CN104599832A - Flexible rare earth magnet with high surface magnetism and manufacturing method of flexible rare earth magnet - Google Patents
Flexible rare earth magnet with high surface magnetism and manufacturing method of flexible rare earth magnet Download PDFInfo
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- CN104599832A CN104599832A CN201510023610.8A CN201510023610A CN104599832A CN 104599832 A CN104599832 A CN 104599832A CN 201510023610 A CN201510023610 A CN 201510023610A CN 104599832 A CN104599832 A CN 104599832A
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Abstract
The invention discloses a flexible rare earth magnet with high surface magnetism and a manufacturing method of the flexible rare earth magnet. The flexible rare earth magnet comprises the following components: 92wt%-97wt% of NdFeB alloy magnetic powder, 2wt%-3wt% of a binding agent and 1wt%-5wt% of a processing auxiliary agent, wherein the NdFeB alloy magnetic powder contains Tb element; the binding agent is F48 thermosetting phenolic aldehyde epoxy resin; the processing auxiliary agent comprises a coupling agent and a curing agent; the coupling agent is titanate; the curing agent is a dicyandiamide curing agent. The production method of the flexible rare earth magnet with the high surface magnetism, disclosed by the invention, has a simple process and low cost; the produced flexible rare earth magnet has a good magnetic performance and has very high surface magnetism; large-scale automatic production can be realized and the economic benefits are high.
Description
Technical field
The present invention relates to technical field of magnetic materials, particularly a kind of flexible rare-earth magnet and manufacture method thereof with high table magnetic.
Background technology
Permanent magnetic material is an important branch of electronic material, and its performance height directly reflects the development level of a National Electrical material.Along with high performance permanent magnetic materials is in the extensive use of the industries such as computer, automobile, space flight, office equipment, household electrical appliances and medical treatment, its market demand cumulative year after year.
At present, the high performance permanent magnetic materials on market is rare-earth bond magnet mostly; So-called rare-earth bond magnet refers to and rare earth permanent-magnet powder is mixed into a certain proportion of binding agent and a kind of magnet made by certain processing technology, and its final form can be divided into rigidity rare-earth bond magnet and flexible rare-earth cementing magnet.Binding rare earth permanent magnet is compared with sintered magnet, and have that process costs is low, dimensional accuracy is high, be easy to shaping complicated shape device, be easy to realize the advantages such as mass automatic production, development in recent years is rapid.
Existing flexible rare-earth cementing magnet magnetic property is poor, and table magnetic is not high, can not meet the demand of application.Prior art adopts the method improving magnetic loading to improve the performance of magnet, then this magnet can lose pliability gradually, and serious meeting causes magnet cannot be shaping, does not reach the requirement of actual use.Prior art also by increasing typed pressure, makes magnet density improve, and then the method for the table magnetic of raising magnet, but pressure increases, and the degree that the magnetic of sheet is destroyed also increases, and domain wall sustains damage, and wall energy declines, thus causes the table magnetic of magnet to decline.
For this reason, need to develop a kind of new flexible rare-earth magnet with high table magnetic and manufacture method thereof.
Summary of the invention
The technical problem that the invention solves is: rare earth permanent-magnetic material magnetic property of the prior art is poor, the low and complicated process of preparation of table magnetic.For this reason, the present invention proposes a kind of flexible rare-earth magnet and the manufacture method thereof with high table magnetic, the process aspect selected, prepare of its composition from alloy, binding agent and curing agent improves, and can eliminate one or more problems that restriction and defect due to prior art cause fully.
Additional advantages of the present invention, object and characteristic, a part will be elucidated in the following description, and another part for those of ordinary skill in the art by being obvious to the investigation of explanation below or acquiring from enforcement of the present invention.Can realize and obtain the object of the invention and advantage by the structure pointed out especially in the specification of word and claims and accompanying drawing.
The invention provides a kind of manufacture method with the flexible rare-earth magnet of high table magnetic, it is characterized in that, described method specifically comprises the following steps:
Step 1, manufacture the NdFeB alloy containing Tb element, the percentage by weight of described Tb element in NdFeB alloy is 1%, and step 1 specifically comprises:
According to the proportional arrangement raw material of the percentage by weight 1: 3.5: 75.5: 20 of Tb, Nd, Fe, B element in the alloy of preparation, the raw material configured is put into vacuum arc furnace ignition, stop bleeding when being evacuated down to 3 × 10-3Pa, be filled with an atmospheric argon gas to clean body of heater, after cleaning, continue to be evacuated down to 3 × 10
-3after Pa, be again filled with an atmospheric argon shield, then start molten alloy;
Step 2, gets rid of in band machine in vacuum and alloy prepared by step 1 is got rid of into amorphous thin ribbon;
Step 3, carries out Annealing Crystallization process to amorphous thin ribbon; Step 3 specifically comprises:
The alloy thin band step 2 prepared loads in the cylinder that molybdenum sheet makes, then puts into quartz ampoule and be evacuated down to 3 × 10
-3pa, then smelting furnace quartz ampoule being put into 540 DEG C-570 DEG C, after keeping 10 minutes, take out quartz ampoule from smelting furnace and put into mixture of ice and water rapidly in smelting furnace;
Step 4, obtains magnetic by the strip after annealed Crystallizing treatment through broken, grinding;
Step 5, use coupling agent to carry out surface treatment to magnetic, described coupling agent is titante coupling agent; Step 5 specifically comprises: the titanate esters toluene solution being 0.1wt% by magnetic and concentration mixes, and stirs half an hour with magnetic stirring apparatus with 400 revs/min at 100 DEG C.
Step 6, by the magnetic after surface treatment and curing agent and binding agent evenly mixing, described curing agent is dicyandiamide, and described binding agent is F48 thermosetting phenolic resin; Step 6 specifically comprises:
First dicyandiamide is joined in solvent dimethylformamide, be heated to 120 DEG C, make it to dissolve completely, make dicyandiamide cure agent solution, and magnetic is joined in the dicyandiamide cure agent solution made, fully stir, dry, make curing agent be coated on magnetic surface; Secondly, then the magnetic powder particle after drying is joined in F48 thermosetting phenolic resin binding agent, fully stir, dry, make magnetic Surface coating F48 binding agent;
Step 7, in the alignment magnetic field of 3T, shaping by rubber die static pressure machine;
Step 8, to be cured and to magnetize process to the magnet after compressing.
Preferably, in the process of the melting of step 1, open magnetic control power supply and carry out magnetic stirring.
Preferably, the temperature of the smelting furnace in step 3 is 555 DEG C.
Preferably, in step 4, by the method that hydrogen is broken, strip is broken.
Preferably, the method for described grinding is airflow milling or ball milling.
Preferably, in step 7, briquetting pressure is 600-800Mpa.
Preferably, in step 8, curing temperature is 120 DEG C, and curing time is 120 minutes.
Present invention also offers a kind of flexible rare-earth magnet with high table magnetic, the method of described flexible rare-earth magnet according to any one in the claims 1-7 is made, wherein, the component of described flexible rare-earth magnet comprises: NdFeB alloy magnetic powder 92wt%-97wt%, binding agent 2-3wt%, processing aid 1-5wt%, wherein, described NdFeB alloy magnetic powder comprises Tb element, described binding agent is F48 thermosetting phenolic epoxy resin, described processing aid comprises coupling agent and curing agent, and described coupling agent is titanate esters, and described curing agent is dicy-curing agent.
Preferably, containing in the NdFeB alloy of Tb element, the percentage by weight of described Tb element in NdFeB alloy is 1%.
Preferably, described processing aid also comprises lubricant and plasticizer.
The flexible rare-earth magnet generation method technique with high table magnetic provided by the invention is simple, and cost is low, and the flexible rare-earth magnet magnetic property produced is good, has very high table magnetic, can realize large-scale automated production, high financial profit.
Accompanying drawing explanation
Fig. 1 be according to the embodiment of the present invention, the flow chart of the production method of the flexible rare-earth magnet with high table magnetic.
Embodiment
With reference to the accompanying drawings the present invention is described more fully, exemplary embodiment of the present invention is wherein described.
Inventor is on the basis of actual production in conjunction with a large amount of experimental study work, find that table magnetic and the composition of material, the auxiliary agent of interpolation and the concrete technological process of flexible rare-earth magnet have relation closely, for this reason, the present invention improves emphatically the table magnetic of flexible rare-earth magnet by above-mentioned several aspect.
The object of the invention is to be achieved through the following technical solutions:
A kind of manufacture method with the flexible rare-earth magnet of high table magnetic of the embodiment of the present invention, described method specifically comprises the following steps:
Step 1, manufacture the NdFeB alloy containing Tb element, wherein, the percentage by weight of Tb element in NdFeB alloy is 1%.
Step 1 specifically comprises: according to the proportional arrangement raw material of the percentage by weight 1: 3.5: 75.5: 20 of Tb, Nd, Fe, B element in the alloy of preparation, the raw material configured is put into vacuum arc furnace ignition, stop bleeding when being evacuated down to 3 × 10-3Pa, be filled with an atmospheric argon gas to clean body of heater, after cleaning, continue to be evacuated down to 3 × 10
-3after Pa, be again filled with an atmospheric argon shield, then start molten alloy.Preferably, in order to make alloy homogenizing, in the process of melting, opening magnetic control power supply and carrying out magnetic stirring.
Add the micro-structural that trace element can improve flexible rare-earth magnet, improve magnetic property.The anisotropy energy of rare earth element tb is very high, and a small amount of doping can significantly improve the magnetic property of magnet, therefore the flexible rare-earth magnet of the height table magnetic that can make.But when the doping of Tb exceedes its solid-liquid degree limit in NdFeB, it just likely forms cenotype and is gathered in crystal boundary or phase boundary place, and this will make the magnetic property of alloy significantly decline.Therefore, the doping of Tb is not arbitrary value, must be controlled in certain scope, the present inventor is through many experiments, and find when the doping percentage by weight accounted in NdFeB alloy of Tb is 1%, the hole in magnet is less, even structure, the magnetic property of magnet is the highest.Therefore, in order to obtain the flexible rare-earth magnet of high table magnetic, the percentage by weight of Tb element in NdFeB alloy is restricted to 1% by the present invention.
Step 2, gets rid of in band machine in vacuum and alloy prepared by step 1 is got rid of into amorphous thin ribbon;
Step 3, carries out Annealing Crystallization process to amorphous thin ribbon;
Concrete, alloy thin band step 2 prepared loads in the cylinder that molybdenum sheet makes, then puts into quartz ampoule and be evacuated down to 3 × 10
-3pa, then smelting furnace quartz ampoule being put into 540 DEG C-570 DEG C, after keeping 10 minutes, take out quartz ampoule from smelting furnace and put into mixture of ice and water rapidly in smelting furnace.
Prove by experiment, by arranging the temperature of suitable smelting furnace and the retention time in smelting furnace, can significantly improve the magnetic property of magnet, preferably, the temperature of smelting furnace is set to 555 DEG C by the present invention, and the magnetic property of the magnet now obtained is best.
Step 4, obtains magnetic by the strip after annealed Crystallizing treatment through broken, grinding;
Preferably, the present invention is broken by strip, concrete by the method that hydrogen is broken, to prepare strip loads in hydrogen crushing furnace, after vacuumizing, be filled with high-purity hydrogen, under 0.02-1.2Mpa hydrogen pressure, inhale hydrogen 0.5-5h, hear the cracker of alloy, can detect that the temperature of container is in continuous rising simultaneously, this forms hydride volumetric expansion after RE permanent magnetic alloy inhales hydrogen and bursts, then dehydrogenase 12-10h at 450-650 DEG C, obtains flour.
In the present invention, the flour after described grinding is broken by hydrogen is broken further, thus completes the pulverizing process of alloy.The method of described grinding is airflow milling or ball milling.The present invention preferably adopts airflow milling.The method of airflow milling powder is conventionally known to one of skill in the art, and powder particle is accelerated to supersonic speed for utilizing air-flow by it, makes it mutually head-on collision and broken.Along with the increase of airflow milling granularity of magnet powder, magnet bending strength obviously reduces, and when granularity reduces, the magnetic property of magnet just weakens, and considers, and the average grain diameter of magnetic of the present invention is 3-4 μm.
Step 5, use coupling agent to carry out surface treatment to magnetic, described coupling agent is titante coupling agent;
Coupling agent is in the preparation technology of magnet must be indispensable, therefore magnetic is hydrophilic, and general binding agent is oil loving, the effect of coupling agent is linked together at magnetic and binding agent, thus enhance the affinity of magnetic and interlaminar resin, improve the overlay capacity of magnetic surface resin, thus improve magnetic property.In order to make coupling agent be uniformly dispersed in magnetic, the present invention is by the organic solution of coupling agent and magnetic mixing, and as preferably, the present invention selects titanate coupling agent, selects toluene solution that dissolubility is good as solvent.
Prior art generally uses silane coupling agent, but reacting to each other between the bodies not only deposited by silane coupling agent, but also polymolecular layer can be formed at matrix surface, affect the magnetic property of magnet, and the treatment effect of titante coupling agent to magnetic is better than silane coupling agent, therefore, the coupling agent that the present invention adopts is titante coupling agent.
Step 5 specifically comprises: the titanate esters toluene solution being 0.1wt% by magnetic and concentration mixes, and stirs half an hour with magnetic stirring apparatus with 400 revs/min at 100 DEG C.
Step 6, by the magnetic after surface treatment and curing agent and binding agent evenly mixing, described curing agent is dicyandiamide, and described binding agent is F48 thermosetting phenolic resin;
The density of magnet is higher, and the table magnetic of magnet is also higher.But when similar density, magnet performance difference to some extent prepared by different binding agent, this is because magnet performance is except being determined by magnet density, is also subject to the impact of the degree of injury of magnetic in forming process densification process.Such as, the F48 thermosetting phenolic resin bonded permanent magnet obtained under 1000Mpa pressure is suitable with E-20 epoxy bond magnet density, but because the effect of E20 resin lubrication is obvious not, the densification of magnet will be leaned on the distortion of magnetic and crackedly to be realized, and the viscosity of F48 resin is large, be evenly distributed between magnetic and magnetic, and the lubrication in pressing process is obvious, the densification of magnet can rely on the distortion of binding agent to drive magnetic flowing, and in magnet densification process, magnetic is cracked not serious.
In addition, the degree that in solidification process, magnetic is oxidized also has impact to the performance of magnet.Because bonded permanent magnet is suppressed by the magnetic of surperficial wrapped resin layer to form; binding agent has good protective effect to magnetic; if but to prepare the parcel of binding agent to magnet in blending process uneven; or in pressing process, cause parcel uneven; then when solidifying; magnetic partial oxidation will be made, cause magnetic property to decline.
The F48 thermosetting phenolic resin lubrication that the present invention selects is strong, uniform to magnetic parcel, effectively can improve the magnetic property of magnet.In order to realize the automatic mold filling die mould of automated production, require that batching has good popularity, the F48 resin that the present invention adopts is solid-state or semi-solid at normal temperatures, is convenient to production operation.
In addition, can there is the chemical reactions such as solidification along with the change of time in curing agent, makes the chemistry of batching, physical and mechanical property changes, and then affect compressing process, cause magnet density to decline, and magnetic damage aggravation, finally causes the table magnetic of magnet to decline.For this reason, curing agent of the present invention adopts dicyandiamide class curing agent, dicyandiamide class curing agent has latency, the magnetic property of magnet can be kept substantially constant, but due to dicy-curing agent crystallinity quite by force and be not easily dissolved in epoxy resin, and when preparing NdFeB Bonded Magnets, binding agent is needed to be coated on magnetic surface, curing agent exists the uniformity of binding agent and coated unfavorable with particle, for this reason, the present invention adopts two step cladding process, namely, step 6 specifically comprises: first join in solvent dimethylformamide by dicyandiamide, be heated to 120 DEG C, make it to dissolve completely, make dicyandiamide cure agent solution, and magnetic is joined in the dicyandiamide cure agent solution made, abundant stirring, dry, curing agent is made to be coated on magnetic surface, secondly, again the magnetic powder particle after oven dry is joined in F48 thermosetting phenolic resin binding agent, abundant stirring, dry, make magnetic Surface coating F48 binding agent, like this, curing agent and F48 epoxy resin just form uniform two thin layers on magnetic surface, make binding agent have good solidification effect, be conducive to the table magnetic improving the magnet made.
Step 7, in the alignment magnetic field of 3T, shaping by rubber die static pressure machine;
The present invention, by applying alignment magnetic field in the process of compacting, can improve the degree of orientation of magnetic, and then improves the magnetic property of magnet, and the table magnetic of magnet is improved; In addition, the present invention is undertaken shaping by rubber die static pressure machine, compared with the magnet that existing briquetting process is obtained, can improve the table magnetic of magnet.Preferably, briquetting pressure is 600-800Mpa.
Step 8, to be cured and to magnetize process to the magnet after compressing;
Curing time and the table magnetic of curing temperature to magnet also have a great impact, and in order to make the table magnetic of magnet maximum, through many experiments, the curing temperature chosen is 120 DEG C, and curing time is 120 minutes.
The foregoing describe the manufacture method with the flexible rare-earth magnet of high table magnetic proposed by the invention, by the improvement to the composition of material, the auxiliary agent of interpolation and concrete technological process, effectively can improve the table magnetic of obtained flexible rare-earth magnet, in addition, lubricant and plasticizer can also be added, to improve the magnetic property of magnet further in the process of manufacturing flexible rare earth magnet.
Present invention also offers a kind of flexible rare-earth magnet with high table magnetic, the described flexible rare-earth magnet method above-mentioned according to the present invention is made, concrete, the component of described flexible rare-earth magnet comprises: NdFeB alloy magnetic powder 92wt%-97wt%, binding agent 2-3wt%, processing aid 1-5wt%, wherein, described NdFeB alloy magnetic powder comprises Tb element, described binding agent is F48 thermosetting phenolic epoxy resin, described processing aid comprises coupling agent and curing agent, and described coupling agent is titanate esters, and described curing agent is dicy-curing agent.
Preferably, described processing aid also comprises lubricant and plasticizer.
Above content is only preferred embodiment of the present invention, and for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.
Claims (10)
1. have a manufacture method for the flexible rare-earth magnet of high table magnetic, it is characterized in that, described method specifically comprises the following steps:
Step 1, manufacture the NdFeB alloy containing Tb element, the percentage by weight of described Tb element in NdFeB alloy is 1%, and step 1 specifically comprises:
According to the proportional arrangement raw material of the percentage by weight 1: 3.5: 75.5: 20 of Tb, Nd, Fe, B element in the alloy of preparation, the raw material configured is put into vacuum arc furnace ignition, stop bleeding when being evacuated down to 3 × 10-3Pa, be filled with an atmospheric argon gas to clean body of heater, after cleaning, continue to be evacuated down to 3 × 10
-3after Pa, be again filled with an atmospheric argon shield, then start molten alloy;
Step 2, gets rid of in band machine in vacuum and alloy prepared by step 1 is got rid of into amorphous thin ribbon;
Step 3, carries out Annealing Crystallization process to amorphous thin ribbon; Step 3 specifically comprises:
The alloy thin band step 2 prepared loads in the cylinder that molybdenum sheet makes, then puts into quartz ampoule and be evacuated down to 3 × 10
-3pa, then smelting furnace quartz ampoule being put into 540 DEG C-570 DEG C, after keeping 10 minutes, take out quartz ampoule from smelting furnace and put into mixture of ice and water rapidly in smelting furnace;
Step 4, obtains magnetic by the strip after annealed Crystallizing treatment through broken, grinding;
Step 5, use coupling agent to carry out surface treatment to magnetic, described coupling agent is titante coupling agent; Step 5 specifically comprises: the titanate esters toluene solution being 0.1wt% by magnetic and concentration mixes, and stirs half an hour with magnetic stirring apparatus with 400 revs/min at 100 DEG C.
Step 6, by the magnetic after surface treatment and curing agent and binding agent evenly mixing, described curing agent is dicyandiamide, and described binding agent is F48 thermosetting phenolic resin; Step 6 specifically comprises:
First dicyandiamide is joined in solvent dimethylformamide, be heated to 120 DEG C, make it to dissolve completely, make dicyandiamide cure agent solution, and magnetic is joined in the dicyandiamide cure agent solution made, fully stir, dry, make curing agent be coated on magnetic surface; Secondly, then the magnetic powder particle after drying is joined in F48 thermosetting phenolic resin binding agent, fully stir, dry, make magnetic Surface coating F48 binding agent;
Step 7, in the alignment magnetic field of 3T, shaping by rubber die static pressure machine;
Step 8, to be cured and to magnetize process to the magnet after compressing.
2. the manufacture method with the flexible rare-earth magnet of high table magnetic according to claim 1, is characterized in that, in the process of the melting of step 1, open magnetic control power supply and carry out magnetic stirring.
3. the manufacture method with the flexible rare-earth magnet of high table magnetic according to claim 1, it is characterized in that, the temperature of the smelting furnace in step 3 is 555 DEG C.
4. the manufacture method with the flexible rare-earth magnet of high table magnetic according to claim 1, is characterized in that, in step 4, the method broken by hydrogen is broken by strip.
5. the production method of the rare-earth flexible magnetic stripe of high tenacity according to claim 1, is characterized in that, in step 4, the method for described grinding is airflow milling or ball milling.
6. the manufacture method with the flexible rare-earth magnet of high table magnetic according to claim 1, it is characterized in that, in step 7, briquetting pressure is 600-800Mpa.
7. the manufacture method with the flexible rare-earth magnet of high table magnetic according to claim 1, it is characterized in that, in step 8, curing temperature is 120 DEG C, and curing time is 120 minutes.
8. one kind has the flexible rare-earth magnet of high table magnetic, the method of described flexible rare-earth magnet according to any one in the claims 1-7 is made, wherein, the component of described flexible rare-earth magnet comprises: NdFeB alloy magnetic powder 92wt%-97wt%, binding agent 2-3wt%, processing aid 1-5wt%, wherein, described NdFeB alloy magnetic powder comprises Tb element, described binding agent is F48 thermosetting phenolic epoxy resin, described processing aid comprises coupling agent and curing agent, and described coupling agent is titanate esters, and described curing agent is dicy-curing agent.
9. the flexible rare-earth magnet with high table magnetic according to claim 8, it is characterized in that, containing in the NdFeB alloy of Tb element, the percentage by weight of described Tb element in NdFeB alloy is 1%.
10. the flexible rare-earth magnet with high table magnetic according to claim 8, it is characterized in that, described processing aid also comprises lubricant and plasticizer.
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Cited By (1)
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| CN110473684A (en) * | 2019-08-19 | 2019-11-19 | 中国计量大学 | A kind of preparation method of high-coercive force Sintered NdFeB magnet |
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| CN101281811A (en) * | 2007-04-06 | 2008-10-08 | 浙江工业大学 | Method for preparing NdFeB/PPS injection moulding particle material |
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