CN109676125B - Method for preparing sintered neodymium-iron-boron magnet through 3D printing - Google Patents
Method for preparing sintered neodymium-iron-boron magnet through 3D printing Download PDFInfo
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- CN109676125B CN109676125B CN201910016362.2A CN201910016362A CN109676125B CN 109676125 B CN109676125 B CN 109676125B CN 201910016362 A CN201910016362 A CN 201910016362A CN 109676125 B CN109676125 B CN 109676125B
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Classifications
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- 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
-
- 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
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- 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
- H01F1/0577—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 sintered
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention provides a method for preparing a sintered neodymium-iron-boron magnet through 3D printing, and belongs to the field of powder metallurgy. The surface of the neodymium iron boron magnetic powder is coated with the oxygen-free organic film, the magnetic powder is prevented from being oxidized in the 3D printing process, meanwhile, the printing slurry of the neodymium iron boron is prepared by adopting liquid photosensitive resin, the printing of the slurry with high solid content is realized through the ultrasonic vibration control system, the precision of a printing blank body is ensured, the printing orientation forming of a magnet is realized by adopting the orientation magnetizing system, and finally, the high-performance sintered neodymium iron boron part with a complex shape is obtained. The surface of the neodymium iron boron magnetic powder which is easy to oxidize is coated with oxygen-free organic matters, the oxidation problem of the magnetic powder in the forming process is controlled, and the neodymium iron boron slurry for 3D printing is prepared from liquid photosensitive resin, so that the rapid forming of photocuring is realized. The sintered neodymium-iron-boron magnet prepared by the invention has good magnetic performance, can realize near-net-shape forming of various complex shapes, saves cutting processing of complex parts of the magnet, greatly reduces production cost and saves resources.
Description
Technical Field
The invention belongs to the field of powder metallurgy, and provides a method for preparing a sintered neodymium-iron-boron magnet through 3D printing.
Background
The sintered Nd-Fe-B permanent magnet material is called "magnetic king" because of high energy density, and has become a core functional device in the fields of aerospace, biomedicine, information communication, household appliances, wind power generation, automobile industry and the like. The sintered Nd-Fe-B magnet is usually prepared by powder pressing and sintering processes, the particle size of the sintered Nd-Fe-B magnet powder is generally 3-8 mu m, the particle size of the powder is too large, and Nd is generated2Fe14The magnetic performance of the magnet is seriously affected by the oversize of the B crystal grains. However, the fine neodymium-iron-boron powder is very easy to oxidize, the oxygen condition is strictly controlled in the actual production process of the sintered neodymium-iron-boron magnet, the oxygen content of the magnet is generally not more than 4000ppm at most, and otherwise, the magnetic performance of the magnet is greatly reduced.
With the development of science and technology, the sintered nd-fe-b magnet is more and more widely used, but in order to obtain a part with an ideal shape, a certain amount of machining is usually required to be performed on the sintered magnet, which causes a great deal of resource waste and increases the production cost. Therefore, there is a need to develop a technology that can produce high-performance functional magnetic devices with near-net shape at low cost. The 3D printing technology, also known as additive manufacturing technology, is a novel near-net forming technology, and can print and form parts with complex shapes layer by controlling materials such as metal powder particles or plastics according to a computer output system. The 3D printing technology is very suitable for preparing the neodymium iron boron magnet, the printed magnet does not need further cutting, raw material waste is reduced, a separate manufacturing die is not needed, and production cost is greatly reduced. The most widely studied and applied 3D printing process is currently the SLS selective laser sintering rapid prototyping technique, which manufactures three-dimensional parts by layer-by-layer build-up by melting pre-laid metal powder (spherical, and with a particle size D50 ═ 30-35 μm) or wire through laser beam heating. However, the SLS molding technique is not suitable for preparing sintered nd-fe-b magnets due to the limitation of the powder size and morphology.
Therefore, the invention provides a sintered neodymium-iron-boron magnet prepared by a 3D printing technology, and provides a sintered neodymium-iron-boron magnet prepared by coating neodymium-iron-boron powder with an oxygen-free organic matter, which can effectively control the magnet oxidation problem in the 3D printing process. Meanwhile, the neodymium iron boron magnetic powder printing slurry is prepared from the liquid photosensitive resin, so that photocuring rapid forming is realized. The formability and the blank precision of the high-solid-content slurry are ensured by combining the ultrasonic vibration system and the orientation magnetizing system, and the high-performance neodymium iron boron magnet with a complex shape is successfully prepared.
Disclosure of Invention
The invention aims to provide a method for preparing a sintered neodymium-iron-boron magnet through 3D printing, which obtains a satisfactory result in controlling the oxygenation condition of easily-oxidized neodymium-iron-boron powder in the 3D printing process, prevents the neodymium-iron-boron powder from being oxidized in the printing process by coating a layer of organic matter without oxygen on the surface of the magnetic powder, and realizes photocuring rapid printing and molding by adopting photosensitive resin to prepare printing slurry. Although the viscosity of the slurry is increased by adding fine neodymium iron boron powder into the liquid photosensitive resin, the formability of the slurry with high solid content and the precision of a blank body are ensured by ultrasonic vibration in the printing process. Meanwhile, the orientation of the magnet in the Z-axis direction is realized in the printing process, so that the complex forming of the high-performance sintered neodymium-iron-boron magnet is realized.
In order to obtain the method for preparing the sintered neodymium-iron-boron magnet through 3D printing, the invention adopts the following technical scheme, wherein all the operation steps are carried out in an argon atmosphere glove box or vacuum atmosphere equipment, and the specific steps are as follows:
(1) preparing a coating solution: dissolving the organic matter coating body in an organic solvent, and uniformly stirring to prepare an organic matter coating solution, wherein the concentration of the solution is 0.05g/ml-2.5 g/ml;
(2) powder coating: measuring the organic matter coating solution in the step (1) with the corresponding volume according to the mass percentage that the mass of the organic matter coating body is 0.6-1.5 wt% of the mass of the neodymium iron boron powder, and uniformly mixing the organic matter coating solution and the neodymium iron boron powder to enable the solution to soak all the powder;
(3) powder treatment: putting the coated powder into a vacuum drying oven, drying at 45-60 deg.C for 30-60min, and taking out to obtain neodymium iron boron powder coated with organic matters;
(4) preparing printing slurry: mixing a certain amount of reactive diluent, photoinitiator, photosensitizer and photosensitive oligomer according to the weight percentage to prepare a premixed liquid. Putting the neodymium iron boron powder coated in the step (3) into the premixed liquid, and uniformly stirring, wherein the solid content of the neodymium iron boron powder is 55-70 vol%;
(5) assembling the printing device: installing ultrasonic vibration equipment on a component platform of the photosensitive printer, externally connecting the ultrasonic vibration equipment with a control system, and installing an orientation magnetizing control system;
(6) printing and forming: inputting the model with the required shape into the 3D photosensitive printer assembled in the step (5), loading the slurry in the step (4) into a feeding port of 3D printing equipment, opening an orientation magnetizing control system and an ultrasonic vibration system, irradiating an ultraviolet lamp with the wavelength of 250-400 nm in the whole printing process, continuously ultrasonically vibrating a component platform of the printer, continuously orienting a printed blank under a magnetic field of 1.2-2.0T, and printing the blank with the required shape layer by layer to realize the oriented printing and forming of the magnet;
(7) and (3) vacuum sintering: performing vacuum sintering on the green body printed in the step (6), preserving heat at 600-800 ℃ for 180-fold-processed materials for 420min, preserving heat at 1020-1100 ℃ for 120-fold-processed materials for 360min, and keeping the vacuum degree at 10-2-10-3Pa, then rapidly cooling to room temperature with argon gas to prepare the sintered neodymium iron boron magnet with the required shape.
Further, the organic coating in step (1) is an oxygen-free organic substance, such as one or more of liquid paraffin, styrene or polystyrene.
Further, the organic solvent in step (1) is an oxygen-free solvent, such as one or more of toluene, xylene, dichloromethane, chloroform or cyclohexane.
Further, in the step (2), the neodymium iron boron powder is sintered neodymium iron boron powder, and the particle size of the powder is 3-8 μm.
Further, in the step (4), the reactive diluent is one or more selected from styrene (St), vinyl pyrrolidone (NVP), Vinyl Acetate (VA), Butyl Acrylate (BA), isooctyl acrylate (EHA), hydroxy (meth) acrylate (HEA, HEMA, HPA), 1, 6-hexanediol diacrylate (HDDA), tripropylene glycol diacrylate (TPGDA), neopentyl glycol diacrylate (NPGDA), trimethylolpropane triacrylate (TMPTA), etc., and the mass percentage in the premix is 5.0-20.0 wt.%.
Further, the photoinitiator in the step (4) is one or more of benzoin and derivatives thereof, acetophenone derivatives, triarylsulfonium salts and the like, and the mass percentage of the photoinitiator in the premixed liquid is 0.1-5.0 wt.%.
Further, in the step (4), the photosensitizer is one or more of benzophenone, michaelis mollis ketone, thioxanthone, benzil and the like, and the mass percentage of the photosensitizer in the premix liquid is 0.1-5.0 wt.%.
Further, in the step (4), the photosensitive oligomer is one or more of acrylated epoxy resin, unsaturated polyester, polyurethane, polythiol/polyene photocuring resin and the like.
Further, the orientation magnetization control system in the step (5) is composed of an upper electromagnet, a lower electromagnet and a control unit, wherein the upper electromagnet is fixed on a component platform of the printer, the lower electromagnet is fixed on the resin tank, and the Z-axis direction magnetization is realized through the power supply control unit.
The invention has the advantages that:
1. organic matter of an oxygen-free system is coated on the surface of the neodymium iron boron magnetic powder which is easy to oxidize, so that the problem of oxidation of the magnetic powder in the forming process is solved;
2. preparing 3D printed neodymium iron boron slurry by using photosensitive resin, and realizing photocuring rapid molding of a neodymium iron boron printed blank;
3. ultrasonic vibration is implemented in the printing process, so that the formability of the neodymium iron boron slurry with high solid content is ensured, and the control of the precision of the blank body is facilitated; the orientation of the magnet is realized through the orientation magnetizing system, so that the high-orientation-degree magnet is obtained;
4. sintered neodymium-iron-boron magnets with various complex shapes can be prepared through 3D printing, so that cutting processing of complex parts of the magnets is omitted, production cost is greatly reduced, and resources are saved;
5. the sintered neodymium-iron-boron magnet printed by 3D printing has the advantages of wide application range, stable process and good magnetic performance, and has good industrial application prospect.
Detailed Description
Example 1:
a method for preparing a triangular sintered neodymium-iron-boron magnet through 3D printing comprises the following steps:
(1) mixing the following components in a weight ratio of 1: 1, dissolving the polystyrene and the paraffin in dichloromethane, wherein the concentration of the solution is 0.1g/ml, and uniformly stirring to prepare an organic matter coating solution. Weighing 50ml of coating solution, weighing 500g of 5-micron neodymium-iron-boron powder, and uniformly mixing the organic matter coating solution and the neodymium-iron-boron powder to enable the solution to soak all the powder;
(2) putting the coated powder into a vacuum drying oven, drying for 50min at 45 ℃, and taking out to obtain neodymium iron boron powder coated with organic matters;
(3) 10 wt.% of 1, 6-hexanediol diacrylate, 2.5 wt.% of benzoin derivative, 3 wt.% of benzophenone and 84.5 wt.% of acrylated epoxy resin were mixed to prepare a premix. Putting the coated neodymium iron boron powder into a premix liquid, wherein the solid content is 65 vol%, and uniformly stirring to prepare printing slurry;
(4) installing ultrasonic vibration equipment on a component platform of the photosensitive printer, externally connecting the ultrasonic vibration equipment with a control system, and installing an orientation magnetizing control system;
(5) inputting the triangular model into a 3D printer, loading printing slurry into a feeding port of 3D printing equipment, starting printing, simultaneously opening an ultrasonic vibration control system and an orientation magnetizing control system, continuously orienting a printed blank in a 1.5T magnetic field in the printing process, irradiating an ultraviolet lamp, and printing the blank in a required shape layer by layer;
(6) placing the printed blank into a vacuum sintering furnace, firstly preserving heat at 600 ℃ for 180min, continuously heating to 1050 ℃, preserving heat for 300min, and keeping vacuum degree of 10-3Pa, then rapidly cooling argon to room temperature to prepare the triangular sintered neodymium-iron-boron magnet.
Example 2:
a method for preparing a horseshoe-shaped sintered neodymium-iron-boron magnet through 3D printing comprises the following steps:
(1) dissolving paraffin in cyclohexane to obtain solution with concentration of 0.2g/ml, and stirring to obtain organic matter coating solution. Measuring 15ml of coating solution, weighing 500g of 5-micron neodymium-iron-boron powder, and uniformly mixing the organic matter coating solution and the neodymium-iron-boron powder to enable the solution to soak all the powder;
(2) putting the coated powder into a vacuum drying oven, drying for 30min at 60 ℃, and taking out to obtain neodymium iron boron powder coated with organic matters;
(3) 20 wt.% of vinyl acetate, 1 wt.% of acetophenone derivative, 2 wt.% of thioxanthone and 77 wt.% of polyurethane are mixed to prepare a premixed liquid. Putting the coated neodymium iron boron powder into a premix liquid, wherein the solid content is 58 vol%, and uniformly stirring to prepare printing slurry;
(4) installing ultrasonic vibration equipment on a component platform of the photosensitive printer, externally connecting the ultrasonic vibration equipment with a control system, and installing an orientation magnetizing control system;
(5) inputting the horseshoe-shaped model into a 3D printer, loading printing slurry into a feeding port of 3D printing equipment, starting printing, simultaneously starting an ultrasonic vibration control system and an orientation magnetizing control system, continuously orienting a printed blank in a 2.0T magnetic field in the printing process, irradiating an ultraviolet lamp, and printing the blank in a required shape layer by layer;
(6) placing the printed blank into a vacuum sintering furnace, firstly preserving the heat at 700 ℃ for 300min, and continuously heating to 1080 DEG CKeeping the temperature for 360min, and keeping the vacuum degree at 10-3Pa, then rapidly cooling to room temperature with argon to prepare the horseshoe-shaped sintered neodymium iron boron magnet.
Claims (8)
1. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing is characterized in that all the operation steps are carried out in an argon atmosphere glove box or vacuum atmosphere equipment, and the sintered neodymium-iron-boron magnet is prepared according to the following steps:
(1) preparing a coating solution: dissolving the organic matter coating body in an organic solvent, and uniformly stirring to prepare an organic matter coating solution, wherein the concentration of the solution is 0.05g/ml-2.5 g/ml;
(2) powder coating: measuring the organic matter coating solution in the step (1) with the corresponding volume according to the mass percentage that the mass of the organic matter coating body is 0.6-1.5 wt% of the mass of the neodymium iron boron powder, and uniformly mixing the organic matter coating solution and the neodymium iron boron powder to enable the solution to soak all the powder;
(3) powder treatment: putting the coated powder into a vacuum drying oven, drying at 45-60 deg.C for 30-60min, and taking out to obtain neodymium iron boron powder coated with organic matters;
(4) preparing printing slurry: mixing a certain amount of reactive diluent, photoinitiator, photosensitizer and photosensitive oligomer according to the weight percentage to prepare a premixed solution; putting the neodymium iron boron powder coated in the step (3) into the premixed liquid, and uniformly stirring, wherein the solid content of the neodymium iron boron powder is 55-70 vol%;
(5) assembling the printing device: installing ultrasonic vibration equipment on a component platform of the photosensitive printer, externally connecting the ultrasonic vibration equipment with a control system, and installing an orientation magnetizing control system;
(6) printing and forming: inputting the model with the required shape into the 3D photosensitive printer assembled in the step (5), loading the slurry in the step (4) into a feeding port of 3D printing equipment, opening an orientation magnetizing control system and an ultrasonic vibration system, irradiating an ultraviolet lamp with the wavelength of 250-400 nm in the whole printing process, continuously ultrasonically vibrating a component platform of the printer, continuously orienting a printed blank under a magnetic field of 1.2-2.0T, and printing the blank with the required shape layer by layer to realize the oriented printing and forming of the magnet;
(7) and (3) vacuum sintering: performing vacuum sintering on the green body printed in the step (6), preserving heat at 600-800 ℃ for 180-fold-processed materials for 420min, preserving heat at 1020-1100 ℃ for 120-fold-processed materials for 360min, and keeping the vacuum degree at 10-2-10-3Pa, then rapidly cooling argon to room temperature to prepare the sintered neodymium-iron-boron magnet with the required shape;
in the step (2), the neodymium iron boron powder is sintered neodymium iron boron powder, and the particle size of the powder is 3-8 μm.
2. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing according to claim 1, wherein the method comprises the following steps: the organic matter coating body in the step (1) is an oxygen-free organic matter and comprises one or more of liquid paraffin, styrene or polystyrene.
3. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing according to claim 1, wherein the method comprises the following steps: the organic solvent in the step (1) is an oxygen-free solvent and comprises one or more of toluene, xylene, dichloromethane, trichloromethane or cyclohexane.
4. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing according to claim 1, wherein the method comprises the following steps: in the step (4), the active diluent is one or more of styrene (St), vinyl pyrrolidone (NVP), Vinyl Acetate (VA), Butyl Acrylate (BA), isooctyl acrylate (EHA), hydroxy (meth) acrylate (HEA, HEMA, HPA), 1, 6-hexanediol diacrylate (HDDA), tripropylene glycol diacrylate (TPGDA), neopentyl glycol diacrylate (NPGDA) and trimethylolpropane triacrylate (TMPTA), and the mass percentage of the active diluent in the premix is 5.0-20.0 wt.%.
5. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing according to claim 1, wherein the method comprises the following steps: in the step (4), the photoinitiator is one or more of benzoin and derivatives thereof, acetophenone derivatives and triarylsulfonium salts, and the mass percentage of the photoinitiator in the premixed liquid is 0.1-5.0 wt.%.
6. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing according to claim 1, wherein the method comprises the following steps: in the step (4), the photosensitizer is one or more of benzophenone, michaelis mollis ketone, thioxanthone and benzil, and the mass percentage of the photosensitizer in the premixed liquid is 0.1-5.0 wt.%.
7. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing according to claim 1, wherein the method comprises the following steps: in the step (4), the photosensitive oligomer is one or more of acrylated epoxy resin, unsaturated polyester, polyurethane and polythiol/polyene photocuring resin.
8. The method for preparing the sintered neodymium-iron-boron magnet through 3D printing according to claim 1, wherein the method comprises the following steps: and (5) the orientation magnetizing control system consists of an upper electromagnet, a lower electromagnet and a control unit, wherein the upper electromagnet is fixed on a component platform of the printer, the lower electromagnet is fixed on the resin tank, and the Z-axis direction magnetizing is realized through the power supply control unit.
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| CN111370217B (en) * | 2020-03-19 | 2021-07-13 | 中国科学院宁波材料技术与工程研究所 | Method for preparing permanent magnet through photocuring-assisted direct-writing 3D printing |
| CN111941845B (en) * | 2020-06-23 | 2022-04-12 | 西安理工大学 | Material groove system and particle composite material surface exposure 3D printing system and method |
| CN112349506A (en) * | 2020-09-28 | 2021-02-09 | 辽宁秉航非晶科技有限公司 | Method for manufacturing powder magnetic core by insulating and curing amorphous powder at room temperature |
| CN112916868B (en) * | 2021-01-13 | 2022-05-10 | 中国科学院金属研究所 | Photocuring 3D printing metal part and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103854844A (en) * | 2014-03-19 | 2014-06-11 | 北京科技大学 | Method for preparing complicated shape bonded magnet by utilizing 3D (three-dimensional) printing technology |
| CN104821219A (en) * | 2015-05-18 | 2015-08-05 | 朱春芳 | UV-cured resin coated soft magnetic powder, preparation method and application thereof |
| CN106883347A (en) * | 2017-02-27 | 2017-06-23 | 广东工业大学 | A kind of photosensitive resin synthesis precursor and preparation method thereof and photosensitive resin |
| CN106571219B (en) * | 2016-10-27 | 2017-11-28 | 北京科技大学 | The device and method of magnetic field orientating 3D printing anisotropic neodymium iron boron magnetic body |
| CN108320876A (en) * | 2018-03-05 | 2018-07-24 | 北京科技大学 | A kind of method that hot isostatic pressing low-temperature sintering obtains high magnetic sintered NdFeB |
| CN108465806A (en) * | 2018-03-12 | 2018-08-31 | 北京科技大学 | A kind of method that Coated with Organic Matter alloy powder prepares high-performance powder metallurgy product |
-
2019
- 2019-01-08 CN CN201910016362.2A patent/CN109676125B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103854844A (en) * | 2014-03-19 | 2014-06-11 | 北京科技大学 | Method for preparing complicated shape bonded magnet by utilizing 3D (three-dimensional) printing technology |
| CN104821219A (en) * | 2015-05-18 | 2015-08-05 | 朱春芳 | UV-cured resin coated soft magnetic powder, preparation method and application thereof |
| CN106571219B (en) * | 2016-10-27 | 2017-11-28 | 北京科技大学 | The device and method of magnetic field orientating 3D printing anisotropic neodymium iron boron magnetic body |
| CN106883347A (en) * | 2017-02-27 | 2017-06-23 | 广东工业大学 | A kind of photosensitive resin synthesis precursor and preparation method thereof and photosensitive resin |
| CN108320876A (en) * | 2018-03-05 | 2018-07-24 | 北京科技大学 | A kind of method that hot isostatic pressing low-temperature sintering obtains high magnetic sintered NdFeB |
| CN108465806A (en) * | 2018-03-12 | 2018-08-31 | 北京科技大学 | A kind of method that Coated with Organic Matter alloy powder prepares high-performance powder metallurgy product |
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