CN114171275A - Multi-element alloy neodymium iron boron magnetic material and preparation method thereof - Google Patents

Multi-element alloy neodymium iron boron magnetic material and preparation method thereof Download PDF

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CN114171275A
CN114171275A CN202111479669.XA CN202111479669A CN114171275A CN 114171275 A CN114171275 A CN 114171275A CN 202111479669 A CN202111479669 A CN 202111479669A CN 114171275 A CN114171275 A CN 114171275A
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alloy
magnetic material
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neodymium
boron magnetic
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宁海龙
彭维波
陈斌
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Zhejiang Zhonghang New Material Co ltd
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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
    • 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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  • Crystallography & Structural Chemistry (AREA)
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  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention discloses a multi-element alloy neodymium iron boron magnetic material, which comprises a mother alloy, an auxiliary phase alloy and a heavy rare earth oxide or hydride; the master alloy comprises the following components: (R),Ce,Nd)aFebMcBdWherein Ce is rare earth element cerium, Nd is rare earth element neodymium, Fe is iron element, and B is boron element; r is one or more of other rare earth elements except Nd and Ce, and M is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; wherein a is more than or equal to 30 wt% and less than or equal to 33 wt%, c is more than or equal to 0.1 wt% and less than or equal to 2 wt%, d is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and the balance is b. The magnetic material has the excellent characteristics of high coercive force and comprehensive magnetic performance. The invention also discloses a preparation method of the magnetic material, which has low preparation cost and can effectively improve the coercive force and comprehensive magnetic performance of the magnetic material.

Description

Multi-element alloy neodymium iron boron magnetic material and preparation method thereof
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a multi-element alloy neodymium iron boron magnetic material and a preparation method thereof.
Background
Neodymium-iron-boron magnetic materials are widely used in electronic products, such as hard disks, mobile phones, earphones, battery-powered tools, and the like. According to different components and processes, the material can be divided into single alloy and multi-element alloy neodymium iron boron magnetic materials: most of the existing neodymium iron boron magnetic materials are single-component cerium-containing neodymium iron boron magnetic performance materials, and the traditional neodymium iron boron technology is adopted: smelting, hydrogen breaking, airflow milling, compression molding and sintering/aging process, and no addition is needed in the process.
The cerium-containing neodymium-iron-boron magnetic material of the single alloy process has cerium preferentially distributed in a crystal boundary phase to form CeFe2The phase partially replaces the traditional neodymium-rich phase, so that the epitaxial layer of the main phase particles is easy to form a reverse magnetization domain, and the coercive force is low, so that the cerium-containing neodymium-iron-boron magnet prepared by adopting a single alloy process is usually low in coercive force and mainly used for preparing an N-brand with low performance. In order to further improve the coercive force of the cerium-containing neodymium-iron-boron magnetic material, a common method is to add heavy rare earth elements such as Ho and Dy in a single alloy component, or to mix and add common neodymium-iron-boron magnetic powder which contains the heavy rare earth such as Ho and Dy and does not contain cerium and has high coercive force, wherein the heavy rare earth is mainly distributed in main phase particles, so that the anisotropy field of the main phase particles is improved, and the coercive force is improved; in addition, the addition of heavy rare earths also increases costs.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a multi-element alloy neodymium iron boron magnetic material and a preparation method thereof, and aims to solve the problem that the application of a magnet is influenced because the coercive force and the comprehensive magnetic property of the neodymium iron boron magnetic material prepared by the prior art are low.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a multi-element alloy neodymium iron boron magnetic material comprises a mother alloy, an auxiliary phase alloy and a heavy rare earth oxide or hydride; the master alloy comprises the following components: (R, Ce, Nd)aFebMcBdWherein Ce is rare earth element cerium, Nd is rare earth element neodymium, Fe is iron element, and B is boron element; r is one or more of other rare earth elements except Nd and Ce, and M is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; wherein a is more than or equal to 30 wt% and less than or equal to 33 wt%, c is more than or equal to 0.1 wt% and less than or equal to 2 wt%, d is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and the balance is b.
Preferably, the auxiliaryThe phase alloy comprises the following components: (R' Ce, Nd)xFeyM’zBnWherein Ce is rare earth element cerium, Nd is rare earth element neodymium, Fe is iron element, and B is boron element; r 'is one or more of other rare earth elements except Nd and Ce, and M' is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; wherein x is more than or equal to 40 wt% and less than or equal to 50 wt%, z is more than or equal to 0.1 wt% and less than or equal to 3 wt%, n is more than or equal to 0.8 wt% and less than or equal to 0.9 wt%, and the balance is y.
Preferably, the oxide or hydride of the heavy rare earth is at least one of oxide or hydride of heavy rare earth Ho (holmium), Dy (dysprosium), Tb (terbium).
The invention also provides a preparation method of the multi-element alloy neodymium iron boron magnetic material, which comprises the following steps:
step S1: preparing materials according to the components of the neodymium iron boron magnetic material master alloy, then smelting by adopting a vacuum smelting induction furnace, casting into a cast sheet with the thickness of 0.1-0.5 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace, and crushing the cast sheet into master alloy coarse powder;
step S2: adding hydride or oxide of heavy rare earth Ho, Dy and Tb into the master alloy coarse powder obtained in the step S1, wherein the adding proportion is 0.1-1%, and adding part of lubricant to carry out coarse powder mixing; the hydride or oxide of the heavy rare earth is added before the jet milling, and the grain boundary addition of the heavy rare earth can magnetically harden the epitaxial layer of the main phase master alloy particles, so that the anisotropy field is improved, and the coercivity is improved;
step S3: grinding the neodymium iron boron magnetic material coarse powder mixed in the step S2 into mother alloy fine powder by using an air flow mill, wherein the average particle size is controlled to be 2-5 um;
step S4: the method comprises the following steps of (1) mixing materials according to the components of an auxiliary phase alloy of a neodymium iron boron magnetic material, and obtaining auxiliary phase alloy fine powder after smelting, hydrogen breaking and jet milling operations, wherein the average particle size of the auxiliary phase alloy fine powder is controlled to be 2-4 mu m; the neodymium iron boron auxiliary phase alloy containing cerium is added after the jet milling, so that the distribution of cerium and the uniformity of a grain boundary phase can be improved, and the improvement of coercive force can also be promoted;
step S5: adding the auxiliary phase alloy fine powder obtained in the step S4 into the master alloy fine powder obtained in the step S3 according to the mass ratio of 1-20%, and adding the rest of lubricant to mix the fine powder;
step S6: and (2) performing oriented compression molding on the fine powder mixture after the addition and mixing of the multi-element alloy under the protection of nitrogen, performing isostatic pressing to obtain a pressed compact, then loading the pressed compact into a sintering furnace under the protection of nitrogen for high-temperature sintering, and then performing aging heat treatment.
Preferably, in step S1, the melting temperature of the vacuum melting induction furnace is 1400 to 1500 ℃, and the reaction temperature of the hydrogen furnace is 50 to 200 ℃.
Preferably, in step S3, the jet mill is operated under the conditions of nitrogen grinding, the grinding pressure is 0.5-0.6 MPa, and the oxygen content is less than or equal to 10 ppm.
Preferably, in step S2, the additive amount of the lubricant is 0.03 to 0.1 wt% of the neodymium iron boron magnetic material; in the step S5, the addition amount of the lubricant is 0.03-0.1 wt% of the neodymium iron boron magnetic material; the lubricant is an organic solvent containing zinc stearate. The organic solvent may be a compound known to those skilled in the art, such as ethanol, isopropanol, toluene, acetone, diethyl ether, dichloromethane, acetonitrile, pyridine, and the like.
Preferably, in the step S6, the sintering temperature is 1000 to 1080 ℃, and the aging temperature is 450 to 900 ℃.
The technical scheme is that based on the design of the components of the cerium-containing neodymium iron boron, a multi-alloy method is adopted for production, but the existing single-alloy process cannot improve the magnetic performance by improving the microstructure like the multi-alloy method, and only can obtain the performance of the components, so that the comprehensive magnetic performance of the cerium-containing neodymium iron boron magnetic performance material of the multi-alloy is higher than that of the magnet of the single-alloy process. In addition, by adopting the process of the multi-element alloy, the grain boundary of the cerium-containing neodymium-iron-boron material is effectively improved, and the reduction of the coercive force by cerium is inhibited, so that the coercive force and the comprehensive magnetic property of the magnetic material are improved. Meanwhile, cerium belongs to high-abundance elements in rare earth elements, the price is low, and compared with the conventional neodymium-iron-boron magnet, the cost of the cerium-containing neodymium-iron-boron magnet is greatly reduced.
The invention has the beneficial effects that:
according to the multi-element alloy neodymium iron boron magnetic material and the preparation method thereof, the addition of the multi-element alloy can improve the grain boundary of the cerium-containing neodymium iron boron magnetic material, the heavy rare earth can magnetically harden the grain boundary epitaxial layer, and the grain boundary neodymium-rich phase can be distributed more uniformly, so that the coercive force and the squareness of the magnet can be improved, and the comprehensive magnetic performance of the magnet can be improved.
According to the multi-element alloy neodymium iron boron magnetic material and the preparation method thereof, the cerium-containing neodymium iron boron magnetic material prepared from the multi-element alloy has higher magnetic performance than the cerium-containing neodymium iron boron magnetic material prepared from a single alloy, and can inhibit the reduction of the coercive force caused by cerium.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Example 1
The multi-element alloy neodymium iron boron magnetic material comprises the following components: (PrNd)22Ce7Gd2.0Co0.5Al0.4Cu0.15Zr0.2B0.92Fe66.83。
The auxiliary phase alloy comprises the following components: (PrNd)35.0Ce6.0Ho1.0Co1.0Al0.5Cu0.2B0.88Fe55.42。
The heavy rare earth is hydride of Ho.
The preparation method of the multi-element alloy neodymium iron boron magnetic material comprises the following steps:
step S1: preparing materials according to the components of the neodymium iron boron magnetic material master alloy, then smelting by adopting a vacuum smelting induction furnace, casting into a cast sheet with the thickness of 0.1-0.5 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace, and crushing the cast sheet into master alloy coarse powder; the melting temperature of the vacuum melting induction furnace is 1450-1460 ℃, and the reaction temperature of the hydrogen furnace is 50-200 ℃;
step S2: adding hydride of holmium Ho to the master alloy coarse powder obtained in the step S1, wherein the adding proportion is 0.4%, and adding 0.04% of lubricant to carry out coarse powder mixing;
step S3: grinding the neodymium iron boron magnetic material coarse powder mixed in the step S2 into mother alloy fine powder by using an air flow mill, wherein the average particle size is controlled to be 2.9 um; the jet mill is operated under the conditions of nitrogen grinding, the grinding pressure is 0.5-0.6 MPa, and the oxygen content is less than or equal to 10 ppm;
step S4: the ingredients of the auxiliary phase alloy of the neodymium iron boron magnetic material are proportioned, and the auxiliary phase alloy fine powder is obtained after the operations of smelting, hydrogen breaking and jet milling, wherein the average particle size of the auxiliary phase alloy fine powder is controlled to be 2.8 mu m; the neodymium iron boron auxiliary phase alloy containing cerium is added after the jet milling, so that the distribution of cerium and the uniformity of a grain boundary phase can be improved, and the improvement of coercive force can also be promoted;
step S5: adding the auxiliary phase alloy fine powder obtained in the step S4 into the master alloy fine powder obtained in the step S3 according to the mass ratio of 5%, and adding 0.05% of lubricant to mix the fine powder;
step S6: carrying out orientation compression molding on the fine powder mixture after the addition and the mixing of the multi-component alloy under the protection of nitrogen, carrying out isostatic pressing operation to obtain a pressed compact, then putting the pressed compact into a sintering furnace under the protection of nitrogen, carrying out high-temperature sintering at 1070 ℃ for heat preservation for 5 hours, and cooling to room temperature by filling nitrogen; then carrying out aging heat treatment at 900 ℃ for 2 hours, charging nitrogen gas to cool to room temperature, then carrying out heat preservation at 620 ℃ for 5 hours, charging nitrogen gas to cool to room temperature.
Example 2
The preparation method of the multi-element alloy neodymium-iron-boron magnetic material in the embodiment is basically the same as that in the embodiment 1, except that in the multi-element alloy neodymium-iron-boron magnetic material in the embodiment, the mother alloy comprises the following components: (PrNd)25.2Ce5Ho0.3Co0.5Al0.3Cu0.15Zr0.15Ti0.1Ga0.1B0.98Fe67.22The auxiliary phase alloy comprises the following components: (PrNd)35.0Ce6.0Ho1.0Co1.0Al0.5Cu0. 2B0.88Fe55.42The heavy rare earth is dysprosium oxide.
The preparation method of the multi-element alloy neodymium iron boron magnetic material comprises the following steps:
step S1: preparing materials according to the components of the neodymium iron boron magnetic material master alloy, then smelting by adopting a vacuum smelting induction furnace, casting into a cast sheet with the thickness of 0.1-0.5 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace, and crushing the cast sheet into master alloy coarse powder; the melting temperature of the vacuum melting induction furnace is 1450-1460 ℃, and the reaction temperature of the hydrogen furnace is 50-200 ℃;
step S2: dysprosium oxide is added into the master alloy coarse powder obtained in the step S1, the addition proportion is 0.3%, and 0.04% of lubricant is added for coarse powder mixing;
step S3: grinding the neodymium iron boron magnetic material coarse powder mixed in the step S2 into mother alloy fine powder by using an air flow mill, wherein the average particle size is controlled to be 3.0 um; the jet mill is operated under the conditions of nitrogen grinding, the grinding pressure is 0.5-0.6 MPa, and the oxygen content is less than or equal to 10 ppm;
step S4: the ingredients of the auxiliary phase alloy of the neodymium iron boron magnetic material are proportioned, and the auxiliary phase alloy fine powder is obtained after the operations of smelting, hydrogen breaking and jet milling, wherein the average particle size of the auxiliary phase alloy fine powder is controlled to be 2.8 mu m;
step S5: adding the auxiliary phase alloy fine powder obtained in the step S4 into the master alloy fine powder obtained in the step S3 according to the mass ratio of 5%, and adding 0.05% of lubricant to mix the fine powder;
step S6: carrying out orientation compression molding on the fine powder mixed material after the addition and the mixing of the multi-component alloy under the protection of nitrogen, carrying out isostatic pressing operation to obtain a pressed compact, then putting the pressed compact into a sintering furnace under the protection of nitrogen, carrying out high-temperature sintering at 1075 ℃ for heat preservation for 5 hours, and cooling to room temperature by filling nitrogen; then carrying out aging heat treatment at 900 ℃ for 2 hours, charging nitrogen gas to cool to room temperature, then carrying out heat preservation at 610 ℃ for 5 hours, charging nitrogen gas to cool to room temperature.
Example 3
This example is a magnetic material of multi-element alloy Nd-Fe-BThe preparation method of the material is basically the same as that of the embodiment 1, except that in the multi-element alloy neodymium iron boron magnetic material of the embodiment, the mother alloy comprises the following components: (PrNd)28.3Ce1.5Co0.3Al0.1Cu0.1Zr0.1Nb0.1Ga0.1B0.95Fe68.45The auxiliary phase alloy comprises the following components: (PrNd)40Ce1.5Co0.5Al0.1Cu0.1Zr0.1Ga0. 1B0.85Fe56.75The heavy rare earth is a hydride of dysprosium.
The preparation method of the multi-element alloy neodymium iron boron magnetic material comprises the following steps:
step S1: preparing materials according to the components of the neodymium iron boron magnetic material master alloy, then smelting by adopting a vacuum smelting induction furnace, casting into a cast sheet with the thickness of 0.1-0.4 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace, and crushing the cast sheet into master alloy coarse powder; the smelting temperature of the vacuum smelting induction furnace is 1470-1480 ℃, and the reaction temperature of the hydrogen breaking furnace is 50-200 ℃;
step S2: adding hydride of dysprosium Dy to the master alloy coarse powder obtained in the step S1 at an addition ratio of 0.1%, and adding 0.04% of a lubricant to carry out coarse powder mixing;
step S3: grinding the neodymium iron boron magnetic material coarse powder mixed in the step S2 into mother alloy fine powder by using an air flow mill, wherein the average particle size is controlled to be 3.2 um; the jet mill is operated under the conditions of nitrogen grinding, the grinding pressure is 0.5-0.6 MPa, and the oxygen content is less than or equal to 10 ppm;
step S4: the ingredients of the auxiliary phase alloy of the neodymium iron boron magnetic material are proportioned, and the auxiliary phase alloy fine powder is obtained after the operations of smelting, hydrogen breaking and jet milling, wherein the average particle size of the auxiliary phase alloy fine powder is controlled to be 2.8 mu m;
step S5: adding the auxiliary phase alloy fine powder obtained in the step S4 into the master alloy fine powder obtained in the step S3 according to the mass ratio of 3%, and adding 0.04% of lubricant to mix the fine powder;
step S6: carrying out orientation compression molding on the fine powder mixed material after the addition and the mixing of the multi-component alloy under the protection of nitrogen, carrying out isostatic pressing operation to obtain a pressed compact, then putting the pressed compact into a sintering furnace under the protection of nitrogen, carrying out high-temperature sintering at 1075 ℃ for heat preservation for 5 hours, and cooling to room temperature by filling nitrogen; then carrying out aging heat treatment at 900 ℃ for 2 hours, charging nitrogen gas to cool to room temperature, then carrying out heat preservation at 490 ℃ for 5 hours, charging nitrogen gas to cool to room temperature.
Example 4
The preparation method of the multi-element alloy neodymium iron boron magnetic material of the embodiment is basically the same as that of the embodiment 1, except that the added heavy rare earth is hydride of terbium Tb, and the adding proportion is 0.1%.
Example 5
The preparation method of the multi-element alloy neodymium iron boron magnetic material is basically the same as that of the multi-element alloy neodymium iron boron magnetic material in the embodiment 1, except that the proportion of the added auxiliary phase alloy fine powder is 15%.
Comparative example 1
The comparative example was prepared using a single alloy process, the single alloy having the following composition: (PrNd)22.65Ce6.95Gd1.9Ho0.45Co0.53Al0.4Cu0.15Zr0.19B0.92Fe65.86The composition is identical to the total composition of example 1.
Preparing materials according to the components of the single alloy, then smelting by adopting a vacuum smelting induction furnace at the smelting temperature of 1450-1460 ℃, casting into cast pieces with the thickness of 0.1-0.5 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace at the hydrogen cracking reaction temperature of 50-200 ℃, crushing the cast pieces into coarse powder, and adding 0.04% of lubricant to carry out coarse powder mixing; then, carrying out jet milling, controlling the grinding pressure to be 0.5-0.6 MPa, the oxygen content to be less than or equal to 10ppm and the average particle size to be 2.9um, and adding 0.05% of lubricant to carry out fine powder mixing; carrying out orientation compression molding on the fine powder under the protection of nitrogen, carrying out isostatic pressing operation to obtain a pressed compact, putting the pressed compact into a sintering furnace under the protection of nitrogen, carrying out high-temperature sintering at 1070 ℃ for 5 hours, and filling nitrogen to cool to room temperature; then carrying out aging heat treatment at 900 ℃ for 2 hours, charging nitrogen gas to cool to room temperature, then carrying out heat preservation at 620 ℃ for 5 hours, charging nitrogen gas to cool to room temperature.
Comparative example 2
The comparative example was prepared using a single alloy process, the single alloy having the following composition: (PrNd)25.7Ce5.1Dy0.2 6Ho0.45Co0.53Al0.31Cu0.15Ga0.1Ti0.1Zr0.14B0.98Fe66.18This composition is identical to the overall composition of example 2.
Preparing materials according to the components of the single alloy, then smelting by adopting a vacuum smelting induction furnace at the smelting temperature of 1450-1460 ℃, casting into cast pieces with the thickness of 0.1-0.5 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace at the hydrogen cracking reaction temperature of 50-200 ℃, crushing the cast pieces into coarse powder, and adding 0.04% of lubricant to carry out coarse powder mixing; then, carrying out jet milling, controlling the grinding pressure to be 0.5-0.6 MPa, the oxygen content to be less than or equal to 10ppm and the average particle size to be 2.9um, and adding 0.05% of lubricant to carry out fine powder mixing; carrying out orientation compression molding on the fine powder under the protection of nitrogen, carrying out isostatic pressing operation to obtain a pressed compact, putting the pressed compact into a sintering furnace under the protection of nitrogen, carrying out high-temperature sintering at 1075 ℃, keeping the temperature for 5 hours, and cooling to room temperature by filling nitrogen; then carrying out aging heat treatment at 900 ℃ for 2 hours, charging nitrogen gas to cool to room temperature, then carrying out heat preservation at 610 ℃ for 5 hours, charging nitrogen gas to cool to room temperature.
Comparative example 3
The comparative example was prepared using a single alloy process, the single alloy having the following composition: (PrNd)28.65Ce1.5Dy0. 1Co0.3Al0.1Cu0.1Nb0.1Zr0.1B0.95Fe68.1This composition is identical to the total composition of example 3.
Preparing materials according to the components of a single alloy, smelting by adopting a vacuum smelting induction furnace at 1470-1480 ℃, casting into a cast sheet with the thickness of 0.1-0.5 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace at 50-200 ℃, crushing the cast sheet into coarse powder, and adding 0.04% of lubricant to carry out coarse powder mixing; then, carrying out jet milling, wherein the milling pressure is 0.5-0.6 MPa, the oxygen content is less than or equal to 10ppm, the average particle size is controlled to be 2.9um, and adding 0.05% of lubricant to carry out fine powder mixing; carrying out orientation compression molding on the fine powder under the protection of nitrogen, carrying out isostatic pressing operation to obtain a pressed compact, putting the pressed compact into a sintering furnace under the protection of nitrogen, carrying out high-temperature sintering at 1075 ℃, keeping the temperature for 5 hours, and cooling to room temperature by filling nitrogen; then carrying out aging heat treatment at 900 ℃ for 2 hours, charging nitrogen gas to cool to room temperature, then carrying out heat preservation at 490 ℃ for 5 hours, charging nitrogen gas to cool to room temperature.
The performance test of the multi-element alloy neodymium iron boron magnetic material prepared in the examples 1-5 and the comparative examples 1-3 is carried out, and the performance results are shown in table 1:
TABLE 1
Figure BDA0003394494280000071
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed.

Claims (8)

1. A multi-element alloy neodymium iron boron magnetic material is characterized in that the neodymium iron boron magnetic material comprises a mother alloy, an auxiliary phase alloy and a heavy rare earth oxide or hydride; the master alloy comprises the following components: (R),Ce,Nd)aFebMcBdWherein Ce is rare earth element cerium, Nd is rare earth element neodymium, Fe is iron element, and B is boron element; r is one or more of other rare earth elements except Nd and Ce, and M is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; wherein a is more than or equal to 30 wt% and less than or equal to 33 wt%, c is more than or equal to 0.1 wt% and less than or equal to 2 wt%, d is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and the balance is b.
2. The multi-element alloy neodymium-iron-boron magnetic material as claimed in claim 1, wherein the auxiliary alloy comprises the following components: (R' Ce, Nd)xFeyM’zBnWherein Ce is rare earth element cerium, Nd is rare earth element neodymium, Fe is iron element, and B is boron element; r 'is one or more of other rare earth elements except Nd and Ce, and M' is at least one of Al, Si, Mg, Ti, V, Cr, Mn, Ni, Co, Cu, Zn, Ga, Zr, Nb and W elements; wherein x is more than or equal to 40 wt% and less than or equal to 50 wt%, z is more than or equal to 0.1 wt% and less than or equal to 3 wt%, n is more than or equal to 0.8 wt% and less than or equal to 0.9 wt%, and the balance is y.
3. The multi-element alloy neodymium-iron-boron magnetic material according to claim 1, wherein the oxide or hydride of the heavy rare earth is at least one of oxide or hydride of heavy rare earth Ho, Dy, Tb.
4. The preparation method of the multi-element alloy neodymium-iron-boron magnetic material as claimed in any one of claims 1 to 3, wherein the preparation method comprises the following steps:
step S1: preparing materials according to the components of the neodymium iron boron magnetic material master alloy, then smelting by adopting a vacuum smelting induction furnace, casting into a cast sheet with the thickness of 0.1-0.5 mm, carrying out hydrogen cracking reaction by adopting a hydrogen cracking furnace, and crushing the cast sheet into master alloy coarse powder;
step S2: adding hydride or oxide of heavy rare earth Ho, Dy and Tb into the master alloy coarse powder obtained in the step S1, wherein the adding proportion is 0.1-1%, and adding part of lubricant to carry out coarse powder mixing;
step S3: grinding the neodymium iron boron magnetic material coarse powder mixed in the step S2 into mother alloy fine powder by using an air flow mill, wherein the average particle size is controlled to be 2-5 um;
step S4: the method comprises the following steps of (1) mixing materials according to the components of an auxiliary phase alloy of a neodymium iron boron magnetic material, and obtaining auxiliary phase alloy fine powder after smelting, hydrogen breaking and jet milling operations, wherein the average particle size of the auxiliary phase alloy fine powder is controlled to be 2-4 mu m;
step S5: adding the auxiliary phase alloy fine powder obtained in the step S4 into the master alloy fine powder obtained in the step S3 according to the mass ratio of 1-20%, and adding the rest of lubricant to mix the fine powder;
step S6: and (2) performing oriented compression molding on the fine powder mixture after the addition and mixing of the multi-element alloy under the protection of nitrogen, performing isostatic pressing to obtain a pressed compact, then loading the pressed compact into a sintering furnace under the protection of nitrogen for high-temperature sintering, and then performing aging heat treatment.
5. The method for preparing the multi-element alloy neodymium iron boron magnetic material according to claim 4, wherein in the step S1, the melting temperature of the vacuum melting induction furnace is 1400-1500 ℃, and the reaction temperature of the hydrogen furnace is 50-200 ℃.
6. The method for preparing the multi-element alloy neodymium-iron-boron magnetic material as claimed in claim 4, wherein in step S3, the jet mill is operated under the conditions of nitrogen grinding, the grinding pressure is 0.5-0.6 MPa, and the oxygen content is less than or equal to 10 ppm.
7. The method for preparing the multi-element alloy neodymium-iron-boron magnetic material as claimed in claim 4, wherein in step S2, the addition amount of the lubricant is 0.03-0.1 wt% of the neodymium-iron-boron magnetic material; in the step S5, the addition amount of the lubricant is 0.03-0.1 wt% of the neodymium iron boron magnetic material; the lubricant is an organic solvent containing zinc stearate.
8. The method for preparing the multi-element alloy neodymium-iron-boron magnetic material as claimed in claim 4, wherein in the step S6, the sintering temperature is 1000-1080 ℃ and the aging temperature is 450-900 ℃.
CN202111479669.XA 2021-12-06 2021-12-06 Multi-element alloy neodymium iron boron magnetic material and preparation method thereof Pending CN114171275A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114864259A (en) * 2022-04-14 2022-08-05 浙江大学 Multi-element grain boundary reconstruction method for improving corrosion resistance of mixed rare earth permanent magnetic material through 1:2 phase

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114864259A (en) * 2022-04-14 2022-08-05 浙江大学 Multi-element grain boundary reconstruction method for improving corrosion resistance of mixed rare earth permanent magnetic material through 1:2 phase
CN114864259B (en) * 2022-04-14 2023-09-12 浙江大学 Multicomponent grain boundary reconstruction method for improving corrosion resistance of mixed rare earth permanent magnet material through 1:2 phase

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