CN112435820A - High-performance sintered neodymium-iron-boron magnet and preparation method thereof - Google Patents
High-performance sintered neodymium-iron-boron magnet and preparation method thereof Download PDFInfo
- Publication number
- CN112435820A CN112435820A CN202011291859.4A CN202011291859A CN112435820A CN 112435820 A CN112435820 A CN 112435820A CN 202011291859 A CN202011291859 A CN 202011291859A CN 112435820 A CN112435820 A CN 112435820A
- Authority
- CN
- China
- Prior art keywords
- magnetic powder
- alloy
- raw materials
- sintering
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000956 alloy Substances 0.000 claims abstract description 61
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 59
- 239000006247 magnetic powder Substances 0.000 claims abstract description 55
- 238000005245 sintering Methods 0.000 claims abstract description 46
- 238000005266 casting Methods 0.000 claims abstract description 36
- 230000008719 thickening Effects 0.000 claims abstract description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000001257 hydrogen Substances 0.000 claims abstract description 32
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000003723 Smelting Methods 0.000 claims abstract description 23
- 238000005496 tempering Methods 0.000 claims abstract description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011159 matrix material Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000011049 filling Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 12
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 11
- 239000000314 lubricant Substances 0.000 claims abstract description 11
- 229910052786 argon Inorganic materials 0.000 claims abstract description 10
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 29
- 239000010949 copper Substances 0.000 claims description 26
- 238000010902 jet-milling Methods 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 17
- 229910052802 copper Inorganic materials 0.000 claims description 15
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 12
- 229910052771 Terbium Inorganic materials 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052779 Neodymium Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052733 gallium Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 239000013078 crystal Substances 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 18
- 239000012071 phase Substances 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 235000021355 Stearic acid Nutrition 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- 239000008117 stearic acid Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007792 addition Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000001808 coupling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005324 grain boundary diffusion Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- -1 silicate ester Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- 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
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
- H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
-
- 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
-
- 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
- H01F41/0266—Moulding; Pressing
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention provides a preparation method of a high-performance sintered neodymium-iron-boron magnet, which comprises the following steps: (1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials to obtain a casting sheet A; filling hydrogen into the cast piece A for crushing, sieving in an inert atmosphere to obtain coarse crushed powder A, and then grinding in an airflow mill protected by the inert atmosphere to obtain airflow mill magnetic powder A; (2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; filling hydrogen into the cast ingot B for crushing, sieving in an argon protection box to obtain coarse crushed powder B, and then grinding in an airflow mill under the protection of argon atmosphere to obtain airflow mill magnetic powder B; (3) mixing the jet mill magnetic powder A and the jet mill magnetic powder B, adding a lubricant, stirring for 2-6 hours, then performing orientation molding, and performing isostatic pressing; (4) the blank after isostatic pressing treatment enters a sintering furnace, is subjected to dehydrogenation treatment, and then is subjected to presintering, high-temperature sintering and tempering heat treatment.
Description
Technical Field
The invention belongs to the field of rare earth permanent magnet material preparation, and relates to a high-performance sintered neodymium-iron-boron magnet and a preparation method thereof.
Background
Since the sintered neodymium iron boron appeared in 1983, the sintered neodymium iron boron is widely applied to the fields of IT, medical treatment, household appliances, new energy automobiles and the like due to the excellent magnetic property. With the development of the market, the sintered nd-fe-b magnet is required to have high magnetic property and high heat resistance, that is, the magnet is required to have a high maximum energy product and a high intrinsic coercive force. Therefore, it becomes a hot spot in technical research and development to improve the coercive force of the magnet while ensuring the magnetism of the magnet.
In the industry, a method for improving the coercive force by partially replacing Nd in an original magnet by using heavy rare earth metal elements such as Dy or Tb and the like can obtain the obviously improved coercive force, but the Dy or Tb can enter a main phase to greatly reduce the magnetism of the magnet while improving the coercive force along with the increase of the replacement amount of the Dy or Tb; on the other hand, heavy rare earth metals such as Dy and Tb are more expensive than Nd, and therefore, partial substitution of Nd with Dy or Tb also increases the cost of the magnet. In order to overcome the defects, in recent years, heavy rare earth is distributed at the crystal grain boundary of the magnet by a thermal diffusion mode of the sintered magnet crystal grain boundary, so that the aim of improving the coercive force can be achieved by using a small amount of Dy and Tb, and the magnetic property of the magnet is reduced little. However, the grain boundary diffusion technology exists: 1. the large-scale production technology is difficult, expensive equipment needs to be configured, and corresponding technical support is needed; 2. the method has the limit to the size of the magnet and is not suitable for producing large-block magnets. Therefore, research on more suitable technology is needed to prepare the ndfeb magnet in the cost-effective and full-application field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a high-performance sintered neodymium iron boron magnet and a preparation method thereof.
The invention provides a high-performance sintered neodymium-iron-boron magnet, which is prepared from the raw materials of a matrix alloy A and a grain boundary thickening alloy B;
the composition component of the base alloy A is RxTyMzB(1-x-y-z)Wherein R is one or more of Nd, Pr, La, Ce, Dy and Tb, M is one or more of Cu, Al and Ga and one or two of Nb and Zr, T is Fe and Co, and the mass ratio of Fe to Co is (40-100): 1, x is 28 to 33 wt%, y is 58 to 72 wt%, and z is 0 to 2.0 wt%.
The component R of the alloy B with thickened grain boundaryxM(1-x), wherein R is one or more of Nd, Pr, Dy and Tb, M is one or more of Cu, Al and Ga, and x is 80-95 wt%.
The invention provides a preparation method of the high-performance sintered neodymium-iron-boron magnet, which comprises the following steps:
(1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials by adopting a rapid hardening process to obtain a cast piece A; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in inert atmosphere to obtain coarse broken powder A, and then grinding the coarse broken powder A in an airflow mill protected by inert atmosphere to obtain airflow mill magnetic powder A;
(2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B;
(3) mixing the jet mill magnetic powder A and the jet mill magnetic powder B, adding a lubricant, stirring for 2-6 hours, then carrying out orientation molding in an inert atmosphere, and then carrying out isostatic pressing treatment;
(4) and (3) feeding the blank subjected to isostatic pressing treatment into a sintering furnace, preserving heat for 2-5 hours at 550-600 ℃ for dehydrogenation treatment, and then performing presintering, high-temperature sintering and tempering heat treatment.
The smelting temperature of the step (1) and the step (2) is 1450-1500 ℃, and the casting temperature is 1400-1450 ℃; when the rapid hardening process is adopted, the rotating speed of the copper roller is 1.2-1.5 m/s, and the average thickness of the obtained cast sheet A is 0.2-0.4 mm.
The average particle size of the jet milling magnetic powder A in the step (1) is 4-5 mu m.
The average particle size of the jet milling magnetic powder B in the step (2) is 1-2 μm.
And (4) in the mixture of the jet milling magnetic powder A and the jet milling magnetic powder B in the step (3), the content of the jet milling magnetic powder B is 1-5 wt%.
The magnetic field intensity of the orientation forming in the step (3) is 1.0-1.5T, and the isostatic pressure treatment pressure is 150-220 MPa.
The pre-sintering in the step (4) is carried out at the temperature of 800-1000 ℃ for 10-15 h.
The pre-sintering in the step (4) is carried out for 12-15 h at 850-950 ℃.
The high-temperature sintering temperature in the step (4) is 1030-1100 ℃, and the sintering time is 4-6 h; the tempering heat treatment comprises the following steps: the primary tempering temperature is 800-920 ℃, and the tempering time is 2-4 hours; the secondary tempering temperature is 460-560 ℃, and the tempering time is 4-6 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts double alloy components: the crystal boundary thickening alloy B and the matrix alloy A are respectively cast, crushed and then co-sintered, the crystal boundary thickening alloy B is uniformly and dispersedly distributed around the matrix alloy A crystal grains, the crystal boundary is thickened, the structure and the distribution of the crystal boundary phase of the magnet are regulated, the magnetostatic coupling effect among the crystal grains is reduced, and the performance of the magnet is improved;
(2) according to the invention, the oxidation resistance of the crystal boundary thickening alloy B in the sintering process is effectively improved through the processes of casting the crystal boundary thickening alloy B into an ingot, removing hydrogen after hydrogen crushing, filling argon for protection and the like, and the crystal boundary thickening alloy B is uniformly dispersed around matrix phase crystal grains through pre-sintering, so that the effects of thickening the crystal boundary and improving the performance of a magnet are exerted;
(3) the average particle size of the jet mill magnetic powder B crushed by the crystal boundary thickening alloy B is controlled to be 1-2 mu m, so that the crystal boundary thickness is effectively improved, and the performance of a magnet is improved;
(4) according to the invention, the content of the jet mill magnetic powder B in the mixture of the jet mill magnetic powder A and the jet mill magnetic powder B is controlled to be 1-5 wt%, so that a crystal boundary thickening phase is generated, and components are prevented from entering a matrix phase, thereby effectively improving the performance of the magnet.
Drawings
Fig. 1 is a structural view of a sintered nd-fe-b magnet according to example 1 of the present invention;
FIG. 2 is a structural view of a sintered NdFeB magnet according to a comparative example 3 of the present invention;
Detailed Description
The high-performance sintered ndfeb magnet and the method for manufacturing the same according to the present invention will be described in detail below, and technical terms or scientific terms used at this time have meanings that are generally understood by those skilled in the art of the present invention, if not defined otherwise.
The embodiment of the invention provides a high-performance sintered neodymium-iron-boron magnet, which is prepared from the raw materials of a matrix alloy A and a grain boundary thickening alloy B;
the composition component of the base alloy A is RxTyMzB(1-x-y-z)Wherein R is one or more of Nd, Pr, La, Ce, Dy and Tb, M is one or more of Cu, Al and Ga and one or two of Nb and Zr, T is Fe and Co, and the mass ratio of Fe to Co is (40-100): 1, x is 28 to 33 wt%, y is 58 to 72 wt%, and z is 0 to 2.0wt%。
The component R of the alloy B with thickened grain boundaryxM(1-x)Wherein R is one or more of Nd, Pr, Dy and Tb, M is one or more of Cu, Al and Ga, and x is 80-95 wt%.
The crystal boundary thickening alloy B is uniformly and dispersedly distributed around the crystal grains of the matrix alloy A, so that the crystal boundary is thickened, the magnetostatic coupling effect among the crystal grains is reduced, and the intrinsic coercive force of the magnet is improved.
Another embodiment of the present invention provides a method for preparing a high-performance sintered ndfeb magnet, including the steps of:
(1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials by adopting a rapid hardening process to obtain a cast piece A; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in inert atmosphere to obtain coarse broken powder A, and then grinding the coarse broken powder A in an airflow mill protected by inert atmosphere to obtain airflow mill magnetic powder A;
(2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B;
(3) mixing the jet mill magnetic powder A and the jet mill magnetic powder B, adding a lubricant, stirring for 2-6 hours, then carrying out orientation molding in an inert atmosphere, and then carrying out isostatic pressing treatment;
(4) and (3) feeding the blank subjected to isostatic pressing treatment into a sintering furnace, preserving heat for 2-5 hours at 550-600 ℃ for dehydrogenation treatment, and then performing presintering, high-temperature sintering and tempering heat treatment.
Herein, the ingot and the cast slab are those conventionally defined in the art, that is, the ingot is obtained by casting the alloy raw material after melting into a water-cooled mold, and the cast slab is obtained by casting the alloy raw material after melting onto a copper roller with a certain rotating speed.
In the invention, the smelting temperature of the step (1) and the step (2) is 1450-1500 ℃, and the casting temperature is 1400-1450 ℃; when the cast sheet is prepared, the rotating speed of a copper roller is 1.2-1.5 m/s, and the average thickness of the prepared cast sheet A is 0.2-0.4 mm; when the thickness of the cast piece is too small, ultrafine crystal grains are easily generated, and when the thickness of the cast piece is too large, the crystal grains are too large and a hetero-phase is generated.
The average thickness of the cast piece is defined herein as the average of the measured data of any 100 cast pieces, and the measuring tool can be a vernier caliper or a micrometer screw.
In the general preparation process of the sintered neodymium iron boron magnet, a casting sheet is cast, and the performance of the magnet is improved by sintering in the form of the casting sheet. The crystal boundary thickening alloy B is cast into an ingot and is co-sintered with the base alloy A in the form of a cast sheet. The reason is that the grain boundary thickening alloy B is a rare earth alloy, is easy to oxidize in the preparation process of the magnet, and can effectively resist oxidation when being cast into an ingot form. In addition, in order to further reduce the oxidation effect of the crystal boundary thickening alloy B, after the ingot B is charged with hydrogen and crushed, dehydrogenation treatment is not carried out, and the hydrogen component of the alloy is kept to better isolate the oxidation caused by the reaction of the alloy and oxygen in the powder preparation process; meanwhile, after being charged with hydrogen and crushed, the ingot B is sieved in an argon protection box and ground in an airflow mill in argon atmosphere, so that the crystal boundary thickening alloy B is not easy to oxidize in argon atmosphere.
In order to ensure the uniform dispersion of the grain boundary thickening alloy B at the grain boundary, the invention carries out a pre-sintering process before high-temperature sintering: and (3) preserving the heat for 10-15 hours at 800-1000 ℃, and preserving the heat for a certain time at the temperature to ensure that the crystal boundary thickening alloy B becomes a liquid phase and fully flows among crystal grains of the matrix phase. The pre-sintering process is preferably carried out at 850-950 ℃ for 12-15 h, so that the activity of crystal grains can be increased, the flow of the liquid phase alloy can be improved, and the crystal grains cannot grow.
The invention effectively improves the oxidation resistance of the crystal boundary thickening alloy B in the sintering process by casting the crystal boundary thickening alloy B into an ingot, removing hydrogen after hydrogen crushing, filling argon for protection and other processes, and uniformly disperses the crystal boundary thickening alloy B around matrix phase crystal grains by pre-sintering, thereby playing the roles of thickening the crystal boundary and improving the performance of a magnet.
And after the grain boundary thickening alloy B is milled by an air jet mill, controlling the average grain size of the air jet mill magnetic powder B to be 1-2 mu m. The average particle size of the jet mill magnetic powder B is controlled based on two points: 1. the thickness of the normal grain boundary phase of the sintered neodymium iron boron magnet is 5-50nm, and the average grain diameter of the sintered neodymium iron boron magnet is larger than the thickness of the normal grain boundary phase as an alloy phase which needs to play a role in thickening the grain boundary; 2. if the average grain size of the grain boundary thickening phase is too large, more grains wrap the same matrix phase grains, resulting in a decrease in the number of matrix phases and a decrease in magnetic properties. Therefore, the average particle size of the jet mill magnetic powder B is controlled to be 1-2 mu m, the grain boundary thickness is effectively improved, and the magnet performance is improved.
Herein, the average particle diameter of the jet-milled magnetic powder is defined as a median diameter of a volume-based particle diameter distribution measured by a laser diffraction scattering method.
And controlling the content of the jet milling magnetic powder B to be 1-5 wt% in the mixture of the jet milling magnetic powder A and the jet milling magnetic powder B. The jet milling magnetic powder B is used for forming a crystal boundary thickening phase, the content is not easy to be excessive, and the excessive content can cause components to enter a matrix phase to reduce the performance of the magnet.
The inert atmosphere of the present invention is nitrogen or argon.
The lubricant of the invention is a lubricant which is conventionally used in the field for sintering neodymium iron boron magnets, such as paraffin, glycerol, silicate ester, silicone oil, stearic acid, zinc stearate, tributyl borate and the like. The addition amount of the lubricant is 0.2-0.5 wt% of the mixture of the jet mill magnetic powder A and the jet mill magnetic powder B.
Hereinafter, the technical solution of the present invention will be further described and illustrated by specific examples and drawings. However, these embodiments are exemplary, and the present disclosure is not limited thereto. Unless otherwise specified, the raw materials used in the following specific examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art.
Example 1
The preparation method of the sintered neodymium-iron-boron magnet comprises the following steps:
(1) nd according to the composition A of the base alloy28.0Fe69.57Co1.0Cu0.1Al0.1Ga0.2Zr0.05B0.98Proportioning, smelting raw materials by adopting a rapid hardening process, and casting the raw materials on a copper roller with the rotating speed of 1.5m/s to obtain a casting sheet A with the average thickness of 0.3mm, wherein the smelting temperature is 1460 ℃, and the casting temperature is 1420 ℃; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in nitrogen protection to obtain coarse broken powder A with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder A in an airflow mill protected by nitrogen atmosphere to obtain airflow mill magnetic powder A with the average particle size of 4 mu m;
(2) according to the constituent Pr of the alloy B with the grain boundary thickened23.75Nd71.25Cu3.0Al2.0Burdening, namely smelting and casting the raw materials into a water-cooled mold to obtain an ingot B, wherein the smelting temperature is 1460 ℃, and the casting temperature is 1410 ℃; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B with the average particle size of 2 mu m;
(3) mixing the jet milling magnetic powder A and the jet milling magnetic powder B according to the mass ratio of 96:4, adding 0.3 wt% of lubricant stearic acid, stirring for 4 hours, then carrying out orientation molding in a magnetic field with the magnetic field intensity of 1.4T in an argon atmosphere, and pressing into a green body in a water isostatic pressing at 200 MPa;
(4) and sintering the green body in a vacuum sintering furnace, preserving heat for 3h at 580 ℃ for dehydrogenation treatment, sintering at 900 ℃ for 15h, heating to 1030 ℃ for sintering for 5h, cooling to room temperature, heating to 900 ℃ for primary tempering for 2.5h, cooling to 500 ℃ for secondary tempering for 4.5h, and preparing the sintered neodymium-iron-boron magnet.
Example 2
The preparation method of the sintered neodymium-iron-boron magnet comprises the following steps:
(1) nd according to the composition A of the base alloy30.0Fe67.3Co1.1Cu0.15Al0.12Nb0.08B1.25Proportioning, smelting raw materials by adopting a rapid hardening process, and casting the raw materials on a copper roller with the rotating speed of 1.5m/s to obtain a casting sheet A with the average thickness of 0.3mm, wherein the smelting temperature is 1480 ℃, and the casting temperature is 1420 ℃; placing the casting sheet A in hydrogenCharging hydrogen into a crushing furnace, crushing, sieving in nitrogen protection to obtain coarse crushed powder A with the particle size of less than or equal to 300 mu m, and then grinding the coarse crushed powder A in a jet mill protected by nitrogen atmosphere to obtain jet mill magnetic powder A with the average particle size of 5 mu m;
(2) dy is the component of alloy B with thickened grain boundary10.65Nd83.35Cu4.0Ga2.0Burdening, namely smelting and casting the raw materials into a water-cooled mold to obtain an ingot B, wherein the smelting temperature is 1460 ℃, and the casting temperature is 1410 ℃; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B with the average particle size of 1 mu m;
(3) mixing the jet milling magnetic powder A and the jet milling magnetic powder B according to the mass ratio of 97:3, adding 0.3 wt% of lubricant stearic acid, stirring for 5 hours, then carrying out orientation molding in a magnetic field with the magnetic field intensity of 1.4T in an argon atmosphere, and pressing into a green body in a water isostatic pressing at 180 MPa;
(4) and sintering the green body in a vacuum sintering furnace, preserving heat for 4h at 560 ℃ for dehydrogenation treatment, sintering at 850 ℃ for 14h, heating to 1040 ℃ for sintering for 4h, cooling to room temperature, heating to 890 ℃ for primary tempering for 2h, cooling to 510 ℃ for secondary tempering for 5h, and preparing the sintered neodymium-iron-boron magnet.
Example 3
Example 3 differs from example 1 only in that the mean particle size of the jet mill magnetic powder B is 4 μm, and other steps are the same and are not repeated here.
Example 4
Example 4 differs from example 1 only in that the jet-milled magnetic powder a and the jet-milled magnetic powder B were mixed at a mass ratio of 92:8, and other steps are the same and are not described herein.
Example 5
The difference between the embodiment 5 and the embodiment 1 is only that the pre-sintering of the embodiment 5 is sintering at 850 ℃ for 8h, and other steps are the same as those of the embodiment 1 and are not repeated herein.
Example 6
The difference between the embodiment 6 and the embodiment 1 is only that the pre-sintering of the embodiment 6 is sintering at 850 ℃ for 18h, and other steps are the same as those of the embodiment 1 and are not repeated herein.
Comparative example 1
Comparative example 1 differs from example 1 only in that the grain boundary thickening alloy B of comparative example 1 was cast into a cast slab according to the rapid solidification process of the matrix alloy a, i.e., according to the composition Pr of the grain boundary thickening alloy B23.75Nd71.25Cu3.0Al2.0And (3) burdening, smelting the raw materials by adopting a rapid hardening process, casting the raw materials on a copper roller with the rotating speed of 1.5m/s to obtain a casting sheet B with the average thickness of 0.3mm, wherein the smelting temperature is 1460 ℃, the casting temperature is 1420 ℃, and other steps are the same as those in the embodiment 1 and are not repeated.
Comparative example 2
The difference between the comparative example 2 and the example 1 is only that the comparative example 2 is not pre-sintered, the temperature is kept at 580 ℃ for 3h for dehydrogenation treatment, then the temperature is directly raised to 1030 ℃ for sintering for 5h, and other steps are the same as those of the example 1 and are not repeated.
Comparative example 3
Comparative example 3 the composition Nd of the base alloy A in example 1 was directly used28.0Fe69.57Co1.0Cu0.1Al0.1Ga0.2Zr0.05B0.98And Dy as the constituent of alloy B with thickened grain boundary10.65Nd83.35Cu4.0Ga2.0Mixing according to the mass ratio of 96:4, namely according to Pr0.950Nd29.730Fe66.787Co0.960Cu0.216Al0.176Ga0.192Zr0.048B0.941The components are proportioned, the raw materials are smelted and cast on a copper roller with the rotating speed of 1.5m/s by adopting a rapid hardening process to obtain a casting sheet with the average thickness of 0.3mm, the smelting temperature is 1460 ℃, and the casting temperature is 1420 ℃; placing the cast piece in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in nitrogen protection to obtain coarse broken powder with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder in an airflow mill in nitrogen atmosphere protection to obtain airflow mill magnetic powder with the average particle size of 4 mu m; adding 0.3 wt% of lubricant stearic acid into jet mill magnetic powder, stirring for 4h, and then stirring in argonCarrying out orientation forming in a magnetic field with the magnetic field intensity of 1.4T in the atmosphere, and pressing into a green body in a water isostatic pressing at 200 MPa; and sintering the green body in a vacuum sintering furnace, preserving heat for 3h at 580 ℃ for dehydrogenation treatment, sintering at 900 ℃ for 15h, heating to 1030 ℃ for sintering for 5h, cooling to room temperature, heating to 900 ℃ for primary tempering for 2.5h, cooling to 500 ℃ for secondary tempering for 4.5h, and preparing the sintered neodymium-iron-boron magnet.
Comparative example 4
Comparative example 4 base alloy A composition Nd according to example 2 directly30.0Fe67.3Co1.1Cu0.15Al0.12Nb0.08B1.25And Dy as the constituent of alloy B with thickened grain boundary10.65Nd83.35Cu4.0Ga2.0Mixing according to a mass ratio of 97:3, namely according to Nd31.601Dy0.320Fe65.281Co1.067Cu0.266Al0.116Ga0.06Nb0.078B1.211The components are proportioned, the raw materials are smelted and cast on a copper roller with the rotating speed of 1.5m/s by adopting a rapid hardening process to obtain a casting sheet with the average thickness of 0.3mm, the smelting temperature is 1480 ℃, and the casting temperature is 1420 ℃; placing the cast piece in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in nitrogen protection to obtain coarse broken powder with the granularity of less than or equal to 300 mu m, and then grinding the coarse broken powder in an airflow mill in nitrogen atmosphere protection to obtain airflow mill magnetic powder with the average particle size of 5 mu m; adding 0.3 wt% of lubricant stearic acid into jet mill magnetic powder, stirring for 5h, then carrying out orientation forming in a magnetic field with the magnetic field intensity of 1.4T in the argon atmosphere, and pressing into a green body in a water isostatic pressing at 180 MPa; and sintering the green body in a vacuum sintering furnace, preserving heat for 4h at 560 ℃ for dehydrogenation treatment, sintering at 850 ℃ for 14h, heating to 1040 ℃ for sintering for 4h, cooling to room temperature, heating to 890 ℃ for primary tempering for 2h, cooling to 510 ℃ for secondary tempering for 5h, and preparing the sintered neodymium-iron-boron magnet.
Fig. 1 is a structural view of a sintered ndfeb magnet according to example 1, and fig. 2 is a structural view of a sintered ndfeb magnet according to comparative example 3. As can be seen from fig. 1 and 2, the grain boundaries between the grains of the sintered nd-fe-b magnet of example 1 are uniformly dispersed and have a large thickness, while the grain boundaries of comparative example 3 are non-uniform and have a small thickness.
The sintered nd-fe-b magnets prepared in examples 1-6 and comparative examples 1-4 were measured for magnetic properties using a magnetometer, and the data are shown in table 1 below.
TABLE 1 magnetic Properties of sintered NdFeB magnets of examples 1-6 and comparative examples 1-4
As shown in Table 1, examples 1 and 2 are preferred examples having higher Br, Hcj, (BH) m, Hk/Hcj values; comparative example 1 the grain boundary-thickened alloy B was cast into a cast piece, the oxidation resistance was reduced, and the magnetic properties were reduced; comparative example 2 is not pre-sintered, the grain boundary thickening alloy B is not uniformly dispersed at the grain boundary, the grain boundary thickening effect is greatly reduced, and partial components can enter the matrix phase to reduce the magnetic performance of the magnet; the comparative example 3 and the example 4 directly cast and crush the two alloy components at the same time, so that the grain boundary among the grains of the neodymium iron boron magnet is uneven, the thickness of the grain boundary is smaller, and the magnetic performance is greatly reduced.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. The high-performance sintered neodymium-iron-boron magnet is characterized in that the preparation raw materials of the high-performance sintered neodymium-iron-boron magnet comprise a matrix alloy A and a grain boundary thickening alloy B;
the composition component of the base alloy A is RxTyMzB(1-x-y-z)Wherein R is one or more of Nd, Pr, La, Ce, Dy and Tb, M is one or more of Cu, Al and Ga and one or two of Nb and Zr, T is Fe and Co, and the mass ratio of Fe to Co is (40-100): 1, x is 28-33 wt%, y is 58-72 wt%, and z is 0-2.0 wt%;
the component R of the alloy B with thickened grain boundaryxM(1-x)Wherein R is one or more of Nd, Pr, Dy and Tb, M is one or more of Cu, Al and Ga, and x is 80-95 wt%.
2. The method for preparing a high-performance sintered neodymium-iron-boron magnet according to claim 1, comprising the following steps:
(1) preparing raw materials according to the composition of the matrix alloy A, and smelting and casting the raw materials by adopting a rapid hardening process to obtain a cast piece A; placing the cast piece A in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in inert atmosphere to obtain coarse broken powder A, and then grinding the coarse broken powder A in an airflow mill protected by inert atmosphere to obtain airflow mill magnetic powder A;
(2) preparing raw materials according to the components of the grain boundary thickening alloy B, and smelting and casting the raw materials to obtain an ingot B; placing the ingot B in a hydrogen breaking furnace, filling hydrogen for breaking, sieving in an argon protection box to obtain coarse broken powder B, and then grinding the coarse broken powder B in a jet mill protected by argon atmosphere to obtain jet mill magnetic powder B;
(3) mixing the jet milling magnetic powder A and the jet milling magnetic powder B, adding a lubricant, stirring for 2-6 h, then carrying out orientation forming in an inert atmosphere, and then carrying out isostatic pressing treatment;
(4) and (3) feeding the blank subjected to isostatic pressing treatment into a sintering furnace, preserving heat for 2-5 hours at 550-600 ℃ for dehydrogenation treatment, and then performing presintering, high-temperature sintering and tempering heat treatment.
3. The preparation method of the high-performance sintered neodymium-iron-boron magnet according to claim 2, wherein the smelting temperature in the step (1) and the step (2) is 1450-1500 ℃, and the casting temperature is 1400-1450 ℃; when the rapid hardening process is adopted, the rotating speed of the copper roller is 1.2-1.5 m/s, and the average thickness of the obtained cast sheet A is 0.2-0.4 mm.
4. The method for preparing a high-performance sintered NdFeB magnet according to claim 2, wherein the average particle size of the jet-milled magnetic powder A in the step (1) is 4-5 μm.
5. The method for preparing a high-performance sintered NdFeB magnet according to claim 2, wherein the average particle size of the jet-milled magnetic powder B in the step (2) is 1-2 μm.
6. The method for preparing a high-performance sintered neodymium-iron-boron magnet according to claim 2, wherein in the mixture of the jet milling magnetic powder A and the jet milling magnetic powder B in the step (3), the content of the jet milling magnetic powder B is 1-5 wt%.
7. The method for preparing a high-performance sintered NdFeB magnet according to claim 2, wherein the magnetic field strength of the orientation molding in the step (3) is 1.0-1.5T, and the isostatic pressure is 150-220 MPa.
8. The method for preparing the high-performance sintered neodymium-iron-boron magnet according to claim 2, wherein the pre-sintering in the step (4) is performed at 800-1000 ℃ for 10-15 hours.
9. The method for preparing a high-performance sintered NdFeB magnet according to claim 8, wherein the pre-sintering in the step (4) is performed by keeping the temperature at 850-950 ℃ for 12-15 h.
10. The preparation method of the high-performance sintered neodymium-iron-boron magnet according to claim 2, characterized in that the high-temperature sintering temperature in the step (4) is 1030-1100 ℃, and the sintering time is 4-6 h; the tempering heat treatment comprises the following steps: the primary tempering temperature is 800-920 ℃, and the tempering time is 2-4 hours; the secondary tempering temperature is 460-560 ℃, and the tempering time is 4-6 hours.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011291859.4A CN112435820B (en) | 2020-11-18 | 2020-11-18 | High-performance sintered NdFeB magnet and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011291859.4A CN112435820B (en) | 2020-11-18 | 2020-11-18 | High-performance sintered NdFeB magnet and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN112435820A true CN112435820A (en) | 2021-03-02 |
CN112435820B CN112435820B (en) | 2024-09-24 |
Family
ID=74693139
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011291859.4A Active CN112435820B (en) | 2020-11-18 | 2020-11-18 | High-performance sintered NdFeB magnet and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112435820B (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114171314A (en) * | 2022-02-10 | 2022-03-11 | 京磁材料科技股份有限公司 | Preparation method of high-performance sintered neodymium-iron-boron permanent magnet |
CN114724837A (en) * | 2022-03-28 | 2022-07-08 | 江西理工大学 | Method for preparing neodymium iron boron magnet by utilizing material defects |
CN117275864A (en) * | 2023-10-08 | 2023-12-22 | 江苏普隆磁电有限公司 | Preparation method and application of high-performance neodymium-iron-boron magnet |
Citations (28)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003049234A (en) * | 2001-05-30 | 2003-02-21 | Sumitomo Special Metals Co Ltd | Method for producing sintered compact for rare earth magnet |
CN1688000A (en) * | 2005-06-06 | 2005-10-26 | 浙江大学 | Method for increasing sintering Nd-Fe-B coercive force by adding nano-oxide in crystal boundary phase |
CN101320609A (en) * | 2008-03-21 | 2008-12-10 | 浙江大学 | Grain boundary phase-reconstructed high-corrosion resistance Sintered NdFeB magnet and preparation method thereof |
CN101958171A (en) * | 2010-04-14 | 2011-01-26 | 无锡南理工科技发展有限公司 | Method for preparing corrosion-resistant sintered neodymium iron boron (NdFeB) magnet |
CN102220538A (en) * | 2011-05-17 | 2011-10-19 | 南京理工大学 | Sintered neodymium-iron-boron preparation method capable of improving intrinsic coercivity and anticorrosive performance |
CN102280240A (en) * | 2011-08-23 | 2011-12-14 | 南京理工大学 | Method for preparing sintered NdFeB with low dysprosium content and high performance |
JP2012248827A (en) * | 2011-05-02 | 2012-12-13 | Shin Etsu Chem Co Ltd | Rare earth permanent magnet and method for producing the same |
CN103065787A (en) * | 2012-12-26 | 2013-04-24 | 宁波韵升股份有限公司 | Method for preparing sintered neodymium-iron-boron magnet |
CN103366943A (en) * | 2013-07-17 | 2013-10-23 | 宁波韵升股份有限公司 | Method for improving performance of sintered NdFeB magnetic sheet |
CN103985533A (en) * | 2014-04-16 | 2014-08-13 | 安泰科技股份有限公司 | Method for improving coercivity of sintered neodymium-ferro-boron magnet by doping with eutectic alloy hydrides |
CN103996519A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Manufacturing method for high-performance NdFeB rare earth permanent magnet devices |
US20140292454A1 (en) * | 2013-03-28 | 2014-10-02 | Tdk Corporation | Rare earth based magnet |
CN104269238A (en) * | 2014-09-30 | 2015-01-07 | 宁波科田磁业有限公司 | High-performance sintered neodymium-iron-boron magnet and preparation method |
CN104505206A (en) * | 2014-12-04 | 2015-04-08 | 浙江大学 | Preparation method of high-coercivity sintered Nd-Fe-B and product |
CN104575903A (en) * | 2014-11-26 | 2015-04-29 | 宁波格荣利磁业有限公司 | Neodymium iron boron magnet added with Dy powder and preparation method thereof |
CN105185499A (en) * | 2015-08-07 | 2015-12-23 | 宁波华辉磁业有限公司 | High-performance sintered neodymium-iron-boron rare-earth permanent magnetic material and preparation method thereof |
JP2018029107A (en) * | 2016-08-17 | 2018-02-22 | 日立金属株式会社 | Method of manufacturing r-t-b based sintered magnet |
CN107742564A (en) * | 2017-10-31 | 2018-02-27 | 中钢集团安徽天源科技股份有限公司 | A kind of method that auxiliary alloy addition of high dysprosium prepares low-cost neodymium iron boron magnet |
CN108281270A (en) * | 2018-01-05 | 2018-07-13 | 宁波招宝磁业有限公司 | The method that metal vapors heat treatment prepares high-performance neodymium-iron-boron magnet |
CN108565086A (en) * | 2018-05-11 | 2018-09-21 | 包头稀土研究院 | The preparation method of high energy product high-coercive force Sintered NdFeB magnet |
CN108766753A (en) * | 2018-05-11 | 2018-11-06 | 包头稀土研究院 | The preparation method of high energy product high-coercive force Sintered NdFeB magnet |
JP2018174311A (en) * | 2017-03-30 | 2018-11-08 | 日立金属株式会社 | Method for manufacturing r-t-b based sintered magnet |
CN109585108A (en) * | 2017-09-28 | 2019-04-05 | 日立金属株式会社 | The manufacturing method of R-T-B based sintered magnet and diffusion source |
CN110853856A (en) * | 2019-11-22 | 2020-02-28 | 安泰科技股份有限公司 | High-coercivity cerium-containing magnet and preparation method thereof |
CN111383833A (en) * | 2019-11-11 | 2020-07-07 | 浙江东阳东磁稀土有限公司 | Grain boundary diffusion method for rare earth neodymium iron boron magnet |
CN111378907A (en) * | 2020-04-08 | 2020-07-07 | 甘肃稀土新材料股份有限公司 | Auxiliary alloy for improving coercive force of neodymium iron boron permanent magnet material and application method |
CN111554500A (en) * | 2020-04-26 | 2020-08-18 | 有研稀土(荣成)有限公司 | High-temperature-resistant sintered neodymium-iron-boron permanent magnet and preparation method thereof |
CN111834118A (en) * | 2020-07-02 | 2020-10-27 | 宁波永久磁业有限公司 | Method for improving coercive force of sintered neodymium-iron-boron magnet and sintered neodymium-iron-boron magnet |
-
2020
- 2020-11-18 CN CN202011291859.4A patent/CN112435820B/en active Active
Patent Citations (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003049234A (en) * | 2001-05-30 | 2003-02-21 | Sumitomo Special Metals Co Ltd | Method for producing sintered compact for rare earth magnet |
CN1688000A (en) * | 2005-06-06 | 2005-10-26 | 浙江大学 | Method for increasing sintering Nd-Fe-B coercive force by adding nano-oxide in crystal boundary phase |
CN101320609A (en) * | 2008-03-21 | 2008-12-10 | 浙江大学 | Grain boundary phase-reconstructed high-corrosion resistance Sintered NdFeB magnet and preparation method thereof |
CN101958171A (en) * | 2010-04-14 | 2011-01-26 | 无锡南理工科技发展有限公司 | Method for preparing corrosion-resistant sintered neodymium iron boron (NdFeB) magnet |
JP2012248827A (en) * | 2011-05-02 | 2012-12-13 | Shin Etsu Chem Co Ltd | Rare earth permanent magnet and method for producing the same |
CN102220538A (en) * | 2011-05-17 | 2011-10-19 | 南京理工大学 | Sintered neodymium-iron-boron preparation method capable of improving intrinsic coercivity and anticorrosive performance |
CN102280240A (en) * | 2011-08-23 | 2011-12-14 | 南京理工大学 | Method for preparing sintered NdFeB with low dysprosium content and high performance |
CN103065787A (en) * | 2012-12-26 | 2013-04-24 | 宁波韵升股份有限公司 | Method for preparing sintered neodymium-iron-boron magnet |
US20150071810A1 (en) * | 2012-12-26 | 2015-03-12 | Ningbo Yunsheng Co., Ltd. | Method for preparing neodymium-iron-boron (nd-fe-b)-based sintered magnet |
US20140292454A1 (en) * | 2013-03-28 | 2014-10-02 | Tdk Corporation | Rare earth based magnet |
CN103366943A (en) * | 2013-07-17 | 2013-10-23 | 宁波韵升股份有限公司 | Method for improving performance of sintered NdFeB magnetic sheet |
CN103985533A (en) * | 2014-04-16 | 2014-08-13 | 安泰科技股份有限公司 | Method for improving coercivity of sintered neodymium-ferro-boron magnet by doping with eutectic alloy hydrides |
CN103996519A (en) * | 2014-05-11 | 2014-08-20 | 沈阳中北通磁科技股份有限公司 | Manufacturing method for high-performance NdFeB rare earth permanent magnet devices |
CN104269238A (en) * | 2014-09-30 | 2015-01-07 | 宁波科田磁业有限公司 | High-performance sintered neodymium-iron-boron magnet and preparation method |
CN104575903A (en) * | 2014-11-26 | 2015-04-29 | 宁波格荣利磁业有限公司 | Neodymium iron boron magnet added with Dy powder and preparation method thereof |
CN104505206A (en) * | 2014-12-04 | 2015-04-08 | 浙江大学 | Preparation method of high-coercivity sintered Nd-Fe-B and product |
CN105185499A (en) * | 2015-08-07 | 2015-12-23 | 宁波华辉磁业有限公司 | High-performance sintered neodymium-iron-boron rare-earth permanent magnetic material and preparation method thereof |
JP2018029107A (en) * | 2016-08-17 | 2018-02-22 | 日立金属株式会社 | Method of manufacturing r-t-b based sintered magnet |
JP2018174311A (en) * | 2017-03-30 | 2018-11-08 | 日立金属株式会社 | Method for manufacturing r-t-b based sintered magnet |
CN109585108A (en) * | 2017-09-28 | 2019-04-05 | 日立金属株式会社 | The manufacturing method of R-T-B based sintered magnet and diffusion source |
CN107742564A (en) * | 2017-10-31 | 2018-02-27 | 中钢集团安徽天源科技股份有限公司 | A kind of method that auxiliary alloy addition of high dysprosium prepares low-cost neodymium iron boron magnet |
CN108281270A (en) * | 2018-01-05 | 2018-07-13 | 宁波招宝磁业有限公司 | The method that metal vapors heat treatment prepares high-performance neodymium-iron-boron magnet |
CN108766753A (en) * | 2018-05-11 | 2018-11-06 | 包头稀土研究院 | The preparation method of high energy product high-coercive force Sintered NdFeB magnet |
CN108565086A (en) * | 2018-05-11 | 2018-09-21 | 包头稀土研究院 | The preparation method of high energy product high-coercive force Sintered NdFeB magnet |
CN111383833A (en) * | 2019-11-11 | 2020-07-07 | 浙江东阳东磁稀土有限公司 | Grain boundary diffusion method for rare earth neodymium iron boron magnet |
CN110853856A (en) * | 2019-11-22 | 2020-02-28 | 安泰科技股份有限公司 | High-coercivity cerium-containing magnet and preparation method thereof |
CN111378907A (en) * | 2020-04-08 | 2020-07-07 | 甘肃稀土新材料股份有限公司 | Auxiliary alloy for improving coercive force of neodymium iron boron permanent magnet material and application method |
CN111554500A (en) * | 2020-04-26 | 2020-08-18 | 有研稀土(荣成)有限公司 | High-temperature-resistant sintered neodymium-iron-boron permanent magnet and preparation method thereof |
CN111834118A (en) * | 2020-07-02 | 2020-10-27 | 宁波永久磁业有限公司 | Method for improving coercive force of sintered neodymium-iron-boron magnet and sintered neodymium-iron-boron magnet |
Non-Patent Citations (1)
Title |
---|
郑华均, 黄建国, 马淳安, 郑国渠: "退火处理对烧结钕铁硼永磁体磁性能的影响", 金属热处理, no. 11, 25 November 2003 (2003-11-25), pages 22 - 25 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114171314A (en) * | 2022-02-10 | 2022-03-11 | 京磁材料科技股份有限公司 | Preparation method of high-performance sintered neodymium-iron-boron permanent magnet |
CN114171314B (en) * | 2022-02-10 | 2022-04-26 | 京磁材料科技股份有限公司 | Preparation method of high-performance sintered neodymium-iron-boron permanent magnet |
CN114724837A (en) * | 2022-03-28 | 2022-07-08 | 江西理工大学 | Method for preparing neodymium iron boron magnet by utilizing material defects |
CN117275864A (en) * | 2023-10-08 | 2023-12-22 | 江苏普隆磁电有限公司 | Preparation method and application of high-performance neodymium-iron-boron magnet |
CN117275864B (en) * | 2023-10-08 | 2024-05-03 | 江苏普隆磁电有限公司 | Preparation method and application of high-performance neodymium-iron-boron magnet |
Also Published As
Publication number | Publication date |
---|---|
CN112435820B (en) | 2024-09-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101266855B (en) | Rare earth permanent magnetism material and its making method | |
CN102568807B (en) | Method for preparing high-coercivity SmCoFeCuZr (samarium-cobalt-ferrum-copper-zirconium) high-temperature permanent magnet by doping nano-Cu powder | |
CN106920617B (en) | High-performance Ne-Fe-B rare earth permanent-magnetic material and preparation method thereof | |
CN112435820B (en) | High-performance sintered NdFeB magnet and preparation method thereof | |
JP7418598B2 (en) | Heavy rare earth alloys, neodymium iron boron permanent magnet materials, raw materials and manufacturing methods | |
CN103426578B (en) | A kind of rare earth permanent-magnetic material and preparation method thereof | |
CN103971875B (en) | Mg-Cu grain boundary modified high-magnetism sintered Nd-Fe-B magnet and preparation process thereof | |
EP4020505B1 (en) | Preparation method for a neodymium-iron-boron magnet | |
CN109712770B (en) | Samarium cobalt magnet and method of making same | |
KR102631761B1 (en) | Neodymium iron boron magnetic material, raw material composition, manufacturing method and application | |
CN107958760B (en) | Rare earth permanent magnetic material and preparation method thereof | |
JP6828027B2 (en) | A method for producing an R-Fe-B-based rare earth sintered magnet containing a composite of Pr and W. | |
KR102632991B1 (en) | Neodymium iron boron magnetic material, raw material composition, manufacturing method and application | |
CN108269665A (en) | A kind of neodymium iron boron magnetic body and preparation method thereof | |
CN112750587A (en) | Preparation method of high-performance sintered samarium-cobalt magnet | |
CN107689279A (en) | One kind improves the coercitive method of sintered NdFeB built-up magnet | |
CN110957090A (en) | A samarium cobalt 1: 5-type permanent magnet material and preparation method thereof | |
CN105118655A (en) | Method for preparing high-coercivity magnet by modifying nano zinc powder crystal boundary | |
CN112582122A (en) | Preparation method of high-knee-point coercive force sintered samarium-cobalt magnet | |
CN114823027A (en) | High-boron neodymium-iron-boron permanent magnet material and preparation method thereof | |
JP2011014631A (en) | R-t-b-based rare-earth permanent magnet, and motor, automobile, generator and wind turbine generator | |
CN112420306B (en) | High-performance sintered NdFeB magnetic ring and preparation method thereof | |
CN104299743A (en) | Rare earth magnet | |
CN112582123B (en) | Preparation method of sintered samarium-cobalt magnet with low temperature coefficient and high use temperature | |
CN104752048B (en) | A kind of preparation method of sintered Nd-Fe-B permanent magnet |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |