CN116844810A - High-cerium-content high-performance neodymium-iron-boron magnet and preparation method thereof - Google Patents
High-cerium-content high-performance neodymium-iron-boron magnet and preparation method thereof Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 57
- 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 claims abstract description 92
- 239000000843 powder Substances 0.000 claims abstract description 57
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 20
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005496 tempering Methods 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000009792 diffusion process Methods 0.000 claims description 42
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 34
- 229910001279 Dy alloy Inorganic materials 0.000 claims description 20
- 229910001117 Tb alloy Inorganic materials 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 16
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 13
- 229910000636 Ce alloy Inorganic materials 0.000 claims description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 238000005324 grain boundary diffusion Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 39
- 238000001514 detection method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012071 phase Substances 0.000 description 8
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 229910052779 Neodymium Inorganic materials 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
-
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The application discloses a high-cerium-content high-performance neodymium-iron-boron magnet and a preparation method thereof, wherein the high-cerium-content high-performance neodymium-iron-boron magnet comprises a magnet core structure, and the magnet core structure comprises a main phase alloy I and a main phase alloy II; the main phase alloy I comprises (Ce x ,Nd 1‑x ) a Fe b B c X is more than or equal to 0.6 and less than or equal to 0.9, and a+b+c=100 wt%; major phase alloy II includes Nd 2 Fe 14 B. The preparation method of the neodymium-iron-boron magnet with high cerium content and high performance comprises the following steps: preparing powder of a main phase alloy I and powder of a main phase alloy II, and mixing to obtain mixed powder; placing the mixed powder in an orientation magnetic field, and performing stamping forming to obtain a green body; and sintering and tempering the green body, and cooling to obtain the magnet core structure. The application has the advantages that the light rare earth element Ce is adopted to replace the heavy rare earth element Nd, and the NdFeB is realized at lower cost while the heavy rare earth element with lower content is usedThe magnet also has high performance.
Description
Technical Field
The application relates to the technical field of rare earth permanent magnet materials, in particular to a neodymium-iron-boron magnet with high cerium content and high performance and a preparation method thereof.
Background
The neodymium-iron-boron magnet is a tetragonal crystal formed by neodymium, iron and boron, has excellent magnetic performance, extremely high magnetic energy product and extremely strong coercive force, and is widely applied to the fields of electronics, electric machinery, medical equipment, toys, packaging, hardware machinery, aerospace, and the like. Thus, neodymium-iron-boron magnets have a wide range of commercial applications.
The existing neodymium-iron-boron magnet is mostly prepared by adopting heavy rare earth elements to replace neodymium elements. However, the heavy rare earth element belongs to a rare and non-renewable resource, and the preparation of the neodymium-iron-boron magnet by excessively relying on the heavy rare earth element is high in cost and easy to cause unbalance of the resource, so that the sustainable development concept is contrary. However, when the light rare earth element is used to partially replace the neodymium element, the performance of the neodymium-iron-boron magnet is reduced more rapidly with the increase of the replacement amount of the light rare earth element. Therefore, when preparing neodymium-iron-boron magnets with lower contents of heavy rare earth elements, the performance of the neodymium-iron-boron magnets tends to be poor.
In view of the foregoing, there is a need for a neodymium-iron-boron magnet with a low content of heavy rare earth elements to achieve a low cost and high performance, so as to solve the problems in the prior art.
Disclosure of Invention
In order to solve at least one of the technical problems, a neodymium-iron-boron magnet with lower cost and higher performance is developed by using a heavy rare earth element with lower content.
On one hand, the neodymium-iron-boron magnet with high cerium content and high performance comprises a magnet core structure, wherein the magnet core structure comprises a main phase alloy I and a main phase alloy II, and the mass ratio of the main phase alloy I to the main phase alloy II is 3-5:1; the main phase alloy I comprises the following components: (Ce) x ,Nd 1-x ) a Fe b B c X is more than or equal to 0.6 and less than or equal to 0.9, and a+b+c=100 wt%; wherein, b is more than or equal to 20wt% and less than or equal to 30wt%, c is more than or equal to 1wt% and less than or equal to 2wt%, and the rest is a; the main phase alloy II comprises the following components: nd 2 Fe 14 B。
By adopting the technical scheme, the neodymium iron boron magnet provided by the application is formed by adopting a double main phase alloy, and the content of the main phase alloy I containing the light rare earth element Ce is obviously higher than that of the main phase alloy II without the light rare earth element Ce; namely, in the known Nd 2 Fe 14 B main phase, incorporating the specific (Ce x ,Nd 1-x ) a Fe b B c The main phase is formed by (Ce x ,Nd 1-x ) a Fe b B c The component-based neodymium-iron-boron magnet with high cerium content reduces heavy rare earthThe proportion and the utilization rate of the element Nd in the neodymium-iron-boron magnet improve the utilization rate of the light rare earth element Ce with relatively rich reserves, and can effectively reduce the cost when the neodymium-iron-boron magnet uses the heavy rare earth element; meanwhile, compared with the neodymium-iron-boron magnet in the prior art, which directly adopts light rare earth element Ce to partially replace heavy rare earth element Nd, the neodymium-iron-boron magnet provided by the application has high cerium content and is more similar to Nd 2 Fe 14 The component proportion of B can effectively reduce the rapid deterioration of the magnetic performance of the neodymium-iron-boron magnet caused by the substitution of the light rare earth element Ce for the heavy rare earth element Nd, so that the neodymium-iron-boron magnet provided by the application can meet the requirement of high performance while realizing lower cost by using the heavy rare earth element with lower content.
Optionally, the main phase alloy i comprises the following components: (Ce) x ,Nd 1-x ) a Fe b B c X=0.83, a+b+c=100 wt%; wherein a=75.3 wt%, b=23.5 wt%, c=1.2 wt%.
By adopting the technical scheme, when the components of the main phase alloy I adopt a specific proportion, the performance of the neodymium iron boron magnet provided by the application is better.
Optionally, the magnetic diffusion source is attached to the surface of the magnetic core structure, and forms a shell layer on the periphery of the crystal grains of the main phase alloy I and the main phase alloy II after being diffused through the crystal boundary.
By adopting the technical scheme, the magnet diffusion source is also attached to the surface of the magnet core structure of the neodymium-iron-boron magnet provided by the application, and can be diffused from outside to inside to the inside of the magnet core structure after being diffused by the grain boundary, and a shell layer is formed on the periphery of crystal grains of the main phase alloy I and the main phase alloy II, so that the neodymium-iron-boron magnet provided by the application forms a 'core-shell structure', the coercive force of the neodymium-iron-boron magnet provided by the application can be further improved, and the performance of the neodymium-iron-boron magnet provided by the application is further improved.
Optionally, the magnet diffusion source includes a Dy/Tb alloy diffusion source and an Al-Ce alloy diffusion source, the Dy/Tb alloy diffusion source is disposed along a magnetic pole edge of the magnet core structure, an area of attachment of the Dy/Tb alloy diffusion source is 20-30% of an area of the magnetic pole of the magnet core structure, and the remaining surfaces of the magnet core structure are all attached by the Al-Ce alloy diffusion source.
By adopting the technical scheme, the magnet diffusion source of the neodymium-iron-boron magnet provided by the application is further limited, the adopted magnet diffusion source is composed of an alloy formed by heavy rare earth elements Dy/Tb and an Al-Ce alloy containing light rare earth elements Ce, a composite diffusion source formed by the heavy rare earth elements and the light rare earth elements is formed, and the attachment positions and the attachment areas of the Dy/Tb alloy diffusion source and the Al-Ce alloy diffusion source are limited, so that the Dy/Tb alloy diffusion source can provide more liquid phases with low melting points while strengthening the easily demagnetized part of the magnet core structure of the neodymium-iron-boron magnet provided by the application, and the grain boundary diffusion of the Dy/Tb alloy diffusion source is promoted, thereby realizing the purpose of reducing the consumption of the heavy rare earth elements and further improving the coercive force of the neodymium-iron-boron magnet provided by the application, and further improving the performance of the neodymium-iron-boron magnet provided by the application.
In a second aspect, the application provides a preparation method of the neodymium-iron-boron magnet with high cerium content and high performance, which comprises the following steps:
s1, preparing powder of a main phase alloy I and powder of a main phase alloy II;
s2, mixing the powder of the main phase alloy I and the powder of the main phase alloy II according to the mass ratio of 3-5:1 to obtain mixed powder;
s3, placing the mixed powder in an orientation magnetic field, and performing stamping forming to obtain a green body;
s4, sintering and tempering the green body, and cooling to obtain a magnet core structure, wherein the magnet core structure forms the neodymium-iron-boron magnet with high cerium content and high performance.
By adopting the technical scheme, the catalyst (Ce x ,Nd 1-x ) a Fe b B c Powder of main phase alloy I is introduced with Nd 2 Fe 14 In the powder of the B main phase alloy II, the application is adoptedThe neodymium-iron-boron magnet prepared by the preparation method provided by the application has the characteristic of high cerium content, reduces the proportion and the utilization rate of the heavy rare earth element Nd in the neodymium-iron-boron magnet, and can effectively reduce the cost when the heavy rare earth element Nd is used for preparing the neodymium-iron-boron magnet; meanwhile, the application adopts the double main phase alloy method to prepare the neodymium-iron-boron magnet, so that the prepared neodymium-iron-boron magnet has high cerium content and is more similar to Nd 2 Fe 14 The component proportion of B effectively reduces the rapid deterioration of the magnetic performance of the neodymium-iron-boron magnet caused by the substitution of the light rare earth element Ce for the heavy rare earth element Nd, so that the prepared neodymium-iron-boron magnet can meet the requirement of high performance while realizing lower cost by using the heavy rare earth element with lower content.
Optionally, in the step S1, the method for preparing the powder of the main phase alloy i is as follows:
step one: weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the components of the main phase alloy I to obtain a target raw material I;
step two: smelting and casting the target raw material I to obtain an alloy sheet I;
step three: carrying out hydrogen crushing treatment on the alloy sheet I to obtain coarse powder of main phase Jin;
step four: and further grinding the coarse powder of the main phase alloy I by adopting an air flow mill to obtain powder of the main phase alloy I.
By adopting the technical scheme, the coarse powder of the main phase alloy I is further ground by adopting the air flow mill, so that the prepared powder of the main phase alloy I is easier to mix with the powder of the main phase alloy II, and the uniformity of the mixed powder is further improved; meanwhile, the waste after further grinding is recycled by adopting the double cyclone air flow mill, and the waste of raw materials is reduced.
Optionally, in the step S1, the method for preparing the powder of the main phase alloy ii is as follows:
step one: weighing and proportioning pure Nd, pure Fe and boron powder according to the components of a main phase alloy II to obtain a target raw material II; step two: smelting and casting the target raw material II to obtain an alloy sheet II;
step three: carrying out hydrogen crushing treatment on the alloy sheet II to obtain coarse powder of main phase Jin;
step four: and further grinding the coarse powder of the main phase alloy II by adopting an air flow mill to prepare powder of the main phase alloy II.
By adopting the technical scheme, the coarse powder of the main phase alloy II is further ground by adopting the air flow mill, so that the prepared powder of the main phase alloy II is easier to mix with the powder of the main phase alloy I, and the uniformity of the mixed powder is further improved; meanwhile, the waste after further grinding is recycled by adopting the double cyclone air flow mill, and the waste of raw materials is reduced.
Optionally, in the step S4, the sintering process conditions are as follows: the sintering temperature is 1050-1200 ℃ and the sintering time is 3-5 h; the tempering treatment conditions are as follows: the tempering temperature is 600-900 ℃ and the tempering time is 5-8 h.
Optionally, the method further comprises a step S5 of performing grain boundary diffusion treatment on the magnet core structure, and the method comprises the following steps:
s5.1, cleaning the surface of the magnet core structure to obtain a magnet core structure with a clean surface;
s5.2, performing magnetron sputtering of a Dy/Tb alloy diffusion source along the magnetic pole edge of the magnet core structure with the clean surface, performing magnetron sputtering of an Al-Ce alloy diffusion source on the other surfaces of the magnet core structure with the clean surface, wherein the magnetron sputtering area of the Dy/Tb alloy diffusion source is 20-30% of the magnetic pole area of the magnet core structure with the clean surface, and preparing a preparation magnet block; s5.3, placing the prepared magnet block in an environment with the temperature of 750-900 ℃, carrying out heat preservation treatment for 6-8 h, then placing in an environment with the temperature of 450-550 ℃, carrying out tempering treatment for 2-3 h, and cooling.
By adopting the technical scheme, in the preparation method of the neodymium-iron-boron magnet, when grain boundary diffusion is carried out, the selected diffusion source is a composite diffusion source consisting of an alloy consisting of heavy rare earth elements Dy/Tb and an Al-Ce alloy containing light rare earth elements Ce, and the positions and the attachment areas of magnetron sputtering of the Dy/Tb alloy diffusion source and the Al-Ce alloy diffusion source are limited, so that the performance of the neodymium-iron-boron magnet provided by the application is further improved.
Optionally, the preparation method of the high-cerium-content high-performance neodymium-iron-boron magnet is carried out in a closed environment, and the oxygen content is controlled within 20 ppm.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the neodymium-iron-boron magnet provided by the application is formed by adopting double main phase alloy, and is prepared from the known Nd 2 Fe 14 B main phase, incorporating the specific (Ce x ,Nd 1-x ) a Fe b B c The main phase is formed by (Ce x ,Nd 1-x ) a Fe b B c The neodymium-iron-boron magnet with high cerium content mainly contains the components, reduces the proportion and the use ratio of the heavy rare earth element Nd in the neodymium-iron-boron magnet, improves the use ratio of the light rare earth element Ce with relatively rich reserves, and can effectively reduce the cost when the heavy rare earth element is used by the neodymium-iron-boron magnet.
2. Compared with the prior art, the neodymium-iron-boron magnet provided by the application is formed by adopting the double main phase alloy, so that the neodymium-iron-boron magnet provided by the application has high cerium content and is more similar to Nd 2 Fe 14 The component proportion of B can effectively reduce the rapid deterioration of the magnetic performance of the neodymium-iron-boron magnet caused by the substitution of the light rare earth element Ce for the heavy rare earth element Nd, so that the neodymium-iron-boron magnet provided by the application can meet the requirement of high performance while realizing lower cost by using the heavy rare earth element with lower content.
Detailed Description
The present application will be described in further detail with reference to examples and comparative examples.
The application designs a neodymium-iron-boron magnet with high cerium content and high performance, which comprises a magnet core structure, wherein the magnet core structure comprises a main phase alloy I and a main phase alloy II, and the mass ratio of the main phase alloy I to the main phase alloy II is 3-5:1; by a means ofThe main phase alloy I comprises the following components: (Ce) x ,Nd 1-x ) a Fe b B c X is more than or equal to 0.6 and less than or equal to 0.9, and a+b+c=100 wt%; wherein, b is more than or equal to 20wt% and less than or equal to 30wt%, c is more than or equal to 1wt% and less than or equal to 2wt%, and the rest is a; the main phase alloy II comprises the following components: nd 2 Fe 14 B。
The preparation method of the high-cerium-content high-performance neodymium-iron-boron magnet comprises the following steps:
s1, preparing powder of a main phase alloy I and powder of a main phase alloy II;
s2, mixing the powder of the main phase alloy I and the powder of the main phase alloy II according to the mass ratio of 3-5:1 to obtain mixed powder;
s3, placing the mixed powder in an orientation magnetic field, and performing stamping forming to obtain a green body;
s4, sintering and tempering the green body, and cooling to obtain a magnet core structure, wherein the magnet core structure forms the neodymium-iron-boron magnet with high cerium content and high performance.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following are preparation examples 1 to 7 of the present application, preparation examples 1 to 6 provide a powder of a main phase alloy I, respectively, and preparation example 7 provides a powder of a main phase alloy II; wherein, unless otherwise specified, the raw materials used in preparation examples 1 to 7 are all commercial products:
pure Ce: cerium metal powder, shanghai's metal materials Co., ltd., purity 99.0%;
pure Nd: neodymium powder, jiangxi middle tin metal material Co., ltd, purity 99.5%;
pure Fe: metal iron powder, shanghai super-wei nano technology limited company, purity 99.99%;
boron powder: shanghai Charpy technology Co., ltd., purity 99.9%.
Preparation example 1
Weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the molar ratio of 4.74:3.16:2:0.1 to obtain a target raw material I; smelting and casting a target raw material I to obtain an alloy sheet I; carrying out hydrogen crushing treatment on the alloy sheet I to obtain coarse powder of main phase Jin; and further grinding coarse powder of the main phase alloy I by adopting an air flow mill to obtain powder of the main phase alloy I.
Preparation example 2
Based on preparation example 1, this preparation example differs from preparation example 1 in that: weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the molar ratio of 5.32:2.28:2.2:0.2; the remaining steps, conditions and parameters were the same as in preparation example 1.
Preparation example 3
Based on preparation example 1, this preparation example differs from preparation example 1 in that: weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the molar ratio of 5.96:1.49:2.4:0.15; the remaining steps, conditions and parameters were the same as in preparation example 1.
Preparation example 4
Based on preparation example 1, this preparation example differs from preparation example 1 in that: weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the molar ratio of 6.18:0.69:3:0.13; the remaining steps, conditions and parameters were the same as in preparation example 1.
Preparation example 5
Based on preparation example 1, this preparation example differs from preparation example 1 in that: weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the molar ratio of 6.05:1.07:2.7:0.18; the remaining steps, conditions and parameters were the same as in preparation example 1.
Preparation example 6
Based on preparation example 1, this preparation example differs from preparation example 1 in that: weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the molar ratio of 6.25:1.28:2.35:0.12; the remaining steps, conditions and parameters were the same as in preparation example 1.
Preparation example 7
Weighing and proportioning pure Nd, pure Fe and boron powder according to the molar ratio of 2:14:1 to obtain a target raw material II; smelting and casting a target raw material II to obtain an alloy sheet II; carrying out hydrogen crushing treatment on the alloy sheet II to obtain coarse powder of main phase Jin; and further grinding coarse powder of the main phase alloy II by adopting an air flow mill to prepare powder of the main phase alloy II.
Examples 1 to 17 and comparative examples of the present application, examples 1 to 17 and comparative examples, respectively, provide a neodymium-iron-boron magnet; unless otherwise specified, the raw materials used in examples 1 to 17 and comparative examples were all commercially available products: dy/Tb alloy: the Dy and Tb are melted according to the mass ratio of 1:1;
pure Dy: dysprosium metal powder, pan (Shanghai) international trade company, purity 99.0%;
pure Tb: terbium metal powder, shanghai Ala Biochemical technology Co., ltd., purity 99.9%;
Al-Ce alloy: the alloy is prepared by melting pure Al and pure Ce according to the mass ratio of 1:1;
pure Al: metal aluminum powder, shandong Lu Chi New Material Co., ltd, purity 99.8%;
pure Ce: cerium metal powder, shanghai's metal materials Co., ltd., purity 99.0%.
Example 1
In a closed environment, controlling the oxygen content to be within 20 ppm: mixing 1.21kg of powder of the main phase alloy I prepared in preparation example 1 and 0.4kg of powder of the main phase alloy II prepared in preparation example 7 to obtain mixed powder; placing the mixed powder in an orientation magnetic field, and performing stamping forming to obtain a green body; and (3) placing the green body at a sintering temperature of 1050 ℃, performing sintering treatment for 5 hours, then placing at a tempering temperature of 600 ℃, performing tempering treatment for 8 hours, and cooling to obtain a magnet core structure, wherein the magnet core structure forms a neodymium-iron-boron magnet with high cerium content and high performance.
Examples 2 to 6
Based on example 1, the differences between examples 2 to 6 and example 1 are shown in Table 1; wherein m is Ⅰ Meaning the mass, m, of the powder of the major phase alloy I Ⅱ Meaning the mass of the powder of the main phase alloy II; the remaining steps, conditions and parameters were the same as in example 1.
Table 1 examples 2 to 6 differ from example 1 in summary table
| Powder of main phase alloy I | m Ⅰ (kg) | m Ⅱ (kg) | |
| Example 1 | Preparation example 1 | 1.21 | 0.4 |
| Example 2 | Preparation example 2 | 1.36 | 0.34 |
| Example 3 | Preparation example 3 | 1.52 | 0.38 |
| Example 4 | Preparation example 4 | 1.68 | 0.42 |
| Example 5 | Preparation example 5 | 1.84 | 0.46 |
| Example 6 | Preparation example 6 | 2.01 | 0.49 |
Comparative example
Based on example 1, this comparative example differs from example 1 in that: in this comparative example, only 1.61kg of the powder of the main phase alloy I prepared in preparation example 1 was used for the preparation of the neodymium-iron-boron magnet, and the powder of the main phase alloy II prepared in preparation example 7 was not used; the remaining steps, conditions and parameters were the same as in example 1.
Experimental detection of magnetic properties: experimental detection related to magnetic properties was performed on the NdFeB magnets provided in examples 1 to 6 and the NdFeB magnets provided in comparative examples according to GB/T42160-2022; the detection results are recorded in table 2.
Table 2 summary of the results of the test in examples 1 to 6 and comparative example
Referring to Table 2, the results of Table 2 show that the magnetic properties of the NdFeB magnets provided in examples 1 to 6 are all better than those of the NdFeB magnets provided in comparative examples, thereby illustrating the superiority of the present application in preparing NdFeB magnets by the double main phase alloy method; meanwhile, in the neodymium-iron-boron magnets provided in examples 1 to 6, the magnetic performance of the neodymium-iron-boron magnet provided in example 6 is better, so that the neodymium-iron-boron magnet provided by the application has better superiority due to the fact that the main phase alloy I with specific component proportions is adopted.
Examples 7 to 10
Based on example 6, examples 7 to 10 differ from example 6 by the reference to Table 3; the remaining steps, conditions and parameters were the same as in example 6.
Table 3 examples 7 to 10 differ from example 6 in summary table
Experimental detection of magnetic properties: experimental detection related to magnetic performance is carried out on the NdFeB magnets provided in examples 7-10 according to GB/T42160-2022; the detection results are recorded in table 4.
Table 4 summary of the results of the tests of examples 7 to 10 and example 6
Referring to table 4, it is apparent from the results of table 4 that the neodymium iron boron magnets provided in examples 7 to 10 all have superior magnetic properties, and that the sintering treatment and tempering treatment performed at the temperature and time provided in example 8 have superior properties.
Example 11
Based on example 8, this example differs from example 8 in that: the present example further includes subjecting the produced magnet core structure to grain boundary diffusion treatment:
cleaning the surface of the magnet core structure prepared in the embodiment 8 to obtain a magnet core structure with a clean surface; performing magnetron sputtering Dy/Tb alloy diffusion sources along the magnetic pole edges of the magnet core structure with clean surfaces, and controlling the magnetron sputtering area of the Dy/Tb alloy diffusion sources to be 20% of the magnetic pole area of the magnet core structure with clean surfaces; performing magnetron sputtering of an Al-Ce alloy diffusion source on the other surfaces of the magnet core structure with the clean surfaces to prepare a preparation magnet block; placing the prepared magnet block in an environment with the temperature of 750 ℃, carrying out heat preservation treatment for 8 hours, then placing in an environment with the temperature of 450 ℃, carrying out tempering treatment for 3 hours, and cooling;
at this time, the Dy/Tb alloy diffusion source and the Al-Ce alloy diffusion source jointly form a magnet diffusion source, and after being diffused by a grain boundary, the magnet diffusion source forms a shell layer on the periphery of crystal grains of the main phase alloy I and the main phase alloy II; the remaining steps, conditions and parameters were the same as in example 8.
Example 12
Based on embodiment 11, this embodiment differs from embodiment 11 in that: 25% of the magnetic pole area of a magnet core structure with clean magnetron sputtering area surface of a Dy/Tb alloy diffusion source is controlled; the remaining steps, conditions and parameters were the same as in example 8.
Example 13
Based on embodiment 11, this embodiment differs from embodiment 11 in that: 30% of the magnetic pole area of a magnet core structure with clean magnetron sputtering area surface of a Dy/Tb alloy diffusion source is controlled; the remaining steps, conditions and parameters were the same as in example 8.
Experimental detection of magnetic properties: experimental detection related to magnetic performance was performed on the NdFeB magnets provided in examples 11 to 13 according to GB/T42160-2022; the detection results are recorded in table 5.
Table 5 summary of the results of the measurements of examples 11 to 13 and example 8
Referring to Table 5, it is apparent from the results of Table 5 that the magnetic properties of the NdFeB magnets provided in examples 11 to 13 are all superior to those of the NdFeB magnet provided in example 8, thereby illustrating the superiority of the present application in further grain boundary diffusion treatment of the obtained magnet core structure.
Examples 14 to 17
Based on example 12, examples 14 to 17 differ from example 12 in Table 6; the remaining steps, conditions and parameters were the same as in example 12.
TABLE 6 EXAMPLES 14 TO 17 different from EXAMPLE 12 summary tables
Experimental detection of magnetic properties: experimental detection related to magnetic performance was performed on the NdFeB magnets provided in examples 14 to 17 according to GB/T42160-2022; the detection results are recorded in table 7.
Table 7 summary of the results of the measurements in examples 14 to 17 and example 12
Referring to table 7, it is understood from the results of table 7 that the neodymium iron boron magnets provided in examples 14 to 17 all have relatively excellent magnetic properties.
In conclusion, the neodymium-iron-boron magnet obtained by the neodymium-iron-boron magnet and the preparation method thereof have the advantages of high cerium content and high performance.
The above embodiments are not intended to limit the scope of the present application, so: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.
Claims (10)
1. The neodymium-iron-boron magnet with high cerium content and high performance is characterized by comprising a magnet core structure, wherein the magnet core structure comprises a main phase alloy I and a main phase alloy II, and the mass ratio of the main phase alloy I to the main phase alloy II is 3-5:1; the main phase alloy I comprises the following components: (Ce) x ,Nd 1-x ) a Fe b B c X is more than or equal to 0.6 and less than or equal to 0.9, and a+b+c=100 wt%; wherein, b is more than or equal to 20wt% and less than or equal to 30wt%, c is more than or equal to 1wt% and less than or equal to 2wt%, and the rest is a; the main phase alloy II comprises the following components: nd 2 Fe 14 B。
2. The high cerium content high performance neodymium iron boron magnet according to claim 1, wherein said main phase alloy i comprises the following components: (Ce) x ,Nd 1-x ) a Fe b B c X=0.83, a+b+c=100 wt%; wherein a=75.3wt%，b=23.5wt%，c=1.2wt%。
3. The high-cerium-content high-performance neodymium-iron-boron magnet according to claim 1 or 2, further comprising a magnet diffusion source attached to the surface of the magnet core structure, wherein the magnet diffusion source forms a shell layer around the crystal grain periphery of the main phase alloy i and the main phase alloy ii after being diffused through a grain boundary.
4. A high-cerium-content high-performance neodymium-iron-boron magnet according to claim 3, wherein the magnet diffusion source comprises a Dy/Tb alloy diffusion source and an Al-Ce alloy diffusion source, the Dy/Tb alloy diffusion source is arranged along the magnetic pole edge of the magnet core structure, the attached area of the Dy/Tb alloy diffusion source occupies 20-30% of the magnetic pole area of the magnet core structure, and the rest of the surface of the magnet core structure is attached by the Al-Ce alloy diffusion source.
5. A method for preparing the high-cerium-content high-performance neodymium-iron-boron magnet according to claim 1, which is characterized by comprising the following steps:
s1, preparing powder of a main phase alloy I and powder of a main phase alloy II;
s2, mixing the powder of the main phase alloy I and the powder of the main phase alloy II according to the mass ratio of 3-5:1 to obtain mixed powder;
s3, placing the mixed powder in an orientation magnetic field, and performing stamping forming to obtain a green body;
s4, sintering and tempering the green body, and cooling to obtain a magnet core structure, wherein the magnet core structure forms the neodymium-iron-boron magnet with high cerium content and high performance.
6. The method for preparing a high-cerium-content high-performance neodymium iron boron magnet according to claim 5, wherein in the step S1, the method for preparing the powder of the main phase alloy i is as follows:
step one: weighing and proportioning pure Ce, pure Nd, pure Fe and boron powder according to the components of the main phase alloy I to obtain a target raw material I;
step two: smelting and casting the target raw material I to obtain an alloy sheet I;
step three: carrying out hydrogen crushing treatment on the alloy sheet I to obtain coarse powder of main phase Jin;
step four: and further grinding the coarse powder of the main phase alloy I by adopting an air flow mill to obtain powder of the main phase alloy I.
7. The method for preparing a high-cerium-content and high-performance neodymium-iron-boron magnet according to claim 5, wherein in the step S1, the method for preparing the powder of the main phase alloy ii is as follows:
step one: weighing and proportioning pure Nd, pure Fe and boron powder according to the components of a main phase alloy II to obtain a target raw material II;
step two: smelting and casting the target raw material II to obtain an alloy sheet II;
step three: carrying out hydrogen crushing treatment on the alloy sheet II to obtain coarse powder of main phase Jin;
step four: and further grinding the coarse powder of the main phase alloy II by adopting an air flow mill to prepare powder of the main phase alloy II.
8. The method for preparing a high-cerium-content and high-performance neodymium-iron-boron magnet according to claim 5, wherein in the step S4, the sintering process conditions are as follows: the sintering temperature is 1050-1200 ℃, and the sintering time is 3-5 h; the tempering treatment conditions are as follows: the tempering temperature is 600-900 ℃, and the tempering time is 5-8 hours.
9. The method for preparing a high-cerium-content and high-performance neodymium-iron-boron magnet according to claim 5, further comprising the step of S5, performing grain boundary diffusion treatment on the magnet core structure, and comprising the following steps:
s5.1, cleaning the surface of the magnet core structure to obtain a magnet core structure with a clean surface;
s5.2, performing magnetron sputtering of a Dy/Tb alloy diffusion source along the magnetic pole edge of the magnet core structure with the clean surface, performing magnetron sputtering of an Al-Ce alloy diffusion source on the other surfaces of the magnet core structure with the clean surface, wherein the magnetron sputtering area of the Dy/Tb alloy diffusion source is 20-30% of the magnetic pole area of the magnet core structure with the clean surface, and preparing a preparation magnet block;
s5.3, placing the prepared magnet block in an environment with the temperature of 750-900 ℃, carrying out heat preservation treatment for 6-8 hours, placing the prepared magnet block in an environment with the temperature of 450-550 ℃, carrying out tempering treatment for 2-3 hours, and cooling.
10. The method for preparing the high-cerium-content and high-performance neodymium-iron-boron magnet according to any one of claims 5 to 9, wherein the method for preparing the high-cerium-content and high-performance neodymium-iron-boron magnet is carried out in a closed environment, and the oxygen content is controlled within 20 ppm.
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