A kind of preparation method of high temperature resistant high magnetic characteristics permanent-magnet material
Technical field
The present invention relates to a kind of field of rare-earth permanent magnetic technology, especially a kind of high temperature resistant high magnetic characteristics permanent-magnet material
Preparation method.
Background technique
The advantages of ndfeb magnet is cost performance height, has good mechanical property;It is disadvantageous in that Curie point is low,
Temperature characterisitic is poor, and is easy to dusting corrosion, it is necessary to by adjusting its chemical component and surface treatment method be taken to be allowed to be changed
Into can be only achieved the requirement of practical application.
Neodymium iron boron magnetic body is divided into slug type and two kinds of binding type according to production method difference.Compared with sintered permanent magnet, glue
Connect magnet with cost performance high, special-shaped magnet convenient formation, machining accuracy height, good toughness, magnetic deviation is small and is easy to minimize
Many advantages, such as, these features have conformed exactly to the developing direction of electronic information complete product " light, thin, short, small ", therefore are bonded
Magnet is widely used in the fields such as computer, mobile communication, advanced audio, small and special electric machine, sensor and magneto-electric instrument and meter.
With the continuous expansion of rare-earth magnet application range, such as starting motor of automobile, Motor product and integrated CO-ROM, hard disk master
Spindle motor HDD, other micro- special direct current generator and automation instrument etc. fields are widely used to Agglutinate neodymium-iron-boron range of needs
Expansion, how to improve the temperature tolerance of Sintered NdFeB magnet is a kind of new challenge to its market application range is expanded.
In the prior art, Chinese invention patent CN101740193B, it is entitled:A kind of high magnetic characteristics high resistivity
It is referred in the patent of rare-earth permanent magnet and preparation method thereof from high-performance magnetic powder surface insulation processing technique and magnet temperature and pressure
Oriented moulding technology is started with, and does not add insulation additive, has studied magnetic powder surface coupling process, is resin dedicated with coupling magnetic powder
Hybrid technique, magnet temperature and pressure oriented moulding technique etc., solve magnetic powder with it is resin dedicated it is Nian Jie loosely, it is resin dedicated in magnetic powder table
Magnet magnetic property improves a series of problems, such as limited after bread covers imperfect, resin dedicated easy to reunite during processing, molding,
In terms of its result, electrical insulation capability is obviously improved really, but high temperature resistance is unsatisfactory, how to develop high temperature resistant
Permanent-magnet material becomes development trend.
Summary of the invention
Technical problem:Technical problem to be solved by the invention is to provide a kind of systems of high temperature resistant high magnetic characteristics permanent-magnet material
Preparation Method, the preparation method pass through magnetic powder surface coupling process, the resin dedicated hybrid technique with coupling bonded magnetic powder, magnet temperature
The Technology Ways such as pressure oriented moulding technology obtain a kind of high temperature resistant high magnetic characteristics permanent-magnet material.
Technical solution:In order to realize the purpose for solving above-mentioned technical problem, present invention employs following technical solutions:
The preparation method of high temperature resistant high magnetic characteristics permanent-magnet material provided by the invention, specific preparation step are:
1) by the Nd of 100 parts by weight2Fe14The graphene oxide powder of B magnetic powder and 0.2~3 parts by weight is stirred mixing
Uniformly it is configured to mixing magnetic powder;The titanate coupling agent of 0.1~5 parts by weight is mixed with the organic solvent of 20~50 parts by weight again
After be added to mixing magnetic powder in, then the ferrocene magnetic powder of mixing magnetic powder and 0.1~0.3 parts by weight after coupling processing is mixed
It closes, it is dry, it is dried in vacuo and is granulated after finally mixing the mixing magnetic powder after drying with 1~10 parts by weight of bisphenol A epoxy resin,
Gained mixing magnetic powder should can pass through 100~400 meshes;
2) it is in the temperature field that setting thermostat temperature is 20~200 DEG C and magnetic field strength by the resulting mixing magnetic powder of step 1
10~30min of molding is carried out under the combinational environment of the orientation field of 0.5~3T, briquetting pressure range is 2~8ton/cm2, it is made resistance to
High temperature high magnetic characteristics permanent-magnet material.
Preferably, the Nd2Fe14B granularity of magnet powder be 20~200 μm and performance requirement be iHc >=400KA/m, Br >=
0.65T、BHmax≥120KJ/m3。
Preferably, the organic solvent be toluene, benzene, ethylbenzene, dimethylbenzene, acetone or absolute alcohol any or
Its two or more mixture.
Preferably, carbon content is 300~2500ppm in high temperature resistant high magnetic characteristics permanent-magnet material obtained.
Preferably, the Nd2Fe14100 parts of B magnetic powder, 0.3 part of ferrocene magnetic powder, 3 parts of titanate coupling agent, bisphenol-A epoxy
8 parts and 2.6 parts of graphene oxide powder of resin.
Preferably, the granularity of the graphene oxide powder is 40~60 μm.
Beneficial effect:By using above-mentioned technical proposal, the present invention compared with the magnet obtained under the conditions of the prior art,
Beneficial effect is:
1. the preparation method of high temperature resistant high magnetic characteristics permanent-magnet material provided by the invention is high to introduce coupling agent, metallocene
Molecule ferromagnet, epoxy resin surface insulationization processing NdFeB- graphene mixing magnetic powder for, institute's pressing magnetic body compared to shows
There is bonding NdFeB magnet magnetic property in technology to be obviously improved.
2. the collocation of element of the Optimization of preparation of high temperature resistant high magnetic characteristics permanent-magnet material provided by the invention, passes through idol
The techniques such as connection, mixing, post-processing make magnetic powder surface insulation performance be improved significantly, then the modified magnetic powder in surface is existed again
It is formed under the combinational environment of temperature field and orientation field, improves the bad disadvantage of Agglutinate neodymium-iron-boron material temperature tolerance, expand
Can the Agglutinate neodymium-iron-boron scope of application, Agglutinate neodymium-iron-boron can be made up and use the low disadvantage of temperature.
3. the preparation method of high temperature resistant high magnetic characteristics permanent-magnet material provided by the invention during mixing magnetic powder by adding
Add graphene oxide powder, since graphene oxide powder disperse is in the Grain-Boundary Phase of neodymium iron boron magnetic body, and with tetragonal structure
Structure exists, and effectively improves the oxygen content distribution of magnet, therefore can rationally control crystallite dimension and make magnet full densification,
Effectively crystal grain can be inhibited to grow up, improve Hcj and have obvious effect to grain structure structure is improved.Improve Agglutinate neodymium-iron-boron
The bad disadvantage of material temperature tolerance expands the Agglutinate neodymium-iron-boron scope of application.
4. the preparation method of high temperature resistant high magnetic characteristics permanent-magnet material provided by the invention, which passes through, improves ingredient and technical process,
Epoxy resin bonded permanent magnet is replaced with metallocene macromolecule ferromagnet, makes in bonded permanent magnet magnetic between NdFeB magnetic powder particle
Field structure state changes, and substantially increases the magnetic property of magnet under high temperature, and can effectively reduce magnet weightlessness, improves
The corrosion resistance of magnet.
5. the present invention assesses Agglutinate neodymium-iron-boron temperature tolerance as a result, the prior art is made to pass through conjunction by practical technique and method
The technological factors such as optimisation technique technique, component prescription are managed, Agglutinate neodymium-iron-boron material is improved and obtains temperature tolerance.
6. high temperature resistant high magnetic characteristics permanent-magnet material obtained has light-weight, high mechanical properties, resistance to by the method for the invention
Burn into is anti-aging, advantage resistant to high temperature, can use for a long time in high-temperature service, can significantly extend product service life, subtract
The number of component is replaced less.
Specific embodiment
The present invention is further described combined with specific embodiments below:
Titanate coupling agent as used in the following examples is that dawn chemical industry in Nanjing is produced, during bisphenol A epoxide resin is
The 7th 25 research institute of company of Shipbuilding Industry Corporation of state produces 725-2-A bisphenol A epoxide resin, and graphene oxide powder uses
The preparation of Hummers method.
Embodiment 1
(1) magnetic powder surface is coupled:By the Nd of 100 parts by weight2Fe14The graphene oxide powder of B magnetic powder and 0.2 parts by weight into
Row stirring and mixing is uniformly configured to mixing magnetic powder;Again by the diformazan of 0.1 parts by weight titanate coupling agent NDZ401 and 30 parts by weight
Benzene organic solvent is added in the magnetic powder of 100.2 parts by weight, will be upper by the high shear agitation 0.5h of 2000 revs/min of speed
It states solution to be uniformly mixed, and by supersonic oscillations 0.5h magnetic powder is sufficiently mixed with coupling agent, then by mixture side
Side heating is stirred, until solvent volatilization finishes, it is stand-by by being ground after the drying of modified mixing magnetic powder;
(2) then modified mixing magnetic powder will be mixed with the ferrocene magnetic powder of 0.1 parts by weight, is dried, then by bisphenol-A
The mixed liquor of 1 parts by weight of epoxy resin and acetone is added in the mixing magnetic powder after drying, under 2000 revs/min of mixing speed
Above-mentioned mixed liquor is uniformly mixed by stirring 0.5h, and so that magnetic powder is sufficiently mixed with resin by supersonic oscillations 0.5h, then
Mixture is heated while stirring, until solvent volatilization finishes, will be ground after the drying of modified mixing magnetic powder, it is mixed after grinding
Conjunction magnetic powder, which should lead to, to be sieved with 100 mesh sieve;
(3) complex loop for the orientation field for being 0.5T in 20 DEG C of temperature fields and magnetic field strength by the modified mixing magnetic powder in surface
Molding 30min, briquetting pressure 3ton/cm are carried out under border2, obtain high temperature resistant high magnetic characteristics permanent-magnet material.
Obtained high temperature resistant high magnetic characteristics permanent-magnet material, resistivity are 1.3 × 10-4Ω m, in magnetic field strength 0.5T
When, being in the 1h temperature rise off field of 50KHz high-frequency alternating is 75 DEG C.
Embodiment 2
(1) magnetic powder surface is coupled:By the Nd of 100 parts by weight2Fe14The graphene oxide powder of B magnetic powder and 3 parts by weight carries out
Stirring and mixing is uniformly configured to mixing magnetic powder, and the titanate coupling agent NDZ401 of 2 parts by weight and the alcohol of 35 parts by weight are added
Into the mixing magnetic powder of 103 parts by weight, above-mentioned solution is uniformly mixed by the high shear agitation 1h of 500 revs/min of speed,
And by supersonic oscillations 1h mixing magnetic powder is sufficiently mixed with coupling agent, then mixture is heated while stirring, directly
It is finished to solvent volatilization, it is stand-by by being ground after the drying of modified mixing magnetic powder;(2) then by modified mixing magnetic powder and
The ferrocene magnetic powders of 0.3 parts by weight mixes, dry, then by the mixing of bisphenol A epoxide resin 6.5 parts by weight and organic solvent-acetone
Liquid is added in the mixing magnetic powder after the coupling of surface, and 1h is stirred under 500~2000 revs/min of mixing speed by above-mentioned mixed liquor
It is uniformly mixed, and so that mixing magnetic powder is sufficiently mixed with resin by supersonic oscillations 1h, then add mixture while stirring
Heat will be ground, the magnetic powder after grinding should pass through 250 meshes until solvent volatilization finishes after the drying of modified mixing magnetic powder;
(3) the modified mixing magnetic powder in surface is carried out under the combinational environment for the orientation field for being 2T in 80 DEG C of temperature fields and magnetic field strength
Form 15min, briquetting pressure 5ton/cm2, obtain high temperature resistant high magnetic characteristics permanent-magnet material.
Obtained high temperature resistant high magnetic characteristics permanent-magnet material, resistivity are 1.5 × 10-4Ω m, in magnetic field strength 0.5T
When, being in the 1h temperature rise off field of 50KHz high-frequency alternating is 73 DEG C.
Embodiment 3
(1) magnetic powder surface is coupled:By the Nd of 100 parts by weight2Fe14The graphene oxide powder of B magnetic powder and 2 parts by weight carries out
Stirring and mixing is uniformly configured to mixing magnetic powder, and the dimethylbenzene of the titanate coupling agent NDZ401 of 5 parts by weight and 30 parts by weight are added
Enter into the mixing magnetic powder of 102 parts by weight, is mixed above-mentioned solution by the high shear agitation 1.5h of 800 revs/min of speed
Uniformly, and by supersonic oscillations 1.5h mixing magnetic powder is sufficiently mixed with coupling agent, then while stirring by mixture
Heating, until solvent volatilization finishes, it is stand-by by being ground after the drying of modified mixing magnetic powder;(2) then by modified mixing
Magnetic powder is mixed with the ferrocene magnetic powder of 0.2 parts by weight, dry, then the mixed liquor of bisphenol A epoxide resin and organic solvent-acetone adds
Enter to surface in the mixing magnetic powder after being coupled, 1.5h is stirred under 500~2000 revs/min of mixing speed and mixes above-mentioned mixed liquor
It closes uniformly, and so that magnetic powder is sufficiently mixed with resin by supersonic oscillations 1.5h, then heat mixture while stirring, directly
It finishes, will be ground after the drying of modified mixing magnetic powder, the magnetic powder after grinding should pass through 400 meshes to solvent volatilization;(3) by table
The modified mixing magnetic powder in face is formed under the combinational environment for the orientation field for being 3T in 200 DEG C of temperature fields and magnetic field strength
10min, briquetting pressure 8ton/cm2, obtain high temperature resistant high magnetic characteristics permanent-magnet material.
Obtained high temperature resistant high magnetic characteristics permanent-magnet material, resistivity are 1.8 × 10-3Ω m, in magnetic field strength 0.5T
When, being in the 1h temperature rise off field of 50KHz high-frequency alternating is 71 DEG C.
The high temperature resistant high magnetic characteristics permanent-magnet material as made from the method for the present invention is inventors tested a larged in embodiment 1 a series of
At a temperature of magnetic property, see Table 1 for details;
Table 1 implements magnetic property of the 1 resulting NdFeB Bonded Magnets under series of temperature
Temperature |
Residual magnetic flux density mT |
Coercivity kA/m |
Intrinsic coercivity kA/m |
Magnetic energy product kJ/m3 |
120 |
656 |
406 |
801 |
120 |
150 |
654 |
394 |
793 |
116 |
200 |
651 |
391 |
786 |
112 |
280 |
646 |
384 |
780 |
108 |
360 |
641 |
379 |
778 |
106 |
450 |
635 |
376 |
770 |
103 |
From the point of view of the result of table 1, for the resulting high temperature resistant high magnetic characteristics permanent-magnet material of embodiment 1 at 450 DEG C, magnet can also
Reach practical horizontal, magnet can also maintain higher magnetic property.At high temperature compared with the Agglutinate neodymium-iron-boron magnet magnetic of same class
Performance can all be greatly improved, and can reach the effect for maintaining high magnetic characteristics in the event of high temperatures.