WO2022193820A1 - 一种r-t-b磁体及其制备方法 - Google Patents

一种r-t-b磁体及其制备方法 Download PDF

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WO2022193820A1
WO2022193820A1 PCT/CN2022/072253 CN2022072253W WO2022193820A1 WO 2022193820 A1 WO2022193820 A1 WO 2022193820A1 CN 2022072253 W CN2022072253 W CN 2022072253W WO 2022193820 A1 WO2022193820 A1 WO 2022193820A1
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magnet
component
intergranular
phase
triangular region
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PCT/CN2022/072253
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English (en)
French (fr)
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陈大崑
牟维国
黄佳莹
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福建省长汀金龙稀土有限公司
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Priority to KR1020237031356A priority Critical patent/KR20230145174A/ko
Priority to JP2023544209A priority patent/JP2024513632A/ja
Priority to EP22770180.2A priority patent/EP4303894A1/en
Publication of WO2022193820A1 publication Critical patent/WO2022193820A1/zh
Priority to US18/458,290 priority patent/US20230411054A1/en

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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/0555—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together
    • H01F1/0557—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • 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
    • H01F41/0293—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

Definitions

  • the invention relates to an R-T-B magnet and a preparation method thereof.
  • NdFeB permanent magnet materials As an important rare earth functional material, NdFeB permanent magnet materials have excellent comprehensive magnetic properties and are widely used in the electronics industry, electric vehicles and many other fields. However, the comprehensive magnetic properties of the current NdFeB magnet materials are poor, and it is difficult to prepare products with better properties, which cannot meet the needs of society.
  • NdFeB permanent magnet material which is composed of the following components by weight percentage: PrNd 15-30%, Gd 3-6%, Ga 0.05-0.15%, B 0.5-1.2%, Co 0.6 ⁇ 1.2%, Al 0.3 ⁇ 0.8%, Cu 0.05 ⁇ 0.3%, Mo 0.05 ⁇ 0.3%, Ti 0.05 ⁇ 0.3%, the balance is Fe.
  • a finer grain structure is obtained through the addition of the above formula, the low melting point metal is first dissolved in the intergranular, the solubility of the high melting point metal in the liquid phase is improved, and it is uniformly distributed in the intergranular region, while the High melting point metals can hinder the growth of grains and refine the grains.
  • the remanence and coercivity of NdFeB magnets under this formula are still at a low level.
  • NdFeB magnet It is a technical problem that needs to be solved at present to seek a formula of NdFeB magnet, which can obtain magnetic properties such as remanence, coercivity and squareness at a relatively high level to meet the current application in high-demand fields.
  • the present invention provides an R-T-B magnet. and its preparation method.
  • the specific coordination between the components in the R-T-B magnet of the present invention can be prepared as a magnet material with magnetic properties such as remanence, coercivity and squareness at a relatively high level.
  • the present invention mainly solves the above technical problems through the following technical solutions.
  • the present invention provides an R-T-B magnet, which includes the following components:
  • R ⁇ 30.0wt.%
  • R is rare earth element
  • Fe 58-69 wt.%; wt.% is the percentage of the mass of each component to the total mass of each component; the R-T-B magnet also contains Co and Ti; in the R-T-B magnet, the mass content of the Co The ratio to the total mass content of "the Nb and the Ti" is 4-10.
  • the total mass of the above components includes the mass content of Co and Ti.
  • the content of the R is preferably 30-32 wt.%, such as 30.5 wt.%, 30.6 wt.% or 30.7 wt.%.
  • the R can generally also include Nd.
  • the content of the Nd can be conventional in the field, and the Nd is preferably 22-32wt.%, such as 28.2wt.%, 28.4wt.%, 29.2wt.%, 29.3wt.%, 29.4wt.% %, 29.5 wt. %, 29.8 wt. %, 29.9 wt. % or 30.3 wt. %, wt. % is the percentage of the total mass of each component.
  • the type of R generally includes Pr and/or RH, and the RH is a heavy rare earth element.
  • the content of the Pr is preferably below 0.3 wt. %, for example, 0.2 wt. %, and wt. % is the percentage of the total mass of each component.
  • the content of the RH is preferably below 3wt.%, such as 0.2wt.%, 0.6wt.%, 0.8wt.%, 1.1wt.%, 1.2wt.%, 1.4wt.%, 2.3wt.% % or 2.5wt.%, wt.% is the percentage of the total mass of each component.
  • the type of RH preferably includes Tb or Dy.
  • the content of Tb is preferably 0.2-1.1 wt.%, such as 0.2 wt.%, 0.5 wt.%, 0.6 wt.%, 0.8 wt.% or 1.1 wt.% , wt.% is the percentage of the total mass of each component.
  • the content of Dy is preferably 0.5 to 2.5 wt.%, such as 0.6 wt.%, 1.2 wt.%, 1.8 wt.% or 2.5 wt.%, where the wt.% is percentage of the total mass of each component.
  • the ratio of the atomic percent content of RH to the atomic percent content of R may be less than 0.1, such as 0.02, 0.04, 0.06 or 0.08, and the atomic percent content refers to the total content of each component atomic percent.
  • the content of Nb is preferably 0.15-0.25wt.%, such as 0.16wt.%, 0.18wt.%, 0.2wt.%, 0.22wt.%, 0.23wt.% or 0.24wt.% .
  • the ratio of the mass content of Co to the total mass content of "the Nb and the Ti" is preferably 4.6-8.4, such as 4.6, 5.3, 5.5, 6.5, 6.6 , 6.7, 6.8, 7.9 or 8.4, more preferably 4-7.
  • the content of Co is preferably 1.5-3.5 wt.%, such as 2 wt.%, 2.5 wt.%, 2.6 wt.%, 2.8 wt.% or 3 wt.%.
  • the content of Ti is preferably 0.15-0.35wt.%, such as 0.15wt.%, 0.18wt.%, 0.23wt.%, 0.25wt.% or 0.35wt.%.
  • the content of the B is preferably 0.955-1.1 wt.%, for example, 0.99 wt.%.
  • the ratio of the atomic percentage of B to the atomic percentage of R in the R-T-B magnet may be above 0.38, such as 0.41, 0.42, 0.43 or 0.44, and the atomic percentage refers to The atomic percentage of the total content of each component.
  • the Fe content is preferably 65-66wt.%, such as 64.67wt.%, 64.71wt.%, 64.88wt.%, 64.89wt.%, 64.98wt.%, 65.07wt.%, 65.13 wt. %, 65.14 wt. %, 65.33 wt. %, 65.38 wt. % or 65.64 wt. %.
  • the R-T-B magnet may further contain Cu.
  • the content of the Cu may be 0.1-0.4wt.%, such as 0.1wt.%, 0.15wt.%, 0.25wt.%, 0.3wt.%, 0.36wt.% or 0.39wt.%, wt.% as a percentage of the total mass of each component.
  • the R-T-B magnet generally introduces inevitable impurities, such as one or more of C, O and Mn, during the preparation process.
  • the R-T-B magnet preferably further comprises Co-Ti-Nb, the Co-Ti-Nb phase is located in the intergranular triangular region, and the area of the Co-Ti-Nb phase in the intergranular triangular region is equal to The ratio of the total area of the intercrystalline triangular region is 1.1-2.5%.
  • the intergranular triangular region can be the meaning commonly understood in the art, and generally refers to the grain boundary phase formed between three or more main phase particles.
  • the area of the Co-Ti-Nb phase and the total area of the intergranular triangular region generally refer to the area respectively occupied by the detected cross-section of the R-T-B magnet during FE-EPMA detection.
  • the atomic percentage content ratio among Co, Ti and Nb is close to 8:1:1.
  • the Co-Ti-Nb phase is preferably Co 8 Ti 1 Nb 1 phase.
  • the ratio of the area of the Co-Ti-Nb phase in the intergranular triangular region to the total area of the intergranular triangular region is, for example, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7% , 1.8%, 1.9% or 2%.
  • the RTB magnet includes the following components: Nd 29.5wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.07wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 2%.
  • the RTB magnet includes the following components: Nd 29.5wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.23wt.%, Nb 0.24wt.%, B 0.99wt.% and Fe 64.98wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.8%.
  • the RTB magnet includes the following components: Nd 29.5wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.35wt.%, Nb 0.22wt.%, B 0.99wt.% and Fe 64.88wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.7%.
  • the RTB magnet includes the following components: Nd 29.5wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.15wt.%, Nb 0.16wt.%, B 0.99wt.% and Fe 65.14wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.5%.
  • the RTB magnet includes the following components: Nd 29.5wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 3wt.%, Ti 0.18wt.%, Nb 0.2 wt.%, B 0.99wt.% and Fe 64.67wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 2%.
  • the RTB magnet includes the following components: Nd 29.8wt.%, Tb 0.8wt.%, Cu 0.3wt.%, Co 2.6wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.13wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.9%.
  • the RTB magnet includes the following components: Nd 29.9wt.%, Tb 0.6wt.%, Cu 0.25wt.%, Co 2.5wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.38wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 2%.
  • the RTB magnet includes the following components: Nd 30.3wt.%, Tb 0.2wt.%, Cu 0.39wt.%, Co 2.8wt.%, Ti 0.23wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 64.89wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.8%.
  • the RTB magnet includes the following components: Nd 28.2wt.%, Dy 2.5wt.%, Cu 0.15wt.%, Co 3wt.%, Ti 0.25wt.%, Nb 0.2 wt.%, B 0.99wt.% and Fe 64.71wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.8%.
  • the RTB magnet includes the following components: Nd 28.4wt.%, Tb 0.5wt.%, Dy 1.8wt.%, Cu 0.1wt.%, Co 2.5wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.33wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet It contains Co 8 Ti 1 Nb 1 phase, and the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.8%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Dy 1.2wt.%, Cu 0.39wt.%, Co 2wt.%, Ti 0.18wt.%, Nb 0.2 wt.%, B 0.99wt.% and Fe 65.64wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.7%.
  • the RTB magnet includes the following components: Nd 29.2wt.%, Tb 0.8wt.%, Dy 0.6wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.07wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet It contains Co 8 Ti 1 Nb 1 phase, and the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.6%.
  • the RTB magnet includes the following components: Nd 29.3wt.%, Pr 0.2wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.07wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet It contains Co 8 Ti 1 Nb 1 phase, and the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.7%.
  • the RTB magnet includes the following components: Nd 29.5wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.07wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.2%.
  • the RTB magnet includes the following components: Nd 29.5wt.%, Tb 1.1wt.%, Cu 0.36wt.%, Co 2.6wt.%, Ti 0.18wt.%, Nb 0.2wt.%, B 0.99wt.% and Fe 65.07wt.%, wt.% is the percentage of the mass of each component to the total mass of each component; the intergranular triangular region of the RTB magnet contains Co 8 Ti 1 Nb 1 phase, the ratio of the area of the Co 8 Ti 1 Nb 1 phase to the total area of the intergranular triangular region is 1.1%.
  • the invention provides a preparation method of an R-T-B magnet, which comprises the following steps: after the raw material mixture of each component of the above-mentioned R-T-B magnet is sintered, air cooling treatment and aging treatment are performed in sequence.
  • the process of the sintering treatment can be conventional in the art.
  • the temperature of the sintering treatment is preferably 1000-1100°C, for example, 1080°C.
  • the sintering is preferably carried out under vacuum conditions.
  • vacuum conditions For example, 5 ⁇ 10 -3 Pa vacuum conditions.
  • the time of the sintering treatment may be conventional in the art, and may be 4 to 8 hours, for example, 6 hours.
  • the temperature of the air cooling treatment is preferably 550 to 950°C, such as 550°C, 600°C, 650°C, 700°C, 750°C, 800°C or 950°C.
  • the temperature of the air cooling treatment generally refers to the temperature at which the fan is turned on to rapidly cool to room temperature after the sintering treatment is naturally cooled to the temperature of the air cooling treatment.
  • the time of the air-cooling treatment in the present invention is not particularly limited, and may be appropriately adjusted according to the temperature of the air-cooling treatment.
  • the aging treatment can adopt the conventional aging process in the art, generally including primary aging and secondary aging.
  • the temperature of the primary aging treatment may be 860-920°C, for example, 880°C or 900°C.
  • the time of the first-stage aging treatment may be 2.5 to 4 hours, for example, 3 hours.
  • the temperature of the secondary aging treatment may be 460-530°C, for example, 500°C, 510°C or 520°C.
  • the time of the secondary aging treatment may be 2.5-4 hours, for example, 3 hours.
  • grain boundary diffusion can generally be performed after the aging treatment.
  • the grain boundary diffusion can be a conventional process in the field, generally, the grain boundary diffusion of heavy rare earth elements is performed.
  • the temperature of the grain boundary diffusion may be 800-900°C, for example, 850°C.
  • the time for the grain boundary diffusion may be 5-10 hours, for example, 8 hours.
  • the addition method of the heavy rare earth elements in the R-T-B magnet can refer to the routine in the field, generally 0-80% of the heavy rare earth elements are added during smelting and the rest are added during smelting, such as 25%, 30%, 40%, 50% or 67%.
  • the heavy rare earth element added at the time of smelting is, for example, Tb.
  • the heavy rare earth element in the R-T-B magnet when the heavy rare earth element in the R-T-B magnet is Tb and Tb is greater than 0.5 wt.%, 25-67% of Tb is added during smelting, and the rest is added during grain boundary diffusion.
  • the heavy rare earth elements in the R-T-B magnet are Tb and Dy
  • the Tb is added during smelting
  • the Dy is added during grain boundary diffusion.
  • the heavy rare earth element in the R-T-B magnet is Tb and Tb is less than or equal to 0.5 wt.% or when the heavy rare earth element in the R-T-B magnet is Dy
  • the heavy rare earth element in the R-T-B magnet diffuses at grain boundaries added when.
  • the temperature of the grain boundary diffusion may be 800-900°C, for example, 850°C.
  • the time for the grain boundary diffusion may be 5-10 hours, for example, 8 hours.
  • the raw material mixture of each component of the R-T-B magnet is sequentially subjected to smelting, casting, hydrogen crushing, pulverizing and magnetic field molding.
  • the smelting can adopt a conventional smelting process in the art.
  • the vacuum degree of the melting is, for example, 5 ⁇ 10 -2 Pa.
  • the smelting temperature is, for example, 1550°C or lower.
  • the smelting is generally carried out in a high-frequency vacuum induction smelting furnace.
  • the casting process can be conventional in the art.
  • the casting process is, for example, a rapid-setting sheet casting method.
  • the casting temperature may be 1390-1460°C, preferably 1410-1440°C, for example, 1430°C.
  • the thickness of the alloy ingot obtained after the casting may be 0.25-0.40 mm, for example, 0.29 mm.
  • the process of hydrogen crushing and pulverization can generally be followed by hydrogen absorption, dehydrogenation, and cooling.
  • the hydrogen absorption can be carried out under the condition of a hydrogen pressure of 0.085 MPa.
  • the dehydrogenation can be carried out under the condition of raising the temperature while drawing a vacuum.
  • the temperature of the dehydrogenation may be 480-520°C, eg 500°C.
  • the process of the micro-pulverization may adopt a conventional process in the art, such as jet mill pulverization.
  • the gas atmosphere during the fine pulverization may be carried out with an oxidizing gas content below 1000 ppm, and the oxidizing gas content refers to the content of oxygen or moisture.
  • the pressure during the fine pulverization is, for example, 0.68 MPa.
  • a lubricant such as zinc stearate, is generally also added.
  • the added amount of the lubricant may be 0.05-0.15%, for example, 0.12%, of the mass of the powder obtained after the fine pulverization.
  • the process of forming the magnetic field may adopt a conventional process in the art.
  • the magnetic field forming can be carried out under the protection of a magnetic field strength above 1.8T and a nitrogen atmosphere. For example, it is performed under a magnetic field strength of 1.8 to 2.5T.
  • the present invention also provides an R-T-B magnet, which is prepared by the above preparation method.
  • the reagents and raw materials used in the present invention are all commercially available.
  • the positive improvement effect of the present invention is that: the present invention provides elements such as Co, Ti, Nb, and B with a specific coordination relationship, further optimizes the formula of the R-T-B magnet, the coercivity of the obtained R-T-B magnet is significantly improved, and the remanence , high stability performance and magnetic properties such as squareness are also at a high level.
  • FIG. 1 is a SEM image of the R-T-B magnet in Example 1.
  • FIG. The arrow A in Fig. 1 points to the Co-Ti-Nb phase of single-point quantitative analysis in the intergranular triangular region.
  • the raw materials were prepared, and the raw material mixture (0.4wt. Forming, sintering treatment, air cooling treatment, aging treatment and grain boundary diffusion.
  • Jet mill pulverization is performed in an atmosphere with an oxidizing gas content of 100 ppm or less, and the oxidizing gas refers to oxygen or moisture content.
  • the pressure of the grinding chamber of the jet mill pulverization is 0.68MPa.
  • the lubricant zinc stearate was added in an amount of 0.12% by weight of the powder after mixing.
  • Magnetic field molding carried out under the protection of a magnetic field strength of 1.8-2.5T and a nitrogen atmosphere.
  • Sintering treatment sintering at 1080°C for 6 hours under the vacuum condition of 5 ⁇ 10 -3 Pa; Ar gas can be introduced to make the gas pressure reach 0.05MPa before cooling.
  • Air-cooling treatment After the sintering treatment, it is naturally cooled to 650°C, and the fan is turned on to quickly cool to room temperature.
  • / means that the element is not added. Ga and Zr are not detected in the R-T-B magnets of the above-mentioned embodiments and comparative examples, and C, O and Mn are inevitably introduced into the R-T-B magnets of the final product during the preparation process. These impurities are not included.
  • Example 1 14.4 26.5 49.30 0.99
  • Example 2 14.3 26.8 48.89 0.99
  • Example 3 14.3 26.9 48.69 0.98
  • Example 4 14.4 26.4 49.23 0.99
  • Example 5 14.4 26.9 49.30 0.98
  • Example 6 14.4 25.3 49.58 0.99
  • Example 7 14.5 24.4 49.99 0.99
  • Example 8 14.7 23.5 51.24 0.99
  • Example 9 13.9 24.4 46.00 0.99
  • Example 10 14.0 28.7 46.67 0.99
  • Example 11 14.3 21.7 48.55 0.99
  • Example 12 14.3 26.8 48.35 0.99
  • Example 13 14.4 26.6 49.37 0.99
  • Example 14 14.4 25.4 49.30 0.95
  • Example 15 14.4 25.5 49.30 0.94
  • Comparative Example 1 14.4 24.4 49.30 0.98 Comparative Example 2 14.4 24.6 49.30 0.99 Comparative Example 3 14.4 24.5 49.30 0.97
  • FE-EPMA Field Emission Electron Probe Microanalyzer
  • FIG. 1 it is the SEM microstructure diagram of the RTB magnet in Example 1 detected by FE-EPMA.
  • the position indicated by the arrow A in Figure 1 refers to the Co-Ti-Nb phase quantitatively analyzed at a single point in the intergranular triangular region.
  • Co 8 Ti 1 Nb 1 phase is formed in the intergranular triangular region of the RTB magnet of the present invention, and the ratio of the area of this phase in the intergranular triangular region to the total area of the intergranular triangular region (the following The area ratio of the Co 8 Ti 1 Nb 1 phase for short) is 2%.
  • the area of the Co 8 Ti 1 Nb 1 phase and the area of the intergranular triangular region respectively refer to the area occupied by the detected cross section (the above-mentioned vertical orientation plane).
  • the test results of Examples 2 to 15 and Comparative Examples 1 to 4 are shown in Table 3 below.

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Abstract

本发明公开了一种R-T-B磁体及其制备方法。该R-T-B磁体包括以下组分：R：≥30.0wt.％，R为稀土元素，Nb：0.1～0.3wt.％；B：0.955～1.2wt.％；Fe：58～69wt.％；wt.％为各组分的质量占各组分总质量的百分比；所述的R-T-B磁体中还含有Co和Ti；所述R-T-B磁体中，所述Co的质量含量与"所述Nb和所述Ti"的总质量含量的比值为4～10。本发明进一步优化了R-T-B磁体中各组分之间的配合关系，可制备为剩磁、矫顽力和方形度等磁性能均在较高水平的磁体材料。

Description

一种R-T-B磁体及其制备方法 技术领域
本发明涉及一种R-T-B磁体及其制备方法。
背景技术
钕铁硼永磁体材料作为一类重要的稀土功能材料，拥有优良的综合磁性能，被广泛应用于电子行业、电动汽车等诸多领域。但目前的钕铁硼磁体材料的综合磁性能较差，难以制备得到性能更优异的产品，无法满足社会需求。
例如中国专利文献CN106158204A公开了一种钕铁硼永磁体材料，其由如下重量百分比的组分组成：PrNd 15～30％、Gd 3～6％、Ga 0.05～0.15％、B 0.5～1.2％、Co 0.6～1.2％、Al 0.3～0.8％、Cu 0.05～0.3％、Mo 0.05～0.3％、Ti 0.05～0.3％，余量为Fe。该专利文献中通过上述配方的添加获得了较细的晶粒组织，低熔点金属先在晶间溶解，提高了高熔点金属在液相中的溶解性，使之在晶间区域均匀分布，而高熔点金属能够阻碍晶粒的长大，细化晶粒。但是该配方下的钕铁硼磁体的剩磁和矫顽力仍然在较低的水平。
寻求一种钕铁硼磁体的配方，能够得到剩磁、矫顽力和方形度等磁性能均在较高水平，以符合目前高要求领域的应用，是目前需要解决的技术问题。
发明内容
本发明为了解决现有技术中存在的R-T-B磁体配方的协同配合效果较低，得到的磁体材料的剩磁、矫顽力和方形度无法同时达到较高水平的缺陷，而提供了一种R-T-B磁体及其制备方法。本发明中的R-T-B磁体中各组分之间的特定配合，可制备为剩磁、矫顽力和方形度等磁性能均在较高水平的磁体材料。
本发明主要是通过以下技术方案解决以上技术问题的。
本发明提供了一种R-T-B磁体，其包括以下组分：
R：≥30.0wt.％，R为稀土元素，
Nb：0.1～0.3wt.％；
B：0.955～1.2wt.％；
Fe：58～69wt.％；wt.％为各组分的质量占各组分总质量的百分比；所述的R-T-B磁体中还含有Co和Ti；所述R-T-B磁体中，所述Co的质量含量与“所述Nb和所述Ti”的总质量含量的比值为4～10。
本发明中，根据所述的R-T-B磁体可知，上述的各组分总质量包括Co和Ti的质量含量。
本发明中，所述R的含量较佳地为30～32wt.％，例如30.5wt.％、30.6wt.％或30.7wt.％。
本发明中，所述R中一般还可包括Nd。
其中，所述Nd的含量可为本领域常规，所述Nd较佳地为22～32wt.％，例如28.2wt.％、28.4wt.％、29.2wt.％、29.3wt.％、29.4wt.％、29.5wt.％、29.8wt.％、29.9wt.％或30.3wt.％，wt.％为占各组分总质量的百分比。
本发明中，所述R的种类一般还包括Pr和/或RH，所述RH为重稀土元素。
其中，所述Pr的含量较佳地在0.3wt.％以下，例如0.2wt.％，wt.％为占各组分总质量的百分比。
其中，所述RH的含量较佳地在3wt.％以下，例如0.2wt.％、0.6wt.％、0.8wt.％、1.1wt.％、1.2wt.％、1.4wt.％、2.3wt.％或2.5wt.％，wt.％为占各组分总质量的百分比。
其中，所述的RH的种类较佳地包括Tb或Dy。
当所述的RH包括Tb时，所述Tb的含量较佳地为0.2～1.1wt.％，例如0.2wt.％、0.5wt.％、0.6wt.％、0.8wt.％或1.1wt.％，wt.％为占各组分总质量的百分比。
当所述的RH包括Dy时，所述Dy的含量较佳地为0.5～2.5wt.％，例如0.6wt.％、1.2wt.％、1.8wt.％或2.5wt.％，wt.％为占各组分总质量的百分比。
其中，所述RH的原子百分含量与所述R的原子百分含量的比值可为0.1以下，例如0.02、0.04、0.06或0.08，所述的原子百分含量是指占各组分总含量的原子百分比。
本发明中，所述Nb的含量较佳地为0.15～0.25wt.％，例如0.16wt.％、0.18wt.％、0.2wt.％、0.22wt.％、0.23wt.％或0.24wt.％。
本发明中，所述R-T-B磁体中，所述Co的质量含量与“所述Nb和所述Ti”的总质量含量的比值较佳地为4.6～8.4，例如4.6、5.3、5.5、6.5、6.6、6.7、6.8、7.9或8.4，更佳地为4～7。
本发明中，所述Co的含量较佳地为1.5～3.5wt.％，例如2wt.％、2.5wt.％、2.6wt.％、2.8wt.％或3wt.％。
本发明中，所述Ti的含量较佳地为0.15～0.35wt.％，例如0.15wt.％、0.18wt.％、0.23wt.％、0.25wt.％或0.35wt.％。
本发明中，所述B的含量较佳地为0.955～1.1wt.％，例如0.99wt.％。
本发明中，所述B的原子百分含量与所述R-T-B磁体中R的原子百分含量的比值可在0.38以上，例如0.41、0.42、0.43或0.44，所述的原子百分含量是指占各组分总含量的原子百分比。
本发明中，所述Fe的含量较佳地为65～66wt.％，例如64.67wt.％、64.71wt.％、64.88wt.％、64.89wt.％、64.98wt.％、65.07wt.％、65.13wt.％、65.14wt.％、65.33wt.％、65.38wt.％或65.64wt.％。
本发明中，所述的R-T-B磁体中还可包含Cu。
其中，所述Cu的含量可为0.1～0.4wt.％，例如0.1wt.％、0.15wt.％、0.25wt.％、0.3wt.％、0.36wt.％或0.39wt.％，wt.％为占各组分总质量的百分比。
本发明中，本领域技术人员知晓，所述R-T-B磁体在制备的过程中一般还会引入不可避免的杂质，例如C、O和Mn中的一种或多种。
发明人发现，上述元素及其含量之间的特定配合关系的磁体组分配方，在制备成R-T-B磁体后，得到的磁体材料的矫顽力、剩磁和方形度等磁性能均在较高的水平。进一步分析之后发现，该配方下的R-T-B磁体相比于不是 该配方的磁体材料，在晶间三角区中形成了Co-Ti-Nb相。所述Co-Ti-Nb相的存在显著地阻碍了晶粒长大。
本发明中，所述的R-T-B磁体较佳地还包括Co-Ti-Nb，所述Co-Ti-Nb相位于晶间三角区，所述晶间三角区中Co-Ti-Nb相的面积与所述晶间三角区总面积的比为1.1～2.5％。其中，所述的晶间三角区可为本领域内常规理解的含义，一般是指3个以上的主相颗粒之间形成的晶界相。所述Co-Ti-Nb相的面积与所述晶间三角区总面积一般是指，FE-EPMA检测时，分别在所检测的所述R-T-B磁体的截面中所占的面积。
其中，所述的Co-Ti-Nb相中，Co、Ti和Nb之间的原子百分含量的比值接近8：1：1。所述的Co-Ti-Nb相较佳地为Co 8Ti 1Nb 1相。
其中，所述晶间三角区中Co-Ti-Nb相的面积与所述晶间三角区总面积的比例如为1.1％、1.2％、1.3％、1.4％、1.5％、1.6％、1.7％、1.8％、1.9％或2％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为2％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.23wt.％、Nb 0.24wt.％、B 0.99wt.％和Fe 64.98wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.8％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.35wt.％、Nb 0.22wt.％、B 0.99wt.％和Fe 64.88wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间 三角区总面积的比为1.7％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.15wt.％、Nb 0.16wt.％、B 0.99wt.％和Fe 65.14wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.5％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 3wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 64.67wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为2％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.8wt.％、Tb 0.8wt.％、Cu 0.3wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.13wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.9％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.9wt.％、Tb 0.6wt.％、Cu 0.25wt.％、Co 2.5wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.38wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为2％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 30.3wt.％、Tb 0.2wt.％、Cu 0.39wt.％、Co 2.8wt.％、Ti 0.23wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 64.89wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.8％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 28.2wt.％、 Dy 2.5wt.％、Cu 0.15wt.％、Co 3wt.％、Ti 0.25wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 64.71wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.8％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 28.4wt.％、Tb 0.5wt.％、Dy 1.8wt.％、Cu 0.1wt.％、Co 2.5wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.33wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.8％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Dy 1.2wt.％、Cu 0.39wt.％、Co 2wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.64wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.7％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.2wt.％、Tb 0.8wt.％、Dy 0.6wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.6％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.3wt.％、Pr 0.2wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.7％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B 磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.2％。
本发明一较佳实施例中，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.1％。
本发明提供了一种R-T-B磁体的制备方法，其包括以下步骤：上述R-T-B磁体各组分的原料混合物经烧结处理后，再依次进行风冷处理和时效处理。
本发明中，所述烧结处理的工艺可为本领域常规。
其中，所述烧结处理的温度较佳地为1000～1100℃，例如1080℃。
其中，所述烧结较佳地在真空条件下进行。例如5×10 -3Pa真空条件。
其中，所述烧结处理的时间可采用本领域常规，可为4～8h，例如6h。
本发明中，所述风冷处理的温度较佳地为550～950℃，例如550℃、600℃、650℃、700℃、750℃、800℃或950℃。
本发明中，本领域技术人员知晓，所述风冷处理的温度一般是指在所述烧结处理之后自然冷却到所述风冷处理的温度时，开启风机快速冷却至室温的温度。本发明中所述风冷处理的时间无特别的限定，根据不同所述风冷处理的温度适当调节即可。
本发明中，所述的时效处理可采用本领域常规的时效工艺，一般包括一级时效和二级时效。
其中，所述一级时效处理的温度可为860～920℃，例如880℃或900℃。
其中，所述一级时效处理的时间可为2.5～4h，例如3h。
其中，所述二级时效处理的温度可为460～530℃，例如500℃、510℃或520℃。
其中，所述二级时效处理的时间可为2.5～4h，例如3h。
本发明中，当所述的R-T-B磁体中含有重稀土元素时，所述时效处理之 后一般还可进行晶界扩散。
其中，所述晶界扩散可为本领域常规的工艺，一般是将重稀土元素进行晶界扩散。
所述晶界扩散的温度可为800～900℃，例如850℃。所述晶界扩散的时间可为5～10h，例如8h。
其中，所述R-T-B磁体中的重稀土元素的添加方式可参照本领域常规，一般采用0～80％的重稀土元素在熔炼时添加且其余在熔炼时添加的方式，例如25％、30％、40％、50％或67％。在熔炼时添加的重稀土元素例如为Tb。
例如，当所述R-T-B磁体中的重稀土元素为Tb且Tb大于0.5wt.％时，25～67％的Tb在熔炼时添加，剩余部分在晶界扩散时添加。例如，当所述R-T-B磁体中的重稀土元素为Tb和Dy时，所述的Tb在熔炼时添加，所述的Dy在晶界扩散时添加。例如，当所述R-T-B磁体中的重稀土元素为Tb且Tb小于等于0.5wt.％时或者所述R-T-B磁体中的重稀土元素为Dy时，所述R-T-B磁体中的重稀土元素在晶界扩散时添加。
所述晶界扩散的温度可为800～900℃，例如850℃。所述晶界扩散的时间可为5～10h，例如8h。
本发明中，所述烧结处理之前一般还包括将所述R-T-B磁体各组分的原料混合物依次经熔炼、铸造、氢破粉碎、微粉碎和磁场成型。
其中，所述熔炼可采用本领域常规的熔炼工艺。
所述熔炼的真空度例如为5×10 -2Pa。
所述熔炼的温度例如在1550℃以下。
所述的熔炼一般在高频真空感应熔炼炉中进行。
其中，所述铸造的工艺可采用本领域常规。
所述铸造的工艺例如采用速凝铸片法。
所述铸造的温度可为1390～1460℃，较佳地为1410～1440℃，例如为1430℃。
所述铸造之后得到的合金铸片的厚度可为0.25～0.40mm，例如0.29mm。
其中，所述氢破粉碎的工艺一般可为依次经吸氢、脱氢、冷却处理。
所述吸氢可在氢气压力0.085MPa的条件下进行。
所述脱氢可在边抽真空边升温的条件下进行。所述脱氢的温度可为480-520℃，例如500℃。
其中，所述微粉碎的工艺可采用本领域常规的工艺，例如气流磨粉碎。
所述微粉碎时的气体氛围可为氧化气体含量在1000ppm以下进行，所述氧化气体含量是指氧气或水分的含量。
所述微粉碎时的压力例如为0.68MPa。
所述微粉碎后，一般还添加润滑剂，例如硬脂酸锌。
所述润滑剂的添加量可为所述微粉碎后得到的粉体质量的0.05～0.15％，例如0.12％。
其中，所述磁场成型的工艺可采用本领域常规的工艺。
所述磁场成型可在1.8T以上的磁场强度和氮气气氛保护下进行。例如1.8～2.5T的磁场强度下进行。
本发明还提供了一种R-T-B磁体，其采用上述制备方法制得。
在符合本领域常识的基础上，上述各优选条件，可任意组合，即得本发明各较佳实例。
本发明所用试剂和原料均市售可得。
本发明的积极进步效果在于：本发明提供了特定配合关系的Co、Ti和Nb，以及B等元素，进一步优化了R-T-B磁体的配方，得到的R-T-B磁体的矫顽力得到显著提升，且剩磁、高稳定性能以及方形度等磁性能同时也在较高水平。
附图说明
图1为实施例1中R-T-B磁体的SEM图。图1中A箭头所指为晶间三角区中单点定量分析的Co-Ti-Nb相。
具体实施方式
下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法，按照常规方法和条件，或按照商品说明书选择。
实施例1
按照下述表1中实施例1的R-T-B磁体的成分配制原料，将原料混合物(表1配方中0.4wt.％的Tb在熔炼时添加)依次经熔炼、铸造、氢破粉碎、微粉碎、磁场成型、烧结处理、风冷处理、时效处理和晶界扩散即得。
该R-T-B磁体的制备工艺如下所示：
(1)熔炼：在真空度为5×10 -2Pa的高频真空感应熔炼炉中熔炼，熔炼的温度为1550℃以下。
(2)铸造：采用速凝铸片法，获得厚度为0.29mm的合金铸片，浇铸的温度为1430℃。
(3)氢破粉碎：经吸氢、脱氢、冷却处理。吸氢在氢气压力0.085MPa的条件下进行。脱氢在边抽真空边升温的条件下进行，脱氢温度为500℃。
(4)微粉碎工序：在氧化气体含量100ppm以下的气氛下进行气流磨粉碎，氧化气体指的是氧气或水分含量。气流磨粉碎的研磨室压力为0.68MPa。粉碎后，添加润滑剂硬脂酸锌，添加量为混合后粉末重量的0.12％。
(6)磁场成型：在1.8～2.5T的磁场强度和氮气气氛保护下进行。
(7)烧结处理：在5×10 -3Pa真空条件下、在1080℃下烧结6h；冷却前可通入Ar气体使气压达到0.05MPa。
(8)风冷处理：烧结处理结束后，自然冷却至650℃，开启风机快速冷却至室温。
(9)时效处理：一级时效的温度900℃、时间3h；二级时效的温度510℃、时间3h。
(10)晶界扩散，将剩余重稀土元素(0.7wt.％的Tb)熔融后附着在材料表面，在850℃下进行晶界扩散8h。
2、实施例2～15和对比例1～4中R-T-B磁体的原料和风冷处理的温度如下表1所示，其余制备工艺同实施例1。其中，实施例2～7、13～15和对比例1～4中均是在熔炼时添加0.4wt％的Tb，其余Tb通过晶界扩散进入R-T-B磁体中；实施例8、9和11中的重稀土元素均是在晶界扩散时添加进入R-T-B磁体中；实施例10和12中的Tb在熔炼时添加，Dy通过晶界扩散进入R-T-B磁体中。
效果实施例1
1、成分测定：实施例1～15和对比例1～4中的R-T-B磁体使用高频电感耦合等离子体发射光谱仪(ICP-OES)进行测定。测试结果如下表1所示。
表1 R-T-B磁体的组分及含量(wt.％)
Figure PCTCN2022072253-appb-000001
注：/表示未添加该元素。上述各实施例和对比例的R-T-B磁体中未检测到Ga和Zr， 终产品的R-T-B磁体在制备过程中不可避免引入了C、O和Mn，各实施例和对比例中所记载的含量百分比并未将这些杂质包括在内。
2、磁性能的测试
在室温20℃条件下，实施例1～15和对比例1～4中的R-B-T磁体使用PFM脉冲式BH退磁曲线测试设备进行测试，得到剩磁(Br)、内禀矫顽力(Hcj)、最大磁能积(BHmax)和方形度(Hk/Hcj)的数据，测试结果如下表2所示。
表2
  Br(kGs) Hcj(kOe) BHmax(MGOe) Hk/Hcj
实施例1 14.4 26.5 49.30 0.99
实施例2 14.3 26.8 48.89 0.99
实施例3 14.3 26.9 48.69 0.98
实施例4 14.4 26.4 49.23 0.99
实施例5 14.4 26.9 49.30 0.98
实施例6 14.4 25.3 49.58 0.99
实施例7 14.5 24.4 49.99 0.99
实施例8 14.7 23.5 51.24 0.99
实施例9 13.9 24.4 46.00 0.99
实施例10 14.0 28.7 46.67 0.99
实施例11 14.3 21.7 48.55 0.99
实施例12 14.3 26.8 48.35 0.99
实施例13 14.4 26.6 49.37 0.99
实施例14 14.4 25.4 49.30 0.95
实施例15 14.4 25.5 49.30 0.94
对比例1 14.4 24.4 49.30 0.98
对比例2 14.4 24.6 49.30 0.99
对比例3 14.4 24.5 49.30 0.97
对比例4 14.4 24.3 49.30 0.99
3、微观结构的测试
采用FE-EPMA检测：对实施例1～15和对比例1～4中的R-T-B磁体的垂直取向面进行抛光，采用场发射电子探针显微分析仪(FE-EPMA)(日本电子株式会社(JEOL)，8530F)检测。首先通过FE-EPMA面扫描确定R-T-B磁体中Co、Ti和Nb元素的分布，然后通过FE-EPMA单点定量分析确定Co-Ti-Nb相中各元素的含量，测试条件为加速电压15kv，探针束流50nA。经检测，实施例1～15中Co-Ti-Nb相的Co、Ti和Nb元素的原子百分含量的比值接近8：1：8。测试结果如下表3所示。
如图1所示，为实施例1中的R-T-B磁体经FE-EPMA检测得到的SEM图微观结构图。图1中A箭头所指的位置是指：晶间三角区中单点定量分析的Co-Ti-Nb相。经检测和计算可得，在本发明R-T-B磁体的晶间三角区中形成了Co 8Ti 1Nb 1相，且晶间三角区中该物相的面积与晶间三角区总面积的比(以下简称Co 8Ti 1Nb 1相的面积占比)为2％。其中，Co 8Ti 1Nb 1相的面积和晶间三角区的面积分别是指在所检测的截面(上述的垂直取向面)中所占的面积。实施例2～15和对比例1～4的测试结果如下表3所示。
表3
  是否形成Co 8Ti 1Nb 1相 Co 8Ti 1Nb 1相的面积占比(％)
实施例1 是 2.0
实施例2 是 1.8
实施例3 是 1.7
实施例4 是 1.9
实施例5 是 2.0
实施例6 是 1.9
实施例7 是 2.0
实施例8 是 1.8
实施例9 是 1.8
实施例10 是 1.8
实施例11 是 1.7
实施例12 是 1.8
实施例13 是 1.8
实施例14 是 1.2
实施例15 是 1.1
对比例1 否 /
对比例2 否 /
对比例3 是 0.7
对比例4 是 1.0
由上述实验数据可知，发明人设计的上述R-T-B磁体的配方经制备为磁体材料后，可得到剩磁、矫顽力、高温稳定性、磁能积和方形度均在较高水平，综合磁性能优异的磁体材料，能够满足高要求领域的应用。经过进一步的微观结构分析，发明人发现，上述特定配方的R-T-B磁体经制备成磁体材料后，在磁体的晶间三角区中形成了特定面积占比的Co 8Ti 1Nb 1相，该物相的存在显著地阻碍了晶粒长大，进而提升了R-T-B磁体的矫顽力和其他磁性能。若本发明中R-T-B磁体的配方不在本发明的范围，无法得到Co 8Ti 1Nb 1相或者很少含量的该物相，难以显著提升R-T-B磁体的磁性能。

Claims (10)

  1. 一种R-T-B磁体，其特征在于，其包括以下组分：
    R：≥30.0wt.％，R为稀土元素，
    Nb：0.1～0.3wt.％；
    B：0.955～1.2wt.％；
    Fe：58～69wt.％；wt.％为各组分的质量占各组分总质量的百分比；
    所述的R-T-B磁体中还含有Co和Ti；所述R-T-B磁体中，所述Co的质量含量与“所述Nb和所述Ti”的总质量含量的比值为4～10。
  2. 如权利要求1所述的R-T-B磁体，其特征在于，所述R的含量为30～32wt.％，例如30.5wt.％、30.6wt.％或30.7wt.％；
    和/或，所述R中还包括Nd；
    其中，所述Nd的含量较佳地为22～32wt.％，例如28.2wt.％、28.4wt.％、29.2wt.％、29.3wt.％、29.4wt.％、29.5wt.％、29.8wt.％、29.9wt.％或30.3wt.％，wt.％为占各组分总质量的百分比；
    和/或，所述R的种类还包括Pr和/或RH，所述RH为重稀土元素；
    其中，所述Pr的含量较佳地在0.3wt.％以下，例如0.2wt.％，wt.％为占各组分总质量的百分比；
    其中，所述RH的含量较佳地在3wt.％以下，例如0.2wt.％、0.6wt.％、0.8wt.％、1.1wt.％、1.2wt.％、1.4wt.％、2.3wt.％或2.5wt.％，wt.％为占各组分总质量的百分比；
    其中，所述RH的种类较佳地包括Tb或Dy；
    当所述的RH包括Tb时，所述Tb的含量较佳地为0.2～1.1wt.％，例如0.2wt.％、0.5wt.％、0.6wt.％、0.8wt.％或1.1wt.％，wt.％为占各组分总质量的百分比；
    当所述的RH包括Dy时，所述Dy的含量较佳地为0.5～2.5wt.％，例如0.6wt.％、1.2wt.％、1.8wt.％或2.5wt.％，wt.％为占各组分总质量的百分比；
    其中，所述RH的原子百分含量与所述R的原子百分含量的比值较佳地在0.1以下。
  3. 如权利要求1所述的R-T-B磁体，其特征在于，所述Nb的含量为0.15～0.25，例如0.16wt.％、0.18wt.％、0.2wt.％、0.22wt.％、0.23wt.％或0.24wt.％；
    和/或，所述Co的质量含量与“所述Nb和所述Ti”的总质量含量的比值为4.6～8.4，例如4.6、5.3、5.5、6.5、6.6、6.7、6.8、7.9或8.4，较佳地为4～7；
    和/或，所述Co的含量为1.5～3.5wt.％，例如2wt.％、2.5wt.％、2.6wt.％、2.8wt.％或3wt.％；
    和/或，所述Ti的含量为0.15～0.35wt.％，例如0.15wt.％、0.18wt.％、0.23wt.％、0.25wt.％或0.35wt.％。
  4. 如权利要求1所述的R-T-B磁体，其特征在于，所述B的含量为0.955～1.1wt.％，例如0.99wt.％；
    和/或，所述B的原子百分含量与所述R-T-B磁体中R的原子百分含量的比值在0.38以上；
    和/或，所述Fe的含量为65～66wt.％，例如64.67wt.％、64.71wt.％、64.88wt.％、64.89wt.％、64.98wt.％、65.07wt.％、65.13wt.％、65.14wt.％、65.33wt.％、65.38wt.％或65.64wt.％；
    和/或，所述的R-T-B磁体中还包含Cu；
    其中，所述Cu的含量较佳地为0.1～0.4wt.％，例如0.1wt.％、0.15wt.％、0.25wt.％、0.3wt.％、0.36wt.％或0.39wt.％，wt.％为占各组分总质量的百分比。
  5. 如权利要求1～4中任一项所述的R-T-B磁体，其特征在于，所述的R-T-B磁体还包括Co-Ti-Nb相，所述的Co-Ti-Nb相位于晶间三角区，所述晶间三角区中Co-Ti-Nb相的面积与所述晶间三角区总面积的比为1.1～2.5％；
    其中，所述的Co-Ti-Nb相较佳地为Co 8Ti 1Nb 1相；
    其中，所述晶间三角区中Co-Ti-Nb相的面积与所述晶间三角区总面积的比例如为1.1％、1.2％、1.3％、1.4％、1.5％、1.6％、1.7％、1.8％、1.9％或2％。
  6. 如权利要求1所述的R-T-B磁体，其特征在于，所述的R-T-B磁体包 括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为2％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.23wt.％、Nb 0.24wt.％、B 0.99wt.％和Fe 64.98wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.8％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.35wt.％、Nb 0.22wt.％、B 0.99wt.％和Fe 64.88wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.7％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.15wt.％、Nb 0.16wt.％、B 0.99wt.％和Fe 65.14wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.5％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 3wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 64.67wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为2％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.8wt.％、Tb 0.8wt.％、Cu 0.3wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.13wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角 区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.9％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.9wt.％、Tb 0.6wt.％、Cu 0.25wt.％、Co 2.5wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.38wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为2％；
    或者，所述的R-T-B磁体包括以下组分：Nd 30.3wt.％、Tb 0.2wt.％、Cu 0.39wt.％、Co 2.8wt.％、Ti 0.23wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 64.89wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.8％；
    或者，所述的R-T-B磁体包括以下组分：Nd 28.2wt.％、Dy 2.5wt.％、Cu 0.15wt.％、Co 3wt.％、Ti 0.25wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 64.71wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1的面积与所述晶间三角区总面积的比为1.8％；
    或者，所述的R-T-B磁体包括以下组分：Nd 28.4wt.％、Tb 0.5wt.％、Dy 1.8wt.％、Cu 0.1wt.％、Co 2.5wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.33wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.8％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Dy 1.2wt.％、Cu 0.39wt.％、Co 2wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.64wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.7％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.2wt.％、Tb 0.8wt.％、Dy 0.6wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有C Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.6％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.3wt.％、Pr 0.2wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.7％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.2％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.5wt.％、Tb 1.1wt.％、Cu 0.36wt.％、Co 2.6wt.％、Ti 0.18wt.％、Nb 0.2wt.％、B 0.99wt.％和Fe 65.07wt.％，wt.％为各组分的质量占各组分总质量的百分比；所述R-T-B磁体的晶间三角区中含有Co 8Ti 1Nb 1相，所述Co 8Ti 1Nb 1相的面积与所述晶间三角区总面积的比为1.1％。
  7. 一种R-T-B磁体的制备方法，其特征在于，如权利要求1～4和6中任一项所述R-T-B磁体各组分的原料混合物经烧结处理后，再依次进行风冷处理和时效处理。
  8. 如权利要求7所述的R-T-B磁体的制备方法，其特征在于，所述烧结处理的温度为1000～1100℃，例如1080℃；
    和/或，所述烧结处理的时间为4～8h，例如6h；
    和/或，所述风冷处理的温度为550～950℃，例如550℃、600℃、650℃、 700℃、750℃、800℃或950℃；
    和/或，所述时效处理包括一级时效处理和二级时效处理；
    其中，所述一级时效处理的温度较佳地为860～920℃，例如880℃或900℃；
    其中，所述一级时效处理的时间较佳地为2.5～4h，例如3h；
    其中，所述二级时效处理的温度较佳地为460～530℃，例如500℃、510℃或520℃；
    其中，所述二级时效处理的时间较佳地为2.5～4h，例如3h；
    和/或，当所述R-T-B磁体中含有重稀土元素时，所述的时效处理之后还包括晶界扩散；
    其中，所述晶界扩散的温度较佳地800～900℃，例如850℃；
    其中，所述晶界扩散的时间较佳地为5～10h，例如8h；
    其中，所述R-T-B磁体中重稀土元素添加的方式优选采用0～80％的重稀土元素在熔炼时添加且其余重稀土元素在晶界扩散时添加的方式；例如，当所述R-T-B磁体中的重稀土元素为Tb且Tb大于0.5wt.％时，25～67％的Tb在熔炼时添加，剩余部分在晶界扩散时添加；或者例如，当所述R-T-B磁体中的重稀土元素为Tb和Dy时，所述的Tb在熔炼时添加，所述的Dy在晶界扩散时添加；或者例如，当所述R-T-B磁体中的重稀土元素为Tb且Tb小于等于0.5wt.％时或者所述R-T-B磁体中的重稀土元素为Dy时，所述R-T-B磁体中的重稀土元素在晶界扩散时添加。
  9. 如权利要求7或8所述的R-T-B磁体的制备方法，其特征在于，所述烧结处理之前还包括将熔炼、铸造、氢破粉碎、微粉碎和成型处理；
    其中，所述熔炼的温度例如在1550℃以下；
    其中，所述铸造的温度较佳地为1410～1440℃，例如为1430℃；
    其中，所述铸造之后得到的合金铸片的厚度较佳地为0.25～0.40mm，例如0.29mm；
    其中，所述氢破粉碎的工艺较佳地为依次经吸氢、脱氢、冷却处理；
    其中，所述磁场成型的磁场强度较佳地在1.8T以上，例如1.8～2.5T。
  10. 一种如权利要求7～9中任一项所述的R-T-B磁体的制备方法制得的R-T-B磁体。
PCT/CN2022/072253 2021-03-17 2022-01-17 一种r-t-b磁体及其制备方法 WO2022193820A1 (zh)

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