CN102360918A - Adhesive composite magnet and preparation method thereof - Google Patents
Adhesive composite magnet and preparation method thereof Download PDFInfo
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- CN102360918A CN102360918A CN 201110236408 CN201110236408A CN102360918A CN 102360918 A CN102360918 A CN 102360918A CN 201110236408 CN201110236408 CN 201110236408 CN 201110236408 A CN201110236408 A CN 201110236408A CN 102360918 A CN102360918 A CN 102360918A
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Abstract
The invention provides an adhesive composite magnet and a preparation method thereof. The preparation method comprises the following specific steps of: (1), uniformly dispersing magnetic powder, an adhesion agent and a coupling agent by using a dispersing agent, and drying the obtained mixture to obtain a mixed material, wherein the adhesion agent is epoxy resin or phenolic resin, and on the basis of the total weight of the material, the contents of the magnetic powder, the adhesion agent, a curing agent and the coupling agent are respectively 93.0-98.0%, 1.0-6.0%, 0.1-0.4% and 0.1-0.6%; (2), carrying out press molding on the mixed material to obtain a green blank; and (3), cooling the green blank subjected to the press molding to a room temperature along with a furnace, and magnetizing the cooled green blank to obtain the adhesive composite magnet. The adhesive composite magnet has the following advantages that the flowability of the mixed material is good in a molding process; the filling amount of the magnetic powder is high; the adhesive magnet with high density is prepared easily; and furthermore, the preparation method has the advantages of low equipment manufacturing cost, good processability, high yield and the like, and can realize automatic production easily on large scale.
Description
Technical field
The invention belongs to the binding electromagnetic material field; The preparation method who relates to warm flow compaction moulding bonded permanent magnet; And the bonding built-up magnet that uses this method preparation, be particularly useful for the compound of ferrite and NdFeB magnetic powder, equally also be applicable to the compound of magnetics such as SmCo, neodymium iron nitrogen, manganese bismuth.
Background technology
Bonded permanent magnet is compared with sintered magnet; Have that the technology cost is low, dimensional accuracy is high, be easy to moulding complicated shape device, be easy to realize advantages such as mass automatic production; Development in recent years is rapid, so the preparation technology of bonded permanent magnet and performance study have caused people's attention.Bonded permanent magnet mainly is bonded ferrite and Agglutinate neodymium-iron-boron at present, and what occupy bonded permanent magnet market mainly is Agglutinate neodymium-iron-boron.There is temperature stability poor (coercive force temperature coefficient-about (0.45～0.6) %/K), perishable in Agglutinate neodymium-iron-boron, and machine-shaping is prone to shortcoming such as deterioration to be had to be solved.And bonded ferrite is cheap, and coercive force temperature coefficient is about (0.2～0.6) %/K, and temperature stability is better, in electronics, household electrical appliances, machine product, is widely used.Therefore, explore an optimal path that can guarantee that certain performance reduces production costs again in practice and become noticeable research focus.Utilize ferromagnetic oxide powder and neodymium iron boron fast quenching magnetic compound, or the magnetic of low price and the compound of neodymium iron boron fast quenching magnetic not only can obtain the built-up magnet that bonds cheaply, and can fill up the blank on Agglutinate neodymium-iron-boron and the bonded ferrite performance.If satisfying under the prerequisite of user to the magnet performance requirement; In order to save cost and the product of high performance-price ratio to be provided; It is only adopting Agglutinate neodymium-iron-boron/ferrite built-up magnet, but the lower magnetic property of built-up magnet, to a great extent limit its development space.There are two approach can improve the magnetic property of built-up magnet to greatest extent at present; Approach one is exactly under the identical prerequisite of magnetic raw material, to improve the density and the degree of orientation of magnet, mainly realizes that with the increase alignment magnetic field increase of pressure must promote the densification process of magnet through increasing pressure at present; When pressure acquires a certain degree; Two kinds of factors are depended in the raising of magnet magnetic property: the one, and the displacement of powder particle and filling space, the 2nd, stressed generation plastic deformation of powder even fragmentation, compactedness improves can improve magnetic property; The fragmentation of powder then causes the decline of magnet performance; Increase pressure and also can increase the loss of mould and equipment, increase alignment magnetic field and can improve the degree of orientation of magnet, but also increased the complexity of the production cost and the operating procedure of magnet.Approach two is exactly under the prerequisite that guarantees the magnet mechanical property requirements, to reduce the percent by volume of non magnetic phases such as binding agent as far as possible; Binding agent percent by volume as the bonded permanent magnet matrix can not be too low; Binding agent provides the magnet mechanical property as the support skeleton of keeping whole bonded permanent magnet on the one hand, and binding agent can play lubricated effect on the other hand.
" warm flow compaction forming technique " is on the basis of powder compaction, warm compaction molding technology; In conjunction with advantage and a kind of novel powder metallurgical parts near-net-shape technology that puts forward of metallic powder injection moulding process, improved flowability, fillibility and the mouldability of mixed-powder greatly through the content that adds an amount of meal and attritive powder, surfactant or plasticizer and increasing thermoplasticity lubricant.Because mixed-powder becomes the rheid with good fluidity when compacting; The advantage that had both had liquid; Very high viscosity is arranged again; And reduced in the forming process between the powder and the frictional force between powder and the die cavity, make in the pressing process applied pressure can be in powder equably, transmit effectively.Like this, powder can flow to each corner and not crack in pressing process.Thereby can moulding has a part of complex geometric shapes." warm flow compaction forming technique " both overcome the deficiency of prior powder metallurgy aspect the moulding complex geometric shapes, avoided the expensive of metal injection molded technology again, was a new technology that has potentiality, had broad application prospects.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists in the prior art, the preparation method of the Agglutinate neodymium-iron-boron that a kind of cost is cheap than Agglutinate neodymium-iron-boron, thermal stability is better and magnetic property is higher/ferrite built-up magnet is provided.
The object of the invention is realized through following technical proposals:
A kind of preparation method of the built-up magnet that bonds, concrete steps are following:
(1) with dispersant magnetic, binding agent and coupling agent are uniformly dispersed, obtain mixed material after the drying; Said binding agent is epoxy resin or phenolic resinoid; Said magnetic, binding agent, curing agent and coupling agent account for respectively the material total weight 93.0～98.0%, 1.0～6.0%, 0.1～0.4wt.% and 0.1～0.6%;
(2) mixed material is pressed, obtains green part;
(3) green part after the above-mentioned compression moulding is cured processing, cools to room temperature with the furnace, obtain the built-up magnet that bonds after magnetizing.
Preferably, the said magnetic of step (1) is selected from the mixing of any two or more magnetic in MnBi permanent-magnet powder, ferrite permanent-magnet powder and the rare earth permanent-magnet powder; Said epoxy resin is E-20 or E-12 thermosetting epoxy resin; Said phenolic resinoid is a kind of in phenol formaldehyde resin, alkynyl or pi-allyl phenol-formaldehyde resin modified and the modified rubber phenolic resins; Said coupling agent is a silane coupler; Said dispersant is an acetone.
Preferably, said curing agent is maleic anhydride, mellophanic acid dianhydride or benzophenone tetracarboxylic dicarboxylic anhydride.
Preferably, said ferrite permanent-magnet powder is SrFe
12O
19(strontium ferrite) or BaFe
12O
19(barium ferrite) magnetic; Said rare earth permanent-magnet powder is SmCo
5, Sm
2Co
17, Sm
2Fe
17N
xOr R
2Fe
14The B magnetic, wherein, x=0～6, R is neodymium (Nd), dysprosium (Dy) or praseodymium (Pr) rare earth element.
Preferably, said magnetic is that rare earth permanent-magnet powder mixes with the mass ratio of ferrite permanent-magnet powder by 3: 2, and granularity of magnet powder is 45～100 μ m.
Preferably, the step of mixed material is in the step (1): magnetic is joined carry out coupling processing in the dispersant that is dissolved with coupling agent earlier, place the ultrasonic wave dispersion treatment, treat the dispersant volatilization after, coupling agent evenly coats magnetic; Again binding agent and curing agent are dissolved in the dispersant, process numberator height dispersed solids sol solution; Above-mentioned solid gum solution is fully mixed with the magnetic that above-mentioned coupling agent coats, after the drying mixed material is placed high-performance batch mixer batch mixing 12h, the material that obtains mixing.The purpose of wherein said coupling processing is the interface binding power that improves between hydrophilic magnetic and the hydrophobic binding agent, strengthens the affinity between them, makes magnetic can evenly spread in the binding agent and can improve the non-oxidizability of magnetic.Wherein cured is curing agent and binding agent generation chemical reaction at a certain temperature, makes the linear structure of binding agent become three-dimensional-structure, thereby reaches the effect of bonding.
Preferably; What said compression moulding was adopted is the warm flow compaction moulding; Be about to mixed material and on the warm flow compaction moulding press, carry out the warm flow compaction moulding, preferably, the step of said warm flow compaction moulding is homogeneous mixture of material to be put into mould be heated to; Apply the pressure compression moulding of 500～1100MPa, pressurize 10～15min.The heating system of this warm flow compaction moulding press and temperature-controlling system can be controlled at certain steady temperature with mould.Under the effect of heating system; Binding agent in the compound reaches the molten state temperature and becomes molten, and mixed-powder becomes the rheid with good fluidity, has both had the advantage of liquid; Very high viscosity is arranged again; This can reduce in the forming process between the powder and the frictional force between powder and the die cavity, make in the pressing process applied pressure can be in powder equably, transmit effectively, only need apply the bonded permanent magnet that lower pressure just can obtain high-compactness.
Preferably, said cured is 150～200 ℃ of following heat treatment 1～4 hour in vacuum tube furnace.
The present invention compared with prior art has following advantage and effect:
(1) adopts warm flow compaction forming technique preparation bonding built-up magnet; Compared with prior art, can be according to the different choice of binding agent suitable warm flow compaction forming temperature helps the pressing result that reaches better; The good fluidity of mixed material during moulding; The loading of magnetic is high, under the effect of lower pressure, just can obtain the bonded permanent magnet of higher-density, is easy to prepare the high bonding built-up magnet of magnetic property.And the equipment making cost is low, machinability good, rate of finished products is high and be easy to realize advantages such as mass automatic production.
Improved the magnetic property of bonded permanent magnet when (2) advantage of maximum of the present invention is not improve production cost, promptly the magnetic of identical component is through behind the warm flow compaction forming technique of the present invention, and magnetic property is significantly improved.
(3) the present invention is prepared into Agglutinate neodymium-iron-boron/ferrite built-up magnet through neodymium iron boron and the ferritic compound that the warm flow compaction forming technique will mix by a certain percentage; With the ferromagnetic oxide powder cheap, that temperature stability is higher (coercive force temperature coefficient is about (0.2～0.6) %/K) with cost an arm and a leg, the NdFeB magnetic powder of temperature stability poor (coercive force temperature coefficient-about (0.45～0.6) %/K) is compound; Not only can obtain Agglutinate neodymium-iron-boron/ferrite built-up magnet cheaply; Fill up the blank on Agglutinate neodymium-iron-boron and the bonded ferrite performance; And improved the coercive force temperature coefficient of Agglutinate neodymium-iron-boron magnet, can be applicable to the motor of work under the higher temperature.
(4) preparation method adopts " warm flow compaction moulding " new technology to prepare Agglutinate neodymium-iron-boron/ferrite built-up magnet, has both overcome the deficiency of prior powder metallurgy aspect the moulding complex geometric shapes, has avoided the expensive of metal injection molded technology again.Technology is simple, and is with low cost, is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 warm flow compaction moulding Agglutinate neodymium-iron-boron/ferrite built-up magnet manufacturing process flow diagram.
Fig. 2 embodiment 1 is at the magnetic hysteresis loop of 90 ℃ of warm compaction molding Agglutinate neodymium-iron-boron/ferrite built-up magnets.
Fig. 3 comparative example 1 is at the magnetic hysteresis loop of normal temperature compacting Agglutinate neodymium-iron-boron/ferrite built-up magnet.
Fig. 4 comparative example 2 is at the magnetic hysteresis loop of 90 ℃ of warm compaction molding Agglutinate neodymium-iron-boron magnets.
Fig. 5 embodiment 2 is at the magnetic hysteresis loop of 90 ℃ of warm compaction molding Agglutinate neodymium-iron-boron/ferrite built-up magnets.
Fig. 6 comparative example 3 is at the magnetic hysteresis loop of normal temperature compacting Agglutinate neodymium-iron-boron/ferrite built-up magnet.
Fig. 7 comparative example 4 is at the magnetic hysteresis loop of 90 ℃ of warm compaction molding Agglutinate neodymium-iron-boron magnets.
Fig. 8 embodiment 3 is at the magnetic hysteresis loop of 70 ℃ of warm compaction molding Agglutinate neodymium-iron-boron/ferrite built-up magnets.
Fig. 9 comparative example 5 is at the magnetic hysteresis loop of 70 ℃ of warm compaction molding Agglutinate neodymium-iron-boron magnets.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but execution mode of the present invention is not limited thereto.
Embodiment 1:
(1) with the brilliant magneto plumbite type ferrite powder of hexagonal SrFe
12O
19In two hours annealing in process of 900 ℃ of insulations, ferrite particle is reunited after the annealing in process, after grinding and screening, makes its particle size range between 45～100 μ m.
(2) be Nd with nominal composition
11.5Fe
81.1Co
1.9B
5.5Neodymium iron boron fast quenching magnetic through broken, grind, after the screening, make its particle size range between 45～100 μ m.
(3) take by weighing above-mentioned pretreated neodymium iron boron fast quenching magnetic 3g and ferromagnetic oxide powder 2g; Join in the 100mL acetone that is dissolved with 0.026g coupling agent KH550 and carry out coupling processing; Place ultrasonic wave dispersion treatment 30min, treat acetone volatilization after, coupling agent evenly coats magnetic.
(4) epoxy resin E-20 0.143g and curing agent maleic anhydride 0.012g are dissolved in the 50mL acetone dispersant, process numberator height dispersed solids sol solution.
(5) above-mentioned solid gum solution is fully mixed with the magnetic that above-mentioned coupling agent coats, after the drying mixed material is placed high-performance batch mixer batch mixing 12h, the material that obtains mixing.
(6) place the warm compaction molding press to carry out the warm flow compaction moulding the above-mentioned material that mixes, the warm flow compaction temperature is 90 ℃, and moulding pressure is 1100MPa, and pressurize 10min stops heating and remove the pressure of exerting pressure obtaining green part.
(7) with the green part after the above-mentioned compression moulding, in vacuum atmosphere oven, behind 180 ℃ of cured 2h, cool to room temperature with the furnace, obtain high-performance Agglutinate neodymium-iron-boron/ferrite built-up magnet after magnetizing.Manufacturing process flow is seen Fig. 1, and the Agglutinate neodymium-iron-boron that obtains after the moulding/magnetic hysteresis loop of ferrite built-up magnet under the 300K temperature is as shown in Figure 2, and its magnetic property is: B
r=0.39T, H
Cj=451kA/m, (BH)
Max=21.4kJ/m
3, the result lists in table 1.
Be the effect of checking warm flow compaction forming technique, the bonding built-up magnet that reaction mass is passed through normal temperature compression moulding and warm flow compaction moulding preparation carries out performance relatively, sees comparative example 1.
Comparative example 1:
The magnet prescription is with embodiment 1.Agglutinate neodymium-iron-boron/the magnetic hysteresis loop of ferrite built-up magnet under the 300K temperature that often obtains after temperature and pressure system (operating procedure is with embodiment 1, and different is the moulding of the normal temperature pressed) moulding is as shown in Figure 3, and its magnetic property is: B
r=0.36T, H
Cj=443kA/m, (BH)
Max=19.2kJ/m
3, the result lists in table 1.
Variation for the bonding built-up magnet coercive force temperature coefficient among the checking embodiment 1; The magnetic that to reaction mass is neodymium iron boron carries out the Performance Detection comparison through the Agglutinate neodymium-iron-boron magnet of warm flow compaction forming technique preparation and the embodiment 1 Agglutinate neodymium-iron-boron/ferrite built-up magnet through the preparation of warm flow compaction forming technique, sees comparative example 2.
Comparative example 2:
Magnetic is merely the neodymium iron boron quenched powder among the embodiment 1, and quality is 5g, and other each composition proportion and operating procedure are with embodiment 1.The magnetic hysteresis loop of the Agglutinate neodymium-iron-boron magnet that obtains after the moulding under the 300K temperature is as shown in Figure 4, and its magnetic property is: B
r=0.6T, H
Cj=612kA/m, (BH)
Max=54.3kJ/m
3, the result lists in table 1.
The magnetic property of table 1 embodiment 1, comparative example 1 and comparative example 2
Remarks: the computing formula of coercive force temperature coefficient β is following:
Can know from the result of table 1; The warm flow compaction forming technique can be applied in the die press technology for forming well; Use manufacturing approach of the present invention can obtain to have the bonded permanent magnet of good magnetic property and coercive force temperature coefficient, compare the bonding built-up magnet that normal temperature is suppressed, magnetic property has improved 11%.And compare Agglutinate neodymium-iron-boron magnet, coercive force temperature coefficient has then improved 31%.
Embodiment 2:
Step (1), step (2) and step (3) are with embodiment 1.
Step (4) is dissolved in epoxy resin of binder E-12 0.148g and curing agent maleic anhydride 0.008g in the 50mL acetone dispersant, processes numberator height dispersed solids sol solution.
Step (5), step (6) and step (7) are with embodiment 1.
The Agglutinate neodymium-iron-boron that obtains after the moulding/magnetic hysteresis loop of ferrite built-up magnet under the 300K temperature is as shown in Figure 5, and its magnetic property is: B
r=0.4T, H
Cj=556kA/m, (BH)
Max=23.6kJ/m
3, the result lists in table 2.
Comparative example 3:
The magnet prescription is with embodiment 2, and the Agglutinate neodymium-iron-boron/magnetic hysteresis loop of ferrite built-up magnet under the 300K temperature that often obtains after temperature and pressure system (operating procedure is with embodiment 2, and different is the to adopt formed at normal temp) moulding is as shown in Figure 6, and its magnetic property is: B
r=0.37T, H
Cj=553kA/m, (BH)
Max=20.4kJ/m
3, the result lists in table 2.
Comparative example 4:
Magnetic is merely the neodymium iron boron quenched powder among the embodiment 1, and quality is 5g, and other each composition proportion and operating procedure are with embodiment 2.The magnetic hysteresis loop of Agglutinate neodymium-iron-boron magnet after the moulding under the 300K temperature is as shown in Figure 7, and concrete magnetic property is: B
r=0.62T, H
Cj=623kA/m, (BH)
Max=59.4kJ/m
3, the result lists in table 2.
The magnetic property of table 2 embodiment 2, comparative example 3 and comparative example 4
Remarks: the computing formula of coercive force temperature coefficient β is with embodiment 1.
Can know from the result of table 2; Use manufacturing approach of the present invention can obtain to have the bonded permanent magnet of good magnetic property and coercive force temperature coefficient; Compare the bonding built-up magnet of normal temperature compacting preparation; Magnetic property has improved 16%, and compares Agglutinate neodymium-iron-boron magnet, and coercive force temperature coefficient has then improved 11%.
Embodiment 3
The magnet prescription is with embodiment 1, and in the step (6), the warm flow compaction forming temperature is 70 ℃; Other steps are with embodiment 1.The Agglutinate neodymium-iron-boron that obtains after the moulding/magnetic hysteresis loop of ferrite built-up magnet under the 300K temperature is as shown in Figure 8, and its magnetic property is: B
r=0.39T, H
Cj=449kA/m, (BH)
Max=22.5kJ/m
3, the result lists in table 3.
Comparative example 5
Magnetic is merely the neodymium iron boron quenched powder among the embodiment 1, and quality is 5g, and other each composition proportion and operating procedure are with embodiment 3.The magnetic hysteresis loop of the Agglutinate neodymium-iron-boron magnet that obtains after the moulding under the 300K temperature is as shown in Figure 9, and its magnet performance is: B
r=0.6T, H
Cj=611kA/m, (BH)
Max=54.1kJ/m
3, the result lists in table 3.
The magnetic property of table 3 embodiment 3, comparative example 5 and comparative example 1
Remarks: the computing formula of coercive force temperature coefficient β is with embodiment 1.
Can know from the result of table 3; Use manufacturing approach of the present invention can obtain to have the bonded permanent magnet of good magnetic property and coercive force temperature coefficient; Compare the bonding built-up magnet of normal temperature compacting preparation; Magnetic property has improved 17%, and compares Agglutinate neodymium-iron-boron magnet, and coercive force temperature coefficient has then improved 27%.
Claims (10)
1. the preparation method of the built-up magnet that bonds is characterized in that, concrete steps are following:
(1) with dispersant magnetic, binding agent and coupling agent are uniformly dispersed, obtain mixed material after the drying; Said binding agent is epoxy resin or phenolic resinoid; Said magnetic, binding agent, curing agent and coupling agent account for respectively the material total weight 93.0～98.0%, 1.0～6.0%, 0.1～0.4wt.% and 0.1～0.6%;
(2) mixed material is pressed, obtains green part;
(3) green part after the above-mentioned compression moulding is cured processing, cools to room temperature with the furnace, obtain the built-up magnet that bonds after magnetizing.
2. according to the preparation method of the said bonding built-up magnet of claim 1, it is characterized in that the said magnetic of step (1) is selected from the mixing of any two or more magnetic in MnBi permanent-magnet powder, ferrite permanent-magnet powder and the rare earth permanent-magnet powder; Said epoxy resin is E-20 or E-12 thermosetting epoxy resin; Said phenolic resinoid is a kind of in phenol formaldehyde resin, alkynyl or pi-allyl phenol-formaldehyde resin modified and the modified rubber phenolic resins; Said coupling agent is a silane coupler; Said dispersant is an acetone.
3. the preparation method of built-up magnet according to claim 2 is characterized in that, said curing agent is maleic anhydride, mellophanic acid dianhydride or benzophenone tetracarboxylic dicarboxylic anhydride.
4. according to the preparation method of claim 1 or 2 or 3 said bonding built-up magnets, it is characterized in that said ferrite permanent-magnet powder is SrFe
12O
19Or BaFe
12O
19Magnetic; Said rare earth permanent-magnet powder is SmCo
5, Sm
2Co
17, Sm
2Fe
17N
xOr R
2Fe
14The B magnetic, wherein, x=0～6, R is neodymium, dysprosium or praseodymium rare earth element.
5. according to the preparation method of the said bonding built-up magnet of claim 4, it is characterized in that said magnetic is that rare earth permanent-magnet powder mixes with the mass ratio of ferrite permanent-magnet powder by 3: 2, granularity of magnet powder is 45～100 μ m.
6. according to the preparation method of the said bonding built-up magnet of claim 5; It is characterized in that; The step of mixed material is in the step (1): magnetic is joined carry out coupling processing in the dispersant that is dissolved with coupling agent earlier; Place the ultrasonic wave dispersion treatment, treat dispersant volatilization after, coupling agent evenly coats magnetic; Again binding agent and curing agent are dissolved in the dispersant, process numberator height dispersed solids sol solution; Above-mentioned solid gum solution is fully mixed with the magnetic that above-mentioned coupling agent coats, after the drying mixed material is placed high-performance batch mixer batch mixing 12h, the material that obtains mixing.
7. according to the preparation method of the said bonding built-up magnet of claim 6, it is characterized in that what said compression moulding was adopted is the warm flow compaction moulding.
8. according to the preparation method of the said bonding built-up magnet of claim 7; It is characterized in that; The step of said warm flow compaction moulding is homogeneous mixture of material to be put into mould be heated to 70～110 ℃, applies the pressure compression moulding of 500～1100MPa, pressurize 10～15min.
9. the preparation method of said according to Claim 8 bonding built-up magnet is characterized in that, said cured is 150～200 ℃ of following heat treatment 1～4 hour in vacuum tube furnace.
10. a bonding built-up magnet is characterized in that, this bonding built-up magnet is by any method preparation of claim 1～9.
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