CN105225780A - 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 PDF

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CN105225780A
CN105225780A CN201510659428.1A CN201510659428A CN105225780A CN 105225780 A CN105225780 A CN 105225780A CN 201510659428 A CN201510659428 A CN 201510659428A CN 105225780 A CN105225780 A CN 105225780A
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magnetic
magnet
bond
iron nitrogen
samarium iron
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CN105225780B (en
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尹玉霞
胡瑞金
岳明
刘卫强
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Beijing University of Technology
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Beijing University of Technology
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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 with anisotropy samarium iron nitrogen magnetic for magnetisable material, take sodium metasilicate as main binder, take high-temperature-resistant epoxy resin as additional adhesive, obtained anisotropic bond samarium iron nitrogen magnet not only has higher magnetic property, its temperature tolerance is also largely increased, operating ambient temperature can reach 200 DEG C, and has impermeabilisation, the advantage such as corrosion-resistant.One of the present invention is high temperature resistant anisotropic bond samarium iron nitrogen magnet and preparation method thereof, gained magnet has high magnetic performance, higher serviceability temperature, in implementation process, equipment is simple, easy and simple to handle, cost is lower, be easy to large-scale production, economic worth is high, has very large application prospect in permanent magnetic material field.

Description

A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet and preparation method thereof
Technical field
A kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet of invention and preparation method thereof, belongs to technical field of function materials.
Background technology
Nineteen ninety, the interstitial atom intermetallic compound R that utilized gas-solid phase reaction to synthesize such as HongSun and Coey 2fe 17n x, cause the extensive concern of magnetics circle, become the focus of domestic and international magnetics circle research immediately.Country " 12 " 863 major project born by Peking University's applied magnetics center, successfully have developed samarium iron nitrogen anisotropic magnet powder production line, and achieves product supply market.
In recent years, the high speed development of wind power generation, electric automobile and magnetic suspension train motor, had higher requirement to magnet serviceability temperature.The Curie temperature of samarium iron nitrogen magnetic is 470 DEG C, and higher than NdFeB magnetic (312 DEG C), therefore, samarium iron nitrogen series permanent magnetic material faces new opportunity to develop with its good resistance to elevated temperatures.Contrast with existing rare-earth magnetic, not only magnetic energy product is high, heat-resisting quantity good but also the cost of material is low for anisotropy samarium iron nitrogen magnetic.The bonding samarium iron nitrogen magnet adopting anisotropy samarium iron nitrogen magnetic to prepare not only has acted on the high energy product of magnetic, can also reduce required magnet volume, adapt to the growth requirement of current electrical equipment miniaturization.Therefore, the research and development of high temperature resistant bonding samarium iron nitrogen magnet have good realistic meaning and application prospect.
Binding agent at first for samarium-ferronitrogen permanent magnet has rubber, nylon, epoxy resin, phenolic resins, PS, PPS, polyimides-composite epoxy resin etc., but due to the shortcoming of binding agent itself, (the Ye Jinwen that all has much room for improvement such as mechanical property, thermal stability of obtained magnet, Liu Ying, Zhang Ran, Chen Mei, Zhu Guoli, promotion is lucky, be coated with an inscription ancient type of banner hoisted on a featherdecked mast. the preparation [J] of isotropism samarium iron nitrogen magnetic and bonded permanent magnet thereof. Rare Metals Materials and engineering, 2007,36 (2): 329-331.).Recent study finds that low-melting-point metal Zn, Al, Pb, Sn and Pb-Sn alloy etc. can be used as binding agent, obtained magnet can be applicable to higher temperature, serious (the Wang Min but the remanent magnetism of magnet declines, Li Hongwei, Yu Dunbo, Li Kuoshe, Luo Yang. the influencing factor [J] of samarium iron nitrogen bonded permanent magnet magnetic property. Metallic Functional Materials, 2010,17 (2): 72-76.).High temperature resistant anisotropic bond samarium iron nitrogen magnet of the present invention take sodium metasilicate as main binder, take high-temperature-resistant epoxy resin as additional adhesive, not only farthest can keep the magnetic property of samarium iron nitrogen magnetic, also effectively can improve the temperature tolerance of magnet, its operating ambient temperature can reach 200 DEG C.
Adopt sodium metasilicate as bonded permanent magnet binding agent, Japan Patent once reported a kind of sodium metasilicate of preparing and mixed the method that rear mold suppresses standby bonded permanent magnet parts with magnetic, obtained bonded permanent magnet parts normally can work in motor, generator etc. slightly hot environment, but there is the large problem of moisture absorption in magnet assembly, need to carry out necessary surface treatment and could use (MinamiTadashi, NakamuraKatsuya, OdakaneMasaaki.Manufactureofbondmagnet.Japan, H01F41/02,1997.).If sodium metasilicate and High temp. epoxy resins are used for bonded permanent magnet simultaneously, then gained magnet can in conjunction with every advantage of epoxy bonded permanent magnet and sodium metasilicate bonded permanent magnet, high temperature resistant, activeness and quietness, impermeabilisation moisture absorption, corrosion-resistant etc. in have unique advantage.Sodium metasilicate has good thermal endurance and intensity, can make up the shortcoming of epoxy resin non-refractory, and improves the strength character of magnet; Meanwhile, epoxy resin infiltrates sodium metasilicate system with molecular scale, forms the inierpeneirating network structure of sodium metasilicate and epoxy resin, will improve anti-permeability performance and the corrosion resistance of magnet well, a step-down of going forward side by side its moisture absorption low after crosslinking curing.
The present invention with anisotropy samarium iron nitrogen magnetic for magnetisable material, take sodium metasilicate as main binder, take high-temperature-resistant epoxy resin as additional adhesive, obtained anisotropic bond samarium iron nitrogen magnet not only has higher magnetic property, its temperature tolerance is also largely increased, operating ambient temperature can reach 200 DEG C, and has impermeabilisation, the advantage such as corrosion-resistant.
Summary of the invention
The object of this invention is 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.
One of the present invention is high temperature resistant, and anisotropic bond samarium iron nitrogen magnet is with anisotropy samarium iron nitrogen magnetic and binding agent is main constitutive material, then adds proper amount of surfactant and lubricant and obtained bonded permanent magnet.The mass ratio of each main 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%.
Described sodium silicate binder is sodium silicate aqueous solution, modulus 3.1 ~ 3.4, Baume degrees 39 ~ 41 °.
Described surfactant is preferably from KH-550, KH-560, KH-570, stearic acid, Aluminate, titanate esters.
Described lubricant is preferably from paraffin, glycerol, esters of silicon acis, silicone oil.
The preparation method of a kind of high temperature resistant anisotropic bond samarium iron nitrogen magnet of the present invention is as follows:
The first step, mixed with the surfactant of certain mass by anisotropy samarium iron nitrogen magnetic, stir, must bond magnetic A;
Second step, the bonding magnetic A first step obtained and epoxy adhesive, stir than mixing by certain mass, until magnetic is loose shape, must bond magnetic B;
3rd step, the bonding magnetic B obtained by second step mixes in mass ratio with sodium silicate binder, stirs, until magnetic is loose shape, must bond magnetic C;
4th step, the bonding magnetic C that the 3rd step is obtained and the mix lubricant of certain mass, stir, must bond magnetic D;
5th step, in the bonding magnetic D that the 4th step obtains, spray a little organic solvent to accelerate moisture evaporation in binding agent, be stirred to magnetic loose, must bond magnetic E;
6th step, the appropriate bonding magnetic E the 5th step obtained is placed in mould jolt ramming, first magnetic field orientating in orientating molded forming machine, and then compressing, the demoulding obtains initial magnet base F;
7th step, the initial magnet base F the 6th step obtained is placed in equal pressing equipment, makes its densification, obtains densification magnet base G;
8th step, the densification magnet base G the 7th step obtained is placed in vacuum or inert gas environment solidifies, and obtain high temperature resistant anisotropic bond samarium iron nitrogen magnet, curing temperature is 175 ~ 200 DEG C, time 30 ~ 40min.
Described epoxy adhesive first dissolves by a small amount of acetone diluted before use, instantly namely uses.
Described organic solvent is the mixing of one or more in acetone, methyl alcohol, ethanol, ethyl acetate.
Conventional anisotropic bond samarium iron nitrogen magnet many employings epoxy resin is as binding agent, be easy to batch production, size is accurate, it is the forming method that magnetic material is conventional, but there is the shortcoming that Long-Time Service temperature is lower, generally be no more than 110 DEG C, which has limited the use of bonded permanent magnet in some field.Therefore, develop resistant to elevated temperatures anisotropic bond samarium iron nitrogen magnet, not only have important application prospect in permanent magnetic material field, and there is very large economic worth.
The present invention compared with prior art has following beneficial effect.
One of the present invention is high temperature resistant anisotropic bond samarium iron nitrogen magnet and preparation method thereof, not only there is high magnetic performance, higher serviceability temperature (200 DEG C), simultaneously, the present invention's equipment in implementation process is simple, easy and simple to handle, cost is lower, be easy to large-scale production, economic worth is high.Therefore, the present invention has very large application prospect in permanent magnetic material field.
Embodiment
Below in conjunction with 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 Sm 2fe 17n 3the preparation method of magnet, carries out according to the following steps.
The first step, by 96g anisotropy Sm 2fe 17n 3magnetic mixes with 0.3gKH-550, stirs, and must bond magnetic A1;
Second step, the bonding magnetic A1 first step obtained mixes with 0.5g epoxy adhesive, stirs, until magnetic is loose shape, must bond magnetic B1;
3rd step, the bonding magnetic B1 obtained by second step and 3g sodium silicate binder (modulus 3.1, Baume degrees 40 °) mix, and stir, until magnetic is loose shape, must bond magnetic C1;
4th step, the bonding magnetic C1 the 3rd step obtained mixes with 0.2g paraffin, stirs, and must bond magnetic D1;
5th step, in the bonding magnetic D1 that the 4th step obtains, spray 5ml acetone, be stirred to magnetic loose, must bond magnetic E1;
6th step, the appropriate bonding magnetic E1 the 5th step obtained is placed in mould jolt ramming, in orientating molded forming machine, first use 10T magnetic field orientating, and then compressing, the demoulding obtains initial magnet base F1;
7th step, the initial magnet base F1 the 6th step obtained is placed in equal pressing equipment, makes its densification, obtains densification magnet base G1;
8th step, the densification magnet base G1 the 7th step obtained is placed in vacuum environment and solidifies, and obtains high temperature resistant anisotropic bond Sm 2fe 17n 3magnet, curing temperature is 175 DEG C, time 40min.
Adopt the processing step that this embodiment is identical, sodium silicate binder is used instead the epoxy adhesive of equal in quality, obtained anisotropic bond Sm 2fe 17n 3magnet 1 " #.Two kinds of anisotropic bond Sm that this embodiment obtains 2fe 17n 3magnet 1# and 1 " the temperature coefficient data of # are as shown in table 1.The anisotropic bond Sm of this embodiment gained 2fe 17n 3magnet 1# and 1 " magnetic property at the room temperature of # and 200 DEG C is as shown in table 2.
Table 1 anisotropic bond Sm 2fe 17n 3magnet 1# and 1 " the magnetic property temperature coefficient (easy axle) of #
Note: bonded permanent magnet 1 " # only uses epoxy resin for binding agent, and its operational environment is no more than 110 DEG C.
Table 2 anisotropic bond Sm 2fe 17n 3magnet 1# and 1 " magnetic property (easy axle) of #
Note: bonded permanent magnet 1 " # only uses epoxy resin for binding agent, cracked when it tests at 200 DEG C, do not have data.
Embodiment 2: a kind of high temperature resistant anisotropic bond Sm 2fe 17n 3the preparation method of magnet, carries out according to the following steps.
The first step, by 93g anisotropy Sm 2fe 17n 3magnetic mixes with 0.2gKH-560, stirs, and must bond magnetic A2;
Second step, the bonding magnetic A2 first step obtained mixes with 1.5g epoxy adhesive, stirs, until magnetic is loose shape, must bond magnetic B2;
3rd step, the bonding magnetic B2 obtained by second step and 5g sodium silicate binder (modulus 3.2, Baume degrees 39 °) mix, and stir, until magnetic is loose shape, must bond magnetic C2;
4th step, the bonding magnetic C2 the 3rd step obtained mixes with 0.3g silicone oil, stirs, and must bond magnetic D2;
5th step, in the bonding magnetic D2 that the 4th step obtains, spray 4ml ethanol, be stirred to magnetic loose, must bond magnetic E2;
6th step, the appropriate bonding magnetic E2 the 5th step obtained is placed in mould jolt ramming, in orientating molded forming machine, first use 10T magnetic field orientating, and then compressing, the demoulding obtains initial magnet base F2;
7th step, the initial magnet base F2 the 6th step obtained is placed in equal pressing equipment, makes its densification, obtains densification magnet base G2;
8th step, the densification magnet base G2 the 7th step obtained is placed in ar gas environment and solidifies, and obtains high temperature resistant anisotropic bond Sm 2fe 17n 3magnet, curing temperature is 188 DEG C, time 35min.
Adopt the processing step that this embodiment is identical, sodium silicate binder is used instead the epoxy adhesive of equal in quality, obtained anisotropic bond Sm 2fe 17n 3magnet 2 " #.Two kinds of anisotropic bond Sm that this embodiment obtains 2fe 17n 3magnet 2# and 2 " the temperature coefficient data of # are as shown in table 3.The anisotropic bond Sm of this embodiment gained 2fe 17n 3magnet 2# and 2 " magnetic property at the room temperature of # and 200 DEG C is as shown in table 4.
Table 3 anisotropic bond Sm 2fe 17n 3magnet 2# and 2 " the magnetic property temperature coefficient (easy axle) of #
Note: bonded permanent magnet 2 " # only uses epoxy resin for binding agent, and its operational environment is no more than 110 DEG C.
Table 4 anisotropic bond Sm 2fe 17n 3magnet 2# and 2 " magnetic property (easy axle) of #
Note: bonded permanent magnet 1 " # only uses epoxy resin for binding agent, cracked when it tests at 200 DEG C, do not have data.
Embodiment 3: a kind of high temperature resistant anisotropic bond Sm 2fe 17n 3the preparation method of magnet, carries out according to the following steps.
The first step, by 90g anisotropy Sm 2fe 17n 3magnetic mixes with 0.1gKH-570, stirs, and must bond magnetic A3;
Second step, the bonding magnetic A3 first step obtained mixes with 3.3g epoxy adhesive, stirs, until magnetic is loose shape, must bond magnetic B3;
3rd step, the bonding magnetic B3 obtained by second step and 6.5g sodium silicate binder (modulus 3.4, Baume degrees 41 °) mix, and stir, until magnetic is loose shape, must bond magnetic C3;
4th step, the bonding magnetic C3 the 3rd step obtained mixes with 0.1g paraffin, stirs, and must bond magnetic D3;
5th step, in the bonding magnetic D3 that the 4th step obtains, spray 5ml acetone, be stirred to magnetic loose, must bond magnetic E3;
6th step, the appropriate bonding magnetic E3 the 5th step obtained is placed in mould jolt ramming, in orientating molded forming machine, first use 10T magnetic field orientating, and then compressing, the demoulding obtains initial magnet base F3;
7th step, the initial magnet base F3 the 6th step obtained is placed in equal pressing equipment, makes its densification, obtains densification magnet base G3;
8th step, the densification magnet base G3 the 7th step obtained is placed in vacuum environment and solidifies, and obtains high temperature resistant anisotropic bond Sm 2fe 17n 3magnet, curing temperature is 200 DEG C, time 30min.
Adopt the processing step that this embodiment is identical, sodium silicate binder is used instead the epoxy adhesive of equal in quality, obtained anisotropic bond Sm 2fe 17n 3magnet 3 " #.Two kinds of anisotropic bond Sm that this embodiment obtains 2fe 17n 3magnet 3# and 3 " the temperature coefficient data of # are as shown in table 5.The anisotropic bond Sm of this embodiment gained 2fe 17n 3magnet 3# and 3 " magnetic property at the room temperature of # and 200 DEG C is as shown in table 6.
Table 5 anisotropic bond Sm 2fe 17n 3magnet 3# and 3 " the magnetic property temperature coefficient (easy axle) of #
Note: bonded permanent magnet 3 " # only uses epoxy resin for binding agent, and its operational environment is no more than 110 DEG C.
Table 6 anisotropic bond Sm 2fe 17n 3magnet 3# and 3 " magnetic property (easy axle) of #
Note: bonded permanent magnet 1 " # only uses epoxy resin for binding agent, cracked when it tests at 200 DEG C, do not have data.

Claims (7)

1. a high temperature resistant anisotropic bond samarium iron nitrogen magnet, is characterized in that, is be main constitutive material with anisotropy samarium iron nitrogen magnetic and binding agent, then adds proper amount of surfactant and lubricant and obtained bonded permanent magnet.The mass ratio of each main 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%.
2., according to the one of claim 1 high temperature resistant anisotropic bond samarium iron nitrogen magnet, it is characterized in that, described sodium silicate binder is sodium silicate aqueous solution, modulus 3.1 ~ 3.4, Baume degrees 39 ~ 41 °.
3. according to the one of claim 1 high temperature resistant anisotropic bond samarium iron nitrogen magnet, it is characterized in that, it is characterized in that, surfactant is preferably from KH-550, KH-560, KH-570, stearic acid, Aluminate, titanate esters.
4. according to the one of claim 1 high temperature resistant anisotropic bond samarium iron nitrogen magnet, it is characterized in that, it is characterized in that, lubricant is preferably from paraffin, glycerol, esters of silicon acis, silicone oil.
5. prepare the method for the high temperature resistant anisotropic bond samarium iron nitrogen magnet of claim 1, it is characterized in that, comprise the following steps:
The first step, mixed with the surfactant of certain mass by anisotropy samarium iron nitrogen magnetic, stir, must bond magnetic A;
Second step, the bonding magnetic A first step obtained and epoxy adhesive, stir than mixing by certain mass, until magnetic is loose shape, must bond magnetic B;
3rd step, the bonding magnetic B obtained by second step mixes in mass ratio with sodium silicate binder, stirs, until magnetic is loose shape, must bond magnetic C;
4th step, the bonding magnetic C that the 3rd step is obtained and the mix lubricant of certain mass, stir, must bond magnetic D;
5th step, in the bonding magnetic D that the 4th step obtains, spray a little organic solvent accelerate moisture evaporation in binding agent, be stirred to magnetic loose, must bond magnetic E;
6th step, the appropriate bonding magnetic E the 5th step obtained is placed in mould jolt ramming, first magnetic field orientating in orientating molded forming machine, and then compressing, the demoulding obtains initial magnet base F;
7th step, the initial magnet base F the 6th step obtained is placed in equal pressing equipment, makes its densification, obtains densification magnet base G;
8th step, the densification magnet base G the 7th step obtained is placed in vacuum or inert gas environment solidifies, and obtain high temperature resistant anisotropic bond samarium iron nitrogen magnet, curing temperature is 175 ~ 200 DEG C, time 30 ~ 40min.
6. according to the method for claim 5, it is characterized in that, described epoxy adhesive first dissolves by acetone diluted before use, instantly namely uses.
7. according to the method for claim 5, it is characterized in that, described organic solvent is the mixing of one or more in acetone, methyl alcohol, ethanol, ethyl acetate.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN112789701A (en) * 2018-10-09 2021-05-11 株式会社Ihi Method for producing Sm-Fe-N magnet, and motor having Sm-Fe-N magnet

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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
CN103119664A (en) * 2010-09-24 2013-05-22 户田工业株式会社 Ferromagnetic particle powder, method for producing same, anisotropic magnet, and bonded magnet
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
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
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112789701A (en) * 2018-10-09 2021-05-11 株式会社Ihi Method for producing Sm-Fe-N magnet, and motor having Sm-Fe-N magnet
JP7294347B2 (en) 2018-10-09 2023-06-20 株式会社Ihi Manufacturing method of Sm-Fe-N magnet, Sm-Fe-N magnet and motor provided with Sm-Fe-N magnet
CN112789701B (en) * 2018-10-09 2023-08-08 株式会社Ihi Method for producing 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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