WO2022193818A1 - 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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WO2022193818A1
WO2022193818A1 PCT/CN2022/072251 CN2022072251W WO2022193818A1 WO 2022193818 A1 WO2022193818 A1 WO 2022193818A1 CN 2022072251 W CN2022072251 W CN 2022072251W WO 2022193818 A1 WO2022193818 A1 WO 2022193818A1
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content
phase
ratio
component
magnet
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PCT/CN2022/072251
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French (fr)
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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 JP2023544206A priority Critical patent/JP2024513631A/ja
Priority to KR1020237029961A priority patent/KR20230142567A/ko
Priority to EP22770178.6A priority patent/EP4303892A1/en
Priority to US18/277,116 priority patent/US20240127995A1/en
Publication of WO2022193818A1 publication Critical patent/WO2022193818A1/zh

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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 magnet materials have been widely used in electronics, electrical machinery, medical equipment and other fields. In recent years, the improvement of the magnetic properties of NdFeB magnet materials has become a current research focus.
  • Chinese patent document CN108831650A discloses a NdFeB magnet material and its preparation method.
  • the reduction of The amount of heavy rare earth elements in the material can also unify the secondary aging temperature of each brand and improve the universality of secondary aging.
  • the addition of these four composite elements achieves the purpose of refining the grains and improving the fluidity of the rare-earth-rich phase at the grain boundary, improving various performance indicators of the material, especially the intrinsic coercivity and squareness, and reducing the amount of heavy rare earths.
  • Example 5 of the patent contains the following components: PrNd 30.3%, Dy 0%, B 0.97%, Co 0.5%, Cu 0.15%, Al 0.1%, Ti 0.08%, Nb 0.1%, Ga 0.2 %, Zr 0.05%, the balance is Fe.
  • the fine powder of 3.0 ⁇ m was prepared by jet milling, the sintering temperature was 1040 °C, the primary aging temperature was 900 °C, and the secondary aging temperature was 520 °C.
  • the remanence was 14.4, Hcj was 12.5, and the maximum magnetic energy product was 50.82.
  • NdFeB magnet material with squareness of 97%.
  • the formula of the magnet material has not been further optimized, and the coercive force of the obtained magnet material is at a low level, and the magnetic property temperature at high temperature is also at a low level, which cannot be applied to products with higher requirements.
  • the present invention provides an R-T-B magnet. and its preparation method.
  • the combination of specific element types and specific contents in the R-T-B magnet of the present invention can prepare a magnet material with higher remanence, coercivity and squareness, and better high temperature stability.
  • the present invention mainly solves the above technical problems through the following technical solutions.
  • the invention provides an R-T-B magnet, which comprises the following components: R: ⁇ 30.0wt.%, R is a 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 content of the R is preferably 30-33 wt.%, such as 30 wt.%, 30.3 wt.% or 30.8 wt.%.
  • the type of R can be conventional in the art, and generally includes Nd.
  • the content of the Nd is preferably 29-31wt.%, such as 29wt.%, 29.4wt.%, 29.7wt.%, 29.9wt.%, 30wt.%, 30.1wt.% or 30.4wt.% , wt.% is the percentage of the total mass of each component.
  • the R generally also includes Pr and/or RH, and the RH is a heavy rare earth element.
  • the content of Pr is preferably below 0.3 wt.%, and wt.% is the percentage of the mass of each component to the total mass of each component.
  • the heavy rare earth element is preferably Tb.
  • the content of the RH may be below 1.4 wt.%, for example, 0.2 wt.%, 0.4 wt.%, 0.6 wt.%, 1 wt.%, and wt.% is a 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 or 0.06, and the atomic percent content refers to the atomic percentage of the total content of each component. percentage.
  • the content of "Ti+Nb" is preferably 0.1-0.24wt.%, for example, 0.1wt.%, 0.2wt.%, 0.23wt.% or 0.24wt.%.
  • the content of the Nb is preferably 0.05-0.14wt.%, for example, 0.05wt.%, 0.09wt.%, 0.1wt.%, 0.12wt.% or 0.14wt.%.
  • the content of Ti is preferably below 0.24wt.% and not 0wt.%, such as 0.05wt.%, 0.09wt.%, 0.11wt.%, 0.14wt.% or 0.15wt.% .
  • the content of "Al+Cu” is preferably below 0.44wt.% and not 0wt.%, more preferably 0.1-0.44wt.%, such as 0.23wt.%, 0.25wt.% , 0.32 wt. %, 0.33 wt. %, 0.34 wt. %, 0.43 wt. %, 0.44 wt. %, or 0.45 wt. %.
  • the content of Al is preferably below 0.08wt.% and not 0wt.%, such as 0.02wt.%, 0.03wt.%, 0.04wt.%, 0.05wt.%, 0.06wt.% or 0.08wt.%.
  • the content of the Cu is preferably 0.2-0.46wt.%, such as 0.2wt.%, 0.3wt.%, 0.39wt.%, 0.4wt.% or 0.46wt.%.
  • the content of the B is preferably 0.955-1.15 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 0.4, 0.41, 0.42, 0.43 or 0.44, and the atomic percentage is Refers to the atomic percentage of the total content of each component.
  • the Fe content is preferably 67-69wt.%, such as 67.53wt.%, 67.58wt.%, 67.63wt.%, 67.68wt.%, 67.74wt.%, 68.02wt.%, 68.03 wt. %, 68.04 wt. %, 68.16 wt. %, 68.31 wt. %, 68.38 wt. %, 68.49 wt. %, 68.57 wt. % or 68.58 wt. %.
  • the R-T-B magnet may also contain conventional additive elements in the art, such as Co.
  • the content of Co is preferably below 1 wt.%, for example, or 0.8 wt.%, and wt.% is the percentage of the mass of each component to 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 inventor found that the combination of the above-mentioned specific content of elements such as Ti, Nb, Cu, etc., the magnetic properties of the obtained R-T-B magnet such as coercivity, high temperature stability and squareness have been significantly improved. . Further analysis found that after the components of the above-mentioned specific formula were prepared into R-T-B magnets, part of Fe in the two-grain grain boundary phase aggregated with Nb and Cu elements to form a Cu-Nb-Fe phase. The Cu-Nb-Fe phase The existence of Fe can significantly reduce the Fe content in the two-grain grain boundary phase, and increase the magnetic isolation effect of the Nd-rich phase, thereby obtaining the R-T-B magnet of the present invention.
  • the R-T-B magnet preferably includes a Cu-Nb-Fe phase, and the Cu-Nb-Fe phase is located in the intergranular triangular region.
  • the intergranular triangular region can be the meaning commonly understood in the field, and generally refers to the grain boundary phase formed between three or more main phase particles.
  • the two-grain grain boundary phase is generally the grain boundary phase between two main phase grains.
  • the ratio of the area of the Cu-Nb-Fe phase to the total area of the intergranular triangular region is preferably 1.3-2%, such as 1.3%, 1.4%, 1.5% or 1.6%.
  • the area of the Cu-Nb-Fe phase or the total area of the intergranular triangular region generally refers to the area respectively occupied in the detected R-T-B cross-section during FE-EPMA detection.
  • the comparison between the content of Fe in the two grain boundary phase and the total content of all elements in the two grain boundary phase is preferably below 46wt.%, such as 40wt.%, 41wt.%, 42wt.%, 43wt.%, 44wt% .%, 45wt.% or 46wt.%.
  • All elements in the two-grain boundary phase are, for example, Fe, rare earth elements, Cu, Nb, and the like.
  • the Cu-Nb-Fe phase is preferably Cu 5 Nb 1 Fe 94 phase.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Cu 0.3wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.49wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.5%, and the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 45 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Co 0.8wt.%, Cu 0.3wt.%, Al 0.03wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 67.68wt.%, wt.% is the mass ratio of the content of each component to the total content of each component; the crystallite of the RTB magnet
  • the inter-triangular region also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the inter-granular triangular region is 1.5%, and the content of Fe in the two-grain grain boundary phase is related to the two-grain The ratio of the total content of all elements in the grain boundary phase is 46 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Co 0.5wt.%, Cu 0.2wt.%, Al 0.05wt.%, Nb 0.05wt.%, Ti 0.05wt.%, B 0.99wt.% and Fe 68.16wt.%, wt.% is the mass ratio of the content of each component to the total content of each component; the crystallite of the RTB magnet
  • the inter-triangular region also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the inter-granular triangular region is 1.4%, and the content of Fe in the two-grain grain boundary phase is related to the two-grain The ratio of the total content of all elements in the grain boundary phase is 45 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Co 0.6wt.%, Cu 0.4wt.%, Al 0.04wt.%, Nb 0.14wt.%, Ti 0.09wt.%, B 0.99wt.% and Fe 67.74wt.%, wt.% is the mass ratio of the content of each component to the total content of each component; the crystal of the RTB magnet
  • the inter-triangular region also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the inter-granular triangular region is 1.6%, and the content of Fe in the two-grain grain boundary phase is related to the two-grain The ratio of the total content of all elements in the grain boundary phase is 43 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Cu 0.2wt.%, Al 0.03wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.58wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.5%, and the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 43 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Cu 0.39wt.%, Al 0.04wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.38wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.5%, and the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 42 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Cu 0.46wt.%, Al 0.04wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.31wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.4%, the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 46 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Cu 0.3wt.%, Al 0.04wt.%, Nb 0.05wt.%, Ti 0.05wt.%, B 0.99wt.% and Fe 68.57wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.4%, the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 44 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Co 0.8wt.%, Cu 0.3wt.%, Al 0.03wt.%, Nb 0.1wt.%, Ti 0.14wt.%, B 0.99wt.% and Fe 67.64wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the inter-triangular region also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the inter-granular triangular region is 1.5%, and the content of Fe in the two-grain grain boundary phase is related to the two-grain The ratio of the total content of all elements in the grain boundary phase is 43 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Co 0.8wt.%, Cu 0.3wt.%, Al 0.03wt.%, Nb 0.12wt.%, Ti 0.11wt.%, B 0.99wt.% and Fe 67.65wt.%, wt.% is the mass ratio of the content of each component to the total content of each component; the crystallinity of the RTB magnet
  • the inter-triangular region also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the inter-granular triangular region is 1.4%, and the content of Fe in the two-grain grain boundary phase is related to the two-grain The ratio of the total content of all elements in the grain boundary phase is 45 wt.%.
  • the RTB magnet includes the following components: Nd 29.7wt.%, Tb 0.6wt.%, Cu 0.39wt.%, Al 0.04wt.%, Nb 0.1wt.%, Ti 0.14wt.%, B 0.99wt.% and Fe 68.04wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.6%, the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 45 wt.%.
  • the RTB magnet includes the following components: Nd 30.4wt.%, Tb 0.4wt.%, Cu 0.39wt.%, Al 0.05wt.%, Nb 0.1wt.%, Ti 0.14wt.%, B 0.99wt.% and Fe 67.53wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.4%, the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 45 wt.%.
  • the RTB magnet includes the following components: Nd 29.9wt.%, Tb 0.4wt.%, Cu 0.39wt.%, Al 0.06wt.%, Nb 0.1wt.%, Ti 0.14wt.%, B 0.99wt.% and Fe 68.02wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.4%, the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 43 wt.%.
  • the RTB magnet includes the following components: Nd 30.1wt.%, Tb 0.2wt.%, Cu 0.39wt.%, Al 0.05wt.%, Nb 0.09wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.03wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.4%, the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 44 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Cu 0.3wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.49wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.5%, and the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 42 wt.%.
  • the RTB magnet includes the following components: Nd 29.4wt.%, Tb 0.6wt.%, Cu 0.3wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.49wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.5%, and the content of Fe in the two-grain boundary phase is related to all elements in the two-grain boundary phase The ratio of the total content was 45 wt.%.
  • the RTB magnet includes the following components: Nd 30wt.%, Cu 0.3wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.49wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, The ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.5%, and the ratio of the Fe content in the two-grain grain boundary phase to the total content of all elements in the two-grain grain boundary phase is 43 wt.% .
  • the RTB magnet includes the following components: Nd 29wt.%, Tb 1wt.%, Cu 0.3wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15 wt.%, B 0.99wt.% and Fe 68.49wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.4%, and the content of Fe in the two-grain boundary phase is equal to the total content of all elements in the two-grain grain boundary phase. The ratio is 45 wt.%.
  • the RTB magnet includes the following components: Nd 28.2wt.%, Tb 0.6wt.%, Dy 1.2wt.%, Cu 0.36wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.43wt.%, wt.% is the mass ratio of the content of each component to the total content of each component; the intergranular of the RTB magnet
  • the triangular zone also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular zone is 1.4%, and the content of Fe in the two-grain grain boundary phase is related to the two-grain crystal.
  • the ratio of the total content of all elements in the boundary phase is 44 wt.%.
  • the RTB magnet includes the following components: Nd 28.4wt.%, Tb 0.6wt.%, Dy 1wt.%, Co 0.5wt.%, Cu 0.36wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 67.93wt.%, wt.% is the mass ratio of the content of each component to the total content of each component; the The intergranular triangular region of the RTB magnet also includes a Cu 5 Nb 1 Fe 94 phase, and the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.3%. The ratio of the content to the total content of all elements in the two-grain boundary phase is 46 wt.%.
  • the RTB magnet includes the following components: Nd 28.8wt.%, Tb 0.6wt.%, Dy 0.6wt.%, Cu 0.36wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.43wt.%, wt.% is the mass ratio of the content of each component to the total content of each component; the intergranular of the RTB magnet
  • the triangular zone also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular zone is 1.3%, and the content of Fe in the two-grain grain boundary phase is related to the two-grain crystal.
  • the ratio of the total content of all elements in the boundary phase is 46 wt.%.
  • the RTB magnet includes the following components: Nd 28.2wt.%, Tb 0.7wt.%, Dy 0.3wt.%, Co 0.8wt.%, Cu 0.36wt.%, Al 0.02wt.%, Nb 0.05wt.%, Ti 0.15wt.%, B 0.99wt.% and Fe 68.43wt.%, wt.% is the mass ratio of the content of each component to the total content of each component;
  • the intergranular triangular region of the RTB magnet also includes a Cu 5 Nb 1 Fe 94 phase, the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.3%, and Fe in the two-grain grain boundary phase The ratio of the content to the total content of all elements in the two-grain boundary phase is 46 wt.%.
  • the present invention also provides a method for preparing the above-mentioned R-T-B magnet, which includes the following steps: the raw material mixture of the above-mentioned components is finely pulverized, and then sintered;
  • the particle size of the powder obtained by the fine pulverization is 3.9 to 4.4 ⁇ m.
  • the particle size of the powder obtained by the fine pulverization is, for example, 3.9 ⁇ m, 4.0 ⁇ m, 4.1 ⁇ m, 4.2 ⁇ m or 4.3 ⁇ m.
  • the inventor found that if the particle size of the powder after the micro-pulverization is larger than 4.4 ⁇ m, or smaller than 3.9 ⁇ m, the R-T-B magnet in the intergranular triangular region will be reduced.
  • the particle size of the powder generally refers to D50.
  • the micro-pulverization process can adopt a conventional process in the art, such as jet mill pulverization.
  • the gas atmosphere during the micro-pulverization may have 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 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 temperature of the sintering treatment can be a conventional temperature in the art, preferably 1000-1100°C, for example 1080°C.
  • the sintering treatment is preferably performed 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.
  • micro-pulverization generally further includes the following steps: the raw material mixture of each component of the R-T-B magnet is sequentially smelted, cast, and hydrogen crushed.
  • 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 for example, adopts the rapid-setting casting method.
  • the casting temperature may be 1390-1460°C, for example, 1400, 1420°C or 1430°C.
  • the thickness of the alloy slab obtained after the casting may be 0.25-0.40mm, for example, 0.29mm.
  • 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.
  • a conventional forming process in the field is generally included.
  • the forming can adopt the magnetic field forming method.
  • the forming is 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 sintering treatment generally further includes conventional aging treatment in the art.
  • the aging treatment generally includes 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 2.5-4 hours, for example, 3 hours.
  • the temperature of the secondary aging treatment may be 460-530°C, for example, 490°C, 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 is generally included after the aging treatment.
  • the grain boundary diffusion can be a conventional process in the art, 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 method of adding heavy rare earth elements in the R-T-B magnet can refer to the conventional method in the field, generally adopt the method of adding 0-80% heavy rare earth elements during smelting and adding the rest during smelting, such as 33%, 38%, 40% %, 57% 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.%, 40-67% 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 R-T-B magnet when the R-T-B magnet contains 0.08 wt. % or less of Al, generally no additional Al is added when preparing the raw material mixture of each component. Those skilled in the art know that Al below 0.08 wt. % is generally introduced during the preparation process.
  • the present invention also provides an R-T-B magnet 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 further optimizes the formula of the R-T-B magnet through the combination of elements such as Ti, Nb, and Cu with a specific content, and the coercivity of the obtained R-T-B magnet is significantly improved, and the remanence, high stability Magnetic properties such as performance and squareness are also at a high level.
  • FIG. 1 is a SEM image of the R-T-B magnet in Example 1.
  • the raw materials were prepared, and the raw material mixture (0.4 wt.% of Tb in Table 1 was added in the smelting process, and the remaining 0.2 wt. Add) through smelting, casting, hydrogen crushing, micro-grinding, magnetic field forming, sintering, aging treatment and grain boundary diffusion in sequence.
  • the smelting is carried out in a high-frequency vacuum induction melting furnace, the vacuum degree of the melting furnace is 5 ⁇ 10 -2 Pa, and the temperature is below 1530 °C;
  • Casting was carried out by the quick-setting casting method to obtain an alloy casting sheet with a thickness of 0.29 mm, and the casting temperature was 1420 °C;
  • Hydrogen crushing is followed by hydrogen absorption, dehydrogenation and cooling.
  • Hydrogen absorption can be carried out under the condition of hydrogen pressure of 0.085MPa;
  • dehydrogenation can be carried out under the condition of vacuuming and heating, and the dehydrogenation temperature is 500°C;
  • the fine pulverization is performed by jet mill pulverization in an atmosphere with an oxidizing gas content of 100 ppm or less, and the particle size of the obtained powder is 4.1 ⁇ m.
  • the oxidizing gas refers to the oxygen or moisture content.
  • the pressure of the grinding chamber of the jet mill pulverization is 0.68MPa. After pulverizing, add lubricant zinc stearate in an amount of 0.12% by weight of the powder after mixing;
  • Magnetic field forming is carried out under the protection of magnetic field strength of 1.8-2.5T and nitrogen atmosphere;
  • the temperature of primary aging is 900°C and the time is 3h; the temperature of secondary aging is 490°C and the time is 3h.
  • Grain boundary diffusion The remaining heavy rare earth elements (0.2 wt. % of Tb) were attached to the surface of the material, and grain boundary diffusion was performed at 850° C. for 8 h.
  • Example 2 The raw materials and powder particle sizes of the R-T-B magnets of Examples 2 to 22 and Comparative Examples 1 to 7 are shown in Table 1 below, and the rest of the preparation processes are carried out according to Example 1. Among them, in Examples 1-11, 15, 16, 18 and Comparative Examples 1-7, 0.4wt% of Tb was added during smelting, and the rest Tb diffused into the R-T-B magnet through grain boundaries; Heavy rare earth elements are added at grain boundary diffusion; Example 17 does not include grain boundary diffusion. In Examples 19 to 22, Tb was added during melting, and Dy was added during grain boundary diffusion.
  • / means that the element is not detected.
  • Ga and Zr are not detected in the R-T-B magnets of the above-mentioned embodiments and comparative examples, and the R-T-B magnets of the final product inevitably introduce C, O, Mn in the preparation process, and the contents recorded in each embodiment and the comparative examples are not. Include these impurities.
  • Al below 0.08wt% is introduced in the preparation process, and is not specially added in the form of raw materials.
  • FE-EPMA Field Emission Electron Probe Microanalyzer
  • Figure 1 shows the SEM image of the RTB magnet in Example 1 detected by FE-EPMA.
  • the arrow of a in Figure 1 points to the Cu-Nb-Fe phase quantitatively analyzed at a single point in the intergranular triangular region.
  • the ratio of the area of the Cu 5 Nb 1 Fe 94 phase to the total area of the intergranular triangular region is 1.5%
  • the area of the Cu 5 Nb 1 Fe 94 phase and the total area of the intergranular triangular region respectively refer to the area occupied in the cross-section (the aforementioned vertical orientation plane) of the RTB magnet detected during FE-EPMA detection.
  • the content of Fe in the two-grain boundary phase was analyzed by FE-EPMA. It was found that the ratio of the Fe content in the two-grain boundary phase to the total content of all elements in the two-grain boundary phase was 45wt.%.
  • the inventor found that after the RTB magnet with the above specific formula was prepared into a magnet material, a Cu 5 Nb 1 Fe 94 phase with a specific area ratio was formed in the intergranular triangular region of the magnet. The existence of the phase aggregates and distributes the Fe element in the two-grain boundary phase, thereby reducing the Fe distributed in the two-grain boundary phase, enhancing the magnetic isolation of the neodymium-rich phase, thereby improving the magnetic properties.
  • the content of a certain element in the formula of the RTB magnet is not within the scope of the present invention, only a small amount of Cu 5 Nb 1 Fe 94 phase is formed, and it is difficult to significantly reduce Fe in the two-grain boundary phase.
  • the content of Cu in Comparative Example 1 is too low, Cu is only concentrated in the phase interface between the main phase and the grain boundary phase, and the Cu 5 Nb 1 Fe 94 phase cannot be formed in the grain boundary phase.
  • Comparative Example 4 where Al+Cu is greater than 0.5 wt.%, the excess Cu enters the grain boundary phase, which reduces the interface stability and reduces the formation of the Cu 5 Nb 1 Fe 94 phase.
  • the Nb+Ti in Comparative Example 5 is greater than 0.24wt%, which leads to excessive pinning of high-melting elements at the grain boundaries and affects the fluidity of the Nd-rich phase, resulting in a decrease in the content of the Cu 5 Nb 1 Fe 94 phase.

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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：0.02～0.14wt.％；Cu：0.2～0.48wt.％；Ti+Nb：≤0.24wt.％；Al+Cu：≤0.50wt.％；B：≥0.955wt.％；Fe：58～69wt.％；wt.％为各组分的质量占各组分总质量的百分比。本发明中的R-T-B磁体的剩磁、矫顽力、高温稳定性和方形度均在较佳的水平。

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
钕铁硼磁体材料目前已广泛应用于电子、电力机械、医疗器具等领域。近年来，对钕铁硼磁体材料磁性能的提升成为目前的研究热点。
例如中国专利文献CN108831650A公开了一种钕铁硼磁体材料及其制备方法，通过在钕铁硼材料中复合添加钛、锆、铌、镓各0.05～0.5％，采用少量多种的添加原则，降低材料中重稀土元素的用量，同时可统一各牌号二级时效温度、提高二级时效的普适性。这四种复合元素的添加，达到细化晶粒的同时提高晶界富稀土相流动性的目的，提高材料的各项性能指标尤其是内禀矫顽力及方形度，在降低重稀土用量的同时改善产品方形度，提高产品一致性和高温稳定性。例如该专利实施例5的配方中含有如下质量含量的组分PrNd 30.3％、Dy 0％、B 0.97％、Co 0.5％、Cu 0.15％、Al 0.1％、Ti 0.08％、Nb 0.1％、Ga 0.2％、Zr 0.05％，余量为Fe。采用气流磨制备为3.0μm的细粉，烧结温度为1040℃、一级时效温度为900℃、二级时效温度为520℃的制备工艺得到剩磁为14.4、Hcj为12.5、最大磁能积为50.82、方形度为97％的钕铁硼磁体材料。但该磁体材料的配方未进行进一步优化，得到的磁体材料的矫顽力在较低水平，且高温时的磁性能温度性也在较低水平，无法适用于更高要求的产品中。
寻求一种钕铁硼磁体的配方，使经制备后得到高矫顽力、高剩磁、矫顽力的高温度稳定性、高方形度的综合磁性能优异的磁体材料，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钕铁硼磁体材料的配方得到的磁体的剩磁、矫顽力、高温稳定性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磁体中特定元素种类和特定含量之间的配合，能够制备得到较高的剩磁、矫顽力和方形度、高温稳定性也较佳的磁体材料。
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：0.02～0.14wt.％；
Cu：0.2～0.48wt.％；
Ti+Nb：≤0.24wt.％；
Al+Cu：≤0.50wt.％；
B：≥0.955wt.％；
Fe：58～69wt.％；wt.％为各组分的质量占各组分总质量的百分比。
本发明中，所述R的含量较佳地为30～33wt.％，例如30wt.％、30.3wt.％或30.8wt.％。
本发明中，所述R的种类可为本领域常规，一般包括Nd。
其中，所述Nd的含量较佳地为29～31wt.％，例如29wt.％、29.4wt.％、29.7wt.％、29.9wt.％、30wt.％、30.1wt.％或30.4wt.％，wt.％为占各组分总质量的百分比。
本发明中，所述R中一般还包括Pr和/或RH，所述的RH为重稀土元素。
其中，所述Pr的含量较佳地在0.3wt.％以下，wt.％为各组分的质量占各组分总质量的百分比。
其中，所述重稀土元素较佳地为Tb。
其中，所述RH的含量可在1.4wt.％以下，例如0.2wt.％、0.4wt.％、0.6wt.％、1wt.％，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或0.06，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“Ti+Nb”的含量较佳地为0.1～0.24wt.％，例如0.1wt.％、0.2wt.％、0.23wt.％或0.24wt.％。
本发明中，所述Nb的含量较佳地为0.05～0.14wt.％，例如0.05wt.％、0.09wt.％、0.1wt.％、0.12wt.％或0.14wt.％。
本发明中，所述Ti的含量较佳地在0.24wt.％以下且不为0wt.％，例如0.05wt.％、0.09wt.％、0.11wt.％、0.14wt.％或0.15wt.％。
本发明中，所述“Al+Cu”的含量较佳地在0.44wt.％以下且不为0wt.％，更佳地为0.1～0.44wt.％，例如0.23wt.％、0.25wt.％、0.32wt.％、0.33wt.％、0.34wt.％、0.43wt.％、0.44wt.％或0.45wt.％。
本发明中，所述Al的含量较佳地在0.08wt.％以下且不为0wt.％，例如0.02wt.％、0.03wt.％、0.04wt.％、0.05wt.％、0.06wt.％或0.08wt.％。
本发明中，所述Cu的含量较佳地为0.2～0.46wt.％，例如0.2wt.％、0.3wt.％、0.39wt.％、0.4wt.％或0.46wt.％。
本发明中，所述B的含量较佳地为0.955～1.15wt.％，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0.4、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67～69wt.％，例如67.53wt.％、67.58wt.％、67.63wt.％、67.68wt.％、67.74wt.％、68.02wt.％、68.03wt.％、68.04wt.％、68.16wt.％、68.31wt.％、68.38wt.％、68.49wt.％、68.57wt.％或68.58wt.％。
本发明中，所述的R-T-B磁体中还可含有本领域内常规的添加元素，例如Co。
其中，所述Co的含量较佳地在1wt.％以下，例如或0.8wt.％，wt.％为各 组分的质量占各组分总质量的百分比。
本发明中，本领域技术人员知晓，所述的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。
发明人通过对R-T-B磁体的配方的优化发现，上述特定含量的Ti、Nb、Cu等元素之间的配合，得到的R-T-B磁体的矫顽力、高温稳定性和方形度等磁性能有显著的提升。进一步分析发现，上述特定配方的组分在制备成R-T-B磁体后，使得二颗粒晶界相中的部分Fe与Nb、Cu元素聚集形成了Cu-Nb-Fe相，所述Cu-Nb-Fe相的存在使得二颗粒晶界相中Fe的含量明显降低，增加了富Nd相的隔磁作用，从而得到本发明的R-T-B磁体。
本发明中，所述的R-T-B磁体较佳地包括Cu-Nb-Fe相，所述Cu-Nb-Fe相位于晶间三角区。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，所述的晶界相一般为二颗粒晶界相和晶间三角区形成的区域的统称。所述的二颗粒晶界相一般为两个主相颗粒之间的晶界相。
其中，晶间三角区中，所述Cu-Nb-Fe相的面积与晶间三角区总面积的比较佳地为1.3～2％，例如1.3％、1.4％、1.5％或1.6％。本发明中，所述Cu-Nb-Fe相的面积或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的截面中所占的面积。
其中，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比较佳地在46wt.％以下，例如40wt.％、41wt.％、42wt.％、43wt.％、44wt.％、45wt.％或46wt.％。所述二颗粒晶界相中的所有元素例如为Fe、稀土元素、Cu和Nb等。
其中，经检测，所述Cu-Nb-Fe相中，Cu、Nb和Fe的原子百分含量的比值接近5：1：94。因此，本发明中，所述的Cu-Nb-Fe相较佳地为Cu 5Nb 1Fe 94相。
在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.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、 B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％。
在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.％、Tb 0.6wt.％、Co 0.8wt.％、Cu 0.3wt.％、Al 0.03wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 67.68wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％。
在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.％、Tb 0.6wt.％、Co 0.5wt.％、Cu 0.2wt.％、Al 0.05wt.％、Nb 0.05wt.％、Ti 0.05wt.％、B 0.99wt.％和Fe 68.16wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％。
在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.％、Tb 0.6wt.％、Co 0.6wt.％、Cu 0.4wt.％、Al 0.04wt.％、Nb 0.14wt.％、Ti 0.09wt.％、B 0.99wt.％和Fe 67.74wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.6％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％。
在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.％、Tb 0.6wt.％、Cu 0.2wt.％、Al 0.03wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.58wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二 颗粒晶界相中所有元素总含量的比为43wt.％。
在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.％、Tb 0.6wt.％、Cu 0.39wt.％、Al 0.04wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.38wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为42wt.％。
在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.％、Tb 0.6wt.％、Cu 0.46wt.％、Al 0.04wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.31wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％。
在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.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.04wt.％、Nb 0.05wt.％、Ti 0.05wt.％、B 0.99wt.％和Fe 68.57wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为44wt.％。
在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.％、Tb 0.6wt.％、Co 0.8wt.％、Cu 0.3wt.％、Al 0.03wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 67.64wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％。
在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.％、Tb 0.6wt.％、Co 0.8wt.％、Cu 0.3wt.％、Al 0.03wt.％、Nb 0.12wt.％、 Ti 0.11wt.％、B 0.99wt.％和Fe 67.65wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％。
在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 29.7wt.％、Tb 0.6wt.％、Cu 0.39wt.％、Al 0.04wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 68.04wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.6％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％。
在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 30.4wt.％、Tb 0.4wt.％、Cu 0.39wt.％、Al 0.05wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 67.53wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％。
在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 0.4wt.％、Cu 0.39wt.％、Al 0.06wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 68.02wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％。
在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 30.1wt.％、Tb 0.2wt.％、Cu 0.39wt.％、Al 0.05wt.％、Nb 0.09wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.03wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二 颗粒晶界相中所有元素总含量的比为44wt.％。
在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.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为42wt.％。
在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.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％。
在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 30wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％。
在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 29wt.％、Tb 1wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％。
在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.％、Tb 0.6wt.％、Dy 1.2wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、 Ti 0.15wt.％、B 0.99wt.％和Fe 68.43wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为44wt.％。
在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 0.6wt.％、Dy 1wt.％、Co 0.5wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 67.93wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.3％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％。
在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 28.8wt.％、Tb 0.6wt.％、Dy 0.6wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.43wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.3％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％。
在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.％、Tb 0.7wt.％、Dy 0.3wt.％、Co 0.8wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.43wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.3％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％。
本发明还提供了上述R-T-B磁体的制备方法，其包括以下步骤：上述各组分的原料混合物，经微粉碎后，再进行烧结处理；
所述微粉碎得到的粉体的粒径为3.9～4.4μm。
本发明中，所述微粉碎得到的粉体的粒径例如为3.9μm、4.0μm、4.1μm、4.2μm或4.3μm。
本发明中，在制备所述R-T-B磁体的过程中，发明人发现，在所述微粉碎之后的粉体粒径若大于4.4μm、或小于3.9μm会降低所述的R-T-B磁体在晶间三角区中Cu-Nb-Fe相的面积占比。所述粉体的粒径一般是指D50。
本发明中，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。
其中，所述微粉碎时的气体氛围可为氧化气体含量在1000ppm以下，所述氧化气体含量是指氧气或水分的含量。
其中，所述微粉碎时的压力例如为0.68MPa。
其中，所述微粉碎后，一般还添加润滑剂，例如硬脂酸锌。
其中，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％。
本发明中，所述烧结处理的温度可采用本领域常规的温度，较佳地为1000～1100℃，例如1080℃。
本发明中，所述烧结处理较佳地在真空条件下进行。例如5×10 -3Pa真空条件。
本发明中，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，本领域技术人员知晓，所述的微粉碎之前一般还包括以下步骤：所述R-T-B磁体各组分的原料混合物依次进行熔炼、铸造和氢破粉碎。
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。
其中，所述铸造的工艺例如采用速凝铸片法。
其中，所述铸造的温度可为1390～1460℃，例如为1400、1420℃或1430℃。
其中，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℃。
本发明中，所述微粉碎之后、所述烧结处理之前一般还包括本领域内常规的成型工艺。
其中，所述的成形可采用磁场成型法。
其中，所述成型在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。
本发明中，所述烧结处理之后一般还包括本领域内常规的时效处理。
其中，所述的时效处理一般包括一级时效和二级时效。
所述一级时效处理的温度可为860～920℃，例如880℃或900℃。
所述一级时效处理的时间可为2.5～4h，例如3h。
所述二级时效处理的温度可为460～530℃，例如490℃、500℃、510℃或520℃。
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磁体中还含有重稀土元素时，所述时效处理之后一般还包括晶界扩散。
其中，所述的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33％、38％、40％、57％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磁体中重稀土元素为Tb且Tb大于0.5wt.％时，40～67％ 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。
本发明中，当所述的R-T-B磁体中含有0.08wt.％以下的Al时，在配制各组分的原料混合物时，一般不额外添加Al。本领域技术人员知晓，0.08wt.％以下的Al一般是在制备过程中引入的。
本发明还提供了一种采用上述制备方法制得的R-T-B磁体。
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：本发明通过特定含量的Ti、Nb、Cu等元素的配合，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附图。其中，图1中a的箭头所指为晶间三角区中单点定量分析的Cu-Nb-Fe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，将该原料混合物(表1中的Tb有0.4wt.％在熔炼中添加，剩余的0.2wt.％在下述的晶界扩 散中添加)依次经熔炼、铸造、氢破粉碎、微粉碎、磁场成型、烧结、时效处理和晶界扩散即得。
其中，熔炼在高频真空感应熔炼炉中进行，熔炼炉的真空度为5×10 -2Pa，温度为1530℃以下；
采用速凝铸片法进行铸造，获得厚度为0.29mm的合金铸片，浇铸的温度为1420℃；
氢破粉碎为依次经吸氢、脱氢、冷却处理。吸氢可在氢气压力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℃；
微粉碎为在氧化气体含量100ppm以下的气氛下进行气流磨粉碎，得到粉体的粒径为4.1μm，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％；
磁场成型在1.8～2.5T的磁场强度和氮气气氛保护下进行；
烧结在5×10 -3Pa真空条件和1080℃下烧结6h，再冷却；冷却前可通入Ar气体使气压达到0.05MPa；
时效处理：一级时效的温度900℃、时间3h；二级时效的温度490℃、时间3h。
晶界扩散：将剩余的重稀土元素(0.2wt.％的Tb)附着在材料表面，在850℃下进行晶界扩散8h。
2、实施例2～22和对比例1～7的R-T-B磁体的原料以及粉体粒径按照如下表1所示，其余制备工艺按照实施例1进行。其中，实施例1～11、15、16、18和对比例1～7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12～14中的重稀土元素在晶界扩散时添加；实施例17不包括晶界扩散。实施例19～22中的Tb在熔炼时添加、Dy在晶界扩散时添加。
效果实施例1
1、成分测定：对实施例1～22和对比例1～7中的R-T-B系永磁材料使用 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.％)
表1
Figure PCTCN2022072251-appb-000001
Figure PCTCN2022072251-appb-000002
注：/表示未检测到该元素。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、Mn，各实施例和对比例中所记载的含量并未将这些杂质包括在内。同时，0.08wt％以下的Al为制备过程中引入的，并非以原料的形式特别添加。
2、磁性能的测试
实施例1～22和对比例1～7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
Figure PCTCN2022072251-appb-000003
Figure PCTCN2022072251-appb-000004
3、微观结构的测试
采用FE-EPMA检测：对实施例1～22和对比例1～7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Cu、Nb、Fe等元素的分布，然后通过FE-EPMA单点定量分析确定Cu-Nb-Fe相中Cu、Nb、Fe等元素的含量，测试条件为加速电压15kv，探针束流50nA。经检测，实施例1～18中Cu-Nb-Fe相的Cu、Nb、Fe元素的原子比接近5：1：94，因此，Cu-Nb-Fe相为Cu 5Nb 1Fe 94相。
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。图1中a的箭头所指为晶间三角区中单点定量分析的Cu-Nb-Fe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Cu 5Nb 1Fe 94相，且Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，Cu 5Nb 1Fe 94相的面积与晶间三角区总面积分别是指FE-EPMA检测时，在所检测的R-T-B磁体的截面(前述的垂直取向面)中所占的面积。同时，通过FE-EPMA检测分析 了二颗粒晶界相中Fe的含量，可得，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素的总含量的比为45wt.％。
实施例1～22和对比例1～7中的R-T-B磁体中FE-EPMA的测试结果如下表3所示。
表3
Figure PCTCN2022072251-appb-000005
Figure PCTCN2022072251-appb-000006
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的分析，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Cu 5Nb 1Fe 94相，该物相的存在聚集了分布二颗粒晶界相中的Fe元素，进而减少了二颗粒晶界相中分布的Fe，增强了富钕相的隔磁作用，进而提升了磁性能。
若R-T-B磁体的配方中某一元素的含量不在本发明范围内，只形成了少量的Cu 5Nb 1Fe 94相，难以显著的减少二颗粒晶界相中的Fe。例如，对比例1中Cu的含量过低，Cu仅会富集于主相和晶界相的相界面中，在晶界相中无法形成Cu 5Nb 1Fe 94相。例如，对比例4中，Al+Cu大于0.5wt.％，过量Cu进入晶界相中，降低界面稳定性，减少了Cu 5Nb 1Fe 94相的生成。例如，对比例5中Nb+Ti大于0.24wt％，导致过多的高熔点元素钉扎在晶界影响富Nd相的流动性，从而导致Cu 5Nb 1Fe 94相含量降低。

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：0.02～0.14wt.％；
    Cu：0.2～0.48wt.％；
    Ti+Nb：≤0.24wt.％；
    Al+Cu：≤0.50wt.％；
    B：≥0.955wt.％；
    Fe：58～69wt.％；wt.％为各组分的质量占各组分总质量的百分比。
  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30～33wt.％，例如30wt.％、30.3wt.％或30.8wt.％；
    和/或，所述R的种类还包括Nd；
    其中，所述Nd的含量较佳地为29～31wt.％，例如29wt.％、29.4wt.％、29.7wt.％、29.9wt.％、30wt.％、30.1wt.％或30.4wt.％，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，wt.％为占各组分总质量的百分比；
    其中，所述RH的种类较佳地为Tb；
    其中，所述RH的含量较佳地在1.4wt.％以下，例如0.2wt.％、0.4wt.％、0.6wt.％或1wt.％，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为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“Ti+Nb”的含量为0.1～0.24wt.％，例如0.1wt.％、0.2wt.％、0.23wt.％或0.24wt.％；
    和/或，所述Nb的含量为0.05～0.14wt.％，例如0.05wt.％、0.09wt.％、0.1wt.％、0.12wt.％或0.14wt.％；
    和/或，所述Ti的含量在0.24wt.％以下且不为0wt.％，例如0.05wt.％、 0.09wt.％、0.11wt.％、0.14wt.％或0.15wt.％，wt.％为占各组分总质量的百分比；
    和/或，所述“Al+Cu”的含量在0.44wt.％以下且不为0wt.％，较佳地为0.1～0.44wt.％，例如0.23wt.％、0.25wt.％、0.32wt.％、0.33wt.％、0.34wt.％、0.43wt.％或0.44wt.％；
    和/或，所述Al的含量在0.08wt.％以下且不为0wt.％，例如0.02wt.％、0.03wt.％、0.04wt.％、0.05wt.％、0.06wt.％或0.08wt.％，wt.％为占各组分总质量的百分比；
    和/或，所述Cu的含量为0.2～0.46wt.％，例如0.2wt.％、0.3wt.％、0.39wt.％、0.4wt.％或0.46wt.％。
  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0.955～1.15wt.％，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67～69wt.％，例如67.53wt.％、67.64wt.％、67.65wt.％、67.68wt.％、67.74wt.％、68.02wt.％、68.03wt.％、68.04wt.％、68.16wt.％、68.31wt.％、68.38wt.％、68.49wt.％、68.57wt.％或68.58wt.％；
    和/或，所述的R-T-B磁体中还含有Co；
    其中，所述Co的含量较佳地在1wt.％以下，例如0.8wt.％。
  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，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为40～46wt.％，例如42wt.％、43wt.％、44wt.％、45wt.％或46wt.％；
    和/或，所述的R-T-B磁体包括Cu-Nb-Fe相，所述Cu-Nb-Fe相位于晶间三角区；
    其中，所述Cu-Nb-Fe相的总面积与晶间三角区的总面积的比较佳地为1.3～2％，例如1.3％、1.4％、1.5％或1.6％；
    其中，所述Cu-Nb-Fe相中，Cu、Nb和Fe的原子百分比含量的比值较 佳地为5：1：94。
  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 29.4wt.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Co 0.8wt.％、Cu 0.3wt.％、Al 0.03wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 67.68wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Co 0.5wt.％、Cu 0.2wt.％、Al 0.05wt.％、Nb 0.05wt.％、Ti 0.05wt.％、B 0.99wt.％和Fe 68.16wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Co 0.6wt.％、Cu 0.4wt.％、Al 0.04wt.％、Nb 0.14wt.％、Ti 0.09wt.％、B 0.99wt.％和Fe 67.74wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.6％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Cu 0.2wt.％、Al 0.03wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.58wt.％， wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Cu 0.39wt.％、Al 0.04wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.38wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为42wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Cu 0.46wt.％、Al 0.04wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.31wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.04wt.％、Nb 0.05wt.％、Ti 0.05wt.％、B 0.99wt.％和Fe 68.57wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述的R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为44wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Co 0.8wt.％、Cu 0.3wt.％、Al 0.03wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 67.64wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所 有元素总含量的比为43wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Co 0.8wt.％、Cu 0.3wt.％、Al 0.03wt.％、Nb 0.12wt.％、Ti 0.11wt.％、B 0.99wt.％和Fe 67.65wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.7wt.％、Tb 0.6wt.％、Cu 0.39wt.％、Al 0.04wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 68.04wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.6％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 30.4wt.％、Tb 0.4wt.％、Cu 0.39wt.％、Al 0.05wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 67.53wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.9wt.％、Tb 0.4wt.％、Cu 0.39wt.％、Al 0.06wt.％、Nb 0.1wt.％、Ti 0.14wt.％、B 0.99wt.％和Fe 68.02wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 30.1wt.％、Tb 0.2wt.％、Cu 0.39wt.％、Al 0.05wt.％、Nb 0.09wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.03wt.％， wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为44wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为42wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29.4wt.％、Tb 0.6wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为45wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 30wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.5％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为43wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 29wt.％、Tb 1wt.％、Cu 0.3wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.49wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的 比为45wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 28.2wt.％、Tb 0.6wt.％、Dy 1.2wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.43wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.4％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为44wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 28.4wt.％、Tb 0.6wt.％、Dy 1wt.％、Co 0.5wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 67.93wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.3％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 28.8wt.％、Tb 0.6wt.％、Dy 0.6wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.43wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.3％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％；
    或者，所述的R-T-B磁体包括以下组分：Nd 28.2wt.％、Tb 0.7wt.％、Dy 0.3wt.％、Co 0.8wt.％、Cu 0.36wt.％、Al 0.02wt.％、Nb 0.05wt.％、Ti 0.15wt.％、B 0.99wt.％和Fe 68.43wt.％，wt.％为各组分的含量占各组分总含量的质量比；所述R-T-B磁体的晶间三角区中还包括Cu 5Nb 1Fe 94相，所述Cu 5Nb 1Fe 94相的面积与晶间三角区总面积的比为1.3％，二颗粒晶界相中Fe的含量与二颗粒晶界相中所有元素总含量的比为46wt.％。
  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，经微粉碎后，再进行烧结处理；
    所述微粉碎得到的粉体的粒径为3.9～4.4μm。
  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，所述微粉碎得到的粉体的粒径为3.9μm、4.0μm、4.1μm、4.2μm或4.3μm；
    和/或，所述微粉碎为气流磨粉碎；
    和/或，所述微粉碎时的气体氛围为氧化气体含量在1000ppm以下，所述氧化气体含量是指氧气或水分的含量；
    和/或，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，所述微粉碎之前还包括以下步骤：所述R-T-B磁体各组分的原料混合物依次进行熔炼、铸造和氢破粉碎；
    其中，所述熔炼的真空度例如为5×10 -2Pa；
    其中，所述熔炼的温度例如在1550℃以下；
    其中，所述铸造的工艺例如采用速凝铸片；
    其中，所述铸造的温度较佳地为1390～1460℃，例如为1400、1420℃或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；
    和/或，所述微粉碎之后、所述烧结处理之前还包括磁场成型。
  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，所述烧结处理之后还包括时效处理；
    其中，所述时效处理较佳地包括一级时效处理和二级时效处理；
    所述一级时效处理的温度较佳地为860～920℃，例如880℃或900℃；
    所述一级时效处理的时间较佳地为2.5～4h，例如3h；
    所述二级时效处理的温度较佳地为460～530℃，例如490℃、500℃、510℃或520℃；
    所述二级时效处理的时间较佳地为2.5～4h，例如3h；
    其中，当所述的R-T-B磁体中还含有重稀土元素时，所述时效处理之后 还包括晶界扩散；所述晶界扩散的温度较佳地为800～900℃，例如850℃；所述晶界扩散的时间较佳地为5～10h，例如8h；
    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磁体中重稀土元素为Tb且Tb大于0.5wt.％时，40～67％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。
  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。
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