CN100590758C - Method for preparing powder for bound rare-earth permanent-magnet by quasi-compression method - Google Patents
Method for preparing powder for bound rare-earth permanent-magnet by quasi-compression method Download PDFInfo
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- CN100590758C CN100590758C CN200710045130A CN200710045130A CN100590758C CN 100590758 C CN100590758 C CN 100590758C CN 200710045130 A CN200710045130 A CN 200710045130A CN 200710045130 A CN200710045130 A CN 200710045130A CN 100590758 C CN100590758 C CN 100590758C
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Abstract
The invention provides a method for preparing a powder material for bonding rare earth permanent magnet before compression, which comprises the following steps: (1) mixing permanent magnet powder, non-magnetic metal powder and hot-curing solid binder powder in the presence of protective gases to obtain a mixture; (2) melting the resulting mixture of the step (1) in a mixing machine capable of heating and kneading the mixture by external force; (3) mechanically pulverizing the agglomerate powder after melting; and (4) adding an auxiliary agent into the powder obtained in the step (3) and compressing to make high-density magnets. The inventive method is used to replace the prior quasi-compression melting method using organic solvents to dissolve the binder and has the advantages of strong bonding force between hot-curing epoxy resin and powder material for bonding rare earth permanent magnet, uniform adhesion and no air pollution. Compared with the prior art, the density and property ofthe prepared magnet are increased by 3-5 percent, and the antioxidant property and mechanical strength of the prepared magnet are also improved.
Description
Technical field
The present invention relates to a kind of method for preparing powder for bound rare-earth permanent-magnet by quasi-compression.
Background technology
In the bonding rare earth permanent magnet preparation process, one of key technology is the granulating technique that mixes of terres rares permanent-magnet powder and binding agent, auxiliary agent.
According to the physicochemical characteristics of binding agent, can synthesize two big class---thermosetting adhesive and thermoplastic adhesives.Prilling process also should be differentiated mutually.
At present, mixing of bonding rare earth permanent-magnet powder and thermosetting adhesive, the general wet method that adopts is mixed, promptly binding agent, auxiliary agent evenly are dissolved in organic solvent, evenly mix with the bonding rare earth permanent-magnet powder again, in atmosphere or in the airtight molten device, mix, in the mixed process or after mixing end, allow organic solvent all volatilize (or partially recycled), then the powder after mixing is pulverized.Be shaped and curing for next process.
Adopt above-mentioned wet method to mix and be difficult to be referred to as to call a kind of mixing, more suitable should be a kind of mixing, makes bonding rare earth permanent-magnet powder surface be stained with as thin as a wafer binding agent and auxiliary agent, and the process of mixing stirs, and lacks powder, the compression of mixed with resin body, kneading; If the process of mixing is carried out in atmosphere, will be subjected to the influence of atmospheric temperature, humidity, therefore, the factor of amblent air temperature is brought certain difference to the quality of mixing, and the magnet mechanical property fluctuation of the binding rare earth permanent magnet powder after mixing is bigger.
In the process of mixing, the bonding rare earth permanent-magnet powder is to mix at normal temperatures by the dissolving of binding agent, therefore, bonding between bonding rare earth permanent-magnet powder and the binding agent, main adhesive by the binding agent under mechanical force and the normal temperature, its adhesive may not be in optimum state, the magnet powder after the granulation, technological fluctuation is big in filling mould, compression molding and solidification process, and consistency of product is relatively poor.Therefore, bring undesirable element for the consistency of magnet.
The common organic solvent that adopts, for example acetone, ethylene glycol, butanone ..., these solvents all have certain harmfulness to health, and environment is caused certain pollution.
Describe bonding rare earth permanent magnetism powder composition and preparation method in formerly patent of invention (ZL 9612194.6) " rare earth-like bonded permanent magnet and rare earth magnet composition " of applicant, (ZL 96119267.4) " rare earth-like bonded permanent magnet and rare earth-like bonded permanent magnet composition ", but do not described the method for mixing of permanent-magnet powder and binding agent; Patent of invention (ZL99801184.3) " rare-earth bond magnet composition; the manufacture method of rare-earth bond magnet and rare-earth bond magnet " (being the technology of mixing) at the binding agent thermoplastic resin, write the composition of understanding permanent-magnet powder and binding agent, rare earth-like bonded permanent magnet comprises that with the composition operation the above temperature of softening temperature of binder resin mixes.In the patent description, the adhesive of employing is a thermoplastic resin, in the patent, mix to be preferably under the low state of binder resin viscosity and mix, the temperature of mixing is not given in the temperature upper limit scope and makes the low method of binder resin viscosity all greater than 150 ℃, does not describe the technology of mixing in detail yet.
Patent of invention ZL99107654.0 " R-T-B alloy powder resin compound particle and production method and bonding rare earth magnet ", relate to " mixture of R-T-B alloy powder and thermosetting resin; pack into be furnished with diameter 300 μ m or more the small nozzle hole extrude to form particle ", " mixture is extruded by said when mixing under pressure; by rotating the particle cavetto; with the particle heat treatment of cavetto ", patent characteristic is to pack into to be furnished with diameter 300 μ m or small nozzle more, extrude form with aperture, the loaded condition harshness is not spoken of pressure limit again.Extrude to form particle from the small nozzle hole, need cavetto, also want heat treatment, operation is many, and efficient is low.
Application for a patent for invention number 200410088953.4 " containing cohesive composite permanent magnetic material of neodymium iron nitrogen and preparation method thereof ", binding agent is rubber or haloflex, " will contain the permanent-magnet powder of 10% neodymium iron nitrogen and 0.1～0.8% coupling agent and organic solvent mixing at least and carry out coating processing ... ", " ... send into internal mixer or the machine of beginning to pratise in mix or begin to pratise; after mixing/begin to pratise evenly; mix with the experienced glue machines of two rollers again ", also comprise vulcanisation step.Its patent characteristic be process transplanting will be in the ferrite rubber magnet commonly used to rare earth permanent magnet, use rubber or haloflex be as binding agent, mixes in the internal mixer or the machine of beginning to pratise or begin to pratise.Operation is many, and organic solvent can cause certain pollution to environment.
Application for a patent for invention number 200410052150.3 " a kind of flexible adhesion Nd-Fe-B magnets and manufacture methods thereof ", be will be the rubber-like binding agent handled of modification and neodymium iron boron class magnetic and processing aid mix in proportion, mixed method adopts close experienced method, the method for beginning to pratise, paddling process or the screw rod method of mixing, or the screw rod method mixed method of mixing, complex procedures, process time is long, and all is to be the occasion of binding agent at what thermoplastic elastic body was done.
Patent of invention ZL93108279.X " is used to produce the solid resin coated magnetic and the manufacture method thereof of anisotropic bonded magnet ", " mediate at following anisotropic magnet powder of reduced atmosphere and the solid resin that is dissolved in the solvent; to the mixture pelleting that is produced; form solid resin coated combination magnetic; with the cracking of ball milling cracking mode, make it be separated into the single anisotropic magnetic powder particles that scribbles solid resin with the aluminium ball." patent use solvent, can cause certain pollution to environment, need under reduced atmosphere, carry out, also will be with the cracking of ball milling cracking mode, operation is many, has increased cost.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing powder for bound rare-earth permanent-magnet by quasi-compression, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
(1) permanent-magnet powder, nonmagnetic powder, thermosetting solid binder powder are mixed in protective gas, obtain mixture;
Said protective gas such as nitrogen, argon gas;
(2) with the mixture of step (1) in muller, under 80-125 ℃, 0.1-30MPa condition under mix, make solid binder be in molten condition, make permanent magnetism powder, nonmagnetic powder and solid binder compress mutually, push, mix, make the solid binder coating permanent-magnet powder of fusion and the surface of nonmagnetic powder;
(3) powder after will mixing carries out mechanical crushing, the powder after the pulverizing, and through the powder of mechanical classification screening granularity at 15 μ m-450 μ m, the powder of granularity 〉=450 μ m returns crushing and screening once more;
(4) auxiliary agent is added the powder process body that step (3) obtains, be pressed into magnet in atmosphere, density is 3.5-6.4/cm
3, the maximum magnetic energy product of magnet is (BH)
mBe 3-14MGOe.
In the step (1), the weight percent content of each component is:
1. permanent-magnet powder 45-99%;
2. thermosetting solid binder powder 1～5%;
3. nonmagnetic metal/non-metal powder 0-40%
Auxiliary agent is selected from the zinc stearate powder, and the adding weight of auxiliary agent is 0～1% of permanent-magnet powder, thermosetting solid binder powder and nonmagnetic powder total weight;
Said permanent-magnet powder is the permanent magnetism of terres rares or in the non-terres rares permanent-magnet powder more than one;
The terres rares permanent-magnet powder is meant the magnetic that contains following composition:
With Nd
2Fe
14B is principal phase (R-Fe-B-M) magnetic, and wherein R is Nd or Pr, and R is D
y, Tb etc., M is transition metal Co, Al, Cu, Nb, V, Mo, Cr, Ni;
With Sm-Co
5Or Sm
2Co
17R (R ')-Co-M R-Sm R '-other rare earths M-Fe-Cu for principal phase
With Sm
2Fe
17N
3(R-R ')-Fe-M-N for principal phase
3-8Magnetic, R are that Sm R ' is other
With NdFe
12-xM
xN be principal phase (R-R ')-; M is Co, Al, Cu, Nb, V, Mo, Cr
The permanent magnetism powder of non-terres rares-Al Ni Co magnetic, ferromagnetic oxide powder;
Said nonmagnetic powder is as Al powder, copper powder, zinc powder, stainless steel powder, SiO
2, Al
2O
3
Said thermosetting solid binder powder is selected from the bisphenol-A/powder of F type epoxy resin, the powder of phenol aldehyde type epoxy resin or the powder of o-cresol epoxy resin;
Method of the present invention, do not use the standard of the organic solvent of dissolving binding agent to compress the method for mixing, after the shaping, the density of prepared magnet, performance are than the high 3-5% of other methods of mixing, oxidation resistance is stronger, adhesion between thermosetting epoxy resin and the bonding rare earth permanent magnetism powder is strong, adheres to evenly, and the mechanical strength of magnet improves.
Embodiment
Among the embodiment, if no special instructions, all be weight percentage.Adopt mixing facilities.
Embodiment 1
Powder with terres rares permanent magnetism NdFeB magnetic (containing Pr, Co) and phenol aldehyde type epoxy resin mixes under the protective gas condition of nitrogen gas, forms uniform mixture,
120 ℃ of temperature, that compresses in the equipment of mixing, pushes, mixes under the pressure 8Mpa condition mixes then.Powder after mixing carries out mechanical crushing, the powder after the pulverizing, and at 35 μ m-355 μ m, the powder of granularity 〉=355 μ m returns crushing and screening once more through mechanical classification screening powder granularity;
The accurate compression bonded rare-earth permanent magnet powder of making is suppressed in atmosphere, and pressure is 14 tons/cm
2, the magnet that is pressed into, at 170 ℃, under 60 minutes conditions of cure, its density is 6.4g/cm
3, the maximum magnetic energy product of magnet is (BH)
mBe 14MGOe.
Wherein: permanent-magnet powder is 98%, and thermosetting solid binder powder is 2%.
Embodiment 2
Powder and 40% ferrite powder with terres rares permanent magnetism NdFeB magnetic (containing Pr, Co element), phenol aldehyde type epoxy resin mix under the condition of protective gas argon gas, form uniform mixture,
85 ℃ of temperature, that compresses in the equipment of mixing, pushes, mixes under the pressure 25Mpa condition mixes then.Powder after mixing carries out mechanical crushing, the powder after the pulverizing, and at 35 μ m-355 μ m, the powder of granularity 〉=355 μ m returns crushing and screening once more through mechanical classification screening powder granularity;
The accurate compression bonded rare-earth permanent magnet powder of making adds the zinc stearate powder and suppresses in atmosphere, and pressure is 10 tons/cm
2, the magnet that is pressed into, at 200 ℃, under 5 minutes conditions of cure, its density is 3.5g/cm
3, the maximum magnetic energy product of magnet is (BH)
mBe 3MGOe.
Wherein: permanent-magnet powder is 57%, and the ferrite nonmagnetic powder is 40%, and thermosetting solid binder powder is 3%, and the auxiliary agent that other adds is 1% of permanent-magnet powder, ferrite nonmagnetic powder and a thermosetting solid binder powder total weight.
Embodiment 3
Other are identical with embodiment 1, and wherein: the temperature of mixing is 80 ℃, and pressure is 0.1Mpa, and testing result is substantially the same manner as Example 1.
Embodiment 4
Other are identical with embodiment 2, and wherein: the temperature of mixing is 125 ℃, and pressure is 30Mpa, and testing result is substantially the same manner as Example 2.
Claims (3)
1. a method for preparing powder for bound rare-earth permanent-magnet by quasi-compression is characterized in that, comprises the steps:
(1) permanent-magnet powder, nonmagnetic powder and thermosetting solid binder powder are mixed in protective gas, obtain mixture;
The weight percent content of each component is:
1. permanent-magnet powder 45-99%;
2. thermosetting solid binder powder 1～5%;
3. nonmagnetic metal/non-metal powder 0-40%;
Each above-mentioned percentages of ingredients sum is 100%,
Said permanent-magnet powder is the permanent-magnet powder of terres rares;
(2) with the mixture of step (1) in mixing roll, under 80-125 ℃, mixing under the condition of 0.1-30Mpa;
(3) powder after mixing is carried out mechanical crushing, the powder after the pulverizing is through the powder of mechanical classification screening granularity at 15 μ m-450 μ m;
(4) auxiliary agent is added the powder that step (3) obtains, in atmosphere, be pressed into magnet.
2. method according to claim 1 is characterized in that, said thermosetting solid binder powder is selected from the bisphenol-A/powder of F type epoxy resin, the powder of phenol aldehyde type epoxy resin or the powder of o-cresol epoxy resin.
3. method according to claim 1 is characterized in that, the powder of granularity 〉=450 μ m returns crushing and screening once more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710045130A CN100590758C (en) | 2007-08-22 | 2007-08-22 | Method for preparing powder for bound rare-earth permanent-magnet by quasi-compression method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710045130A CN100590758C (en) | 2007-08-22 | 2007-08-22 | Method for preparing powder for bound rare-earth permanent-magnet by quasi-compression method |
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| Publication Number | Publication Date |
|---|---|
| CN101145418A CN101145418A (en) | 2008-03-19 |
| CN100590758C true CN100590758C (en) | 2010-02-17 |
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|---|---|---|---|
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102568730A (en) * | 2010-12-31 | 2012-07-11 | 上海爱普生磁性器件有限公司 | High mechanical strength bonding neodymium iron boron permanent magnet and preparation method thereof |
| CN103854844B (en) * | 2014-03-19 | 2016-09-07 | 北京科技大学 | A kind of method that the 3D of utilization printing technique prepares complicated shape bonded permanent magnet |
| CN108987011A (en) * | 2017-06-01 | 2018-12-11 | 宜宾金原复合材料有限公司 | Compound bonded permanent magnet |
| CN111566766B (en) * | 2017-12-28 | 2022-11-15 | 昭和电工材料株式会社 | Method for producing rare earth metal bonded magnet and rare earth metal bonded magnet |
| CN108122656B (en) * | 2017-12-31 | 2020-06-19 | 包头市英思特稀磁新材料股份有限公司 | Rare earth permanent magnetic material |
| CN108538560A (en) * | 2018-03-01 | 2018-09-14 | 安徽艾贤磁体器件科技有限公司 | A kind of Agglutinate neodymium-iron-boron magnet and rapid curing preparation method |
| CN111739725B (en) * | 2020-07-10 | 2021-11-09 | 太原科技大学 | Method and equipment for preparing anisotropic bonded magnet |
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Address after: 201807 No. 3210 Chengbei Road, Jiading Industrial Zone, Shanghai, Jiading District Patentee after: SHANGHAI SAN HUAN MAGNETICS CO., LTD. Patentee after: Beijing Zhongke Sanhuan High-Tech Co., Ltd. Address before: 201800 No. 18 Chengbei Road, Shanghai, Jiading District Patentee before: Shanghai Epson Magnetics Co., Ltd. Patentee before: Beijing Zhongke Sanhuan High-Tech Co., Ltd. |