CN101740193B - Rare-earth permanent magnet with high magnetic performance and high electric resistance and preparation method thereof - Google Patents
Rare-earth permanent magnet with high magnetic performance and high electric resistance and preparation method thereof Download PDFInfo
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- CN101740193B CN101740193B CN200910227793XA CN200910227793A CN101740193B CN 101740193 B CN101740193 B CN 101740193B CN 200910227793X A CN200910227793X A CN 200910227793XA CN 200910227793 A CN200910227793 A CN 200910227793A CN 101740193 B CN101740193 B CN 101740193B
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Abstract
The invention relates to the technology of rare-earth permanent magnet materials, and particularly discloses a rare-earth permanent magnet with high magnetic performance and high electric resistance and a preparation method thereof. The permanent magnet comprises the following components in part by mass: 100 parts of neodymium iron boron and samarium cobalt type magnetic powder with granularity of 20 to 300 microns, 0.1 to 5 parts of titanate coupling agent, 1 to 10 parts of bisphenol A epoxy resin and 0.2 to 2 parts of bisphenol F epoxy resin; the components are evenly mixed, and then are molded to form a cured substance at the temperature field of between 20 and 200 DEG C under the orientation field of which the magnetic field intensity is 0.5 to 3T; and the preparation method for the rare-earth permanent magnet comprises the following steps: coupling the surface of the magnetic powder and the coupling agent, then mixing the magnetic powder, the coupling agent and the resin, drying and grinding the mixture, and molding the mixture at the temperature field under the orientation field. The magnetic performance of the permanent magnet of the invention can keep higher level and has no obvious decline compared with the magnetic performance of the high-end adhesive NdFeB magnet, and the electric resistance of the magnet is improved by over 10 times; and the permanent magnet has no obvious temperature rise under the high-frequency alternating field for 1 hour.
Description
Technical field
The present invention relates to a kind of rare earth permanent-magnetic material art, particularly a kind of high magnetic characteristics high resistivity rare-earth permanent magnet and preparation method thereof.
Background technology
Compare with sintered permanent magnet, bonded magnet has cost performance height, special-shaped magnet convenient formation, machining accuracy height, good toughness, magnetic deviation is little and be easy to plurality of advantages such as miniaturization, these characteristics have just in time met the developing direction of electronic information machine product " light, thin, short, little ", so bonded magnet has been widely used in fields such as computer, mobile communication, advanced audio, small and special electric machine, transducer and magneto-electric instrument and meter.When bonded magnet is applied in high frequency alternating field following time, because its resistivity is lower, magnet surface is easy to generate strong eddy current, cause magnet temperature to raise rapidly, the magnet magnetic property will be had a strong impact on, and therefore, common bonding rare-earth permanent magnet is difficult to realize using under radio-frequency field.
In the prior art, a kind of many magnetic poles electric insulation R-Fe-B permanent magnet that a kind of method is introduced in flat 8-279407 number for the Japanese patent gazette spy opens, this kind magnet is a sintered magnet, it adopts vacuum to steam the method for film after the magnet sinter molding, the polyimide resin film that plates one deck 2～10 μ m in magnet surface to be improving its insulation property, but the magnet that this kind method obtains still can't be avoided causing the magnetic loss of energy because of magnet eddy current self inner heat when using under the alternating magnetic field of higher-frequency.In addition, all mention the method for in rare-earth permanent magnet, adding the insulation additive in the patents such as Chinese patent CN97121777.7 and CN02157615.7 and improved its electrical insulation capability, from its result, electrical insulation capability has obtained obvious lifting really, but because the adding of a large amount of insulation additives has caused the magnet magnetic property seriously to descend, its forming process is no oriented moulding mode simultaneously, this also makes the magnetic property of magnet be difficult to further raising, and the magnet of mentioning in the feasible invention is difficult to be used widely in practice.
Summary of the invention
Technical problem to be solved by this invention provides a kind of high magnetic characteristics high resistivity rare-earth permanent magnet and preparation method thereof.Technology paths such as the hybrid technique of the present invention by magnetic surface coupling process, resin dedicated and coupling bonded magnetic powder, magnet temperature and pressure oriented moulding technology, the bonding rare-earth permanent magnet of a kind of high resistivity that obtains can be used for computer, mobile communication, advanced audio, small and special electric machine, transducer and magneto-electric instrument and meter etc. and needs the technical field of magnet in the radio-frequency field application.
For the purpose that realizes solving the problems of the technologies described above, the present invention has adopted following technical scheme:
A kind of high magnetic characteristics high resistivity rare-earth permanent magnet of the present invention, the even back of mixing that is characterised in that it becomes granularity 20～200 μ m neodymium iron borons and SmCo type for quality group 1～10 part of 0.1～5 part of 100 parts of magnetics, titanate coupling agent, bisphenol A epoxide resin, 0.2～2 part of bisphenol F epoxy resin is being provided with the combinational environment compacted under solidfied material that thermostat temperature is 20～200 ℃ temperature field and the magnetic field intensity orientation field that is 0.5～3T.
A kind of high magnetic characteristics high resistivity rare-earth permanent magnet of the present invention, its optimized technical scheme can also be: described bisphenol A epoxide resin, epoxide number are 0.04～0.06eq/100g.
A kind of high magnetic characteristics high resistivity rare-earth permanent magnet of the present invention, its optimized technical scheme can also be: described bisphenol F epoxy resin, epoxide number are 0.02～0.08eq/100g.
A kind of high magnetic characteristics high resistivity rare-earth permanent magnet of the present invention, its optimized technical scheme can also be: the magnetic of described neodymium iron boron and SmCo type, magnetic consist of Nd
2Fe
14B, Sm
2Co
17Or SmCo
5Any one or two kinds of above mixtures, performance requirement is iHc 〉=400KA/m, Br 〉=0.65T, (BH) max 〉=120KJ/m
3
The preparation method of a kind of high magnetic characteristics high resistivity rare-earth permanent magnet of the present invention comprises following technical process:
(1) magnetic surface coupling: with the titanate coupling agent of 0.1～5 weight portion with join in the magnetic of 100 weight portions after the organic solvent of 20～50 weight portions mixes, high speed shear stirring 0.5～2h by 500～2000 rev/mins speed mixes above-mentioned solution, and make magnetic can fully mix with coupling agent by supersonic oscillations 0.5～2h, then mixture is heated while stirring, finish until solvent evaporates, grind the oven dry of the magnetic after modification back stand-by; Described organic solvent be to titanate esters and epoxy resin inertia, boiling point is at the organic solvent below 200 ℃, for example, toluene, benzene, ethylbenzene, dimethylbenzene, acetone, absolute alcohol or its two or more mixture all can;
(2) with bisphenol A epoxide resin 1～10 weight portion, the mixed liquor of bisphenol F epoxy resin 0.2～2 weight portion and organic solvent 1～100 weight portion joins in the magnetic of 100 weight portions after the surperficial coupling, stirring 0.5～2h under 500～2000 rev/mins mixing speed mixes above-mentioned mixed liquor, and process supersonic oscillations 0.5～2h makes magnetic can fully mix with resin, then mixture is heated while stirring, finish until solvent evaporates, magnetic after surface modification oven dry back grinding is prevented that magnetic from hardening, and the magnetic after the grinding should pass through 100～400 mesh sieves;
(3) magnetic after will grinding carries out moulding 10～30min being provided with under the combinational environment that thermostat temperature is 20～200 ℃ temperature field and the magnetic field intensity orientation field that is 0.5～3T, and the briquetting pressure scope is 2～8ton/cm
2, make high magnetic characteristics, the bonding rare-earth permanent magnet of high resistivity.
The bonding rare earth permanent magnet body and function of the high resistivity surface insulation magnetic of the present invention's preparation is to adopt surperficial coating method to introduce special epoxy resin on the magnetic surface, by technologies such as coupling, mixing, reprocessing make magnetic the surface insulation performance be improved significantly, again with the magnetic after the surface modification the temperature field and the orientation combinational environment under carry out moulding, make last high magnetic characteristics, the bonding rare-earth permanent magnet of high resistivity.The present invention starts with from high-performance magnetic surface insulation treatment technology and magnet temperature and pressure oriented moulding technology, do not add the insulation additive, studied magnetic surface coupling process, the hybrid technique of resin dedicated and coupling magnetic, magnet temperature and pressure oriented moulding technology etc., solved magnetic and resin dedicated bonding not firm, resin dedicated imperfect in the coating of magnetic surface, resin dedicated easily reunion in processing procedure, the magnet magnetic property improves a series of problems such as limited after the moulding, finally obtained a kind of high magnetic characteristics, the preparation method of the bonding rare-earth permanent magnet of high resistivity anisotropic, the bonding rare-earth permanent magnet that utilizes the present invention to suppress can possess higher resistivity simultaneously under the situation that keeps its higher magnetic property, thereby can realize fully using under the high frequency alternating field.
By adopting technique scheme, the magnet that obtains under the present invention and the prior art condition is compared, and its beneficial effect is:
(1) the magnet magnetic property that utilizes the present invention to develop keeps high levels.Surface insulation processing NdFeB magnetic with introducing 0.3wt% coupling agent, 5wt% epoxy resin is an example, and institute's pressing magnetic body is compared high-end bonding NdFeB magnet magnetic property does not have obvious decline.
(2) the magnet resistivity of utilizing the present invention and being developed promotes obviously.Surface insulation processing magnetic with introducing 0.3wt% coupling agent, 5wt% epoxy resin is an example, and institute's pressing magnetic body is compared high-end bonding NdFeB magnet resistivity and improved more than 10 times.
(3) adaptive capacity used under radio-frequency field of the magnet that utilizes the present invention and made promotes obviously.Surface insulation processing magnetic with introducing 0.1wt% coupling agent, 5wt% epoxy resin is an example, the NdFeB magnet of suppressing is in for a long time that 1h does not have obvious temperature rise under the high frequency alternating field, and bonding NdFeB magnet magnet temperature behind about 10min of prior art for preparing begins that promptly bigger rising is arranged.
Embodiment
Embodiment 1
(1) magnetic surface coupling: employed magnetic is a neodymium iron boron, and it consists of the Nd that particle mean size is 20 μ m
2Fe
14B, the titanate coupling agent NDZ401 of 0.1 part of Nanjing dawn chemical industry product and the dimethylbenzene organic solvent of 30 weight portions are joined in the magnetic of 100 weight portions, high speed shear stirring 0.5h by 2000 rev/mins speed mixes above-mentioned solution, and make magnetic can fully mix with coupling agent by supersonic oscillations 0.5h, then mixture is heated while stirring, finish until solvent evaporates, grind the oven dry of the magnetic after modification back stand-by; (2) No.China Shipbuilding Industry Group Co.ltd. 725 Institute is produced 725-2-A bisphenol A epoxide resin 1 weight portion, the mixed liquor of No.China Shipbuilding Industry Group Co.ltd. 725 Institute's product 725-2-F bisphenol F epoxy resin 0.2 weight portion and acetone joins in the magnetic of 100.1 weight portions after the surperficial coupling, stirring 0.5h under 2000 rev/mins mixing speed mixes above-mentioned mixed liquor, and process supersonic oscillations 0.5h makes magnetic can fully mix with resin, then mixture is heated while stirring, finish until solvent evaporates, magnetic after modification oven dry back is ground, and the magnetic after the grinding should pass through 100 mesh sieves;
(3) magnetic after the surface modification is carried out moulding 30min under the combinational environment of orientation field that in 20 ℃ of temperature fields and magnetic field intensity is 0.5T, briquetting pressure is 3ton/cm
2, obtain rare-earth permanent magnet.。
Prepared rare-earth permanent magnet, its resistivity are 1.3 * 10
-4Ω m when magnetic field intensity 0.5T, is in that the 1h temperature rise is 75 ℃ under the 50KHz high frequency alternating field.
Embodiment 2
(1) magnetic surface coupling: employed magnetic is the SmCo magnetic, and it consists of Sm
2Co
17Particle mean size is 40 μ m, the titanate coupling agent NDZ401 that the Nanjing dawn chemical industry of 2 weight portions is produced and the alcohol of 35 weight portions join in the magnetic of 100 weight portions, high speed shear stirring 1h by 500 rev/mins speed mixes above-mentioned solution, and make magnetic can fully mix with coupling agent by supersonic oscillations 1h, then mixture is heated while stirring, finish, grind the oven dry of the magnetic after modification back stand-by until solvent evaporates; (2) No.China Shipbuilding Industry Group Co.ltd. 725 Institute is produced 725-2-A bisphenol A epoxide resin 6.5 weight portions, the mixed liquor of No.China Shipbuilding Industry Group Co.ltd. 725 Institute's product 725-2-F bisphenol F epoxy resin 1.3 weight portions and organic solvent-acetone joins in the magnetic of 102 weight portions after the surperficial coupling, stirring 1h under 500～2000 rev/mins mixing speed mixes above-mentioned mixed liquor, and process supersonic oscillations 1h makes magnetic can fully mix with resin, then mixture is heated while stirring, finish until solvent evaporates, magnetic after modification oven dry back is ground, and the magnetic after the grinding should pass through 250 mesh sieves; (3) magnetic after the surface modification is carried out moulding 15min under the combinational environment of orientation field that in 80 ℃ of temperature fields and magnetic field intensity is 2T, briquetting pressure is 5ton/cm
2, obtain rare-earth permanent magnet.
Prepared rare-earth permanent magnet, its resistivity are 2 * 10
-3Ω m when magnetic field intensity 0.5T, is in that the 1h temperature rise is 40 ℃ under the 50KHz high frequency alternating field.
Embodiment 3
(1) magnetic surface coupling: employed magnetic is the SmCo magnetic, and it consists of SmCo
5The titanate coupling agent NDZ401 that the Nanjing dawn chemical industry of 5 weight portions is produced and the dimethylbenzene of 30 weight portions join in the magnetic of 100 weight portions, high speed shear stirring 1.5h by 800 rev/mins speed mixes above-mentioned solution, and make magnetic can fully mix with coupling agent by supersonic oscillations 1.5h, then mixture is heated while stirring, finish until solvent evaporates, grind the oven dry of the magnetic after modification back stand-by; (2) No.China Shipbuilding Industry Group Co.ltd. 725 Institute is produced the 725-2-A bisphenol A epoxide resin, the mixed liquor of No.China Shipbuilding Industry Group Co.ltd. 725 Institute's product 725-2-F bisphenol F epoxy resin 2 weight portions and organic solvent-acetone joins in the magnetic of 105 weight portions after the surperficial coupling, stirring 1.5h under 500～2000 rev/mins mixing speed mixes above-mentioned mixed liquor, and process supersonic oscillations 1.5h makes magnetic can fully mix with resin, then mixture is heated while stirring, finish until solvent evaporates, magnetic after modification oven dry back is ground, and the magnetic after the grinding should pass through 400 mesh sieves; (3) magnetic after the surface modification is carried out moulding 10min under the combinational environment of orientation field that in 200 ℃ of temperature fields and magnetic field intensity is 3T, briquetting pressure is 8ton/cm
2, obtain rare-earth permanent magnet.
Prepared rare-earth permanent magnet, its resistivity are 5 * 10
-3Ω m when magnetic field intensity 0.5T, is in that the 1h temperature rise is 45 ℃ under the 50KHz high frequency alternating field.
Comparative Examples
A kind of bonding NdFeB magnet of prior art for preparing, its resistivity is 1 * 10
-6Ω m when magnetic field intensity 0.5T, is in that the 1h temperature rise is 165 ℃ under the 50KHz high frequency alternating field.
Claims (5)
1. high magnetic characteristics high resistivity rare-earth permanent magnet, be characterised in that: its quality group becomes 0.2～2 part of 1～10 part of 0.1～5 part of 100 parts of magnetics, titanate coupling agent, the bisphenol A epoxide resin of granularity 20～200 μ m and bisphenol F epoxy resin, evenly mixes the back combinational environment compacted under solidfied material that thermostat temperature is 20～200 ℃ temperature field and the magnetic field intensity orientation field that is 0.5～3T is being set; Described magnetic is Nd
2Fe
14B, Sm
2Co
17Or SmCo
5Any one or two kinds of above mixtures, performance requirement is iHc 〉=400KA/m, Br 〉=0.65T, (BH) max 〉=120KJ/m
3
2. according to the described a kind of high magnetic characteristics high resistivity rare-earth permanent magnet of claim 1, it is characterized in that: described bisphenol A epoxide resin epoxide number is 0.04～0.06eq/100g.
3. according to the described a kind of high magnetic characteristics high resistivity rare-earth permanent magnet of claim 1, it is characterized in that: described bisphenol F epoxy resin epoxide number is 0.02～0.08eq/100g.
4. the preparation method of claim 1 a high magnetic characteristics high resistivity rare-earth permanent magnet is characterized in that preparation technology is:
(1) magnetic surface coupling: with the titanate coupling agent of 0.1～5 weight portion with join in the magnetic of 100 weight portions after the organic solvent of 20～50 weight portions mixes, form solution, high speed shear stirring 0.5～2h by 500～2000 rev/mins speed mixes above-mentioned solution, and make magnetic can fully mix with coupling agent by supersonic oscillations 0.5～2h, then mixture is heated while stirring, finish until solvent evaporates, grind the oven dry of the magnetic after modification back stand-by; Described organic solvent be to titanate esters and epoxy resin inertia, boiling point is at the organic solvent below 200 ℃;
(2) mixed liquor of bisphenol A epoxide resin 1～10 weight portion, bisphenol F epoxy resin 0.2～2 weight portion and organic solvent 1～100 weight portion is joined in the magnetic of 100 weight portions after the surperficial coupling, stirring 0.5～2h under 500～2000 rev/mins mixing speed mixes above-mentioned mixed liquor, and process supersonic oscillations 0.5～2h makes magnetic can fully mix with resin, then mixture is heated while stirring, finish until solvent evaporates, magnetic after surface modification oven dry back grinding is prevented that magnetic from hardening, and the magnetic after the grinding can pass through 100～400 mesh sieves;
(3) magnetic after will grinding carries out moulding 10～30min being provided with under the combinational environment that thermostat temperature is 20～200 ℃ temperature field and the magnetic field intensity orientation field that is 0.5～3T, and the briquetting pressure scope is 2～8ton/cm
2, make high magnetic characteristics, the bonding rare-earth permanent magnet of high resistivity.
5. according to the preparation method of the described a kind of high magnetic characteristics high resistivity rare-earth permanent magnet of claim 4, it is characterized in that: described organic solvent is any or its two or more mixture of toluene, benzene, ethylbenzene, dimethylbenzene, acetone or absolute alcohol.
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| CN102314990A (en) * | 2010-07-08 | 2012-01-11 | 赵立文 | Magnet and preparation method thereof |
| CN102360918A (en) * | 2011-08-17 | 2012-02-22 | 华南理工大学 | Adhesive composite magnet and preparation method thereof |
| CN102945747B (en) * | 2012-10-11 | 2015-07-29 | 厦门钨业股份有限公司 | A kind of manufacture method adopting temperature controlled sintered Nd-Fe-B based magnet |
| CN105469918A (en) * | 2015-12-30 | 2016-04-06 | 江苏大学 | High-resistivity composite permanent magnet and preparation method thereof |
| CN105978175A (en) * | 2016-06-24 | 2016-09-28 | 无锡新大力电机有限公司 | Permanent magnet material of new energy automobile motor |
| CN106077675A (en) * | 2016-06-27 | 2016-11-09 | 无锡新大力电机有限公司 | A kind of preparation method of holmium ferrum nitrogen rare earth permanent-magnet powder |
| CN106952703B (en) * | 2017-03-23 | 2018-12-14 | 南通龙磁电子有限公司 | A kind of high temperature resistant high magnetic characteristics permanent-magnet material |
| CN110098026A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of preparation method of rare-earth permanent magnet |
| CN113130199B (en) * | 2021-04-20 | 2022-11-11 | 中国计量大学 | High-resistivity sintered samarium-cobalt magnet and preparation method thereof |
| CN113223799B (en) * | 2021-05-11 | 2022-03-22 | 宁波市镇海兴强磁性材料有限公司 | Neodymium-iron-boron strip and pulse magnetizing process thereof |
| CN114456540B (en) * | 2022-01-14 | 2023-08-04 | 滁州杰事杰新材料有限公司 | Melamine formaldehyde resin composite material and preparation method thereof |
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