second step is obtained are mixed with 5g sodium silicate binders (modulus 3.2,39 ° of Baume degrees)
Close, stir, until magnetic is in fluffy, obtain cohesive magnetic C2；
4th step, the bonding magnetic C2 that the 3rd step obtains is mixed with 0.3g silicone oil, stirred, obtain cohesive magnetic D2；
5th step, 4ml ethanol is sprayed in the bonding magnetic D2 obtained to the 4th step, stir loose to magnetic, obtain bonding magnetic
Powder E2；
6th step, the appropriate magnetic E2 that bonds that the 5th step is obtained is placed in jolt ramming in mould, in orientating molded forming machine
10T magnetic field orientatings are first used, are then pressed into type, the demoulding obtains initial magnet base F2；
7th step, the initial magnet base F2 that the 6th step obtains is placed in equal pressing equipment, makes its densification, obtains densification
Change magnet base G2；
8th step, the densification magnet base G2 that the 7th step obtains is placed in ar gas environment and solidified, obtain high temperature resistant respectively to
The opposite sex bonds Sm2Fe17N3Magnet, solidification temperature are 188 DEG C, time 35min.
Using this embodiment identical processing step instead, sodium silicate binder is used to the epoxy adhesive of phase homogenous quantities,
Anisotropic bond Sm is made2Fe17N3The # of magnet 2 ".Two kinds of anisotropic bond Sm obtained by this embodiment2Fe17N3Magnet
The # of 2# and 2 " temperature coefficient data are as shown in table 3.Anisotropic bond Sm obtained by this embodiment2Fe17N3Magnet 2# and
Magnetic property at 2 " # room temperature and 200 DEG C is as shown in table 4.
The anisotropic bond Sm of table 32Fe17N3Magnet 2# and 2 " # magnetic property temperature coefficient (easy axle)
Note：The # of bonded permanent magnet 2 " is binding agent using only epoxy resin, and its working environment is no more than 110 DEG C.
The anisotropic bond Sm of table 42Fe17N3Magnet 2# and 2 " # magnetic property (easy axle)
Note：The # of bonded permanent magnet 1 " is binding agent using only epoxy resin, fragmentation when it is tested at 200 DEG C, without data.
Embodiment 3：A kind of high temperature resistant anisotropic bond Sm2Fe17N3The preparation method of magnet, carry out according to the following steps.
The first step, by 90g anisotropy Sm2Fe17N3Magnetic mixes with 0.1gKH-570, stirs, and obtains cohesive magnetic
A3；
Second step, the bonding magnetic A3 that the first step obtains is mixed with 3.3g epoxy adhesives, stirred, until magnetic
In fluffy, cohesive magnetic B3 is obtained；
3rd step, the bonding magnetic B3 that second step is obtained and 6.5g sodium silicate binders (modulus 3.4,41 ° of Baume degrees)
Mixing, stirs, until magnetic is in fluffy, obtains cohesive magnetic C3；
4th step, the bonding magnetic C3 that the 3rd step obtains is mixed with 0.1g paraffin, stirred, obtain cohesive magnetic D3；
5th step, 5ml acetone is sprayed in the bonding magnetic D3 obtained to the 4th step, stir loose to magnetic, obtain bonding magnetic
Powder E3；
6th step, the appropriate magnetic E3 that bonds that the 5th step is obtained is placed in jolt ramming in mould, in orientating molded forming machine
10T magnetic field orientatings are first used, are then pressed into type, the demoulding obtains initial magnet base F3；
7th step, the initial magnet base F3 that the 6th step obtains is placed in equal pressing equipment, makes its densification, obtains densification
Change magnet base G3；
8th step, the densification magnet base G3 that the 7th step obtains is placed in vacuum environment and solidified, obtain high temperature resistant respectively to
The opposite sex bonds Sm2Fe17N3Magnet, solidification temperature are 200 DEG C, time 30min.
Using this embodiment identical processing step instead, sodium silicate binder is used to the epoxy adhesive of phase homogenous quantities,
Anisotropic bond Sm is made2Fe17N3The # of magnet 3 ".Two kinds of anisotropic bond Sm obtained by this embodiment2Fe17N3Magnet
The # of 3# and 3 " temperature coefficient data are as shown in table 5.Anisotropic bond Sm obtained by this embodiment2Fe17N3Magnet 3# and
Magnetic property at 3 " # room temperature and 200 DEG C is as shown in table 6.
The anisotropic bond Sm of table 52Fe17N3Magnet 3# and 3 " # magnetic property temperature coefficient (easy axle)
Note：The # of bonded permanent magnet 3 " is binding agent using only epoxy resin, and its working environment is no more than 110 DEG C.
The anisotropic bond Sm of table 62Fe17N3Magnet 3# and 3 " # magnetic property (easy axle)
Note：The # of bonded permanent magnet 1 " is binding agent using only epoxy resin, fragmentation when it is tested at 200 DEG C, without data.
Claims (6)
1. prepare the method for high temperature resistant anisotropic bond samarium iron nitrogen magnet, it is characterised in that high temperature resistant anisotropic bond samarium
Iron nitrogen magnet, it is characterised in that be using anisotropy samarium iron nitrogen magnetic and binding agent as main constitutive material, add appropriate table
Prepared by face activating agent and lubricant bonded permanent magnet；The mass percent of each constitutive material of magnet is respectively：Anisotropy
Samarium iron nitrogen magnetic 90~96%, sodium silicate binder 3~6.5%, epoxy adhesive 0.5~3.3%, surfactant 0.1~
0.3%, lubricant 0.1~0.3%；Comprise the following steps：
The first step, anisotropy samarium iron nitrogen magnetic is mixed with the surfactant of certain mass, stirs, obtains cohesive magnetic
A；
Second step, the bonding magnetic A that the first step obtains is mixed with epoxy adhesive by certain mass ratio, stirred, until
Magnetic is in fluffy, obtains cohesive magnetic B；
3rd step, the bonding magnetic B that second step obtains is mixed in mass ratio with sodium silicate binder, stirred, until magnetic
Powder is in fluffy, obtains cohesive magnetic C；
4th step, the bonding magnetic C and the mix lubricant of certain mass that the 3rd step is obtained, stirs, and obtains cohesive magnetic
D；
5th step, a little organic solvent is sprayed in the bonding magnetic D obtained to the 4th step and accelerates moisture evaporation in binding agent, stirring
It is loose to magnetic, obtain cohesive magnetic E；
6th step, the appropriate magnetic E that bonds that the 5th step is obtained are placed in jolt ramming in mould, the first magnetic field in orientating molded forming machine
Orientation, is then pressed into type, and the demoulding obtains initial magnet base F；
7th step, the initial magnet base F that the 6th step obtains is placed in equal pressing equipment, makes its densification, obtain being densified magnetic
Body base G；
8th step, the densification magnet base G that the 7th step obtains is placed in vacuum or inert gas environment and solidified, obtains high temperature resistant
Anisotropic bond samarium iron nitrogen magnet, solidification temperature are 175~200 DEG C, 30~40min of time.
2. according to the method for claim 1, it is characterised in that described epoxy adhesive is first molten with acetone dilution before use
Solution, it is instant to use.
3. according to the method for claim 1, it is characterised in that described organic solvent is acetone, methanol, ethanol, ethyl acetate
In one or more of mixing.
4. according to the method for claim 1, it is characterised in that described sodium silicate binder is sodium silicate aqueous solution, modulus 3.1
~3.4,39~41 ° of Baume degrees.
5. according to the method for claim 1, it is characterised in that surfactant is selected from：It is KH-550, KH-560, KH-57 0, hard
Resin acid, Aluminate or titanate esters.
6. according to the method for claim 1, it is characterised in that lubricant is selected from：Paraffin, glycerine, esters of silicon acis or silicone oil.
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| EP3866180A4 (en) * | 2018-10-09 | 2022-08-10 | IHI Corporation | Method for manufacturing sm-fe-n magnet, sm-fe-n magnet, and motor having sm-fe-n magnet |
| CN112564436A (en) * | 2020-11-26 | 2021-03-26 | 浙江英洛华磁业有限公司 | Method of manufacturing a rotor assembly |
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| CN104070161A (en) * | 2014-05-28 | 2014-10-01 | 浙江大学 | Preparation method for inorganic-organic composite adhesive-coated soft magnetic composite |
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| JPH03295204A (en) * | 1990-04-13 | 1991-12-26 | Hitachi Metals Ltd | Permanent magnet and manufacture thereof |
| JP5822188B2 (en) * | 2010-09-24 | 2015-11-24 | 戸田工業株式会社 | Ferromagnetic particle powder and production method thereof, anisotropic magnet and bonded magnet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157779A (en) * | 2007-09-27 | 2008-04-09 | 广州金南磁塑有限公司 | Novel rubber magnet and method for making same |
| CN101465188A (en) * | 2008-07-22 | 2009-06-24 | 北矿磁材科技股份有限公司 | Flexible rare-earth cementing magnet and method of manufacturing the same |
| CN101615475A (en) * | 2009-05-08 | 2009-12-30 | 北京科技大学 | A kind of manufacture method of flexible anisotropic bonding rare earth permanent magnet |
| CN102982961A (en) * | 2012-12-14 | 2013-03-20 | 北京科技大学 | Method for preparing anisotropic bonded magnet by adopting pressure-keeping curing process |
| CN104070161A (en) * | 2014-05-28 | 2014-10-01 | 浙江大学 | Preparation method for inorganic-organic composite adhesive-coated soft magnetic composite |
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