CN105788793A - Surface modification method capable of improving surface lubricating property of anisotropic permanent magnet powder particles - Google Patents

Surface modification method capable of improving surface lubricating property of anisotropic permanent magnet powder particles Download PDF

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Publication number
CN105788793A
CN105788793A CN201610306055.4A CN201610306055A CN105788793A CN 105788793 A CN105788793 A CN 105788793A CN 201610306055 A CN201610306055 A CN 201610306055A CN 105788793 A CN105788793 A CN 105788793A
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magnet powder
permanent
parylene
magnet
powder
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CN201610306055.4A
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Inventor
孙爱芝
马斌
许琛
郎惠珍
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Priority to CN201610306055.4A priority Critical patent/CN105788793A/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0572—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes with a protective layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0576—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together pressed, e.g. hot working
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/026—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0273—Imparting anisotropy

Abstract

The invention discloses a surface modification method capable of improving the surface lubricating property of anisotropic permanent magnet powder particles, belonging to the technical field of preparation of magnetic materials. A chemical vapor deposition polymerization (CVDP) method is adopted, and parylene is deposited and polymerized on the surface of pre-treated anisotropic permanent magnet powder; and the thickness of a parylene thin film is 1-50 microns. The surface lubricating property of the anisotropic permanent magnet powder modified by the parylene is greatly improved, and the density, orientation degree and magnetic property of a room-temperature orientated and molded magnet body are greater than the density, orientation degree and magnetic property of a magnet body molded by unmodified permanent magnet powder through warm pressing, so that when an anisotropic bonding permanent magnet is prepared by adopting mold pressing molding, the surface modification treatment is carried out on the permanent magnet powder particles through the parylene, and a room-temperature orientation and molding process can be used for replacing warm-pressing orientation and molding.

Description

Improve the surface modifying method of anisotropy permanent-magnet powder particle surface lubricity
Technical field
The invention belongs to anisotropy and mold the preparation method of bonded permanent magnet, be specifically related under a kind of room temperature prepare The technology of the anisotropic bond permanent magnet of highly oriented, high density, high magnetic characteristics.
Background technology
Anisotropic bonded permanent magnet is owing to having had good processing characteristics and more excellent magnetic property concurrently, it is possible to Effectively promote the miniaturization of electronic product, high efficiency, energy-saving, lightweight, and become sending out of bonded permanent magnet Exhibition direction.
The molding mode of bonded permanent magnet has compression molding, calendering formation, injection moulding and extruded, wherein Compression molding magnet is most widely used owing to having the highest magnetic property.
At present, in industrialized production, warm compaction process is widely used in preparation compression molding respectively to different Property bonded permanent magnet.So-called warm compaction molding refers to, is heated to glue by the magnetic powder of cladding thermosetting resin adhesive Being orientated compressing when tying the softening temperature of agent, high temperature makes binding agent soften and melts as viscous state, its low viscosity Play certain lubrication, friction resistance between magnetic powder particle rotary resistance and magnetic powder and die wall when reducing orientation The purpose of power, and then it is effectively improved the degree of orientation and the density of magnet, and then improve the magnetic energy product of magnet.
But, due to the high temperature of mould during temperature and pressure, mixing magnetic powder during filler and be heated, binding agent softens easily Cause magnetic powder wall sticking phenomenon, easily cause filler uneven, thus have influence on concordance and the size of magnet magnetic property Precision；Meanwhile, increase due to frictional resistance in pressing process, easily damage mould, reduce its service life.
Use multistep molding technology thereof can solve the problems referred to above, such as the patent of the Ai Zhizhi steel company of Japan And the patent (patent No.: ZL:201310489311.4) of University of Science & Technology, Beijing is described (CN1173028). But due to many one-step formings, adds additional process costs.
Therefore, at ambient temperature, the technology of preparing of preparation high-performance anisotropic bond permanent magnet just becomes in exploitation An important topic for bonded permanent magnet field.
By the surface modification to permanent-magnet powder granule, improve its lubricity, it will help make at ambient temperature Standby high-performance anisotropic bonded permanent magnet.
The present invention develops a kind of process for modifying surface improving anisotropy permanent-magnet powder particle surface lubricity, Can prepare and warm compaction molding magnet under conditions of room temperature molds with the permanent-magnet powder after being modified process Can suitable anisotropic bond permanent magnet, thus substantially increase production efficiency, it is to avoid warm compaction molding magnet The series of problems such as uniformity and poor dimensional precision.
Summary of the invention
It is an object of the invention to provide a kind of surface improving anisotropy permanent-magnet powder particle surface lubricity Modification technology, in order to use room temperature die press technology for forming to prepare each of high-orientation, high density and high energy product Anisotropy bonded permanent magnet.
The core of the present invention is the method using chemical vapor deposition polymerization (CVDP), by Parylene Molecule becomes thin film at anisotropy permanent-magnet powder surface deposition polymerization, and the thickness of thin film is 1-50 μm.Auspicious through sending The lubricity on the permanent-magnet powder surface after woods modification is greatly improved.
A kind of surface modifying method improving anisotropy permanent-magnet powder particle surface lubricity, it is characterised in that adopt With Parylene, anisotropy permanent-magnet powder is carried out surface modification treatment, then by the permanent-magnet powder after modification Mix with type thermosetting resin binding agent, coupling agent, obtain composite permanet magnet powder, the most at room temperature, to multiple It is compressing that conjunction permanent-magnet powder carries out magnetic field orientating, obtains anisotropic bonded permanent magnet blank, and blank is through solid Change obtains anisotropic bond permanent magnet after processing, and concrete preparation process is as follows:
Step (1) Parylene modification to permanent-magnet powder particle surface:
Anisotropy permanent-magnet powder is placed on containing in the ethanol solution that mass fraction is 5% coupling agent, at ultrasound wave Cleaning 1-3h post-drying in washer, the method using chemical vapor deposition polymerization (CVDP), dry Permanent-magnet powder surface deposition polymerization Parylene thin film, the technique of chemical gaseous phase deposition is: first suction is extremely ～2.6Pa, then, Parylene powder is heated to～180 DEG C be allowed to liter Huawei's gas, gas enters～680 DEG C Cracking is cracked into single molecular in chamber, and last monomolecular gases enters～in 25 DEG C of deposit cavities, poly-on magnetic powder surface Synthesis Parylene thin film.
Step (2) prepares composite permanet magnet powder:
Type thermosetting resin binding agent, coupling agent are dissolved in organic solvent, subsequently with cladding Parylene after forever Magnetic powder stirs, and grinds after organic solvent volatilization is removed, and i.e. can get compound permanent magnetic powder end.
Step (3) room temperature magnetic field orientating is compressing:
Composite permanet magnet powder is at room temperature placed in cavity body of mould, magnetic field orientating, extrusion forming, wherein magnetic field Intensity is more than 0.5T, and pressing pressure is 200-1000MPa, and demagnetization, the demoulding subsequently obtains blank, the side of demagnetization Formula uses alternating current pulse demagnetization or the one of reverse impulse demagnetization.
Step (4) solidifies:
Blank is heated to 100-200 DEG C, is incubated 0.5-3 hour, obtains anisotropic bond permanent magnet.
Described anisotropy permanent-magnet powder is all kinds of of neodymium iron boron, SmCo, samarium ferrum nitrogen, aluminum nickel cobalt or ferrite etc. Permanent-magnet powder.
Described binding agent is epoxy resin or phenolic resin, and described coupling agent is silane coupler or titanate esters coupling Agent etc., described Parylene is Parylene C powder, and the thickness of Parylene thin film is 1-50 μm.
The content of binding agent is the 1.0%-5.0wt% of permanent-magnet powder, preferably 2.0%-3.0wt%.Containing of coupling agent Amount is the 0.05%-2wt%, preferably 0.1%-1.0wt% of permanent-magnet powder.
The invention has the beneficial effects as follows: compared with the magnetic property of the warm compaction molding magnet of unmodified permanent-magnet powder, warp Permanent-magnet powder after Parylene modification, the magnetic property of its room temperature forming magnet is quite or more preferably；And use When room temperature forming thoroughly solves warm compaction molding, owing to binding agent softens the magnetic powder that causes, to glue wall, filler uneven and right The problems such as mould damage is big, and enormously simplify production technology, improve production efficiency.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail, and the present invention is not manufactured embodiment by these and limited.
Embodiment:
Permanent-magnet powder is that HDDR Anisotropy NdFeB Powder and powder size are less than 80 mesh, Parylene thin film Thickness is～3um～6um, and epoxy adhesive content is 2.5% (mass fraction), silane coupler Content is 0.5% (mass fraction).
The permanent-magnet powder of cladding Parylene thin film uses room temperature oriented moulding, and process conditions are: alignment magnetic field is 1.8T, pressing pressure is 600MPa.
The permanent-magnet powder of uncoated Parylene thin film uses temperature and pressure oriented moulding, and process conditions are: press temperature is 140 DEG C, temperature retention time 1min, alignment magnetic field is 1.8T, and pressing pressure is 600MPa.
Performance comparison is as shown in table 1.Using identical HDDR NdFeB permanent-magnet powder is raw material, uses identical Alignment magnetic field and pressing pressure, when Parylene film thickness is～during 6um, it is carried out room temperature oriented moulding The magnetic property of the bonded permanent magnet prepared is compared with the magnetic property of the warm compaction molding magnet of uncoated magnetic powder, and performance is notable Improving, wherein maximum magnetic energy product, the degree of orientation and density have been respectively increased 18.64%, 26.92% and 1.04%.
Table 1

Claims (5)

1. the surface modifying method improving anisotropy permanent-magnet powder particle surface lubricity, it is characterised in that Parylene is used anisotropy permanent-magnet powder to carry out surface modification treatment, then by the permanent magnetism powder after modification End mixes with type thermosetting resin binding agent, coupling agent, obtains composite permanet magnet powder, at room temperature, the most right It is compressing that composite permanet magnet powder carries out magnetic field orientating, obtains anisotropic bonded permanent magnet blank, blank warp Obtaining anisotropic bond permanent magnet after cured, concrete preparation process is as follows:
Step (1) Parylene modification to permanent-magnet powder particle surface:
Anisotropy permanent-magnet powder is placed on containing in the ethanol solution that mass fraction is 5% coupling agent, at ultrasound wave Cleaning 1-3h post-drying in washer, the method using chemical vapor deposition polymerization (CVDP), dry Permanent-magnet powder surface deposition polymerization Parylene thin film, the technique of chemical gaseous phase deposition is: first suction is extremely ～2.6Pa, then, Parylene powder is heated to～180 DEG C be allowed to liter Huawei's gas, gas enters～680 DEG C Cracking is cracked into single molecular in chamber, and last monomolecular gases enters～in 25 DEG C of deposit cavities, poly-on magnetic powder surface Synthesis Parylene thin film；
Step (2) prepares composite permanet magnet powder:
Type thermosetting resin binding agent, coupling agent are dissolved in organic solvent, subsequently with cladding Parylene after forever Magnetic powder stirs, and grinds after organic solvent volatilization is removed, and i.e. can get compound permanent magnetic powder end；
Step (3) room temperature magnetic field orientating is compressing:
Composite permanet magnet powder is at room temperature placed in cavity body of mould, magnetic field orientating, extrusion forming, wherein magnetic field Intensity is more than 0.5T, and pressing pressure is 200-1000MPa, and demagnetization, the demoulding subsequently obtains blank, the side of demagnetization Formula uses alternating current pulse demagnetization or the one of reverse impulse demagnetization；
Step (4) solidifies:
Blank is heated to 100-200 DEG C, is incubated 0.5-3 hour, obtains anisotropic bond permanent magnet.
A kind of table improving anisotropy permanent-magnet powder particle surface lubricity the most according to claim 1 Surface modification process, it is characterised in that: described anisotropy permanent-magnet powder is neodymium iron boron, SmCo, samarium ferrum nitrogen, aluminum Nickel cobalt or ferritic all kinds of permanent-magnet powder.
A kind of table improving anisotropy permanent-magnet powder particle surface lubricity the most according to claim 1 Surface modification process, it is characterised in that: described binding agent is epoxy resin or phenolic resin, and described coupling agent is silicon Alkane coupling agent or titanate coupling agent, described Parylene is Parylene C powder, and the thickness of Parylene thin film is 1-50μm。
4. according to a kind of raising anisotropy permanent-magnet powder particle surface lubricity described in claim 1 or 3 Surface modifying method, it is characterised in that: the content of binding agent is the 1.0%-5.0wt% of permanent-magnet powder；Coupling The content of agent is the 0.05%-2.0wt% of permanent-magnet powder.
A kind of table improving anisotropy permanent-magnet powder particle surface lubricity the most according to claim 4 Surface modification process, it is characterised in that: the content of binding agent is the 2.0%-3.0wt% of permanent-magnet powder；Coupling agent Content is the 0.1%-1.0wt% of permanent-magnet powder.
CN201610306055.4A 2016-05-10 2016-05-10 Surface modification method capable of improving surface lubricating property of anisotropic permanent magnet powder particles Pending CN105788793A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106409492A (en) * 2016-08-26 2017-02-15 昆山磁通新材料科技有限公司 Inductor warm-pressing forming method and inductor prepared by using same
CN109192487A (en) * 2018-08-29 2019-01-11 江苏健睡宝健康科技有限公司 A kind of manufacturing method of high-strength magnetic magnetic stripe
CN110706912A (en) * 2019-09-09 2020-01-17 中国科学院宁波材料技术与工程研究所 Preparation method of amorphous nanocrystalline soft magnetic powder core
CN112341759A (en) * 2020-11-18 2021-02-09 重庆大学 Modified nano-alumina composite epoxy resin insulating material and preparation method thereof
CN114678204A (en) * 2022-04-20 2022-06-28 杨杭福 Preparation method of high-performance samarium-iron-nitrogen magnet
CN117820944A (en) * 2024-03-05 2024-04-05 烟台舜康生物科技有限公司 Preparation method of parylene film layer for surface coating of electronic circuit module

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106409492A (en) * 2016-08-26 2017-02-15 昆山磁通新材料科技有限公司 Inductor warm-pressing forming method and inductor prepared by using same
CN109192487A (en) * 2018-08-29 2019-01-11 江苏健睡宝健康科技有限公司 A kind of manufacturing method of high-strength magnetic magnetic stripe
CN110706912A (en) * 2019-09-09 2020-01-17 中国科学院宁波材料技术与工程研究所 Preparation method of amorphous nanocrystalline soft magnetic powder core
CN112341759A (en) * 2020-11-18 2021-02-09 重庆大学 Modified nano-alumina composite epoxy resin insulating material and preparation method thereof
CN114678204A (en) * 2022-04-20 2022-06-28 杨杭福 Preparation method of high-performance samarium-iron-nitrogen magnet
CN114678204B (en) * 2022-04-20 2024-03-26 中国计量大学 Preparation method of high-performance samarium-iron-nitrogen magnet
CN117820944A (en) * 2024-03-05 2024-04-05 烟台舜康生物科技有限公司 Preparation method of parylene film layer for surface coating of electronic circuit module

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