CN115083710A - Double-shell neodymium iron boron magnet and preparation method thereof - Google Patents
Double-shell neodymium iron boron magnet and preparation method thereof Download PDFInfo
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 250
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 238000003723 Smelting Methods 0.000 claims description 12
- 238000010791 quenching Methods 0.000 claims description 9
- 230000000171 quenching effect Effects 0.000 claims description 9
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
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- KJPHTXTWFHVJIG-UHFFFAOYSA-N n-ethyl-2-[(6-methoxypyridin-3-yl)-(2-methylphenyl)sulfonylamino]-n-(pyridin-3-ylmethyl)acetamide Chemical compound C=1C=C(OC)N=CC=1N(S(=O)(=O)C=1C(=CC=CC=1)C)CC(=O)N(CC)CC1=CC=CN=C1 KJPHTXTWFHVJIG-UHFFFAOYSA-N 0.000 description 1
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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
- 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
- H01F1/0572—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 with a protective layer
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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
- 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
- H01F1/0573—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 obtained by reduction or by hydrogen decrepitation or embrittlement
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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
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- 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
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- 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
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- 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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Abstract
The invention discloses a double-shell neodymium iron boron magnet and a preparation method thereof. The double-shell neodymium iron boron magnet comprises main phase crystal grains, double shells of the main phase crystal grains and an Nd-rich phase adjacent to the main phase crystal grains; the main phase grains contain R 2 Fe 14 B; the inner layer of the double shell layer comprises (Nd/Ho) 2 Fe 14 B and/or (Nd/Gd) 2 Fe 14 B; the outer layer of the double shell layer comprises (Nd/Dy) 2 Fe 14 B and/or (Nd/Tb) 2 Fe 14 B; the thickness of the double shell layer is 0.1-6 mu m; the Nd-rich phase contains (R-RH) 6 T 13 And (4) phase X. The invention can obtain the double-shell neodymium iron boron magnet, a thinner shell layer is formed around the main phase, and the diffusion quantity of heavy rare earth elements into the main phase is effectively reduced.
Description
Technical Field
The invention relates to a double-shell neodymium iron boron magnet and a preparation method thereof.
Background
In recent years, with the increasing of green travel, energy conservation and environmental protection, the demand of electric vehicles, variable frequency air conditioner compressors and wind power generation on high coercivity sintered NdFeB magnetic steel is increasing. At present, the preparation of the high-coercivity sintered NdFeB magnetic steel is mainly realized by replacing light rare earth elements by heavy rare earth elements Dy and/or Tb, so that the raw material cost of the sintered NdFeB is increased, the residual magnetism of the magnet is reduced by adding the heavy rare earth elements, and part of the magnetic energy product of the magnet is sacrificed.
In the prior art, the performance of the magnet can be improved by a double-alloy method. The double-alloy method is characterized in that main and auxiliary alloys are respectively smelted, mixed and sintered after being crushed, and the modification of the grain boundary of main phase alloy particles is realized through the change of the components and the proportion of auxiliary alloy powder. However, because the temperature in the sintering stage is higher, heavy rare earth elements such as Dy, Tb and the like added as auxiliary phases can be greatly diffused into the main phase, so that the remanence of the magnet is reduced; meanwhile, heavy rare earth elements are diffused into the main phase in a large amount, and the concentration of the heavy rare earth elements on the peripheral shell of the main phase particles is reduced, so that the improvement value of the heavy rare earth elements on the coercive force is smaller than the effect of improving a crystal boundary structure by distributing the heavy rare earth elements on the surfaces of crystal grains, and the low utilization rate of the heavy rare earth elements and the limited improvement of the coercive force are caused.
Patent document CN111636035A discloses a heavy rare earth alloy, a neodymium iron boron permanent magnet material, a raw material and a preparation method, wherein the auxiliary alloy components are heavy rare earth metals, B, Ti and/or Zr, Fe and/or Co, etc., and Ti and/or Zr and B are combined by controlling the content of Ti and/or Zr and the total amount of the heavy rare earth elements, etc., so as to avoid the excessive heavy rare earth metals from being combined with B, reduce the amount of heavy rare earth metals diffusing to the main phase, and improve the performance of the magnet.
Therefore, it is necessary to find a new process capable of effectively forming a thinner shell layer around the main phase by the expensive heavy rare earth elements such as Dy and Tb, so as to reduce the diffusion degree of the heavy rare earth elements into the main phase.
Disclosure of Invention
The invention provides a double-shell neodymium iron boron magnet and a preparation method thereof, aiming at solving the problem that heavy rare earth elements can be diffused into a main phase in a large quantity by a double-alloy method in the prior art. The invention can obtain the double-shell neodymium iron boron magnet, a thinner shell layer is formed around the main phase, and the diffusion quantity of heavy rare earth elements into the main phase is effectively reduced.
The invention solves the technical problems through the following technical scheme.
The invention provides a double-shell neodymium-iron-boron magnet which comprises main phase grains, double shells of the main phase grains and an Nd-rich phase adjacent to the main phase grains;
the main phase grains contain R 2 Fe 14 B; r is one or more of La, Ce, Pr and Nd;
the inner layer of the double shell layer comprises (Nd/Ho) 2 Fe 14 B and/or (Nd/Gd) 2 Fe 14 B；
The outer layer of the double-shell layer comprises (Nd/Dy) 2 Fe 14 B and/or (Nd/Tb) 2 Fe 14 B；
The thickness of the double shell layer is 0.1-6 mu m;
the Nd-rich phase comprises (R-RH) 6 T 13 And the X phase is one or more of Ho, Gd, Dy and Tb in RH, Fe and/or Co in T, and one or more of Ga, Cu and Al in X.
In the present invention, preferably, the inner layer of the double shell layer comprises (Nd/Ho) 2 Fe 14 B。
In the present invention, preferably, the outer layer of the double shell layer comprises (Nd/Dy) 2 Fe 14 B。
In the present invention, preferably, ZrB is further included in the Nd-rich phase 2 And TiB 2 。
The invention also provides a preparation method of the double-shell neodymium iron boron magnet, which comprises the following steps:
s1, respectively preparing a main alloy sheet, a first auxiliary alloy sheet and a second auxiliary alloy sheet;
wherein the raw materials of the first auxiliary alloy sheet comprise: LH 1 、RH 1 、X 1 And Fe; the LH 1 Is one or more of La, Ce, Pr and Nd, and the RH 1 Is Ho and/or Gd, the X 1 Is one or more of Cu, Co, Ga and Al; in the first auxiliary alloy sheet, the LH 1 The weight percentage of the first auxiliary alloy sheet is 0-80%, and the RH is 1 5-80% of the first auxiliary alloy sheet by mass, and the LH 1 And RH 1 The total amount of the first auxiliary alloy sheet is more than 30 percent by mass, and the X is 1 The mass percentage of the first auxiliary alloy sheet is 1-15%; the sum of the mass percentages of all elements in the first auxiliary alloy sheet is 100%;
the raw materials of the second auxiliary alloy sheet comprise: RH (relative humidity) 2 、X 2 And Fe; the RH 2 Is Dy and/or Tb, the X 2 Is Zr and/or Ti; in the second auxiliary alloy sheet, the RH 2 The mass percentage of the second auxiliary alloy sheet is 0-80% and not 0, and X is 2 The second auxiliary alloy sheet accounts for 3-10% of the mass of the second auxiliary alloy sheet; the sum of the mass percentages of the elements in the second auxiliary alloy sheet is 100%;
and S2, forming and sintering the mixture of the main alloy sheet, the first auxiliary alloy sheet and the second auxiliary alloy sheet after hydrogen crushing or micro crushing to obtain the double-shell neodymium-iron-boron magnet.
In S1, preferably, the melting point of the first superalloy sheet is lower than the melting point of the second superalloy sheet.
In S1, preferably, the LH 1 Take over the firstThe mass percentage of the auxiliary alloy sheet is 0-60%, but not 0, for example 30%.
In S1, preferably, the LH 1 Is Pr and/or Nd.
In S1, preferably, when Pr is contained in the raw material of the first auxiliary alloy sheet, Pr accounts for 0 to 60% by mass of the first auxiliary alloy sheet, for example, 7.5% by mass of the first auxiliary alloy sheet.
In S1, when Nd is contained in the raw material of the first auxiliary alloy sheet, Nd is preferably contained in an amount of 0 to 60 mass%, for example, 22.5 mass%, based on the first auxiliary alloy sheet.
In S1, preferably, the RH is 1 The weight percentage of the first auxiliary alloy sheet is 20-50%.
In S1, preferably, the LH 1 And RH 1 The total amount of (A) is more than 50% of the mass percentage of the first auxiliary alloy sheet.
In S1, preferably, X is 1 Is Cu and/or Co.
In S1, preferably, X is 1 The weight percentage of the first auxiliary alloy sheet is 5-12%, preferably 5-10%.
Wherein, preferably, X is 1 When Cu is contained, the Cu accounts for 1-6% by mass, for example, 5% by mass of the first auxiliary alloy sheet.
Wherein, preferably, X is 1 When Co is contained, the Co accounts for 1-6% by mass, for example, 5% by mass of the first auxiliary alloy sheet.
In S1, in the first master alloy sheet, Fe is preferably present in an amount of 50% or less, more preferably 39 to 45%, for example 39.5% or 44.7% by mass of the first master alloy sheet.
In S1, preferably, the raw material of the first auxiliary alloy sheet further includes B, and in the first auxiliary alloy sheet, B accounts for 0 to 0.6% by mass of the first auxiliary alloy sheet, and is not 0, for example, 0.3% or 0.5%.
In S1, in a preferred embodiment, the raw material of the first secondary alloy consists of: the content of Ho is 50%; the content of Cu is 5%; the Fe content is 44.7%; the content of B is 0.3%; the percentage refers to the mass percentage of the components in the raw material of the first auxiliary alloy.
In S1, in a preferred embodiment, the raw material of the first secondary alloy consists of: the content of Pr is 7.5%; the content of Nd is 22.5%; the content of Ho is 20 percent; the Cu content is 5%; the content of Co is 5%; the content of Fe is 39.5%; the content of B is 0.5%; the percentage refers to the mass percentage of the components in the raw material of the first auxiliary alloy.
In S1, the first master alloy sheet is preferably prepared by melting and casting the raw material of the first master alloy sheet.
Wherein, the smelting temperature of the raw materials of the first auxiliary alloy sheet is preferably above 1000 ℃.
The casting of the first auxiliary alloy sheet may be a casting process conventional in the art, such as strip casting, ingot casting, centrifugal casting, and rapid quenching.
In S1, preferably, the RH is 2 The second auxiliary alloy sheet accounts for 50-80% by mass, for example, 58% or 63%.
In S1, preferably, X is 2 The second auxiliary alloy sheet accounts for 6-10% of the mass of the second auxiliary alloy sheet.
In S1, preferably, X is 2 When Zr is contained, the Zr accounts for 6-10% of the second auxiliary alloy sheet by mass.
In S1, preferably, the raw material of the second master alloy sheet further includes LH 2 The said LH 2 Is one or more of La, Ce, Pr and Nd, the LH is 2 The second auxiliary alloy sheet accounts for less than 80% of the mass of the second auxiliary alloy sheet and is not 0.
In S1, preferably, the raw material of the second master alloy sheet further includes B, and in the second master alloy sheet, B accounts for 0 to 0.6% by mass of the second master alloy sheet, and is not 0, for example, 0.5%.
In S1, in a preferred embodiment, the raw material of the second auxiliary alloy comprises the following components: the content of Dy is 58%; the Zr content is 6 percent; the content of Fe is 36%; the percentage refers to the mass percentage of the components in the raw materials of the second auxiliary alloy.
In S1, in a preferred embodiment, the raw material of the second auxiliary alloy comprises the following components: the Dy content is 63%; the Zr content is 6 percent; the content of Fe is 30.5%; the content of B is 0.5%; the percentage refers to the mass percentage of the components in the raw materials of the second auxiliary alloy.
In S1, in a preferred embodiment, the raw material of the second auxiliary alloy comprises the following components: the content of Dy is 58%; the Zr content is 6 percent; the content of Fe is 35.5%; the content of B is 0.5%; the percentage refers to the mass percentage of the components in the raw materials of the second auxiliary alloy.
In S1, the second master alloy sheet is preferably prepared by melting and casting the raw material of the second master alloy sheet.
Wherein, the smelting temperature of the raw material of the second auxiliary alloy sheet is preferably 1300 ℃ or higher.
The casting of the second auxiliary alloy sheet may be a casting process conventional in the art, such as strip casting, ingot casting, centrifugal casting, and rapid quenching.
In S1, preferably, the material of the main alloy sheet includes LH 3 、X 3 、Y 3 Fe and B; the LH 3 Is Pr and/or Nd, the X 3 Is one or more of Zr, Ti and Nb, and the Y is 3 Is one or more of Cu, Al, Ga and Co, and the Y is 3 Must contain Cu; in the main alloy sheet, the LH 3 The weight percentage of the X accounts for 27-35% of the main alloy sheet, and the X accounts for 3 Accounting for 0.05-0.8% of the mass of the main alloy sheet; the sum of the mass percentages of the elements in the main alloy sheet is 100%.
Wherein, preferably, said LH 3 The alloy sheet is 27 to 30 mass%, for example, 27.6%, 28% or 29 mass% of the main alloy sheet.
Wherein, preferably, X is 3 The mass percentage of the main alloy sheet is 0.1-0.6%, more preferably 0.2-0.3%, for example 0.2%2％。
Wherein, preferably, said Y 3 The alloy sheet is 0.75 to 2.5 mass%, for example, 1.15 mass% or 2.06 mass%.
Preferably, in the main alloy sheet, Cu accounts for 0.1 to 0.6% by mass of the main alloy sheet, for example, 0.21% or 0.25%.
Wherein, preferably, in the main alloy sheet, Y is 3 When Al is contained, the Al accounts for 0.02 to 1.2% by mass, for example, 0.4% by mass of the main alloy sheet.
Wherein, preferably, in the main alloy sheet, Y is 3 When Ga is contained, the content of Ga in the main alloy sheet is 0.25 to 0.4% by mass, for example, 0.26%.
Wherein, preferably, in the main alloy sheet, Y is 3 When Co is contained, the Co accounts for 0.5-1.2% by mass of the main alloy sheet, for example, 1.19% by mass of the main alloy sheet.
Preferably, in the main alloy sheet, B accounts for 0.97-1% of the main alloy sheet by mass.
Wherein, preferably, the raw material of the main alloy sheet further comprises RH 3 The RH of 3 Is Dy and/or Tb, the RH 3 The weight percentage of the main alloy sheet is 0-3% and is not 0.
S1, in a preferred embodiment, the main alloy comprises the following components: the content of Nd was 27.6%; the content of Dy is 3%; the content of Ga is 0.26%; the content of Al is 0.4%; the Cu content is 0.21%; the content of Co is 1.19%; the content of Ti is 0.2%; the content of Nb is 0.02 percent; the content of B is 1%; the Fe content is 66.12%; the percentage refers to the mass percentage of the components in the raw materials of the main alloy.
S1, in a preferred embodiment, the main alloy comprises the following components: the content of Pr is 7 percent; the content of Nd is 21%; the content of Dy is 3%; the content of Ga is 0.4%; the content of Cu is 0.25%; the content of Co is 0.5%; the Zr content is 0.2%; the content of B is 0.97%; the content of Fe is 66.68 percent; the percentage refers to the mass percentage of the components in the raw materials of the main alloy.
S1, in a preferred embodiment, the main alloy comprises the following components: the content of Pr is 7.25%; the content of Nd was 21.75%; the content of Dy is 1%; the content of Ga is 0.4%; the Cu content is 0.25%; the content of Co is 0.5%; the Zr content is 0.2%; the content of B is 0.97%; the content of Fe is 67.68%; the percentage refers to the mass percentage of the components in the raw materials of the main alloy.
In S1, the main alloy sheet is preferably prepared by melting and casting raw materials of the main alloy sheet.
Wherein, the smelting temperature of the raw materials of the main alloy sheet is more than 1400 ℃.
The casting of the main alloy sheet may be a casting process conventional in the art, such as strip casting, ingot casting, centrifugal casting, and rapid quenching.
In S2, the mass percentage of the usage amount of the first auxiliary alloy sheet and the second auxiliary alloy sheet in the usage amount of the raw material of the double-shell neodymium-iron-boron magnet is preferably greater than 1% and less than 15%, and more preferably 5%; the double-shell neodymium iron boron magnet is characterized in that the double-shell neodymium iron boron magnet is composed of the main alloy sheet, the first auxiliary alloy sheet and the second auxiliary alloy sheet.
In S2, preferably, performing hydrogen crushing, micro-crushing, molding and sintering on the mixture of the main alloy sheet and the auxiliary alloy sheet to obtain the double-shell neodymium-iron-boron magnet;
or hydrogen crushing the main alloy sheet and the auxiliary alloy sheet respectively, mixing coarse powder of the main alloy sheet and the auxiliary alloy sheet after the hydrogen crushing, and performing micro-crushing, molding and sintering treatment on the mixed coarse powder to obtain the double-shell neodymium-iron-boron magnet;
or hydrogen crushing and micro-crushing the main alloy sheet and the auxiliary alloy sheet respectively, mixing fine powder obtained by micro-crushing the main alloy sheet and the auxiliary alloy sheet, and forming and sintering the mixed fine powder to obtain the double-shell neodymium-iron-boron magnet.
The operation and conditions of the hydrogen fragmentation may be conventional in the art, among others. The dehydrogenation temperature for hydrogen fragmentation can be 400-650 ℃, for example 500-620 ℃.
Wherein the micro-pulverization process can be a pulverization process conventional in the art, such as jet milling pulverization, and is preferably carried out in an atmosphere with an oxygen content of 50ppm or less. The particle size of the micro-pulverized powder can be 2-7 μm, for example, 3.0-5.3 μm.
Wherein the forming conditions may be conventional in the art, e.g. pressing into a green body in a press with a magnetic field strength of 0.5T to 3.0T, e.g. 1.0 to 2.0T.
Wherein, the conditions of the sintering treatment can be conventional in the field. The sintering temperature can be 1000-1150 ℃, for example 1050-1085 ℃.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
according to the double-shell neodymium-iron-boron magnet, the heavy rare earth shell with low cost Ho and/or Gd is formed around the main phase, excessive diffusion of expensive rare earth elements Dy and/or Tb into the main phase is inhibited, so that the Dy and/or Tb forms a thin shell around the main phase, the diffusion amount of heavy rare earth elements Dy and/or Tb into the main phase is effectively reduced, and the effect of reducing the usage amount of Dy and Tb under the same performance is achieved.
Drawings
FIG. 1 is a graph of EMPA of the sample of example 1.
Fig. 2 is the results of line scanning of the Ho and Dy elements of the sample in example 1.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
(1) A master alloy sheet, a first master alloy sheet and a second master alloy sheet were prepared according to the formulations shown in table 1, respectively.
The smelting temperature of the main alloy sheet is about 1400-1600 ℃, and then the main alloy sheet is obtained by casting through a rapid quenching method.
The smelting temperature of the first auxiliary alloy sheet is about 1400-1600 ℃, and then the first auxiliary alloy sheet is obtained by casting through a rapid quenching method.
The smelting temperature of the second auxiliary alloy sheet is about 1400-1600 ℃, and then the second auxiliary alloy sheet is obtained by casting through a rapid quenching method.
(2) Hydrogen crushing process: and (2) at room temperature, carrying out hydrogen crushing treatment on the mixture of the main alloy sheet, the first auxiliary alloy sheet and the second auxiliary alloy sheet in the step (1) at 500-620 ℃ to obtain coarse crushed powder.
(3) Micro-crushing treatment: and (3) finely grinding the coarsely ground powder in the step (2) in an air flow mill in an atmosphere with an oxygen content of 50ppm or less to obtain a finely ground powder with an average particle size D50 of 3.0 to 5.3 μm.
(4) And (3) forming: pressing the mixture into a green body in a press with the magnetic field intensity of 1.0-2.0T, and then keeping the green body for 15s under the condition that the pressure is 260MPa to obtain the formed body.
(5) And (3) sintering: and sintering the formed body at 1050-1085 ℃, wherein the sintering atmosphere is vacuum or argon, and the double-shell neodymium iron boron magnet is obtained.
TABLE 1 amounts of elements of the main alloy sheet, the first auxiliary alloy sheet and the second auxiliary alloy sheet of examples 1 to 3
Wherein "/" indicates the absence of the component.
Examples 2 to 3
Except for the different amounts of the raw materials as shown in table 1, the process conditions were the same as in example 1, and a double-shell neodymium-iron-boron magnet was obtained.
Effects of the embodiment
And (3) magnetic property testing: the double-shell neodymium iron boron magnet is subjected to magnetic performance detection by using a PFM14.CN molding type ultra-high coercivity permanent magnet measuring instrument of China measurement institute.
| Example 1 | Example 2 | Example 3 | |
| Whether or not a shell structure is formed | Is that | Is that | Is that |
| Thickness of shell layer (mum) | 0.1～6 | 0.1～6 | 0.1～6 |
| Coercive force (kOe) | 29.3 | 28.7 | 24.0 |
| Remanence (kGs) | 12.3 | 12.6 | 13.2 |
According to the invention, the formula of the first auxiliary alloy sheet, the second auxiliary alloy sheet and the main alloy sheet is adjusted, so that the melting point of the first auxiliary alloy sheet is lower than that of the second auxiliary alloy sheet, and therefore, in the sintering process, the first auxiliary alloy sheet is firstly melted and diffused around a main phase to form an inner layer of a double-shell layer; then, an outer layer of a double shell layer with Dy and/or Tb as heavy rare earth elements is further formed, so that Dy and/or Tb can only form a shell layer at the outermost periphery.
FIG. 1 is the EPMA graph of the sample of example 1, in which a clear shell with a high Dy content is formed outside the main phase along the boundary layer, and H can be achieved cj The effect of promotion. From the results of the composition line scan of example 1 in fig. 2, the diffusion degrees of Ho and Dy are close to each other. The phenomenon shows that Ho and Dy can preferentially replace Nd at 4f position in the main phase, and the Ho element is added to occupy a part of diffusion channels of the heavy rare earth element, so that the diffusion amount of the heavy rare earth element Dy from the outer edge layer of the main phase to the inner part of the main phase is reduced, and the effect of improving the concentration increase of Dy in the outer edge layer of the main phase is achieved.
Claims (10)
1. A double-shell neodymium-iron-boron magnet is characterized by comprising main phase crystal grains, double shells of the main phase crystal grains and an Nd-rich phase adjacent to the main phase crystal grains;
the main phase grains contain R 2 Fe 14 B; r is one or more of La, Ce, Pr and Nd;
the inner layer of the double shell layer comprises (Nd/Ho) 2 Fe 14 B and/or (Nd/Gd) 2 Fe 14 B；
The outer layer of the double-shell layer comprises (Nd/Dy) 2 Fe 14 B and/or (Nd/Tb) 2 Fe 14 B；
The thickness of the double shell layer is 0.1-6 mu m;
the Nd-rich phase contains (R-RH) 6 T 13 And the X phase is one or more of Ho, Gd, Dy and Tb in RH, Fe and/or Co in T, and one or more of Ga, Cu and Al in X.
2. The double shell neodymium-iron-boron magnet according to claim 1, wherein the Nd-rich phase further comprises ZrB 2 And TiB 2 。
3. A method for preparing a double-shell neodymium-iron-boron magnet according to claim 1 or 2, characterized by comprising the following steps:
s1, respectively preparing a main alloy sheet, a first auxiliary alloy sheet and a second auxiliary alloy sheet;
wherein the raw materials of the first auxiliary alloy sheet comprise: LH 1 、RH 1 、X 1 And Fe; the LH 1 Is one or more of La, Ce, Pr and Nd, and the RH 1 Is Ho and/or Gd, the X 1 Is one or more of Cu, Co, Ga and Al; in the first auxiliary alloy sheet, the LH 1 The mass percentage of the first auxiliary alloy sheet is 0-80%, and the RH is 1 5-80% of the first auxiliary alloy sheet by mass, and the LH 1 And RH 1 The total amount of the first auxiliary alloy sheet is more than 30 percent by mass, and the X is 1 The mass percentage of the first auxiliary alloy sheet is 1-15%; the sum of the mass percentages of all elements in the first auxiliary alloy sheet is 100%;
the raw materials of the second auxiliary alloy sheet comprise: RH (relative humidity) 2 、X 2 And Fe; the RH 2 Is Dy and/or Tb, the X 2 Is Zr and/or Ti; in the second auxiliary alloy sheet, the RH 2 The weight percentage of the second auxiliary alloy sheet is 0-80%, and is not 0, X 2 The second auxiliary alloy sheet accounts for 3-10% of the mass of the second auxiliary alloy sheet; the sum of the mass percentages of the elements in the second auxiliary alloy sheet is 100%;
and S2, forming and sintering the mixture of the main alloy sheet, the first auxiliary alloy sheet and the second auxiliary alloy sheet after hydrogen crushing or micro crushing to obtain the double-shell neodymium-iron-boron magnet.
4. As claimed in claim 3The preparation method of the double-shell neodymium-iron-boron magnet is characterized in that in S1, LH is added 1 The mass percentage of the first auxiliary alloy sheet is 0-60%, but not 0, for example 30%;
and/or, in S1, the LH 1 Is Pr and/or Nd;
and/or in S1, when the raw material of the first auxiliary alloy sheet contains Pr, the mass percentage of Pr in the first auxiliary alloy sheet is 0-60%, for example, 7.5%;
and/or, in S1, when Nd is contained in the raw material of the first auxiliary alloy sheet, the mass percentage of Nd in the first auxiliary alloy sheet is 0 to 60%, for example, 22.5%;
and/or, in S1, the RH 1 The mass percentage of the first auxiliary alloy sheet is 20-50%;
and/or, in S1, the LH 1 And RH 1 The total amount of the first auxiliary alloy sheet accounts for more than 50% of the mass percentage of the first auxiliary alloy sheet;
and/or, in S1, the X 1 Is Cu and/or Co;
and/or, in S1, the X 1 5-12% of the first auxiliary alloy sheet, preferably 5-10%;
and/or, in S1, the X 1 When Cu is contained, the mass percentage of Cu in the first auxiliary alloy sheet is 1-6%, for example 5%;
and/or, in S1, the X 1 When the alloy sheet contains Co, the Co accounts for 1-6% of the mass of the first auxiliary alloy sheet, for example, 5%;
and/or in S1, in the first master alloy sheet, the mass percentage of Fe in the first master alloy sheet is 50% or less, preferably 39 to 45%, for example 39.5% or 44.7%;
and/or in S1, the raw material of the first auxiliary alloy sheet further comprises B, and in the first auxiliary alloy sheet, B accounts for 0-0.6% by mass of the first auxiliary alloy sheet and is not 0, for example, 0.3% or 0.5%.
5. The method for preparing a double-shell neodymium-iron-boron magnet according to claim 4, wherein the first auxiliary alloy is prepared from the following raw materials in parts by weight: the content of Ho is 50%; the content of Cu is 5%; the Fe content is 44.7%; the content of B is 0.3%; the percentage refers to the mass percentage of the components in the raw materials of the first auxiliary alloy;
or the raw materials of the first auxiliary alloy comprise the following components: the content of Pr is 7.5 percent; the content of Nd is 22.5%; the content of Ho is 20 percent; the Cu content is 5%; the content of Co is 5%; the content of Fe is 39.5%; the content of B is 0.5%; the percentage refers to the mass percentage of the components in the raw material of the first auxiliary alloy.
6. The method of claim 3, wherein in S1, the RH is set to be equal to or greater than RH 2 The mass percentage of the second auxiliary alloy sheet is 50-80%, such as 58% or 63%;
and/or, in S1, the X 2 The mass percentage of the second auxiliary alloy sheet is 6-10%;
and/or, in S1, the X 2 When Zr is contained, the Zr accounts for 6-10% of the second auxiliary alloy sheet by mass percent;
and/or, in S1, the raw material of the second auxiliary alloy sheet further comprises LH 2 The said LH 2 Is one or more of La, Ce, Pr and Nd, and the LH is 2 The second auxiliary alloy sheet accounts for less than 80% of the mass of the second auxiliary alloy sheet and is not 0;
and/or in S1, the raw material of the second auxiliary alloy sheet further comprises B, and in the second auxiliary alloy sheet, B accounts for 0-0.6% by mass of the second auxiliary alloy sheet and is not 0, for example 0.5%.
7. The method for preparing a double-shell neodymium-iron-boron magnet according to claim 6, wherein the second auxiliary alloy is prepared from the following raw materials: the content of Dy is 58%; the Zr content is 6 percent; the content of Fe is 36%; the percentage refers to the mass percentage of the components in the raw materials of the second auxiliary alloy;
or the raw materials of the second auxiliary alloy comprise the following components: the Dy content is 63%; the Zr content is 6 percent; the content of Fe is 30.5%; the content of B is 0.5%; the percentage refers to the mass percentage of the components in the raw materials of the second auxiliary alloy;
or the raw materials of the second auxiliary alloy comprise the following components: the content of Dy is 58%; the Zr content is 6 percent; the content of Fe is 35.5%; the content of B is 0.5%; the percentage refers to the mass percentage of the components in the raw materials of the second auxiliary alloy.
8. The method for preparing a double-shell neodymium-iron-boron magnet according to claim 3, wherein in S1, the melting point of the first auxiliary alloy sheet is lower than the melting point of the second auxiliary alloy sheet;
and/or, in S1, the raw material of the main alloy sheet contains LH 3 、X 3 、Y 3 Fe and B; the LH 3 Is Pr and/or Nd, the X 3 Is one or more of Zr, Ti and Nb, and the Y is 3 Is one or more of Cu, Al, Ga and Co, and the Y is 3 Must contain Cu; in the main alloy sheet, the LH 3 The weight percentage of the X in the main alloy sheet is 27-35 percent 3 The alloy sheet accounts for 0.05-0.8% of the main alloy sheet by mass; the sum of the mass percentages of the elements in the main alloy sheet is 100%.
9. The method of preparing a double shell neodymium-iron-boron magnet according to claim 8, wherein the LH is 3 The mass percentage of the main alloy sheet is 27-30%, such as 27.6%, 28% or 29%;
and/or, said X 3 The mass percentage of the main alloy sheet is 0.1-0.6%, preferably 0.2-0.3%, for example 0.22%;
and/or, said Y 3 The mass percentage of the main alloy sheet is 0.75-2.5%, such as 1.15% or 2.06%;
and/or in the main alloy sheet, Cu accounts for 0.1-0.6% of the main alloy sheet by mass, such as 0.21% or 0.25%;
and/or, in the main alloy sheet, Y 3 When Al is contained, the mass percentage of Al in the main alloy sheet is 0.02-1.2%, for example 0.4%;
and/or, in the main alloy sheet, Y 3 When Ga is contained, the mass percent of Ga in the main alloy sheet is 0.25-0.4%, for example 0.26%;
and/or, in the main alloy sheet, Y 3 When Co is contained, the Co accounts for 0.5-1.2% by mass of the main alloy sheet, for example, 1.19%;
and/or in the main alloy sheet, B accounts for 0.97-1% of the main alloy sheet by mass percent;
and/or the raw material of the main alloy sheet further comprises RH 3 The RH of 3 Is Dy and/or Tb, the RH 3 The alloy sheet accounts for 0-3% of the main alloy sheet by mass and is not 0;
preferably, the raw materials of the main alloy consist of the following components: the content of Nd was 27.6%; the content of Dy is 3%; the content of Ga is 0.26%; the content of Al is 0.4%; the Cu content is 0.21%; the content of Co is 1.19%; the content of Ti is 0.2%; the content of Nb is 0.02 percent; the content of B is 1%; the Fe content is 66.12%; the percentage refers to the mass percentage of the components in the raw materials of the main alloy;
or the raw materials of the main alloy consist of the following components: the content of Pr is 7%; the content of Nd is 21%; the content of Dy is 3%; the content of Ga is 0.4%; the Cu content is 0.25%; the content of Co is 0.5%; the Zr content is 0.2%; the content of B is 0.97%; the content of Fe is 66.68 percent; the percentage refers to the mass percentage of the components in the raw materials of the main alloy;
or the raw materials of the main alloy consist of the following components: the content of Pr is 7.25%; the content of Nd was 21.75%; the content of Dy is 1%; the content of Ga is 0.4%; the Cu content is 0.25%; the content of Co is 0.5%; the Zr content is 0.2%; the content of B is 0.97%; the content of Fe is 67.68%; the percentage refers to the mass percentage of the components in the raw materials of the main alloy.
10. The method for preparing a double-shell neodymium-iron-boron magnet according to claim 3, wherein in S1, the first auxiliary alloy sheet is prepared by smelting and casting raw materials of the first auxiliary alloy sheet; preferably, the smelting temperature of the raw material of the first auxiliary alloy sheet is more than 1000 ℃; the casting of the first auxiliary alloy sheet is preferably a strip continuous casting method, an ingot casting method, a centrifugal casting method or a rapid quenching method;
and/or in S1, the second auxiliary alloy sheet is prepared by smelting and casting the raw material of the second auxiliary alloy sheet; preferably, the smelting temperature of the raw material of the second auxiliary alloy sheet is above 1300 ℃; the casting of the second auxiliary alloy sheet is preferably a strip continuous casting method, an ingot casting method, a centrifugal casting method or a rapid quenching method;
and/or in S1, the main alloy sheet is prepared by smelting and casting raw materials of the main alloy sheet; preferably, the smelting temperature of the raw materials of the main alloy sheet is more than 1400 ℃; the casting of the main alloy sheet is preferably a strip continuous casting method, an ingot casting method, a centrifugal casting method or a rapid quenching method;
and/or in S2, the mass percentage of the first auxiliary alloy sheet and the second auxiliary alloy sheet in the raw material of the double-shell neodymium-iron-boron magnet is more than 1% and less than 15%, preferably 5%; the double-shell neodymium iron boron magnet is characterized in that the double-shell neodymium iron boron magnet is composed of the main alloy sheet, the first auxiliary alloy sheet and the second auxiliary alloy sheet;
and/or in S2, performing hydrogen crushing, micro-crushing, molding and sintering treatment on the mixture of the main alloy sheet and the auxiliary alloy sheet to obtain the double-shell neodymium-iron-boron magnet; or hydrogen crushing the main alloy sheet and the auxiliary alloy sheet respectively, mixing coarse powder of the main alloy sheet and the auxiliary alloy sheet after the hydrogen crushing, and performing micro-crushing, molding and sintering treatment on the mixed coarse powder to obtain the double-shell neodymium-iron-boron magnet; or hydrogen crushing and micro-crushing the main alloy sheet and the auxiliary alloy sheet respectively, mixing fine powder obtained by micro-crushing the main alloy sheet and the auxiliary alloy sheet, and forming and sintering the mixed fine powder to obtain the double-shell neodymium-iron-boron magnet;
and/or in S2, the dehydrogenation temperature of hydrogen crushing is 400-650 ℃, for example, 500-620 ℃;
and/or, in S2, the micro-pulverization is jet mill pulverization;
and/or, in S2, the micro-pulverization is carried out in an atmosphere having an oxygen content of 50ppm or less;
and/or in S2, the particle size of the micro-pulverized powder is 2-7 μm, such as 3.0-5.3 μm;
and/or, in S2, the forming is carried out in a press with the magnetic field intensity of 0.5T to 3.0T, such as 1.0T to 2.0T, so as to obtain a green body;
and/or in S2, the sintering temperature is 1000-1150 ℃, for example 1050-1085 ℃.
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| CN202110289538.9A CN115083710A (en) | 2021-03-10 | 2021-03-10 | Double-shell neodymium iron boron magnet and preparation method thereof |
| KR1020237025813A KR20230125298A (en) | 2021-03-10 | 2022-01-17 | Double angle niodymium iron boron magnetic material and its manufacturing method |
| JP2023544208A JP2024512185A (en) | 2021-03-10 | 2022-01-17 | Double shell layer neodymium iron boron magnet and its manufacturing method |
| PCT/CN2022/072242 WO2022188548A1 (en) | 2021-03-10 | 2022-01-17 | Double-shell neodymium-iron-boron magnet and preparation method therefor |
| EP22766075.0A EP4250317A4 (en) | 2021-03-10 | 2022-01-17 | Double-shell neodymium-iron-boron magnet and preparation method therefor |
| TW111107189A TWI776781B (en) | 2021-03-10 | 2022-02-25 | DOUBLE-SHELL NdFeB MAGNET AND PREPARATION METHOD |
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| TWI496174B (en) * | 2014-12-26 | 2015-08-11 | China Steel Corp | Ndfeb magnet and method for producing the same |
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