CN113643870A - High-performance cerium-iron-boron magnet and preparation method thereof - Google Patents
High-performance cerium-iron-boron magnet and preparation method thereof Download PDFInfo
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- LAIPFIBOCSBYSV-UHFFFAOYSA-N [B].[Fe].[Ce] Chemical compound [B].[Fe].[Ce] LAIPFIBOCSBYSV-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 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 173
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052802 copper Inorganic materials 0.000 claims abstract description 24
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 21
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 16
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 8
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 8
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 8
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 8
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 8
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 8
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 8
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052796 boron Inorganic materials 0.000 claims abstract description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 82
- 229910045601 alloy Inorganic materials 0.000 claims description 36
- 239000000956 alloy Substances 0.000 claims description 36
- 230000032683 aging Effects 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 25
- 238000005245 sintering Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 9
- 239000000696 magnetic material Substances 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000005266 casting Methods 0.000 description 36
- 239000010949 copper Substances 0.000 description 36
- 239000007788 liquid Substances 0.000 description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 238000001816 cooling Methods 0.000 description 20
- 229910052739 hydrogen Inorganic materials 0.000 description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000498 cooling water Substances 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 16
- 230000006698 induction Effects 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 10
- 238000004321 preservation Methods 0.000 description 10
- 238000003825 pressing Methods 0.000 description 10
- 238000007792 addition Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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
-
- 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
Abstract
The invention discloses a high-performance cerium-iron-boron magnet and a preparation method thereof, and relates to the technical field of rare earth magnetic materialsaFebMcBdWherein Ce is rare earth element cerium, and R is at least one of other rare earth elements except cerium; m is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W; fe is iron element, B is boron element; the auxiliary phase alloy comprises the components of R 'in percentage by mass'xFeyM'zBmWherein R' is at least two of other rare earth elements except Ce and must include Nd and Dy; m' is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; fe is iron element, B is boron element. According to the invention, the auxiliary phase alloy is added into the main phase alloy to improve the crystal boundary, promote the improvement of the coercive force and ensure the squareness of the magnet, so thatUnder the condition of adding cerium, the N52 magnet with high magnetic energy product and high coercive force is obtained.
Description
Technical Field
The invention relates to the technical field of rare earth magnetic materials, in particular to a cerium-iron-boron magnet and a preparation method thereof.
Background
The rare earth magnetic material refers to a magnetic material containing rare earth metal as an alloy element, and the application of the rare earth magnetic material is more and more extensive along with the rapid development of the fields of computers, communication and the like. The abundance ranking of cerium in rare earth metals in earth crust elements is 25 th position, and the preparation of the cerium-iron-boron magnet is beneficial to balancing the utilization of the rare earth metals.
Because cerium is added into the cerium-iron-boron magnet, the addition of cerium can cause the performance reduction of the coercive force, remanence and the like of the magnet, the performance of the cerium-iron-boron magnet can be at most N45 at present, and for the use scene that the performance of the magnet is required to reach N52 or above, the traditional cerium-iron-boron magnet cannot meet the use requirement. At present, the high-performance N52 magnet can only be prepared into an N52 magnet meeting the performance requirement by adopting a neodymium-iron-boron preparation process, but the price of neodymium in rare earth elements is far higher than that of cerium, and the cost for preparing the neodymium-iron-boron magnet is high, so that the cerium-iron-boron magnet meeting the high performance requirement needs to be prepared.
Disclosure of Invention
The invention provides a high-performance cerium-iron-boron magnet and a preparation method thereof, which at least solve the technical problems in the prior art.
The invention provides a high-performance cerium-iron-boron magnet, which comprises a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy comprises the components of (R, Ce)aFebMcBdWherein Ce is rare earth element cerium, and R is at least one of other rare earth elements except cerium; m is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W; fe is iron element, B is boron element;
the auxiliary phase alloy comprises the components of R 'in percentage by mass'xFeyM'zBmWherein R' is at least two of other rare earth elements except Ce and must include Nd and Dy; m' is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; fe is iron element, B is boron element.
In one embodiment, the main phase alloy comprises the following components in percentage by mass: a is more than or equal to 29wt% and less than or equal to 32wt%, c is more than or equal to 0.1wt% and less than or equal to 2wt%, d is more than or equal to 0.9wt% and less than or equal to 1wt%, and the balance is b.
In one embodiment, the Ce accounts for 1-2 wt% of the main phase alloy.
In one embodiment, the auxiliary phase alloy comprises the following components in percentage by mass: x is more than or equal to 32 weight percent and less than or equal to 80 weight percent, z is more than or equal to 0.1 weight percent and less than or equal to 2 weight percent, m is more than or equal to 0.3 weight percent and less than or equal to 1.0 weight percent, and the balance is y.
In one embodiment, the auxiliary phase alloy is 1 to 10wt% of the high performance Ce-Fe-B magnet.
The invention also provides a preparation method of the high-performance cerium-iron-boron magnet, which comprises the following steps:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder;
s2, mixing the main-phase alloy powder and the auxiliary-phase alloy powder to obtain mixed alloy powder;
s3, carrying out orientation molding on the mixed alloy powder under the protection of inert gas, and then sintering at 1000-1100 ℃ in a vacuum state to prepare a high-performance cerium-iron-boron magnet to obtain a blank magnet;
and S4, performing aging treatment on the sintered blank magnet at 450-920 ℃ to obtain the high-performance cerium-iron-boron magnet.
In an implementation mode, the step S4 includes a primary aging treatment and a secondary aging treatment, the temperature of the primary aging treatment is 850-920 ℃, and the treatment time is 1-3 hours; the temperature of the secondary aging treatment is 450-520 ℃, and the treatment time is 3-6 h.
In one embodiment, the step S1 includes:
respectively batching the main phase alloy and the auxiliary phase alloy according to the components and mass percentages;
respectively smelting the raw materials of the main phase alloy and the auxiliary phase alloy into cast pieces
And crushing and grinding to obtain main-phase alloy powder and auxiliary-phase alloy powder with the particle size of 2.5-3.5 microns respectively.
In one embodiment, the vacuum degree in step S3 is less than 1 Pa.
According to the invention, the main phase alloy with low rare earth and high magnetic energy product added with cerium is prepared, and then the auxiliary phase alloy is added into the main phase alloy to improve the grain boundary, promote the improvement of the coercive force and ensure the squareness of the magnet, so that the N52 product with high magnetic energy product and high coercive force is obtained under the condition of cerium addition.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a high-performance cerium-iron-boron magnet, which comprises a main phase alloy and an auxiliary phase alloy;
the main phase alloy comprises the following components (R, Ce)aFebMcBdWherein a is more than or equal to 29wt% and less than or equal to 31wt%, c is more than or equal to 0.1wt% and less than or equal to 2wt%, d is more than or equal to 0.9wt% and less than or equal to 1wt%, and the balance is b; r is at least one of other rare earth elements except cerium; m is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W; one or more impurity elements selected from C, N, O, Si, P, S and H are inevitably present in the raw material of the M element.
The auxiliary phase alloy comprises the components of R 'in percentage by mass'xFeyM'zBmWherein x is more than or equal to 32wt% and less than or equal to 80wt%, z is more than or equal to 0.1wt% and less than or equal to 2wt%, m is more than or equal to 0.3wt% and less than or equal to 1.0wt%, and the balance is y; r' is at least two of other rare earth elements except Ce and must include Nd and Dy; m' is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; one or more impurity elements selected from C, N, O, Si, P, S and H are inevitably present in the raw material of the M element.
The present invention will be described in detail with reference to specific embodiments.
Example 1
A high-performance cerium-iron-boron magnet comprises a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy accounts for 95wt%, and the auxiliary phase alloy accounts for 5wt%;
the main phase alloy comprises the following components in percentage by weight: (PrNd)29.0Ce1.0Fe68.15Co0.5Al0.1Cu0.1Ga0.1Zr0.1B0.95；
The auxiliary phase alloy comprises the following components in percentage by weight: (PrNd)31.0Dy1.0Fe65.28Co1.0Al0.4Cu0.15Ga0.1Zr0.15B0.92；
The preparation method of the high-performance cerium-iron-boron comprises the following steps:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder; in particular, the method comprises the following steps of,
s1.1, preparing materials according to the components of the main phase alloy and the mass percentage of each component, then adding all the components of the main phase alloy into a vacuum induction furnace to be smelted to obtain main phase alloy liquid, and casting the main phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after coarse crushing into an airflow grinding container to grind into main phase alloy powder with the average particle size of 3.0-3.5 mu m;
s1.2, preparing materials according to the components of the auxiliary phase alloy and the mass percentage of each component, then adding all the components of the auxiliary phase alloy into a vacuum induction furnace to be smelted to obtain auxiliary phase alloy liquid, and casting the auxiliary phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after the coarse crushing into an airflow grinding container to grind into auxiliary phase alloy powder with the average particle size of 2.8-3.3 mu m;
s2, mixing the main-phase alloy powder and the auxiliary-phase alloy powder according to a ratio of 95:5 to obtain mixed alloy powder;
s3, placing the mixed alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1070-1080 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s4, continuing to heat to 890 ℃ for primary aging treatment, and preserving heat for 2 hours at 890 ℃; cooling to 490 deg.C, secondary aging treatment, keeping the temperature at 490 deg.C for 4 hours, cooling to room temperature to obtain high-performance Ce-Fe-B magnet.
Example 2
A high-performance cerium-iron-boron magnet comprises a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy accounts for 90wt%, and the auxiliary phase alloy accounts for 10 wt%;
the main phase alloy comprises the following components in percentage by weight: (PrNd)28.0Ce2.0Fe68.25Co0.5Cu0.1Ga0.1Zr0. 1B0.95；
The auxiliary phase alloy comprises the following components in percentage by weight: (PrNd)31.0Dy1.0Fe65.28Co1.0Al0.4Cu0.15Ga0.1Zr0.15B0.92；
The preparation method of the high-performance cerium-iron-boron comprises the following steps:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder; in particular, the method comprises the following steps of,
s1.1, preparing materials according to the components of the main phase alloy and the mass percentage of each component, then adding all the components of the main phase alloy into a vacuum induction furnace to be smelted to obtain main phase alloy liquid, and casting the main phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after coarse crushing into an airflow grinding container to grind into main phase alloy powder with the average particle size of 2.5-3.0 mu m;
s1.2, preparing materials according to the components of the auxiliary phase alloy and the mass percentage of each component, then adding all the components of the auxiliary phase alloy into a vacuum induction furnace to be smelted to obtain auxiliary phase alloy liquid, and casting the auxiliary phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after the coarse crushing into an airflow grinding container to grind into auxiliary phase alloy powder with the average particle size of 2.8-3.3 mu m;
s2, mixing the main phase alloy powder and the auxiliary phase alloy powder according to a ratio of 90:10 to obtain mixed alloy powder;
s3, placing the mixed alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1050-1060 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 4 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s4, raising the temperature to 900 ℃ for primary aging treatment, and preserving the heat at 900 ℃ for 2 hours; and then cooling to 450 ℃ for secondary aging treatment, preserving the heat for 4 hours at 450 ℃, and cooling to room temperature to obtain the high-performance cerium-iron-boron magnet.
Example 3
A high-performance cerium-iron-boron magnet comprises a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy accounts for 92wt%, and the auxiliary phase alloy accounts for 8wt%;
the main phase alloy comprises the following components in percentage by mass: nd (neodymium)28.0Gd0.8Ce1.2Fe68.65Mn0.1Cu0.1Ga0.1Ti0. 1B0.95；
The auxiliary phase alloy comprises the following components in percentage by mass: (PrNd)30.0Dy1.0Tb0.5Fe65.73Co1.1Al0.4Cu0.15Ga0.1Ni0.1B0.92；
The preparation method of the high-performance cerium-iron-boron magnet comprises the following steps:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder; in particular, the method comprises the following steps of,
s1.1, preparing materials according to the components of the main phase alloy and the mass percentage of each component, then adding all the components of the main phase alloy into a vacuum induction furnace to be smelted to obtain main phase alloy liquid, and casting the main phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after coarse crushing into an airflow grinding container to grind into main phase alloy powder with the average particle size of 2.7-3.2 mu m;
s1.2, preparing materials according to the components of the auxiliary phase alloy and the mass percentage of each component, then adding all the components of the auxiliary phase alloy into a vacuum induction furnace to be smelted to obtain auxiliary phase alloy liquid, and casting the auxiliary phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after coarse crushing into an airflow grinding container to grind into auxiliary phase alloy powder with the average particle size of 3.0-3.3 mu m;
s2, mixing the main phase alloy powder and the auxiliary phase alloy powder according to a ratio of 92:8 to obtain mixed alloy powder;
s3, placing the mixed alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1010-1020 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s4, raising the temperature to 920 ℃, carrying out primary aging treatment, and preserving the heat at 920 ℃ for 2 hours; and then cooling to 500 ℃ for secondary aging treatment, preserving the heat for 4 hours at 500 ℃, and cooling to room temperature to obtain the high-performance cerium-iron-boron magnet.
Example 4
A high-performance cerium-iron-boron magnet comprises a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy accounts for 95wt%, and the auxiliary phase alloy accounts for 5wt%;
the main phase alloy comprises the following components in percentage by mass: (PrNd)28.0Ho0.5Ce1.2Fe68.4Co0.6Cu0.1Ga0.1Ni0.1B1.0；
The auxiliary phase alloy comprises the following components in percentage by mass: nd (neodymium)30.0Dy1.0Tb0.5Fe65.7Co1.1Al0.4Cu0.15Ga0.1Ni0.1B0.95；
The preparation method of the high-performance cerium-iron-boron magnet comprises the following steps:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder; in particular, the method comprises the following steps of,
s1.1, preparing materials according to the components of the main phase alloy and the mass percentage of each component, then adding all the components of the main phase alloy into a vacuum induction furnace to be smelted to obtain main phase alloy liquid, and casting the main phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after the coarse crushing into an airflow grinding container to grind into main phase alloy powder with the average particle size of 2.8-3.3 mu m;
s1.2, preparing materials according to the components of the auxiliary phase alloy and the mass percentage of each component, then adding all the components of the auxiliary phase alloy into a vacuum induction furnace to be smelted to obtain auxiliary phase alloy liquid, and casting the auxiliary phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after coarse crushing into an airflow grinding container to grind into auxiliary phase alloy powder with the average particle size of 3.0-3.3 mu m;
s2, mixing the main-phase alloy powder and the auxiliary-phase alloy powder according to a ratio of 95:5 to obtain mixed alloy powder;
s3, placing the mixed alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1040-1050 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s4, raising the temperature to 920 ℃, carrying out primary aging treatment, and preserving the heat at 920 ℃ for 2 hours; and then cooling to 500 ℃ for secondary aging treatment, preserving the heat for 4 hours at 500 ℃, and cooling to room temperature to obtain the high-performance cerium-iron-boron magnet.
Example 5
A high-performance cerium-iron-boron magnet comprises a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy accounts for 95wt%, and the auxiliary phase alloy accounts for 5wt%;
the main phase alloy comprises the following components in percentage by weight: (PrNd)29.0Ho0.3Ce1.0Fe68.25Cr0.1Al0.15Cu0.1Ga0.1W0.1B0.9；
The auxiliary phase alloy comprises the following components in percentage by weight: (PrNd)30Dy1.0Tb0.8Fe65.68Co1.0Mg0.1Al0.1Cu0.15Ga0.1Zr0.15B0.92；
The preparation method of the high-performance cerium-iron-boron comprises the following steps:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder; in particular, the method comprises the following steps of,
s1.1, preparing materials according to the components of the main phase alloy and the mass percentage of each component, then adding all the components of the main phase alloy into a vacuum induction furnace to be smelted to obtain main phase alloy liquid, and casting the main phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after coarse crushing into an airflow grinding container to grind into main phase alloy powder with the average particle size of 2.5-3.0 mu m;
s1.2, preparing materials according to the components of the auxiliary phase alloy and the mass percentage of each component, then adding all the components of the auxiliary phase alloy into a vacuum induction furnace to be smelted to obtain auxiliary phase alloy liquid, and casting the auxiliary phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after the coarse crushing into an airflow grinding container to grind into auxiliary phase alloy powder with the average particle size of 2.8-3.3 mu m;
s2, mixing the main-phase alloy powder and the auxiliary-phase alloy powder according to a ratio of 95:5 to obtain mixed alloy powder;
s3, placing the mixed alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1070-1080 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s4, raising the temperature to 900 ℃ for primary aging treatment, and preserving the heat at 900 ℃ for 2 hours; and then cooling to 500 ℃ for secondary aging treatment, preserving the heat for 6 hours at 500 ℃, and cooling to room temperature to obtain the high-performance cerium-iron-boron magnet.
Example 6
A high-performance cerium-iron-boron magnet comprises a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy accounts for 90wt%, and the auxiliary phase alloy accounts for 10 wt%;
the main phase alloy comprises the following components in percentage by weight: (PrNd)29.0Dy0.3Ce1.0Fe67.85Co0.5Mg0.1Cu0.1Ga0.1Zr0.1B0.95；
The auxiliary phase alloy comprises the following components in percentage by weight: (PrNd)30.0Ho1.0Dy1.0Fe66.08Mn0.2Al0.4Cu0.15Ga0.1Ni0.15B0.92；
The preparation method of the high-performance cerium-iron-boron comprises the following steps:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder; in particular, the method comprises the following steps of,
s1.1, preparing materials according to the components of the main phase alloy and the mass percentage of each component, then adding all the components of the main phase alloy into a vacuum induction furnace to be smelted to obtain main phase alloy liquid, and casting the main phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after coarse crushing into an airflow grinding container to grind into main phase alloy powder with the average particle size of 3.0-3.5 mu m;
s1.2, preparing materials according to the components of the auxiliary phase alloy and the mass percentage of each component, then adding all the components of the auxiliary phase alloy into a vacuum induction furnace to be smelted to obtain auxiliary phase alloy liquid, and casting the auxiliary phase alloy liquid on a copper roller filled with cooling water to obtain a casting sheet with the thickness of 0.1-0.5 mm; placing the cast piece into a hydrogen crushing container to carry out coarse crushing on the cast piece, and placing the crushed pieces after the coarse crushing into an airflow grinding container to grind into auxiliary phase alloy powder with the average particle size of 2.8-3.3 mu m;
s2, mixing the main phase alloy powder and the auxiliary phase alloy powder according to a ratio of 90:10 to obtain mixed alloy powder;
s3, placing the mixed alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1050-1060 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 4 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s4, raising the temperature to 890 ℃, carrying out primary aging treatment, and preserving the heat at 890 ℃ for 2 hours; and then cooling to 490 ℃ for secondary aging treatment, preserving the heat for 4 hours at 490 ℃, and cooling to room temperature to obtain the high-performance cerium-iron-boron magnet.
Comparative example
Comparative example 1
A cerium-iron-boron magnet comprises the following components in percentage by weight: (PrNd)29.0Ce1.0Fe68.15Co0.5Al0.1Cu0.1Ga0.1Zr0.1B0.95；
The preparation method of the cerium-iron-boron comprises the following steps:
s1, preparing materials according to the components of the magnet and the mass percentage of each component, then adding all the components of the magnet into a vacuum induction furnace to be smelted to obtain magnet alloy liquid, and casting the magnet alloy liquid on a copper roller filled with cooling water to obtain a cast sheet with the thickness of 0.1-0.5 mm; placing the casting sheet into a hydrogen cracking container to carry out coarse crushing on the casting sheet, and placing the crushed pieces after coarse crushing into an airflow mill container to grind into magnet alloy powder with the average particle size of 3.0-3.5 mu m;
s2, placing the magnet alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1070-1080 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s3, raising the temperature to 890 ℃ for primary aging treatment, and preserving the heat at 890 ℃ for 2 hours; and then cooling to 490 ℃ for secondary aging treatment, preserving the heat for 4 hours at 490 ℃, and cooling to room temperature to obtain the cerium-iron-boron magnet.
Comparative example 2
A cerium-iron-boron magnet comprises the following components in percentage by weight: (PrNd)28.0Ce2.0Fe68.25Co0.5Cu0.1Ga0.1Zr0.1B0.95；
The preparation method of the cerium-iron-boron comprises the following steps:
s1, preparing materials according to the components of the magnet and the mass percentage of each component, then adding all the components of the magnet into a vacuum induction furnace to be smelted to obtain magnet alloy liquid, and casting the magnet alloy liquid on a copper roller filled with cooling water to obtain a cast sheet with the thickness of 0.1-0.5 mm; placing the casting sheet into a hydrogen cracking container to carry out coarse crushing on the casting sheet, and placing the crushed pieces after coarse crushing into an airflow mill container to grind into magnet alloy powder with the average particle size of 3.0-3.5 mu m;
s2, placing the magnet alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1070-1080 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s3, raising the temperature to 890 ℃, carrying out primary aging treatment, and preserving the heat at 890 ℃ for 2 hours; and then cooling to 490 ℃ for secondary aging treatment, preserving the heat for 4 hours at 490 ℃, and cooling to room temperature to obtain the cerium-iron-boron magnet.
Comparative example 3
A cerium-iron-boron magnet comprises the following components in percentage by weight:
Nd28.0Gd0.8Ce1.2Fe68.65Mn0.1Cu0.1Ga0.1Ti0.1B0.95；
the preparation method of the cerium-iron-boron comprises the following steps:
s1, preparing materials according to the components of the magnet and the mass percentage of each component, then adding all the components of the magnet into a vacuum induction furnace to be smelted to obtain magnet alloy liquid, and casting the magnet alloy liquid on a copper roller filled with cooling water to obtain a cast sheet with the thickness of 0.1-0.5 mm; placing the casting sheet into a hydrogen cracking container to carry out coarse crushing on the casting sheet, and placing the crushed pieces after coarse crushing into an airflow milling container to grind into magnet alloy powder with the average particle size of 2.7-3.2 mu m;
s2, placing the magnet alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1010-1020 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s3, raising the temperature to 920 ℃, carrying out primary aging treatment, and preserving the heat at 920 ℃ for 2 hours; and then cooling to 500 ℃ for secondary aging treatment, preserving the heat for 4 hours at 500 ℃, and cooling to room temperature to obtain the cerium-iron-boron magnet.
Comparative example 4
A cerium-iron-boron magnet comprises the following components in percentage by weight:
(PrNd)28.0Ho0.5Ce1.2Fe68.4Co0.6Cu0.1Ga0.1Ni0.1B1.0；
the preparation method of the cerium-iron-boron comprises the following steps:
s1, preparing materials according to the components of the magnet and the mass percentage of each component, then adding all the components of the magnet into a vacuum induction furnace to be smelted to obtain magnet alloy liquid, and casting the magnet alloy liquid on a copper roller filled with cooling water to obtain a cast sheet with the thickness of 0.1-0.5 mm; placing the casting sheet into a hydrogen cracking container to carry out coarse crushing on the casting sheet, and placing the crushed pieces after coarse crushing into an airflow milling container to grind into magnet alloy powder with the average particle size of 2.8-3.3 mu m;
s2, placing the magnet alloy powder in a mold, compacting the fine powder by applying pressure in the direction perpendicular to a magnetic field under the protection of nitrogen to obtain a magnet green body, placing the green body in a sintering furnace, heating the sintering furnace to 1040-1050 ℃ in a vacuum state (the vacuum degree is less than 1 Pa), preserving heat for 5 hours, and reducing the temperature to be lower than 100 ℃ after the heat preservation is finished;
s3, continuously raising the temperature to 920 ℃, carrying out primary aging treatment, and keeping the temperature at 920 ℃ for 2 hours; and then cooling to 500 ℃ for secondary aging treatment, preserving the heat for 4 hours at 500 ℃, and cooling to room temperature to obtain the cerium-iron-boron magnet.
Performance testing
And (3) magnetic property detection: detecting with reference to GB/T3217-2013 magnetic test method for permanent magnet (hard magnetic) materials;
table 1 results of performance testing
| Residual magnetism Br (kGS) | Magnetic coercive force Hcb (kOe) | Intrinsic coercive force Hcj (kOe) | Maximum magnetic energy product (BH) m (MGOe) | |
| Example 1 | 14.27 | 12.48 | 12.74 | 49.45 |
| Example 2 | 14.13 | 12.35 | 12.69 | 48.47 |
| Example 3 | 14.07 | 12.52 | 12.89 | 48.05 |
| Example 4 | 14.30 | 12.59 | 12.86 | 49.63 |
| Example 5 | 14.10 | 13.07 | 13.37 | 48.25 |
| Example 6 | 14.14 | 12.95 | 13.29 | 48.53 |
| Comparative example 1 | 14.31 | 11.07 | 11.43 | 49.70 |
| Comparative example 2 | 14.31 | 10.19 | 10.52 | 49.59 |
| Comparative example 3 | 14.13 | 11.02 | 11.35 | 48.46 |
| Comparative example 4 | 14.35 | 11.19 | 11.56 | 49.88 |
According to the embodiment of the application, the cerium-added main phase alloy with low rare earth and high magnetic energy product is prepared, and then the auxiliary phase alloy is added into the main phase alloy, so that the crystal boundary is improved, the coercive force is improved, the squareness of the magnet is ensured, and the cerium-iron-boron magnet with high magnetic energy product and high coercive force is obtained under the condition of cerium addition. The comparative example is different from the examples in that no secondary alloy is added to the cerium-iron-boron magnet prepared in the comparative example. According to the magnetic performance results of example 1 and comparative example 1, example 2 and comparative example 2, example 3 and comparative example 3, and example 4 and comparative example 4 in table 1, the magnetic performance of the examples is better than that of the comparative examples, and the addition of the auxiliary phase alloy to the main phase alloy containing cerium can prepare the high-performance cerium iron boron magnet.
The foregoing describes the general principles of the present application in conjunction with specific embodiments, however, it is noted that the advantages, effects, etc. mentioned in the present application are merely examples and are not limiting, and they should not be considered essential to the various embodiments of the present application. Furthermore, the foregoing disclosure of specific details is for the purpose of illustration and description and is not intended to be limiting, since the foregoing disclosure is not intended to be exhaustive or to limit the disclosure to the precise details disclosed.
The words such as "including," "comprising," "having," and the like, referred to in this application are open-ended words that mean "including, but not limited to," and are used interchangeably herein. The words "or" and "as used herein mean, and are used interchangeably with, the word" and/or, "unless the context clearly dictates otherwise. The word "such as" is used herein to mean, and is used interchangeably with, the phrase "such as but not limited to".
It is further noted that in the methods of the present application, the steps may be decomposed and/or recombined. These decompositions and/or recombinations are to be considered as equivalents of the present application.
The previous description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present application. Various modifications to these aspects will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other aspects without departing from the scope of the application. Thus, the present application is not intended to be limited to the aspects shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The foregoing description has been presented for purposes of illustration and description. Furthermore, the description is not intended to limit embodiments of the application to the form disclosed herein. While a number of example aspects and embodiments have been discussed above, those of skill in the art will recognize certain variations, modifications, alterations, additions and sub-combinations thereof.
Claims (9)
1. The high-performance cerium-iron-boron magnet is characterized by comprising a main phase alloy and an auxiliary phase alloy, wherein the main phase alloy comprises the following components (R, Ce)aFebMcBdWherein Ce is rare earth element cerium, and R is at least one of other rare earth elements except cerium; m is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W; fe is iron element, B is boron element;
the auxiliary phase alloy comprises the components of R 'in percentage by mass'xFeyM'zBmWherein R' is at least two of other rare earth elements except Ce and must include Nd and Dy; m' is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; fe is iron element, B is boron element.
2. The high-performance cerium-iron-boron magnet according to claim 1, wherein the mass percentages of the components in the main phase alloy are as follows: a is more than or equal to 29wt% and less than or equal to 32wt%, c is more than or equal to 0.1wt% and less than or equal to 2wt%, d is more than or equal to 0.9wt% and less than or equal to 1wt%, and the balance is b.
3. The high-performance Ce-Fe-B magnet according to claim 2, wherein the Ce is 1-2 wt% in the main phase alloy.
4. The high-performance cerium-iron-boron magnet according to claim 1, wherein the auxiliary alloy comprises the following components in percentage by mass: x is more than or equal to 32 weight percent and less than or equal to 80 weight percent, z is more than or equal to 0.1 weight percent and less than or equal to 2 weight percent, m is more than or equal to 0.3 weight percent and less than or equal to 1.0 weight percent, and the balance is y.
5. The high-performance ce-fe-b magnet according to claim 1, wherein the auxiliary alloy accounts for 1 to 10wt% of the high-performance ce-fe-b magnet.
6. A method for producing a high-performance cerium-iron-boron magnet according to any one of claims 1 to 5, comprising:
s1, respectively mixing the materials according to the components and mass percentages of the main phase alloy and the auxiliary phase alloy to obtain main phase alloy powder and auxiliary phase alloy powder;
s2, mixing the main-phase alloy powder and the auxiliary-phase alloy powder to obtain mixed alloy powder;
s3, carrying out orientation forming on the mixed alloy powder under the protection of inert gas, and then sintering at 1000-1100 ℃ in a vacuum state to obtain a blank magnet;
and S4, performing aging treatment on the sintered blank magnet at 450-920 ℃ to obtain the high-performance cerium-iron-boron magnet.
7. The method for preparing a high-performance cerium-iron-boron magnet according to claim 6, wherein the step S4 includes a primary aging treatment and a secondary aging treatment, the temperature of the primary aging treatment is 850-920 ℃, and the treatment time is 1-3 h; the temperature of the secondary aging treatment is 450-520 ℃, and the treatment time is 3-6 h.
8. The method of manufacturing a high-performance cerium-iron-boron magnet according to claim 6, wherein the step S1 includes:
respectively batching the main phase alloy and the auxiliary phase alloy according to the components and mass percentages;
and respectively smelting the raw materials of the main phase alloy and the auxiliary phase alloy into cast pieces, and crushing and grinding the cast pieces to respectively obtain main phase alloy powder and auxiliary phase alloy powder with the particle size of 2.5-3.5 mu m.
9. The method of manufacturing a high-performance cerium-iron-boron magnet according to claim 6, wherein a degree of vacuum in step S3 is less than 1 Pa.
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