WO2023005166A1 - 一种钕铁硼磁体材料及其制备方法和应用 - Google Patents

一种钕铁硼磁体材料及其制备方法和应用 Download PDF

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WO2023005166A1
WO2023005166A1 PCT/CN2022/072256 CN2022072256W WO2023005166A1 WO 2023005166 A1 WO2023005166 A1 WO 2023005166A1 CN 2022072256 W CN2022072256 W CN 2022072256W WO 2023005166 A1 WO2023005166 A1 WO 2023005166A1
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Prior art keywords
magnet material
ndfeb magnet
phase
grain boundary
percentage
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PCT/CN2022/072256
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French (fr)
Inventor
牟维国
黄佳莹
江政
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Fujian Changting Jinlong Rare Earth Co Ltd
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Fujian Changting Jinlong Rare Earth Co Ltd
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Priority to KR1020237025820A priority Critical patent/KR102723858B1/ko
Priority to JP2023544214A priority patent/JP2024519244A/ja
Priority to EP22847787.3A priority patent/EP4379754A4/en
Publication of WO2023005166A1 publication Critical patent/WO2023005166A1/zh
Priority to US18/411,258 priority patent/US20240153681A1/en
Anticipated expiration legal-status Critical
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    • H—ELECTRICITY
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    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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    • H01F41/0266—Moulding; Pressing
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    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Definitions

  • the invention relates to a neodymium-iron-boron magnet material and a preparation method and application thereof.
  • R-T-B series permanent magnet materials are known as the magnets with the highest performance among permanent magnets, and are used in voice coil motors for hard disk drives, motors for electric vehicles, motors for industrial equipment, etc.
  • the Chinese patent document CN110993233A discloses a kind of R-T-B permanent magnet material, which adjusts the rare earth content by increasing the content of X (Al ⁇ Cu ⁇ Ga), so that the ratio of Fe and B is changed, so that only the conventional content is required B can also form a 6:13:1 phase, and then obtain a magnet material with excellent magnetic properties.
  • Chinese patent document CN111180159A also discloses a kind of NdFeB permanent magnet material
  • the specific embodiment in this patent discloses the magnet material of following composition and structure: Nd 29wt.%, Tb 0.1wt.%, Dy 0.4wt .%, Cu 0.4wt.%, Al 0.5wt.%, Co 0.9wt.%, B 1wt.%, Nb 0.25wt.% and Fe 67.45wt.%; the intergranular rare earth-rich phase also generates a specific mass Ratio of phase Tb 0.4 Dy 2.5 -Al 0.59 -Nd 89.6 -Cu 1.4 -Co 5.1 .
  • the above formulas are all improved based on high Cu and high Al magnet materials, mainly because the addition of Cu element can effectively improve the coercive force of NdFeB magnets, but too much Cu (for example, more than 0.35wt.%) in The enrichment of grain boundaries will lead to the formation of microcracks in the magnet after sintering, thereby reducing the compactness and strength of the magnet.
  • the method of adding Al is generally used (for example, Chinese patent document CN110993234A) to solve the above defects.
  • the coercivity and remanence of these magnet materials still have a certain gap with the theoretical values of permanent magnet materials.
  • the main purpose of the present invention is to overcome the defect of low magnetic performance of the NdFeB magnet material containing Al and Cu existing in the prior art, and provide a NdFeB magnet material and its preparation method and application.
  • the neodymium-iron-boron magnet material prepared by optimizing the formula of the present invention increases the coercive force while maintaining high remanence and squareness.
  • the present invention mainly solves the above technical problems through the following technical solutions.
  • the invention provides a neodymium iron boron magnet material, which comprises the following components:
  • R 28-33wt.%, said R is a rare earth element
  • the R includes Nd and Pr, the Nd: 27-31.5wt.%;
  • the content of the Nd and the Pr in the NdFeB magnet material satisfies the following formula: Nd/Pr ⁇ 58.
  • the content of R is preferably 29-32.5wt.%, such as 29.3wt.%, 29.6wt.%, 29.7wt.%, 30.6wt.%, 30.7wt.%, 31.3wt.% , 31.5wt.%, 31.9wt.%, 32wt.%, 32.1wt.% or 32.3wt.%, wt.% refers to the percentage of the total mass of the NdFeB magnet material.
  • the content of Nd is preferably 27-31wt.%, such as 27.5wt.%, 28.3wt.%, 28.9wt.%, 29.1wt.%, 29.3wt.%, 29.5wt.%, 29.7wt.%, 29.8wt.%, 30.2wt.%, 30.5wt.% or 30.7wt.%, wt.% refers to the percentage of the total mass of the NdFeB magnet material.
  • the NdFeB magnet material may further include RH, and the RH is a heavy rare earth element.
  • the content of RH can be conventional in the field, preferably 0.5-2.5wt.%, such as 0.6wt.%, 0.9wt.%, 1wt.%, 1.2wt.%, 1.4wt.%, 1.5 wt.%, 1.7wt.%, 2wt.% or 2.3wt.%, wt.% refers to the percentage of the total mass of the NdFeB magnet material.
  • the type of RH is preferably Dy and/or Tb.
  • the content of Dy is preferably 0.2-2.5wt.%, such as 0.2wt.%, 0.9wt.%, 1.4wt.%, 1.5wt.%, 1.7wt.% or 2.3wt.%, wt.% refers to the percentage of the total mass of the NdFeB magnet material.
  • the content of Tb is preferably 0.5-2.5wt.%, such as 0.6wt.%, 0.8wt.%, 1.2wt.% or 2wt.%.
  • the percentage of the total mass of the NdFeB magnet material is preferably 0.5-2.5wt.%, such as 0.6wt.%, 0.8wt.%, 1.2wt.% or 2wt.%. The percentage of the total mass of the NdFeB magnet material.
  • the value of Nd/Pr is preferably 60-400, such as 98, 135, 275, 283, 289, 291, 295, 297, 298, 302, 305 or 307.
  • the Nd/Pr refers to the ratio of the Nd content to the Pr content.
  • the content of the Pr is preferably 0.1-0.3wt.%, such as 0.2wt.%.
  • the wt.% refers to the percentage of the total mass of the NdFeB magnet material.
  • the content of Al is preferably 0.45-1.15wt.%, such as 0.46wt.%, 0.61wt.%, 0.65wt.% or 0.7wt.%. Percentage of total mass of Fe-B magnet material.
  • the content of Cu is preferably 0.35-0.45wt.%, such as 0.36wt.%, 0.37wt.%, 0.38wt.%, 0.39wt.%, 0.4wt.% or 0.42wt.%.
  • wt.% refers to the percentage of the total mass of the NdFeB magnet material.
  • the content of Co is preferably 0.9-2.5wt.%, such as 1wt.%, 1.1wt.%, 1.2wt.%, 1.3wt.%, 1.4wt.% or 1.5wt.%, wt.% refers to the percentage of the total mass of the NdFeB magnet material.
  • the content of said Nb is preferably 0.25-0.55wt.%, such as 0.26wt.%, 0.3wt.% or 0.35wt.%. percentage of mass.
  • the content of B is preferably 0.98-1.05wt.%, such as 0.99wt.%, 1wt.%, 1.01wt.%, 1.02wt.% or 1.04wt.%, wt.% means The percentage of the total mass of the NdFeB magnet material.
  • the content of Fe is preferably 63-68wt.%, such as 63.71wt.%, 63.84wt.%, 64.17wt.%, 64.75wt.%, 64.82wt.%, 64.83wt.%, 65.25wt.%, 65.61wt.%, 65.78wt.%, 66.23wt.%, 66.84wt.%, 67.04wt.%, 67.24wt.%, 67.34wt.% or 67.35wt.%, wt.% means The percentage of the total mass of the NdFeB magnet material.
  • the ratio of the total area of the phases is preferably 3-7%, more preferably 4.5-5.5%, such as 4.9%, 5%, 5.1%, 5.2% or 5.3%.
  • the area of the Nd x P y Co z phase or the total area of the grain boundary phase respectively refers to the area occupied by the detected vertical orientation plane of the NdFeB magnet material.
  • the x is, for example, 51%, 52%, 53%, 54%, 55% or 56%.
  • said y is, for example, 4%, 5% or 6%.
  • the z is, for example, 40%, 41%, 42%, 43%, 44% or 45%.
  • x (y or z) refers to the percentage of the molar weight of Nd (Pr or Co) in the Nd x Pr y Co z phase to the total molar weight of all elements in the Nd x P y Co z phase.
  • the grain boundary phase can be the meaning commonly understood in the field, and generally refers to the general term of the region formed by the two-grain grain boundary phase and the intergranular triangular region.
  • the two-grain boundary phase is generally a grain boundary phase between two main phase particles.
  • the NdFeB magnet material is composed of the following components: Nd 29.7wt.%, Pr 0.1wt.%, Dy 1.7wt.%, Al 0.61wt.%, Cu 0.4wt. %, Co 1wt.%, Nb 0.25wt.%, B 0.99wt.% and Fe 65.25wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 55 Pr 4 Co 41 phase, and the ratio of the area of the Nd 55 Pr 4 Co 41 phase to the total area of the grain boundary phase is 5.1%.
  • the NdFeB magnet material is composed of the following components: Nd 29.8wt.%, Pr 0.1wt.%, Dy 1.4wt.%, Al 0.46wt.%, Cu 0.38wt. %, Co 1wt.%, Nb 0.25wt.%, B 1wt.% and Fe 65.61wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the boron magnet material contained the Nd 56 Pr 4 Co 40 phase, and the ratio of the area of the Nd 56 Pr 4 Co 40 phase to the total area of the grain boundary phase was 5.2%.
  • the NdFeB magnet material is composed of the following components: Nd 30.2wt.%, Pr 0.1wt.%, Dy 1.7wt.%, Al 0.61wt.%, Cu 0.38wt. %, Co 0.9wt.%, Nb 0.3wt.%, B 0.99wt.% and Fe 64.82wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 55 Pr 5 Co 40 phase, and the ratio of the area of the Nd 55 Pr 5 Co 40 phase to the total area of the grain boundary phase is 5%.
  • the NdFeB magnet material is composed of the following components: Nd 29.3wt.%, Pr 0.3wt.%, Dy 2.3wt.%, Al 0.61wt.%, Cu 0.39wt.
  • %, Co 1wt.%, Nb 0.26wt.%, B 1.01wt.% and Fe 64.83wt.%, wt.% is the percentage of the mass of each component to the total mass of the neodymium-iron-boron magnet material; the neodymium
  • the grain boundary phase of the iron-boron magnet material contains Nd 53 Pr 6 Co 41 phase, and the ratio of the area of the Nd 53 Pr 6 Co 41 phase to the total area of the grain boundary phase is 5.2%.
  • the NdFeB magnet material is composed of the following components: Nd 30.7wt.%, Pr 0.1wt.%, Dy 1.5wt.%, Al 1.15wt.%, Cu 0.37wt. %, Co 1.1wt.%, Nb 0.25wt.%, B 0.99wt.% and Fe 63.84wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 53 Pr 4 Co 43 phase, and the ratio of the area of the Nd 53 Pr 4 Co 43 phase to the total area of the grain boundary phase is 5.1%.
  • the NdFeB magnet material is composed of the following components: Nd 28.9wt.%, Pr 0.1wt.%, Tb 0.6wt.%, Al 0.46wt.%, Cu 0.36wt.
  • wt.% is the percentage of the mass of each component to the total mass of the neodymium-iron-boron magnet material; the neodymium
  • the grain boundary phase of the iron-boron magnet material contains Nd 56 Pr 4 Co 40 phase, and the ratio of the area of the Nd 56 Pr 4 Co 40 phase to the total area of the grain boundary phase is 4.9%.
  • the NdFeB magnet material is composed of the following components: Nd 28.3wt.%, Pr 0.1wt.%, Tb 1.2wt.%, Al 0.45wt.%, Cu 0.35wt.
  • wt.% is the percentage of the mass of each component to the total mass of the neodymium-iron-boron magnet material; the neodymium
  • the grain boundary phase of the iron-boron magnet material contains Nd 56 Pr 4 Co 40 phase, and the ratio of the area of the Nd 56 Pr 4 Co 40 phase to the total area of the grain boundary phase is 5.2%.
  • the NdFeB magnet material is composed of the following components: Nd 27wt.%, Pr 0.2wt.%, Tb 2.5wt.%, Al 0.45wt.%, Cu 0.36wt.% , Co 1wt.%, Nb 0.26wt.%, B 0.99wt.% and Fe 67.24wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the boron magnet material contained the Nd 54 Pr 5 Co 41 phase, and the ratio of the area of the Nd 54 Pr 5 Co 41 phase to the total area of the grain boundary phase was 5.3%.
  • the NdFeB magnet material is composed of the following components: Nd 27.5wt.%, Pr 0.1wt.%, Tb 2wt.%, Al 0.45wt.%, Cu 0.36wt.% , Co 1.3wt.%, Nb 0.26wt.%, B 0.99wt.% and Fe 67.04wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material; the neodymium
  • the grain boundary phase of the iron-boron magnet material contains Nd 55 Pr 4 Co 41 phase, and the ratio of the area of the Nd 55 Pr 4 Co 41 phase to the total area of the grain boundary phase is 4.9%.
  • the NdFeB magnet material is composed of the following components: Nd 28.3wt.%, Pr 0.1wt.%, Dy 0.9wt.%, Al 0.7wt.%, Cu 0.42wt. %, Co 1.5wt.%, Nb 0.25wt.%, B 0.99wt.% and Fe 66.84wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 54 Pr 4 Co 42 phase, and the ratio of the area of the Nd 54 Pr 4 Co 42 phase to the total area of the grain boundary phase is 5.2%.
  • the NdFeB magnet material is composed of the following components: Nd 30.5wt.%, Pr 0.1wt.%, Dy 1.5wt.%, Al 0.65wt.%, Cu 0.45wt .%, Co 1.4wt.%, Nb 0.25wt.%, B 0.98wt.% and Fe 64.17wt.%, wt.% is the percentage of the mass of each component and the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 55 Pr 4 Co 41 phase, and the ratio of the area of the Nd 55 Pr 4 Co 41 phase to the total area of the grain boundary phase is 5.1%.
  • the NdFeB magnet material is composed of the following components: Nd 29.7wt.%, Pr 0.1wt.%, Dy 1.7wt.%, Al 0.61wt.%, Cu 0.4wt. %, Co 2.5wt.%, Nb 0.26wt.%, B 1.02wt.% and Fe 63.71wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 54 Pr 5 Co 41 phase, and the ratio of the area of the Nd 54 Pr 5 Co 41 phase to the total area of the grain boundary phase is 5.1%.
  • the NdFeB magnet material is composed of the following components: Nd 29.7wt.%, Pr 0.1wt.%, Dy 1.7wt.%, Al 0.61wt.%, Cu 0.4wt. %, Co 1.5wt.%, Nb 0.25wt.%, B 0.99wt.% and Fe 64.75wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 51 Pr 4 Co 45 phase, and the ratio of the area of the Nd 51 Pr 4 Co 45 phase to the total area of the grain boundary phase is 5.2%.
  • the NdFeB magnet material is composed of the following components: Nd 29.1wt.%, Pr 0.1wt.%, Tb 1.5wt.%, Al 0.46wt.%, Cu 0.37wt. %, Co 0.9wt.%, Nb 0.35wt.%, B 0.99wt.% and Fe 66.23wt.%, wt.% is the percentage of the mass of each component to the total mass of the NdFeB magnet material;
  • the grain boundary phase of the NdFeB magnet material contains Nd 52 Pr 5 Co 43 phase, and the ratio of the area of the Nd 52 Pr 5 Co 43 phase to the total area of the grain boundary phase is 5.2%.
  • the NdFeB magnet material is composed of the following components: Nd 29.5wt.%, Pr 0.1wt.%, Dy 0.2wt.%, Tb 0.8wt.%, Al 0.46wt. %, Cu 0.37wt.%, Co 1.2wt.%, Nb 0.55wt.%, B 1.04wt.% and Fe 65.78wt.%, wt.% is the mass of each component and the total of the NdFeB magnet material Percentage by mass: the grain boundary phase of the NdFeB magnet material contains Nd 52 Pr 4 Co 44 phase, and the ratio of the area of the Nd 52 Pr 4 Co 44 phase to the total area of the grain boundary phase is 5.3%.
  • the present invention also provides a preparation method of an NdFeB magnet material, which includes the following steps: preparing the raw materials of each component according to the components of the NdFeB magnet material, and then passing the mixture of the raw materials of each component through It can be obtained after smelting, casting, crushing, molding, sintering and aging treatment;
  • the aging treatment includes three-stage aging treatment, wherein the temperature of the first-stage aging treatment is 850-950°C; the temperature of the second-stage aging treatment is 600-650°C; the temperature of the third-stage aging treatment is 450-550°C .
  • the temperature of the first-stage aging treatment is preferably 790-910°C, for example, 900°C.
  • the time for the first-stage aging treatment may be, for example, 2 to 4 hours, such as 3 hours.
  • the temperature of the second aging treatment is preferably 610-640°C, such as 620°C or 630°C.
  • the time of the second-stage aging treatment may be, for example, 1-4 hours, such as 2 hours.
  • the temperature of the third aging treatment is preferably 470-490°C, such as 480°C.
  • the time for the third-stage aging treatment may be, for example, 1 to 4 hours, for example, 3 hours.
  • grain boundary diffusion treatment may also be performed after the third-stage aging treatment.
  • the temperature of the grain boundary diffusion treatment is preferably 850-1000°C, such as 900°C, 910°C or 920°C.
  • the time for the grain boundary diffusion treatment is preferably 10-30 hours, for example, 20 hours.
  • the diffusion source of the grain boundary diffusion treatment is Dy metal powder or an alloy containing Dy.
  • the diffusion source of the grain boundary diffusion treatment is preferably Dy metal powder and/or an alloy containing Dy.
  • the percentage of the mass of the diffusion source to the total mass of the NdFeB magnet material is preferably 0.3-0.5wt.%, for example 0.4wt.%.
  • the smelting process can be conventional in the field.
  • the vacuum degree of the smelting is, for example, 5 ⁇ 10 -2 Pa.
  • the melting temperature is, for example, below 1550°C, such as 1530°C.
  • the casting process can be conventional in the field.
  • the casting process for example, adopts the quick-setting casting method.
  • the casting temperature may be 1390-1460°C, such as 1400°C.
  • the alloy cast sheet obtained after the casting may have a thickness of 0.25-0.40 mm, such as 0.29 mm.
  • the crushing process can be conventional in the field.
  • the crushing is generally carried out in sequence by hydrogen crushing and jet mill crushing.
  • the hydrogen crushing process generally includes hydrogen absorption, dehydrogenation, and cooling in sequence.
  • the hydrogen absorption can be carried out under the condition of hydrogen pressure of 0.085MPa.
  • the dehydrogenation can be carried out under the condition of raising the temperature while evacuating.
  • the dehydrogenation temperature may be 480-520°C, such as 500°C.
  • the gas atmosphere during the pulverization of the jet mill may have an oxidizing gas content below 100 ppm, and the oxidizing gas content refers to the content of oxygen or moisture.
  • 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 pulverization.
  • the forming may adopt a magnetic field forming method.
  • the magnetic field shaping is performed at a magnetic field strength of 1.8-2.5T, for example.
  • the sintering process may be conventional in the field.
  • the sintering temperature may be 1000-1100°C, such as 1080°C.
  • the sintering time may be 4-8 hours, such as 6 hours.
  • the present invention also provides an NdFeB magnet material prepared by the preparation method of the NdFeB magnet material.
  • the invention also provides an application of the NdFeB magnet material as an electronic component.
  • the reagents and raw materials used in the present invention are all commercially available.
  • the positive progress effect of the present invention lies in: the coercive force of the NdFeB magnet material prepared by the present invention is significantly improved through the combination of elements such as Al, Cu, Co, Nb and B in a specific content, and the remanence and squareness maintained at a high level.
  • the NdFeB magnet material is prepared according to the following steps:
  • the alloy cast slab (0.29mm in thickness) was obtained by adopting the quick-setting slab method, and the casting temperature was 1400°C.
  • Pulverization carry out hydrogen crushing pulverization and jet mill pulverization in sequence.
  • Hydrogen crushing is processed by hydrogen absorption, dehydrogenation and cooling. Hydrogen absorption is carried out under the condition of hydrogen pressure of 0.085MPa. The dehydrogenation is carried out under the condition of raising the temperature while evacuating, and the dehydrogenation temperature is 500°C.
  • Jet mill pulverization is carried out at an oxidizing gas content of 100 ppm or less, and the particle size obtained by pulverization is 4.2 ⁇ m.
  • the oxidizing gas refers to the oxygen or water content.
  • the pressure of the grinding chamber of the jet mill is 0.68MPa. After pulverizing, add lubricant zinc stearate, and the addition amount is 0.12% of the powder weight after mixing.
  • Magnetic field forming is carried out under the protection of a magnetic field strength of 1.8-2.5T and a nitrogen atmosphere.
  • Three-level aging the temperature of the first-level aging is 900°C and the time is 3h; the temperature of the second-level aging is 630°C and the time is 2h; the temperature of the third-level aging is 480°C and the time is 3h.
  • Grain boundary diffusion treatment diffuse Dy metal powder into the magnet material obtained after three-stage aging treatment through grain boundary diffusion treatment (the content of added Dy is 0.4wt.%, wt.% refers to the proportion of NdFeB The percentage of the total mass of the magnet material, while the content of the remaining Dy recorded in Table 1 is 1.3wt.% added during smelting), the temperature of the grain boundary diffusion treatment is 910°C, and the time is 20h.
  • Embodiments 1-5 and 10-13, Comparative Examples 1-8 prepare raw materials according to the formula in Table 1 below, the temperature of the secondary aging is shown in Table 1 below, and other preparation processes are the same as in Example 1; wherein, for grain boundary diffusion The content of Dy added is 0.4wt.%, and the remaining Dy in Table 1 is added during smelting.
  • Examples 6-9, 14 and 15 prepared raw materials according to the formula in Table 1 below.
  • the preparation process did not carry out grain boundary diffusion treatment after the third-stage aging treatment, and the temperature of the second-stage aging treatment was shown in Table 1 below.
  • the rest of the preparation Technology is with embodiment 1.
  • NdFeB magnet materials in Examples 1 to 15 and Comparative Examples 1 to 8 are tested using PFM pulse type BH demagnetization curve testing equipment, and the test temperature is 20°C to obtain remanence (Br), intrinsic coercive force (Hcj ), the maximum magnetic energy product (BHmax) and squareness (Hk/Hcj) data, the test results are shown in Table 2 below.
  • Adopt FE-EPMA to detect the vertical orientation surface of the NdFeB magnet material in Examples 1 ⁇ 15 and Comparative Examples 1 ⁇ 8 is polished, adopts Field Emission Electron Probe Microanalyzer (FE-EPMA) (Japan Electronics Co., Ltd. (JEOL), 8530F) detection.
  • FE-EPMA Field Emission Electron Probe Microanalyzer
  • the area of the Nd x Pry Co z phase is the ratio of the area of the Nd x Pry Co z phase to the total area of the grain boundary phase in the section of the detection NdFeB magnet material (the aforementioned vertical orientation plane) .
  • the present invention combines specific content of Co, Al, Cu, Nb, rare earth elements, etc., and adopts specific three-stage aging treatment in the preparation process, so that the correction of NdFeB magnet materials is Compared with the existing technology, the coercive force has been significantly improved, while the remanence and squareness remain at a high level. According to the results of further microscopic inspection, this may be due to the formation of a specific content of Nd x Pry Co z phase in the grain boundary phase after the formulation of the optimized NdFeB magnet material of the present invention is prepared into the NdFeB magnet material , the grain boundary structure is optimized to increase the coercive force.

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Abstract

本发明公开了一种钕铁硼磁体材料及其制备方法和应用。该钕铁硼磁体材料包括以下组分：R：28～33wt.％，所述R为稀土元素；所述R包括Nd和Pr，所述Nd：27～31.5wt.％；Al：0.30～1.3wt.％；Cu：0.35～0.6wt.％；Co≥0.85wt.％；B：0.98～1.2wt.％；Nb≥0.25wt.％；Fe：62～69wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料中所述Nd和所述Pr的含量满足如下公式：Nd/Pr≥58。本发明通过优化配方制得的钕铁硼磁体材料在提高矫顽力的同时，剩磁和方形度均维持在较高水平。

Description

一种钕铁硼磁体材料及其制备方法和应用 技术领域
本发明涉及一种钕铁硼磁体材料及其制备方法和应用。
背景技术
永磁材料作为支撑电子器件的关键材料被开发出来。R-T-B系永磁材料已知为永久磁铁中性能最高的磁铁，被用于硬盘驱动器的音圈电机、电动车用电机、工业设备用电机等。
关于如何进一步提高R-T-B系永磁材料的综合性能是目前本领域内一直在研究的方向。例如中国专利文献CN110993233A公开了一种R-T-B系永磁材料，该永磁材料通过提高X(Al\Cu\Ga)的含量，调整稀土含量，使Fe和B的比例发生变化，从而只需常规含量的B也能够生成6:13:1相，进而得到磁性能优异的磁体材料。
又例如，中国专利文献CN111180159A也公开了一种钕铁硼永磁材料，该专利中的具体实施例公开了以下成分和结构的磁体材料：Nd 29wt.％、Tb 0.1wt.％、Dy 0.4wt.％、Cu 0.4wt.％、Al 0.5wt.％、Co 0.9wt.％、B 1wt.％、Nb 0.25wt.％和Fe 67.45wt.％；在晶间富稀土相还生成了特定质量占比的物相Tb 0.4Dy 2.5-Al 0.59-Nd 89.6-Cu 1.4-Co 5.1。
上述配方均是基于高Cu高Al的磁体材料进行的改进，这主要是由于Cu元素的加入可以有效提高钕铁硼磁体的矫顽力，但是过多的Cu(例如0.35wt.％以上)在晶界的富集会导致磁体烧结后形成微裂纹从而降低磁体的致密性及强度，现有技术中一般会采用添加Al的方式(例如中国专利文献CN110993234A)，来解决上述缺陷。但是这些磁体材料的矫顽力和剩磁与永磁材料的理论值仍有一定的差距。
如何进一步优化磁体材料的配方，得到矫顽力和剩磁综合性能更高的钕铁硼磁体材料是亟需解决的技术问题。
发明内容
本发明主要是为了克服现有技术中存在的含Al和Cu的钕铁硼磁体材料的磁性能较低的缺陷，而提供了一种钕铁硼磁体材料及其制备方法和应用。本发明通过优化配方制得的钕铁硼磁体材料在提高矫顽力的同时，剩磁和方形度维持在较高水平。
本发明主要是通过以下技术方案解决以上技术问题的。
本发明提供了一种钕铁硼磁体材料，其包括以下组分：
R：28～33wt.％，所述R为稀土元素；
所述R包括Nd和Pr，所述Nd：27～31.5wt.％；
Al：0.30～1.3wt.％；
Cu：0.35～0.6wt.％；
Co≥0.85wt.％；
B：0.98～1.2wt.％；
Nb≥0.25wt.％；
Fe：62～69wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；
所述钕铁硼磁体材料中所述Nd和所述Pr的含量满足如下公式：Nd/Pr≥58。
本发明中，所述R的含量较佳地为29～32.5wt.％，例如29.3wt.％、29.6wt.％、29.7wt.％、30.6wt.％、30.7wt.％、31.3wt.％、31.5wt.％、31.9wt.％、32wt.％、32.1wt.％或32.3wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述Nd的含量较佳地为27～31wt.％，例如27.5wt.％、28.3wt.％、28.9wt.％、29.1wt.％、29.3wt.％、29.5wt.％、29.7wt.％、29.8wt.％、30.2wt.％、30.5wt.％或30.7wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述钕铁硼磁体材料还可包括RH，所述RH为重稀土元素。
其中，所述RH的含量可为本领域常规，较佳地为0.5～2.5wt.％，例如 0.6wt.％、0.9wt.％、1wt.％、1.2wt.％、1.4wt.％、1.5wt.％、1.7wt.％、2wt.％或2.3wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
其中，所述RH的种类较佳地为Dy和/或Tb。
当所述RH包含Dy时，所述Dy的含量较佳地为0.2～2.5wt.％，例如0.2wt.％、0.9wt.％、1.4wt.％、1.5wt.％、1.7wt.％或2.3wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
当所述RH包含Tb时，所述Tb的含量较佳地为0.5～2.5wt.％，例如0.6wt.％、0.8wt.％、1.2wt.％或2wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述Nd/Pr的值较佳地为60～400，例如98、135、275、283、289、291、295、297、298、302、305或307。本领域技术人员知晓，所述Nd/Pr是指所述Nd的含量与所述Pr的含量的比值。
本发明中，所述Pr的含量较佳地为0.1～0.3wt.％，例如0.2wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述Al的含量较佳地为0.45～1.15wt.％，例如0.46wt.％、0.61wt.％、0.65wt.％或0.7wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述Cu的含量较佳地为0.35～0.45wt.％，例如0.36wt.％、0.37wt.％、0.38wt.％、0.39wt.％、0.4wt.％或0.42wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述Co的含量较佳地为0.9～2.5wt.％，例如1wt.％、1.1wt.％、1.2wt.％、1.3wt.％、1.4wt.％或1.5wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述Nb的含量较佳地为0.25～0.55wt.％，例如0.26wt.％、0.3wt.％或0.35wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述B的含量较佳地为0.98～1.05wt.％，例如0.99wt.％、1wt.％、1.01wt.％、1.02wt.％或1.04wt.％，wt.％是指占所述钕铁硼磁体材料总质量 的百分比。
本发明中，所述Fe的含量较佳地为63～68wt.％，例如63.71wt.％、63.84wt.％、64.17wt.％、64.75wt.％、64.82wt.％、64.83wt.％、65.25wt.％、65.61wt.％、65.78wt.％、66.23wt.％、66.84wt.％、67.04wt.％、67.24wt.％、67.34wt.％或67.35wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
本发明中，所述钕铁硼磁体材料较佳地包括Nd xPr yCo z相，以所述Nd xPr yCo z物相中Nd、Pr和Co的总摩尔量100％计，x为50～57％，y＝3～7％，z＝39～46％；所述的Nd xPr yCo z相位于晶界相，所述Nd xPr yCo z相的面积与所述晶界相的总面积的比较佳地为3～7％，更佳地为4.5～5.5％，例如4.9％、5％、5.1％、5.2％或5.3％。所述Nd xPr yCo z物相的面积或所述晶界相的总面积分别是指在检测的所述钕铁硼磁体材料的垂直取向面中所占的面积。
其中，所述x例如为51％、52％、53％、54％、55％或56％。
其中，所述y例如为4％、5％或6％。
其中，所述z例如为40％、41％、42％、43％、44％或45％。
其中，x(y或z)是指所述Nd xPr yCo z相中Nd(Pr或Co)的摩尔量与Nd xPr yCo z相中所有元素总摩尔量的百分比。
本发明中，所述的晶界相可为本领域常规理解的含义，一般是指二颗粒晶界相和晶间三角区形成的区域的统称。所述二颗粒晶界相一般为两个主相颗粒之间的晶界相。
发明人发现，通过上述特定元素之间的配合在钕铁硼磁体材料中形成了特定含量的所述Nd xPr yCo z相，该物相的存在降低了晶界相的溶解温度，能够更显著地提高晶界相的流动性、改善晶界相的分布，从而通过增强晶界相的去磁耦合能力极大地提高了钕铁硼材料的矫顽力。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 29.7wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.4wt.％、Co 1wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 65.25wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含 Nd 55Pr 4Co 41相，所述Nd 55Pr 4Co 41相的面积与所述晶界相总面积的比为5.1％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 29.8wt.％、Pr 0.1wt.％、Dy 1.4wt.％、Al 0.46wt.％、Cu 0.38wt.％、Co 1wt.％、Nb 0.25wt.％、B 1wt.％和Fe 65.61wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 56Pr 4Co 40相，所述Nd 56Pr 4Co 40相的面积与所述晶界相总面积的比为5.2％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 30.2wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.38wt.％、Co 0.9wt.％、Nb 0.3wt.％、B 0.99wt.％和Fe 64.82wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 55Pr 5Co 40相，所述Nd 55Pr 5Co 40相的面积与所述晶界相总面积的比为5％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 29.3wt.％、Pr 0.3wt.％、Dy 2.3wt.％、Al 0.61wt.％、Cu 0.39wt.％、Co 1wt.％、Nb 0.26wt.％、B 1.01wt.％和Fe 64.83wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 53Pr 6Co 41相，所述Nd 53Pr 6Co 41相的面积与所述晶界相总面积的比为5.2％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 30.7wt.％、Pr 0.1wt.％、Dy 1.5wt.％、Al 1.15wt.％、Cu 0.37wt.％、Co 1.1wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 63.84wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 53Pr 4Co 43相，所述Nd 53Pr 4Co 43相的面积与所述晶界相总面积的比为5.1％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 28.9wt.％、Pr 0.1wt.％、Tb 0.6wt.％、Al 0.46wt.％、Cu 0.36wt.％、Co 1wt.％、Nb 0.26wt.％、B 0.98wt.％和Fe 67.34wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 56Pr 4Co 40相，所述Nd 56Pr 4Co 40相的面积与所述晶界相总面积的比为4.9％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd  28.3wt.％、Pr 0.1wt.％、Tb 1.2wt.％、Al 0.45wt.％、Cu 0.35wt.％、Co 1wt.％、Nb 0.26wt.％、B 0.99wt.％和Fe 67.35wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 56Pr 4Co 40相，所述Nd 56Pr 4Co 40相的面积与所述晶界相总面积的比为5.2％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 27wt.％、Pr 0.2wt.％、Tb 2.5wt.％、Al 0.45wt.％、Cu 0.36wt.％、Co 1wt.％、Nb 0.26wt.％、B 0.99wt.％和Fe 67.24wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 54Pr 5Co 41相，所述Nd 54Pr 5Co 41相的面积与所述晶界相总面积的比为5.3％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 27.5wt.％、Pr 0.1wt.％、Tb 2wt.％、Al 0.45wt.％、Cu 0.36wt.％、Co 1.3wt.％、Nb 0.26wt.％、B 0.99wt.％和Fe 67.04wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 55Pr 4Co 41相，所述Nd 55Pr 4Co 41相的面积与所述晶界相总面积的比为4.9％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 28.3wt.％、Pr 0.1wt.％、Dy 0.9wt.％、Al 0.7wt.％、Cu 0.42wt.％、Co 1.5wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 66.84wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 54Pr 4Co 42相，所述Nd 54Pr 4Co 42相的面积与所述晶界相总面积的比为5.2％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 30.5wt.％、Pr 0.1wt.％、Dy 1.5wt.％、、Al 0.65wt.％、Cu 0.45wt.％、Co 1.4wt.％、Nb 0.25wt.％、B 0.98wt.％和Fe 64.17wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 55Pr 4Co 41相，所述Nd 55Pr 4Co 41相的面积与所述晶界相总面积的比为5.1％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 29.7wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.4wt.％、Co 2.5wt.％、Nb 0.26wt.％、B 1.02wt.％和Fe 63.71wt.％，wt.％为各组分的质量与所述钕铁 硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 54Pr 5Co 41相，所述Nd 54Pr 5Co 41相的面积与所述晶界相总面积的比为5.1％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 29.7wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.4wt.％、Co 1.5wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 64.75wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 51Pr 4Co 45相，所述Nd 51Pr 4Co 45相的面积与所述晶界相总面积的比为5.2％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 29.1wt.％、Pr 0.1wt.％、Tb 1.5wt.％、Al 0.46wt.％、Cu 0.37wt.％、Co 0.9wt.％、Nb 0.35wt.％、B 0.99wt.％和Fe 66.23wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 52Pr 5Co 43相，所述Nd 52Pr 5Co 43相的面积与所述晶界相总面积的比为5.2％。
本发明一较佳实施例中，所述钕铁硼磁体材料由以下组分组成：Nd 29.5wt.％、Pr 0.1wt.％、Dy 0.2wt.％、Tb 0.8wt.％、Al 0.46wt.％、Cu 0.37wt.％、Co 1.2wt.％、Nb 0.55wt.％、B 1.04wt.％和Fe 65.78wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 52Pr 4Co 44相，所述Nd 52Pr 4Co 44相的面积与所述晶界相总面积的比为5.3％。
本发明还提供了一种钕铁硼磁体材料的制备方法，其包括以下步骤：按照所述钕铁硼磁体材料的组分配制各组分的原料，再将各组分的原料的混合物依次经熔炼、铸造、粉碎、成型、烧结和时效处理后即得；
所述时效处理包括三级时效处理，其中，第一级时效处理的温度为850～950℃；第二级时效处理的温度为600～650℃；第三级时效处理的温度为450～550℃。
本发明中，所述第一级时效处理的温度较佳地为790～910℃，例如900℃。
本发明中，所述第一级时效处理的时间例如可为2～4h，例如3h。
本发明中，所述第二级时效处理的温度较佳地为610～640℃，例如620℃ 或630℃。
本发明中，所述第二级时效处理的时间例如可为1～4h，例如2h。
本发明中，所述第三级时效处理的温度较佳地为470～490℃，例如480℃。
本发明中，所述第三级时效处理的时间例如可为1～4h，例如3h。
本发明中，所述第三级时效处理之后还可进行晶界扩散处理。
其中，所述晶界扩散处理的温度较佳地为850～1000℃，例如900℃、910℃或920℃。
其中，所述晶界扩散处理的时间较佳地为10～30h，例如20h。
其中，所述晶界扩散处理的扩散源为Dy金属粉末或含有Dy的合金。
其中，所述晶界扩散处理的扩散源较佳地为Dy金属粉末和/或含有Dy的合金。
所述扩散源的质量与所述钕铁硼磁体材料总质量的百分比较佳地为0.3～0.5wt.％，例如0.4wt.％。
本发明中，所述熔炼的工艺可为本领域常规。
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，例如1530℃。
本发明中，所述铸造的工艺可为本领域常规。
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1400℃。
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。
本发明中，所述粉碎的工艺可为本领域常规。
其中，所述粉碎一般依次进行氢破粉碎和气流磨粉碎。
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℃。
所述气流磨粉碎时的气体氛围可为氧化气体含量在100ppm以下，所述氧化气体含量是指氧气或水分的含量。
所述气流磨粉碎后，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％。
本发明中，所述成型可采用磁场成型法。
其中，所述磁场成型例如在1.8～2.5T的磁场强度下进行。
本发明中，所述烧结的工艺可为本领域常规。
其中，所述烧结的温度可为1000～1100℃，例如1080℃。
其中，所述烧结的时间可为4～8h，例如6h。
本发明还提供了一种所述钕铁硼磁体材料的制备方法制得的钕铁硼磁体材料。
本发明还提供了一种所述钕铁硼磁体材料作为电子元器件的应用。
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Al、Cu、Co、Nb和B等元素的配合，制备得到的钕铁硼磁体材料的矫顽力有显著的提升，且剩磁和方形度均维持在较高水平。
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
钕铁硼磁体材料按照下述制备步骤：
(1)熔炼：将按照表1配制好的钕铁硼磁体材料的原料放入真空度为5×10 -2Pa的高频真空感应熔炼炉中，在1530℃温度下熔炼成熔融液。
(2)铸造：采用速凝铸片法，获得合金铸片(厚度为0.29mm)，浇铸的温度为1400℃。
(3)粉碎：依次进行氢破粉碎和气流磨粉碎。
氢破粉碎为经吸氢、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℃。
气流磨粉碎为在氧化气体含量100ppm以下进行，粉碎得到的粒径为4.2μm，氧化气体是指氧气或水分含量。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％。
(4)磁场成型，在1.8～2.5T的磁场强度和氮气气氛保护下进行。
(5)烧结：在5×10 -3Pa真空条件下，经烧结、冷却。在1080℃下烧结6h；冷却前可通入Ar气体使气压达到0.05MPa。
(6)三级时效：第一级时效的温度为900℃、时间为3h；第二级时效的温度为630℃、时间为2h；第三级时效的温度为480℃、时间为3h。
(7)晶界扩散处理：通过晶界扩散处理向经三级时效处理后得到的磁体材料中扩散Dy金属粉末(添加的Dy的含量为0.4wt.％，wt.％是指占钕铁硼磁体材料总质量的百分比，而表1中记载的剩余Dy的含量1.3wt.％在熔炼时添加)，晶界扩散处理的温度为910℃、时间为20h。
实施例1～5和10～13、对比例1～8按照如下表1的配方配制原料，二级时效的温度如下表1所示，其他制备工艺同实施例1；其中，对于晶界扩散时添加的Dy的含量均为0.4wt.％，表1中剩余的Dy是在熔炼时添加。
实施例6～9、14和15按照如下表1的配方配制原料，制备工艺在第三级时效处理之后并未进行晶界扩散处理，第二级时效处理的温度如下表1所示，其余制备工艺同实施例1。
效果实施例1
1、成分测定：对实施例1～15和对比例1～8中的钕铁硼磁体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(单位为wt.％，各元素占钕铁硼磁体材料总质量的百分比)
Figure PCTCN2022072256-appb-000001
注：“/”表示未添加且未检测到该元素。上述实施例和对比例中的钕铁硼磁体材料中Fe的含量的数值为100％减去各元素的含量，本领域技术人员知晓，Fe的含量中包含在制备过程中引入的不可避免的一些杂质。
2、磁性能的测试
实施例1～15和对比例1～8中的钕铁硼磁体材料使用PFM脉冲式BH退磁曲线测试设备进行测试，测试温度为20℃，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。
3、微观结构的表征
采用FE-EPMA检测：对实施例1～15和对比例1～8中的钕铁硼磁体材料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面扫描确定钕铁硼磁体材料的晶界相中Nd、Pr、Co元素的分布，然后通过FE-EPMA单点定量分析确定Nd xPr yCo z相中各元素的摩尔含量占比，测试条件为加速电压15kv，探针束流50nA。测试结果如下表2所示。
其中，Nd xPr yCo z相的面积为在检测钕铁硼磁体材料的截面(前述的垂直取向面)中Nd xPr yCo z相的面积与该截面中晶界相的总面积的比。
表2
Figure PCTCN2022072256-appb-000002
Figure PCTCN2022072256-appb-000003
注：表中Nd xPr yCo z相下标中的数值省略了％。
由上表中的数据可知，本发明通过特定含量的Co、Al、Cu、Nb、稀土元素等的配合，结合制备工艺中采用特定的三级时效处理，制得的钕铁硼磁体材料的矫顽力相较于现有技术有显著的提升，同时剩磁和方形度保持在较高水平。根据进一步地微观检测结果可知，这可能是由于本发明优化后的钕铁硼磁体材料的配方在制备成钕铁硼磁体材料后在晶界相中形成了特定含量的Nd xPr yCo z相，优化了晶界结构进而提升了矫顽力。

Claims (10)

  1. 一种钕铁硼磁体材料，其特征在于，其包括以下组分：
    R：28～33wt.％，所述R为稀土元素；
    所述R包括Nd和Pr，所述Nd：27～31.5wt.％；
    Al：0.30～1.3wt.％；
    Cu：0.35～0.6wt.％；
    Co≥0.85wt.％；
    B：0.98～1.2wt.％；
    Nb≥0.25wt.％；
    Fe：62～69wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；
    所述钕铁硼磁体材料中所述Nd和所述Pr的含量满足如下公式：Nd/Pr≥58。
  2. 如权利要求1所述的钕铁硼磁体材料，其特征在于，所述R的含量为29～32.5wt.％，例如29.3wt.％、29.6wt.％、29.7wt.％、30.6wt.％、30.7wt.％、31.3wt.％、31.5wt.％、31.9wt.％、32wt.％、32.1wt.％或32.3wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述Nd的含量为27～31wt.％，例如27.5wt.％、28.3wt.％、28.9wt.％、29.1wt.％、29.3wt.％、29.5wt.％、29.7wt.％、29.8wt.％、30.2wt.％、30.5wt.％或30.7wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述钕铁硼磁体材料还包括RH，所述RH为重稀土元素；
    其中，所述RH的含量较佳地为0.5～2.5wt.％，例如0.6wt.％、0.9wt.％、1wt.％、1.2wt.％、1.4wt.％、1.5wt.％、1.7wt.％、2wt.％或2.3wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    其中，所述RH的种类较佳地为Dy和/或Tb；
    当所述RH包含Dy时，所述Dy的含量较佳地为0.2～2.5wt.％，例如0.2wt.％、0.9wt.％、1.4wt.％、1.5wt.％、1.7wt.％或2.3wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    当所述RH包含Tb时，所述Tb的含量较佳地为0.5～2.5wt.％，例如0.6wt.％、0.8wt.％、1.2wt.％或2wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述Nd/Pr的值为60～400，例如98、135、275、283、289、291、295、297、298、302、305或307；
    和/或，所述Pr的含量为0.1～0.3wt.％，例如0.2wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
  3. 如权利要求1所述的钕铁硼磁体材料，其特征在于，所述Al的含量为0.45～1.15wt.％，例如0.46wt.％、0.61wt.％、0.65wt.％或0.7wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述Cu的含量为0.35～0.45wt.％，例如0.36wt.％、0.37wt.％、0.38wt.％、0.39wt.％、0.4wt.％或0.42wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述Co的含量为0.9～2.5wt.％，例如1wt.％、1.1wt.％、1.2wt.％、1.3wt.％、1.4wt.％或1.5wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述Nb的含量为0.25～0.55wt.％，例如0.26wt.％、0.3wt.％或0.35wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述B的含量为0.98～1.05wt.％，例如0.99wt.％、1wt.％、1.01wt.％、1.02wt.％或1.04wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比；
    和/或，所述Fe的含量为63～68wt.％，例如63.71wt.％、63.84wt.％、64.17wt.％、64.75wt.％、64.82wt.％、64.83wt.％、65.25wt.％、65.61wt.％、65.78wt.％、66.23wt.％、66.84wt.％、67.04wt.％、67.24wt.％、67.34wt.％或67.35wt.％，wt.％是指占所述钕铁硼磁体材料总质量的百分比。
  4. 如权利要求1～3中任一项所述的钕铁硼磁体材料，其特征在于，所述钕铁硼磁体材料包括Nd xPr yCo z相，以所述Nd xPr yCo z物相中Nd、Pr和Co的总摩尔量100％计，其中x为50～57％，y＝3～7％，z＝39～46％；
    所述x例如为51％、52％、53％、54％、55％或56％；
    所述y例如为4％、5％或6％；
    所述z例如为40％、41％、42％、43％、44％或45％；
    所述的Nd xPr yCo z相位于晶界相；
    所述Nd xPr yCo z相的面积与所述晶界相的总面积的比较佳地为3～7％，更佳地为4.5～5.5％，例如4.9％、5％、5.1％、5.2％或5.3％，所述Nd xPr yCo z物相的面积或所述晶界相的总面积分别是指在检测的所述钕铁硼磁体材料的垂直取向面中所占的面积。
  5. 如权利要求1所述的钕铁硼磁体材料，其特征在于，所述钕铁硼磁体材料由以下组分组成：Nd 29.7wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.4wt.％、Co 1wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 65.25wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 55Pr 4Co 41相，所述Nd 55Pr 4Co 41相的面积与所述晶界相总面积的比为5.1％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 29.8wt.％、Pr 0.1wt.％、Dy 1.4wt.％、Al 0.46wt.％、Cu 0.38wt.％、Co 1wt.％、Nb 0.25wt.％、B 1wt.％和Fe 65.61wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 56Pr 4Co 40相，所述Nd 56Pr 4Co 40相的面积与所述晶界相总面积的比为5.2％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 30.2wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.38wt.％、Co 0.9wt.％、Nb 0.3wt.％、B 0.99wt.％和Fe 64.82wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 55Pr 5Co 40相，所述Nd 55Pr 5Co 40相的面积与所述晶界相总面积的比为5％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 29.3wt.％、Pr 0.3wt.％、Dy 2.3wt.％、Al 0.61wt.％、Cu 0.39wt.％、Co 1wt.％、Nb 0.26wt.％、B 1.01wt.％和Fe 64.83wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分 比；所述钕铁硼磁体材料的晶界相中包含Nd 53Pr 6Co 41相，所述Nd 53Pr 6Co 41相的面积与所述晶界相总面积的比为5.2％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 30.7wt.％、Pr 0.1wt.％、Dy 1.5wt.％、Al 1.15wt.％、Cu 0.37wt.％、Co 1.1wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 63.84wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 53Pr 4Co 43相，所述Nd 53Pr 4Co 43相的面积与所述晶界相总面积的比为5.1％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 28.9wt.％、Pr 0.1wt.％、Dy wt.％、Tb 0.6wt.％、Al 0.46wt.％、Cu 0.36wt.％、Co 1wt.％、Nb 0.26wt.％、B 0.98wt.％和Fe 67.34wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 56Pr 4Co 40相，所述Nd 56Pr 4Co 40相的面积与所述晶界相总面积的比为4.9％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 28.3wt.％、Pr 0.1wt.％、Tb 1.2wt.％、Al 0.45wt.％、Cu 0.35wt.％、Co 1wt.％、Nb 0.26wt.％、B 0.99wt.％和Fe 67.35wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 56Pr 4Co 40相，所述Nd 56Pr 4Co 40相的面积与所述晶界相总面积的比为5.2％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 27wt.％、Pr 0.2wt.％、Tb 2.5wt.％、Al 0.45wt.％、Cu 0.36wt.％、Co 1wt.％、Nb 0.26wt.％、B 0.99wt.％和Fe 67.24wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 54Pr 5Co 41相，所述Nd 54Pr 5Co 41相的面积与所述晶界相总面积的比为5.3％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 27.5wt.％、Pr 0.1wt.％、Tb 2wt.％、Al 0.45wt.％、Cu 0.36wt.％、Co 1.3wt.％、Nb 0.26wt.％、B 0.99wt.％和Fe 67.04wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 55Pr 4Co 41相，所述Nd 55Pr 4Co 41相的面积与所述晶界相总面积的比为4.9％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 28.3wt.％、Pr 0.1wt.％、Dy 0.9wt.％、Al 0.7wt.％、Cu 0.42wt.％、Co 1.5wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 66.84wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 54Pr 4Co 42相，所述Nd 54Pr 4Co 42相的面积与所述晶界相总面积的比为5.2％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 30.5wt.％、Pr 0.1wt.％、Dy 1.5wt.％、Al 0.65wt.％、Cu 0.45wt.％、Co 1.4wt.％、Nb 0.25wt.％、B 0.98wt.％和Fe 64.17wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 55Pr 4Co 41相，所述Nd 55Pr 4Co 41相的面积与所述晶界相总面积的比为5.1％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 29.7wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.4wt.％、Co 2.5wt.％、Nb 0.26wt.％、B 1.02wt.％和Fe 63.71wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 54Pr 5Co 41相，所述Nd 54Pr 5Co 41相的面积与所述晶界相总面积的比为5.1％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 29.7wt.％、Pr 0.1wt.％、Dy 1.7wt.％、Al 0.61wt.％、Cu 0.4wt.％、Co 1.5wt.％、Nb 0.25wt.％、B 0.99wt.％和Fe 64.75wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 51Pr 4Co 45相，所述Nd 51Pr 4Co 45相的面积与所述晶界相总面积的比为5.2％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 29.1wt.％、Pr 0.1wt.％、Tb 1.5wt.％、Al 0.46wt.％、Cu 0.37wt.％、Co 0.9wt.％、Nb 0.35wt.％、B 0.99wt.％和Fe 66.23wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 52Pr 5Co 43相，所述Nd 52Pr 5Co 43相的面积与所述晶界相总面积的比为5.2％；
    或者，所述钕铁硼磁体材料由以下组分组成：Nd 29.5wt.％、Pr 0.1wt.％、Dy 0.2wt.％、Tb 0.8wt.％、Al 0.46wt.％、Cu 0.37wt.％、Co 1.2wt.％、Nb 0.55wt.％、 B 1.04wt.％和Fe 65.78wt.％，wt.％为各组分的质量与所述钕铁硼磁体材料总质量的百分比；所述钕铁硼磁体材料的晶界相中包含Nd 52Pr 4Co 44相，所述Nd 52Pr 4Co 44相的面积与所述晶界相总面积的比为5.3％。
  6. 一种钕铁硼磁体材料的制备方法，其特征在于，其包括以下步骤：按照如权利要求1～3和5中任一项所述的钕铁硼磁体材料的组分配制各组分的原料，再将各组分的原料的混合物依次经熔炼、铸造、粉碎、成型、烧结和时效处理后即得；
    所述时效处理包括三级时效处理，其中，第一级时效处理的温度为850～950℃；第二级时效处理的温度为600～650℃；第三级时效处理的温度为450～550℃。
  7. 如权利要求6所述的钕铁硼磁体材料的制备方法，其特征在于，所述第一级时效处理的温度为790～910℃，例如900℃；
    和/或，所述第一级时效处理的时间为2～4h，例如3h；
    和/或，所述第二级时效处理的温度为610～640℃，例如620℃或630℃；
    和/或，所述第二级时效处理的时间为1～4h，例如2h；
    和/或，所述第三级时效处理的温度为470～490℃，例如480℃；
    和/或，所述第三级时效处理的时间为1～4h，例如3h；
    和/或，所述第三级时效处理之后还进行晶界扩散处理；
    其中，所述晶界扩散处理的温度较佳地为850～1000℃，例如900℃、910℃或920℃；
    其中，所述晶界扩散处理的时间较佳地为10～30h，例如20h；
    其中，所述晶界扩散处理的扩散源为较佳地为Dy金属粉末和/或含有Dy的合金；所述扩散源的质量与所述钕铁硼磁体材料总质量的百分比较佳地为0.3～0.5wt.％，例如0.4wt.％。
  8. 如权利要求6或7所述的钕铁硼磁体材料的制备方法，其特征在于，所述熔炼的真空度为5×10 -2Pa；
    和/或，所述熔炼的温度在1550℃以下，例如1530℃；
    和/或，所述铸造采用速凝铸片法；
    和/或，所述铸造的温度为1390～1460℃，例如1400℃；
    和/或，所述铸造之后得到的合金铸片的厚度为0.25～0.40mm，例如0.29mm；
    和/或，所述粉碎为依次进行氢破粉碎和气流磨粉碎；
    其中，所述氢破碎粉的工艺较佳地为依次经吸氢、脱氢和冷却处理；所述吸氢的氢气压力例如为0.085MPa；所述脱氢的温度例如为480～520℃，例如500℃；
    其中，所述气流磨粉碎时的气体氛围较佳地为氧化气体的含量在100ppm以下，所述气体含量是指氧气和/或水分的含量；
    其中，所述气流磨粉碎后，较佳地还添加润滑剂，所述润滑剂例如为硬脂酸锌；所述润滑剂的添加量较佳地为所述气流磨粉碎后得到的粉体质量的0.05～0.15％，例如0.12％；
    和/或，所述成型为磁场成型，所述磁场成型中磁场强度例如为1.8～2.5T；
    和/或，所述烧结的温度为1000～1100℃，例如1080℃；
    和/或，所述烧结的时间为4～8h，例如6h。
  9. 一种如权利要求6～8中任一项所述的钕铁硼磁体材料的制备方法制得的钕铁硼磁体材料。
  10. 一种如权利要求1～5和9中任一项所述的钕铁硼磁体材料作为电子元器件的应用。
PCT/CN2022/072256 2021-07-29 2022-01-17 一种钕铁硼磁体材料及其制备方法和应用 Ceased WO2023005166A1 (zh)

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