CN117012485A - Neodymium-iron-boron magnet and preparation method thereof - Google Patents
Neodymium-iron-boron magnet and preparation method thereof Download PDFInfo
- Publication number
- CN117012485A CN117012485A CN202210475086.8A CN202210475086A CN117012485A CN 117012485 A CN117012485 A CN 117012485A CN 202210475086 A CN202210475086 A CN 202210475086A CN 117012485 A CN117012485 A CN 117012485A
- Authority
- CN
- China
- Prior art keywords
- thin
- percentage
- neodymium
- iron
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims description 85
- 239000000843 powder Substances 0.000 claims description 83
- 239000000203 mixture Substances 0.000 claims description 33
- 229910052742 iron Inorganic materials 0.000 claims description 20
- 238000010791 quenching Methods 0.000 claims description 15
- 230000000171 quenching effect Effects 0.000 claims description 15
- 229910052733 gallium Inorganic materials 0.000 claims description 12
- 238000003723 Smelting Methods 0.000 claims description 11
- 238000007731 hot pressing Methods 0.000 claims description 10
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 33
- 239000000463 material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 150000002910 rare earth metals Chemical class 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 3
- 238000004453 electron probe microanalysis Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000007858 starting material Substances 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
- 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
- H01F1/0576—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 pressed, e.g. hot working
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0273—Imparting anisotropy
Abstract
The application discloses a neodymium-iron-boron magnet and a preparation method thereof. The neodymium-iron-boron magnet comprises a first structure, a second structure and a third structure; the first structure includes Nd 2 Fe 14 A main phase B and a grain boundary phase thereof; the second structure includes R' 2 Fe 14 A main phase B and a grain boundary phase thereof; the third structure is a junction of the first structure and the second structure; the content of the M element in the third structure is lower than that in the first structure or the second structure; the Nd 2 Fe 14 B main phase and R' 2 Fe 14 The main phase B presents nano-sized long strips. The neodymium iron boron magnet provided by the application has good heat resistance and high remanence.
Description
Technical Field
The application relates to a neodymium-iron-boron magnet and a preparation method thereof.
Background
The R-T-B rare earth permanent magnet material is widely applied to hard disk drives, electric automobile driving motors, wind power generation motors and household appliances. With the miniaturization of motors and the increase of heat generation due to high current density, the demand for heat resistance of rare earth permanent magnets used is further increased, and how to maintain the coercive force of magnets at high temperature is one of the important research subjects in this technical field. The prior art generally improves the heat resistance by adding heavy rare earth to improve the coercive force, but the heavy rare earth is expensive and resources are rare earth. Another technical direction of interest is the miniaturization of grains, which is a grain refinement value of 1 μm to nm scale, which can improve the coercive force and heat resistance of a magnet, whereas after refinement to nm scale, grains tend to be isotropic, and the remanence declines so as to not provide enough magnetic flux to satisfy the use of a motor.
The application provides a rare earth permanent magnet material which has good coercive force temperature coefficient and residual magnetization intensity.
Disclosure of Invention
The application provides a neodymium-iron-boron magnet and a preparation method thereof, aiming at solving the problems of higher cost or reduced remanence when preparing a neodymium-iron-boron magnet with good heat resistance in the prior art. The neodymium iron boron magnet provided by the application has good heat resistance and high remanence.
The application solves the technical problems through the following technical proposal.
The application provides a neodymium-iron-boron magnet, which comprises the following components:
Nd：20.0％～30.0％；
r':0 to 10.0% and is not 0; r' is one or more of Pr, dy and Tb;
Co：1.0％～5.0％；
m:0.1 to 1.2 percent; m is one or more of Al, cu and Ga, and M at least comprises Ga;
the content of B is 0.8-0.96%;
the balance being Fe;
the percentage is the mass percentage of each component in the neodymium-iron-boron magnet;
the neodymium-iron-boron magnet comprises a first structure, a second structure and a third structure; the first structure includes Nd 2 Fe 14 A main phase B and a grain boundary phase thereof; the second structure includes R' 2 Fe 14 A main phase B and a grain boundary phase thereof; the third structure is a junction of the first structure and the second structure; the content of the M element in the third structure is lower than that in the first structure or the second structure; the Nd 2 Fe 14 B main phase and R' 2 Fe 14 The main phase B presents nano-sized long strips.
In the present application, the grain boundary phase refers to a phase between adjacent two main phase grains, such as Nd 2 Fe 14 B main phase and Nd 2 Fe 14 B phase between main phases, or R' 2 Fe 14 B main phase and R' 2 Fe 14 And phases between the main phases B.
In the present application, the first structure preferably accounts for 45.0% -70.0% of the volume of the neodymium-iron-boron magnet, for example 58.0%, 62.0% or 68.0%.
In the present application, the second structure preferably occupies 25.0% to 50.0% of the volume of the neodymium-iron-boron magnet, for example 25.0%, 26.0%, 30.0% or 37.0%.
In the present application, the third structure preferably occupies 5.0% to 10.0% of the volume of the neodymium-iron-boron magnet, for example, 6.0% or 8.0%.
In a preferred embodiment of the present application, the neodymium-iron-boron magnet comprises 58.0% of the first structure, 37.0% of the second structure and 5.0% of the third structure, wherein the percentages are in percentage by volume of the neodymium-iron-boron magnet.
In a preferred embodiment of the present application, the neodymium-iron-boron magnet comprises 70.0% of the first structure, 25.0% of the second structure and 5.0% of the third structure, wherein the percentages are in percentage by volume of the neodymium-iron-boron magnet.
In a preferred embodiment of the present application, the neodymium-iron-boron magnet comprises 68.0% of the first structure, 26.0% of the second structure and 6.0% of the third structure, wherein the percentages are in percentage by volume of the neodymium-iron-boron magnet.
In a preferred embodiment of the present application, the neodymium-iron-boron magnet comprises 62.0% of the first structure, 30.0% of the second structure and 8.0% of the third structure, wherein the percentages are in percentage by volume of the neodymium-iron-boron magnet.
In the present application, the nano-sized elongated shape means a shape in which the dimension of the crystal grain in the width direction is less than 1000 nm.
In the present application, preferably, the Nd 2 Fe 14 The grain width of the B main phase is less than 800nm, more preferably less than 500nm, still more preferably less than 200nm, for example 43.7nm, 75.5nm, 115.0nm or 151.0nm.
In the present application, preferably, the R' 2 Fe 14 The grain width of the B main phase is less than 800nm, more preferably less than 500nm, still more preferably less than 200nm, for example 43.7nm, 75.5nm, 115.0nm or 151.0nm.
In the present application, the Nd content is preferably 20.0% to 26.0%, for example 20.65%, 24.0%, 24.8% or 25.5%.
In the present application, preferably, R' is Pr, and the Pr content is preferably 7.0% to 10.0%, for example, 7.15% or 9.59%.
In the present application, preferably, the R' is Pr and Dy, wherein the Pr content is preferably 3.0% to 7.0%, for example 3.36% or 6.49%; the Dy content is preferably 2.0% to 4.0%, for example 2.92% or 3.08%.
In the present application, the Co content is preferably 1.5% to 3.5%, for example 1.7%, 2.4%, 3.0% or 3.5%.
In the present application, preferably, M is Ga, and the content of Ga is preferably 0.1% to 0.2%, for example, 0.18%.
In the present application, preferably, the M is Ga and Cu, wherein the content of Ga is preferably 0.4% -0.5%, for example 0.43%; the Cu content is preferably 0.6% to 0.7%, for example 0.64%.
In the present application, preferably, the M is Ga and Al, wherein the content of Ga is preferably 0.2% to 0.35%, for example 0.23% or 0.32%; the Al content is preferably 0.01% to 0.1%, for example 0.07% or 0.08%.
In the present application, the content of B is preferably 0.85% to 0.92%, for example 0.85%, 0.89%, 0.9% or 0.92%.
In the present application, the "balance of Fe" does not exclude that the neodymium-iron-boron magnet further includes other elements than the elements mentioned in the present application. When the neodymium-iron-boron magnet further comprises other elements except the elements, the dosage of Fe is correspondingly adjusted so that the mass percentage of the elements except Fe in the neodymium-iron-boron magnet is within the range defined by the application.
In the present application, the content of Fe is preferably 62.0% to 66.0%, for example 62.39%, 64.37%, 64.44% or 65.16%.
In one embodiment of the application, the neodymium-iron-boron magnet comprises the following components: nd 20.65%, pr 9.59%, co 3.50%, ga 0.18%, B0.92% and Fe 65.16%.
In one embodiment of the application, the neodymium-iron-boron magnet comprises the following components: 25.5% of Nd, 3.36% of Pr, 3.08% of Dy, 1.70% of Co, 0.43% of Ga, 0.64% of Cu, 0.85% of B and 64.44% of Fe.
In one embodiment of the application, the neodymium-iron-boron magnet comprises the following components: nd 24.8%, pr 7.15%, co 2.4%, ga 0.32%, al 0.07%, B0.89% and Fe 64.37%.
In one embodiment of the application, the neodymium-iron-boron magnet comprises the following components: 24.0% of Nd, 6.49% of Pr, 2.92% of Dy, 3.0% of Co, 0.23% of Ga, 0.08% of Al, 0.9% of B and 62.39% of Fe.
The application provides a preparation method of a neodymium-iron-boron magnet, which comprises the following steps:
s1, preparing a first thin belt, a second thin belt and a third thin belt respectively; wherein,
the first thin belt is obtained by smelting and rapidly quenching raw materials of the first thin belt; the raw materials of the first thin strip comprise 29.5 to 32.0 percent of Nd, 1.0 to 5.0 percent of Co, 0.05 to 0.2 percent of M, 0.86 to 0.96 percent of B and the balance of Fe; wherein M is one or more of Al, cu and Ga, and M at least comprises Ga; the percentage is the mass percentage of the raw material of the first thin belt;
the second thin belt is obtained by smelting and rapidly quenching the raw materials of the second thin belt; the raw materials of the second thin belt comprise 27.0% -30.0% of R', 0.86% -0.96% of B and the balance of Fe; wherein R' is one or more of Pr, dy and Tb; the percentage is the mass percentage of the raw material of the second thin belt;
the third thin belt is obtained by smelting and rapidly quenching the raw materials of the third thin belt; the raw materials of the third thin belt comprise 80.0% -97.5% of R' and 2.5% -18% of M; wherein R' is one or more of Pr, dy and Tb; m is one or more of Al, cu and Ga; the percentage is the mass percentage of the raw materials of the third thin belt;
s2, sequentially carrying out hot pressing and thermal deformation on the powder mixture to obtain the powder;
wherein the powder mixture comprises 70.0% to 90.0% of the powder of the first thin strip, 9.0% to 30.0% of the powder of the second thin strip, and 0.5% to 5.0% of the powder of the third thin strip; the percentages are mass percentages of the powder mixture.
In the present application, in step S1, the Ga content in the raw material of the first thin ribbon is preferably 0.1% to 0.6%, for example, 0.3%, 0.4% or 0.5%.
In a specific embodiment of the present application, in step S1, the raw material of the first thin strip includes nd29.5%, co 5.0%, ga 0.1%, B0.96%, and Fe 64.44%; the percentage is the mass percentage of the raw material of the first thin belt.
In a specific embodiment of the present application, in step S1, the raw material of the first thin strip includes nd30.0%, co 2.0%, ga 0.5%, B0.88%, and Fe 66.62%; the percentage is the mass percentage of the raw material of the first thin belt.
In a specific embodiment of the present application, in step S1, the raw material of the first thin strip includes nd31.0%, co 3.0%, ga 0.4%, B0.9%, and Fe 64.7%; the percentage is the mass percentage of the raw material of the first thin belt.
In a specific embodiment of the present application, in step S1, the raw material of the first thin strip includes nd32.0%, co 5.04%, ga 0.3%, B0.92%, and Fe 62.78%; the percentage is the mass percentage of the raw material of the first thin belt.
In the present application, in step S1, preferably, in the raw material of the second thin strip, R' is Pr, and the content of Pr is preferably 29.0%, 29.5% or 30.0%.
In the present application, in step S1, preferably, in the raw material of the second thin ribbon, R' is Dy, and the Dy content is preferably 28.0%.
In a specific embodiment of the present application, in step S1, the raw material of the second thin strip includes pr30.0%, B0.86%, and Fe 69.14%; the percentage is the mass percentage of the raw material of the second thin belt.
In one embodiment of the present application, in step S1, the raw material of the second thin strip includes dy28.0%, B0.96%, and Fe 71.04%; the percentage is the mass percentage of the raw material of the second thin belt.
In a specific embodiment of the present application, in step S1, the raw material of the second thin strip includes pr29.0%, B0.94%, and Fe 70.06%; the percentage is the mass percentage of the raw material of the second thin belt.
In a specific embodiment of the present application, in step S1, the feedstock of the second ribbon comprises pr29.5%, B0.94%, and Fe 69.56%; the percentage is the mass percentage of the raw material of the second thin belt.
In the present application, in step S1, preferably, the raw material of the second thin strip further includes Co, and the content of Co is preferably 1.0% to 5.0%, where the percentage is the mass percentage of the raw material of the second thin strip.
In the present application, in step S1, preferably, in the raw material of the third thin strip, R' is Pr, and the content of Pr is preferably 89.0%, 84.0% or 96.5%.
In the present application, in step S1, preferably, in the raw material of the third thin strip, R' is Dy, and the Dy content is preferably 97.2%.
In the present application, in step S1, preferably, in the raw material of the third thin strip, M is Ga, and the Ga content is 4.0% to 12.0%, for example, 11.0%.
In the present application, in step S1, preferably, in the raw material of the third thin strip, M is Cu, and the content of Cu is 14.0% to 17.0%, for example, 16.0%.
In the present application, in step S1, preferably, in the raw material of the third thin strip, M is Al, and the content of Al is 2.5% to 3.5%, for example, 2.8%.
In a specific embodiment of the present application, in step S1, the starting material of the third ribbon includes pr89.0% and Ga 11.0%; the percentage is the mass percentage of the raw material of the third thin belt.
In a specific embodiment of the present application, in step S1, the feedstock of the third ribbon includes pr84.0% and Cu 16.0%; the percentage is the mass percentage of the raw material of the third thin belt.
In a specific embodiment of the present application, in step S1, the raw material of the third thin strip includes pr96.5% and Al 3.5%; the percentage is the mass percentage of the raw material of the third thin belt.
In a specific embodiment of the present application, in step S1, the raw material of the third thin strip includes dy97.2% and Al 2.8%; the percentage is the mass percentage of the raw material of the third thin belt.
In the present application, in step S1, the smelting may be performed by a method conventional in the art, preferably including: in an arc melting furnace, the melting is repeated in an inert gas atmosphere. The purpose of the smelting is to fully alloy the raw materials to obtain alloy ingots.
In the present application, in step S1, the rapid quenching may be performed by a method conventional in the art, and preferably includes: and (3) performing rapid quenching treatment in a vacuum rapid quenching furnace in an inert gas protective atmosphere, wherein the rotating speed of the cooling roller is 25m/s. Wherein the inert gas is preferably Ar gas.
In the present application, in step S2, preferably, the powder mixture includes 70.0% of the powder of the first thin strip, 29.0% of the powder of the second thin strip, and 1.0% of the powder of the third thin strip; the percentages are mass percentages of the powder mixture.
In the present application, in step S2, preferably, the powder mixture includes 85.0% of the powder of the first thin strip, 11.0% of the powder of the second thin strip, and 4.0% of the powder of the third thin strip; the percentages are mass percentages of the powder mixture.
In the present application, in step S2, preferably, the powder mixture includes 80.0% of the powder of the first thin strip, 18.0% of the powder of the second thin strip, and 2.0% of the powder of the third thin strip; the percentages are mass percentages of the powder mixture.
In the present application, in step S2, preferably, the powder mixture includes 75.0% of the powder of the first thin strip, 22.0% of the powder of the second thin strip, and 3.0% of the powder of the third thin strip; the percentages are mass percentages of the powder mixture.
In the present application, in step S2, the powder of the first thin strip, the powder of the second thin strip, and the powder of the third thin strip may be obtained by pulverizing the first thin strip, the second thin strip, and the third thin strip by a pulverizing method that is conventional in the art, and the pulverizing may be performed using a pulverizer.
In the present application, in step S2, preferably, the preparation method of the powder mixture includes: respectively crushing the first thin belt, the second thin belt and the third thin belt to obtain powder of the first thin belt, powder of the second thin belt and powder of the third thin belt; the powder of the first ribbon, the powder of the second ribbon, and the powder of the third ribbon are then mixed.
In the present application, in step S2, preferably, the preparation method of the powder mixture includes: and crushing the first thin belt, the second thin belt and the third thin belt together to obtain the composite material.
In the present application, in step S2, it is preferable that the particle diameter D50 of the powder of the first thin strip, the powder of the second thin strip, and the powder of the third thin strip are each independently 150 to 250 μm.
In the present application, in step S2, the purpose of the hot pressing is to obtain a densified isotropic neodymium iron boron magnet material.
In the present application, in step S2, the temperature of the hot pressing is preferably 500 to 650 ℃.
In the present application, in step S2, the time of the hot pressing is preferably 1 to 5min, for example, 2min.
In the present application, in step S2, the pressure of the hot pressing is preferably 50 to 200MPa, for example 150MPa.
In the present application, in step S2, the purpose of the thermal deformation is to obtain an anisotropic neodymium iron boron magnet material.
In the present application, in step S2, the temperature of the thermal deformation is preferably 750 to 900 ℃, for example 840 ℃.
In the present application, in the step S2, the time of the thermal deformation is preferably 1 to 5min, for example, 3min.
In the present application, in step S2, the pressure of the thermal deformation is preferably 100 to 300MPa, for example 270MPa.
In the present application, in step S2, the deformation rate of the thermal deformation is preferably 50% to 90%, for example, 70%.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the application.
The reagents and materials used in the present application are commercially available.
The application has the positive progress effects that:
the neodymium-iron-boron magnet has higher remanence and coercivity, wherein the room-temperature remanence Br is above 13.18kGs, and the room-temperature coercivity Hcj is above 21.8 kOe. In addition, the neodymium-iron-boron magnet has better heat resistance, wherein the temperature coefficient |alpha| of 150 ℃ Br is lower than 0.10%, and the temperature coefficient |beta| of 150 ℃ Hcj is not more than 0.45%.
Drawings
Fig. 1 is an EPMA diagram of a neodymium-iron-boron magnet of example 1 (structure a is a first structure, structure B is a second structure, and structure C is a third structure).
Fig. 2 is an SEM image of the neodymium-iron-boron magnet of example 1.
Detailed Description
The application is further illustrated by means of the following examples, which are not intended to limit the scope of the application. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
Examples 1 to 4
The preparation method of the neodymium-iron-boron magnet comprises the following steps:
(1) Smelting: the three thin belts are respectively subjected to material proportioning according to the component formula of the table 1, the prepared raw materials are respectively put into an arc melting furnace, and are repeatedly melted in an inert gas protective atmosphere, so that the cast ingots are fully alloyed, and the alloy cast ingots are respectively obtained after cooling.
(2) And (3) quick quenching: and (3) placing the alloy ingot into a vacuum rapid quenching furnace, and performing rapid quenching treatment in an Ar gas protective atmosphere, wherein the rotating speed of a cooling roller is 25m/s, so that the first thin strip, the second thin strip and the third thin strip are obtained.
(3) Pulverizing and mixing: mechanically crushing, grinding and screening the first thin belt, the second thin belt and the third thin belt to obtain powder with the size of 150-250 mu m; the three powders were uniformly mixed by a mixer according to the mixing ratio shown in table 1 to obtain a powder mixture.
(4) Hot pressing: and (3) filling the powder mixture into a die, and preserving heat for 2min at the temperature of 150MPa and 650 ℃ to obtain the isotropic NdFeB magnet with the diameter of phi 15mm multiplied by 17 mm.
(5) Thermal deformation: and (3) preserving the temperature of the isotropic magnet for 3min at 840 ℃ and 270MPa to obtain the anisotropic NdFeB magnet with the deformation rate of 70% and the dimension of phi 24mm multiplied by 5 mm.
Comparative example 1
The final composition of example 1 was formulated with only one ribbon and prepared according to steps (1) - (5) above.
Comparative example 2
The final composition was the same as in example 1, except that only two thin tapes were prepared according to steps (1) to (5) above.
Comparative example 3
The final composition was the same as in example 1, except that only two thin tapes were prepared according to steps (1) to (5) above.
Comparative example 4
Three kinds of ribbons were used, but the mixing ratio was not within the scope of the present application, and the final composition was not within the scope of the present application, and the preparation was carried out according to the above-mentioned steps (1) to (5).
Table 1 formulation of components of neodymium-iron-boron magnet
Wherein "/" means that the component is absent.
Effect examples
(1) FE-EPMA test
The neodymium-iron-boron magnet obtained in example 1 was polished in cross section, and subjected to surface scanning analysis by FE-EPMA (JEOL 8530F), and the results are shown in FIG. 1. As can be seen from fig. 1, the neodymium-iron-boron magnet includes three structures, structure a is a first structure, structure B is a second structure, structure C is a third structure, and the third structure is a junction between the first structure and the second structure. In addition, the volume ratios of the three structures in the neodymium-iron-boron magnets prepared in examples 1 to 4 are shown in Table 2.
(2) Scanning Electron Microscope (SEM) testing
The morphology of the material of the neodymium-iron-boron magnet prepared in example 1 was observed by SEM, and the results are shown in FIG. 2. As can be seen from fig. 2, the main phase grains in the neodymium-iron-boron magnet are in nano-sized long strips, and the grain width is less than 200nm, such as 43.7nm, 75.5nm, 115.0nm or 151.0nm.
(3) Magnetic property test
The neodymium-iron-boron magnets prepared in examples 1 to 4 and comparative examples 1 to 4 were subjected to magnetic performance detection by using a NIM-10000 type bulk rare earth permanent magnet nondestructive detection system of China measuring institute, and the results are shown in Table 2.
Table 2 magnetic properties of neodymium-iron-boron magnets
The data in table 2 are stated as follows:
(1) br at 20 ℃): refers to the residual magnetism Br of the neodymium-iron-boron magnet at normal temperature (20 ℃).
(2) Hcj at 20 ℃): refers to the coercive force Hcj of the NdFeB magnet at normal temperature (20 ℃).
(3) Absolute value of Br temperature coefficient |α| (%): refers to a temperature coefficient calculated based on residual magnetism Br of a neodymium-iron-boron magnet material at normal temperature (20 ℃) and high temperature (150 ℃), and the calculation formula is as follows:
br temperature coefficient
(4) Absolute value of Hcj temperature coefficient |β| (%): refers to a temperature coefficient calculated based on coercive force Hcj of a neodymium iron boron magnet material at normal temperature (20 ℃) and high temperature (150 ℃), and the calculation formula is as follows:
hcj temperature coefficient
As can be seen from Table 2, the neodymium-iron-boron magnet prepared by the embodiment of the application has a room temperature remanence Br of 13.18-kGs, a room temperature coercivity Hcj of 21.8kOe and is higher than that of the comparative example. In addition, the Br temperature coefficient |alpha| of the neodymium-iron-boron magnet prepared by the embodiment of the application at 150 ℃ is 0.09% and lower than that of the comparative example; the Hcj temperature coefficient |beta| of the NdFeB magnet at 150 ℃ prepared by the embodiment of the application is not more than 0.45%, and the comparative examples are all above 0.47%. Therefore, the neodymium-iron-boron magnet has better heat resistance.
Claims (10)
1. A neodymium-iron-boron magnet comprising the following components:
Nd：20.0％～30.0％；
r':0 to 10.0% and is not 0; r' is one or more of Pr, dy and Tb;
Co：1.0％～5.0％；
m:0.1 to 1.2 percent; m is one or more of Al, cu and Ga, and M at least comprises Ga;
the content of B is 0.8-0.96%;
the balance being Fe;
the percentage is the mass percentage of each component in the neodymium-iron-boron magnet;
the neodymium-iron-boron magnet comprises a first structure, a second structure and a third structure; the first structure includes Nd 2 Fe 14 A main phase B and a grain boundary phase thereof; the second structure includes R' 2 Fe 14 A main phase B and a grain boundary phase thereof; the third structure is a junction of the first structure and the second structure; the content of the M element in the third structure is lower than that in the first structure or the second structure; the Nd 2 Fe 14 B main phase and R' 2 Fe 14 The main phase B presents nano-sized long strips.
2. A neodymium-iron-boron magnet according to claim 1, wherein the first structure comprises 45.0% -70.0%, such as 58.0%, 62.0% or 68.0% by volume of the neodymium-iron-boron magnet;
and/or the second structure comprises 25.0% -50.0% by volume of the neodymium-iron-boron magnet, such as 25.0%, 26.0%, 30.0% or 37.0%;
and/or, the third structure accounts for 5.0-10.0% of the volume of the neodymium-iron-boron magnet, such as 6.0% or 8.0%;
preferably, the neodymium-iron-boron magnet comprises 58.0% of a first structure, 37.0% of a second structure and 5.0% of a third structure, wherein the percentage is the volume percentage of the neodymium-iron-boron magnet;
preferably, the neodymium-iron-boron magnet comprises 70.0% of a first structure, 25.0% of a second structure and 5.0% of a third structure, wherein the percentage is the volume percentage of the neodymium-iron-boron magnet;
preferably, the neodymium-iron-boron magnet comprises 68.0% of a first structure, 26.0% of a second structure and 6.0% of a third structure, wherein the percentage is the volume percentage of the neodymium-iron-boron magnet;
preferably, the neodymium-iron-boron magnet comprises 62.0% of a first structure, 30.0% of a second structure and 8.0% of a third structure, and the percentage is the volume percentage of the neodymium-iron-boron magnet;
and/or, the Nd 2 Fe 14 The grain width of the B main phase is less than 800nm, preferably less than 500nm, more preferably less than 200nm, for example 43.7nm, 75.5nm, 115.0nm or 151.0nm;
and/or, the R' 2 Fe 14 The grain width of the B main phase is less than 800nm, preferably less than 500nm, more preferably less than 200nm, for example 43.7nm, 75.5nm, 115.0nm or 151.0nm.
3. A neodymium-iron-boron magnet according to claim 1, wherein the Nd content is 20.0% -26.0%, such as 20.65%, 24.0%, 24.8% or 25.5%;
and/or, the R' is Pr, the Pr content is preferably 7.0% -10.0%, such as 7.15% or 9.59%; alternatively, R' is Pr and Dy, wherein the Pr content is preferably 3.0% to 7.0%, such as 3.36% or 6.49%; the Dy content is preferably 2.0% to 4.0%, for example 2.92% or 3.08%;
and/or the Co content is 1.5% to 3.5%, for example 1.7%, 2.4%, 3.0% or 3.5%;
and/or, M is Ga, the content of Ga is preferably 0.1% -0.2%, for example 0.18%; alternatively, the M is Ga and Cu, wherein the Ga content is preferably 0.4-0.5%, for example 0.43%; the Cu content is preferably 0.6% to 0.7%, for example 0.64%; alternatively, the M is Ga and Al, wherein the Ga content is preferably 0.2% -0.35%, such as 0.23% or 0.32%; the Al content is preferably 0.01% to 0.1%, for example 0.07% or 0.08%;
and/or the content of B is 0.85% to 0.92%, for example 0.85%, 0.89%, 0.9% or 0.92%;
and/or the Fe content is 62.0% to 66.0%, such as 62.39%, 64.37%, 64.44% or 65.16%;
preferably, the neodymium-iron-boron magnet comprises the following components: nd 20.65%, pr 9.59%, co 3.50%, ga 0.18%, B0.92% and Fe 65.16%;
preferably, the neodymium-iron-boron magnet comprises the following components: 25.5% of Nd, 3.36% of Pr, 3.08% of Dy, 1.70% of Co, 0.43% of Ga, 0.64% of Cu, 0.85% of B and 64.44% of Fe;
preferably, the neodymium-iron-boron magnet comprises the following components: nd 24.8%, pr 7.15%, co 2.4%, ga 0.32%, al 0.07%, B0.89% and Fe 64.37%;
preferably, the neodymium-iron-boron magnet comprises the following components: 24.0% of Nd, 6.49% of Pr, 2.92% of Dy, 3.0% of Co, 0.23% of Ga, 0.08% of Al, 0.9% of B and 62.39% of Fe.
4. A method of producing the neodymium-iron-boron magnet according to any one of claims 1 to 3, comprising the steps of:
s1, preparing a first thin belt, a second thin belt and a third thin belt respectively; wherein,
the first thin belt is obtained by smelting and rapidly quenching raw materials of the first thin belt; the raw materials of the first thin strip comprise 29.5 to 32.0 percent of Nd, 1.0 to 5.0 percent of Co, 0.05 to 0.2 percent of M, 0.86 to 0.96 percent of B and the balance of Fe; wherein M is one or more of Al, cu and Ga, and M at least comprises Ga; the percentage is the mass percentage of the raw material of the first thin belt;
the second thin belt is obtained by smelting and rapidly quenching the raw materials of the second thin belt; the raw materials of the second thin belt comprise 27.0% -30.0% of R', 0.86% -0.96% of B and the balance of Fe; wherein R' is one or more of Pr, dy and Tb; the percentage is the mass percentage of the raw material of the second thin belt;
the third thin belt is obtained by smelting and rapidly quenching the raw materials of the third thin belt; the raw materials of the third thin belt comprise 80.0% -97.5% of R' and 2.5% -18% of M; wherein R' is one or more of Pr, dy and Tb; m is one or more of Al, cu and Ga; the percentage is the mass percentage of the raw materials of the third thin belt;
s2, sequentially carrying out hot pressing and thermal deformation on the powder mixture to obtain the powder;
wherein the powder mixture comprises 70.0% to 90.0% of the powder of the first thin strip, 9.0% to 30.0% of the powder of the second thin strip, and 0.5% to 5.0% of the powder of the third thin strip; the percentages are mass percentages of the powder mixture.
5. The method of manufacturing a neodymium-iron-boron magnet according to claim 4, wherein in step S1, the Ga content in the raw material of the first ribbon is 0.1% -0.6%, such as 0.3%, 0.4% or 0.5%;
preferably, in step S1, the raw materials of the first thin strip include Nd29.5%, co 5.0%, ga 0.1%, B0.96%, and Fe 64.44%; the percentage is the mass percentage of the raw material of the first thin belt;
preferably, in step S1, the raw materials of the first thin strip include Nd30.0%, co 2.0%, ga 0.5%, B0.88%, and Fe 66.62%; the percentage is the mass percentage of the raw material of the first thin belt;
preferably, in step S1, the raw materials of the first thin strip include Nd31.0%, co 3.0%, ga 0.4%, B0.9%, and Fe 64.7%; the percentage is the mass percentage of the raw material of the first thin belt;
preferably, in step S1, the raw materials of the first thin strip include Nd32.0%, co 5.04%, ga 0.3%, B0.92%, and Fe 62.78%; the percentage is the mass percentage of the raw material of the first thin belt.
6. The method of manufacturing a neodymium-iron-boron magnet according to claim 4, wherein in step S1, in the raw material of the second thin strip, R' is Pr, and the content of Pr is preferably 29.0%, 29.5% or 30.0%; more preferably, in step S1, the raw material of the second thin strip includes Pr30.0%, B0.86%, and Fe 69.14%; the percentage is the mass percentage of the raw material of the second thin belt; more preferably, in step S1, the raw material of the second thin strip includes Pr29.0%, B0.94%, and Fe 70.06%; the percentage is the mass percentage of the raw material of the second thin belt; more preferably, in step S1, the raw materials of the second thin strip include Pr29.5%, B0.94%, and Fe 69.56%; the percentage is the mass percentage of the raw material of the second thin belt;
alternatively, in the raw material of the second thin ribbon, R' is Dy, and the Dy content is preferably 28.0%; more preferably, in step S1, the raw material of the second thin strip includes Dy28.0%, B0.96%, and Fe 71.04%; the percentage is the mass percentage of the raw material of the second thin belt;
and/or in step S1, the raw material of the second thin strip further includes Co, where the content of Co is preferably 1.0% to 5.0%, and the percentage is the mass percentage of the raw material of the second thin strip.
7. The method of manufacturing a neodymium-iron-boron magnet according to claim 4, wherein in step S1, in the raw material of the third thin strip, R' is Pr, and the content of Pr is preferably 89.0%, 84.0% or 96.5%; alternatively, in step S1, in the raw material of the third thin strip, R' is Dy, and the Dy content is preferably 97.2%;
and/or, in step S1, in the raw material of the third thin strip, the M is Ga, and the Ga content is 4.0% to 12.0%, for example 11.0%; alternatively, in step S1, in the raw material of the third thin strip, M is Cu, and the content of Cu is 14.0% to 17.0%, for example, 16.0%; alternatively, in step S1, in the raw material of the third thin strip, M is Al, and the content of Al is 2.5% to 3.5%, for example, 2.8%;
preferably, in step S1, the raw materials of the third thin strip include Pr89.0% and Ga 11.0%; the percentage is the mass percentage of the raw materials of the third thin belt;
preferably, in step S1, the raw materials of the third thin strip include Pr84.0% and Cu 16.0%; the percentage is the mass percentage of the raw materials of the third thin belt;
preferably, in step S1, the raw materials of the third thin strip include Pr96.5% and Al 3.5%; the percentage is the mass percentage of the raw materials of the third thin belt;
preferably, in step S1, the raw materials of the third thin strip include Dy97.2% and Al 2.8%; the percentage is the mass percentage of the raw material of the third thin belt.
8. The method of manufacturing a neodymium-iron-boron magnet according to claim 4, wherein in step S1, the melting includes: repeatedly smelting in an arc smelting furnace in an inert gas protective atmosphere;
and/or, in step S1, the rapid quenching includes: carrying out rapid quenching treatment in a vacuum rapid quenching furnace in an inert gas protective atmosphere, wherein the rotating speed of a cooling roller is 25m/s; the inert gas is preferably Ar gas.
9. The method of manufacturing a neodymium-iron-boron magnet according to claim 4, wherein in step S2, said powder mixture comprises 70.0% of said first thin strip of powder, 29.0% of said second thin strip of powder, and 1.0% of said third thin strip of powder; the percentage is the mass percentage of the powder mixture;
alternatively, in step S2, the powder mixture includes 85.0% of the powder of the first thin strip, 11.0% of the powder of the second thin strip, and 4.0% of the powder of the third thin strip; the percentage is the mass percentage of the powder mixture;
alternatively, in step S2, the powder mixture includes 80.0% of the powder of the first thin strip, 18.0% of the powder of the second thin strip, and 2.0% of the powder of the third thin strip; the percentage is the mass percentage of the powder mixture;
alternatively, in step S2, the powder mixture includes 75.0% of the powder of the first thin strip, 22.0% of the powder of the second thin strip, and 3.0% of the powder of the third thin strip; the percentages are mass percentages of the powder mixture.
10. The method for preparing a neodymium-iron-boron magnet according to claim 4,
in step S2, the preparation method of the powder mixture includes: respectively crushing the first thin belt, the second thin belt and the third thin belt to obtain powder of the first thin belt, powder of the second thin belt and powder of the third thin belt; then mixing the powder of the first thin strip, the powder of the second thin strip and the powder of the third thin strip; alternatively, the preparation method of the powder mixture comprises the following steps: crushing the first thin belt, the second thin belt and the third thin belt together to obtain the composite material;
and/or the particle diameter D50 of the powder of the first thin strip, the powder of the second thin strip, and the powder of the third thin strip is each independently 150 to 250 μm;
and/or, in the step S2, the temperature of the hot pressing is 500-650 ℃;
and/or, in step S2, the hot pressing time is 1-5 min, for example 2min;
and/or, in step S2, the hot pressing pressure is 50-200 MPa, for example 150MPa;
and/or, in step S2, the temperature of the thermal deformation is 750-900 ℃, for example 840 ℃;
and/or, in step S2, the time of thermal deformation is 1 to 5min, for example, 3min;
and/or, in step S2, the pressure of the thermal deformation is 100 to 300MPa, for example 270MPa;
and/or, in step S2, the deformation rate of the thermal deformation is 50% to 90%, for example, 70%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210475086.8A CN117012485A (en) | 2022-04-29 | 2022-04-29 | Neodymium-iron-boron magnet and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210475086.8A CN117012485A (en) | 2022-04-29 | 2022-04-29 | Neodymium-iron-boron magnet and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117012485A true CN117012485A (en) | 2023-11-07 |
Family
ID=88567845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210475086.8A Pending CN117012485A (en) | 2022-04-29 | 2022-04-29 | Neodymium-iron-boron magnet and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117012485A (en) |
-
2022
- 2022-04-29 CN CN202210475086.8A patent/CN117012485A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102959648B (en) | R-T-B based rare earth element permanent magnet, motor, automobile, generator, wind power generation plant | |
| JP7379362B2 (en) | Low B content R-Fe-B sintered magnet and manufacturing method | |
| CN102959647B (en) | R-T-B based rare earth element permanent magnet, motor, automobile, generator, wind power generation plant | |
| US9997284B2 (en) | Sintered magnet | |
| US20150132174A1 (en) | Rare Earth Composite Magnets with Increased Resistivity | |
| JP5754232B2 (en) | Manufacturing method of high coercive force NdFeB magnet | |
| CN110853855A (en) | R-T-B series permanent magnetic material and preparation method and application thereof | |
| EP3291249B1 (en) | Manganese bismuth-based sintered magnet having improved thermal stability and preparation method therefor | |
| JP5439385B2 (en) | R-T-B rare earth permanent magnet manufacturing method and motor | |
| JP7470804B2 (en) | Neodymium iron boron magnet material, raw material composition, and manufacturing method | |
| JP7418598B2 (en) | Heavy rare earth alloys, neodymium iron boron permanent magnet materials, raw materials and manufacturing methods | |
| WO2010113371A1 (en) | Alloy material for r-t-b-type rare-earth permanent magnet, process for production of r-t-b-type rare-earth permanent magnet, and motor | |
| CN111223627B (en) | Neodymium-iron-boron magnet material, raw material composition, preparation method and application | |
| JP7470805B2 (en) | Neodymium Iron Boron Magnet Material | |
| CN111243807B (en) | Neodymium-iron-boron magnet material, raw material composition, preparation method and application | |
| JP2002064010A (en) | High-resistivity rare earth magnet and its manufacturing method | |
| TW202121451A (en) | Ndfeb magnet material, raw material composition, preparation method and application | |
| CN111312461A (en) | Neodymium-iron-boron magnet material, raw material composition, preparation method and application | |
| JP5757394B2 (en) | Rare earth permanent magnet manufacturing method | |
| JP4951703B2 (en) | Alloy material for RTB-based rare earth permanent magnet, method for manufacturing RTB-based rare earth permanent magnet, and motor | |
| JP5288276B2 (en) | Manufacturing method of RTB-based permanent magnet | |
| CN111261355A (en) | Neodymium-iron-boron magnet material, raw material composition, preparation method and application | |
| CN111223626A (en) | Neodymium-iron-boron magnet material, raw material composition, preparation method and application | |
| JP2015122395A (en) | Method for manufacturing r-t-b-based sintered magnet | |
| JP2853838B2 (en) | Manufacturing method of rare earth permanent magnet |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Applicant after: Fujian Jinlong Rare Earth Co.,Ltd. Address before: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Applicant before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. |
|
| CB02 | Change of applicant information |