WO2021169899A1 - 一种稀土永磁材料及其制备方法和应用 - Google Patents
一种稀土永磁材料及其制备方法和应用 Download PDFInfo
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- WO2021169899A1 WO2021169899A1 PCT/CN2021/077185 CN2021077185W WO2021169899A1 WO 2021169899 A1 WO2021169899 A1 WO 2021169899A1 CN 2021077185 W CN2021077185 W CN 2021077185W WO 2021169899 A1 WO2021169899 A1 WO 2021169899A1
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- rare earth
- percentage
- mass
- content
- earth permanent
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 272
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 238
- 239000000463 material Substances 0.000 title claims abstract description 167
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 117
- 239000002994 raw material Substances 0.000 claims abstract description 114
- 230000005291 magnetic effect Effects 0.000 claims abstract description 33
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 15
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 15
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 7
- 239000000696 magnetic material Substances 0.000 claims description 59
- 238000000034 method Methods 0.000 claims description 29
- 230000032683 aging Effects 0.000 claims description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 238000005266 casting Methods 0.000 claims description 12
- 238000010902 jet-milling Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 4
- 229910052689 Holmium Inorganic materials 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052771 Terbium Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000007731 hot pressing Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 1
- 238000009740 moulding (composite fabrication) Methods 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 46
- 230000000052 comparative effect Effects 0.000 description 16
- 239000010949 copper Substances 0.000 description 15
- 229910052742 iron Inorganic materials 0.000 description 13
- 238000000465 moulding Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 229910001172 neodymium magnet Inorganic materials 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000005347 demagnetization Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 101100065878 Caenorhabditis elegans sec-10 gene Proteins 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007780 powder milling Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—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
- 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
Definitions
- the invention specifically relates to a rare earth permanent magnet material and its preparation method and application.
- Rare earth permanent magnet materials are widely used in electronic products, automobiles, wind power, home appliances, elevators and industrial robots due to their excellent magnetic properties, such as hard disks, mobile phones, earphones, and permanent magnet motors such as elevator traction machines and generators.
- As an energy source its demand is increasing, and the requirements of various manufacturers for magnet properties such as remanence, coercivity performance, temperature stability, magnet squareness, etc. are gradually increasing.
- the rare earth permanent magnetic material is mainly composed of a main phase containing an R 2 T 14 B compound and a grain boundary phase located in the grain boundary portion of the main phase.
- the R 2 T 14 B compound has a ferromagnetic material with high saturation magnetization and anisotropic magnetic field.
- the coercive force of rare earth permanent magnetic materials will decrease at high temperatures, resulting in irreversible thermal demagnetization. It is currently known that: replacing part of the light rare earth RL in R in the R 2 T 14 B compound as the main phase with heavy rare earth element RH, the coercive force will increase, and the coercive force will increase with the increase in the amount of substitution. improve. On the other hand, the residual magnetic flux Br will decrease. In addition, RH resources are scarce and expensive.
- a high squareness is a necessary condition for high-quality magnets.
- the invention aims to overcome the need to add a large amount of heavy rare earth elements when the prior art rare earth permanent magnet materials adopt low-B system to improve the magnetic performance, and even if the heavy rare earth elements are added, the magnetic performance (remanence, coercivity, temperature stability)
- it provides a rare earth permanent magnet material and its preparation method and application.
- the rare earth permanent magnetic material of the present invention can still be prepared with a low boron and aluminum-free system without adding heavy rare earth elements to obtain better magnetic properties (remanence, coercivity, temperature stability, squareness), and the same batch
- the magnetic properties of the second permanent magnet materials are uniform.
- rare earth permanent magnet materials usually require the addition of a certain amount of Al to obtain better performance magnet materials.
- the inventors have verified through multiple tests that the addition of Al will increase the magnetic properties of the magnet material. Yes, but in the preparation of the same batch of products, the magnetic properties are not uniform, that is, the difference between the maximum value and the minimum value of the coercive force in the same batch of products is greater than 1.5kOe.
- the final rare earth permanent magnet material obtained has better uniformity.
- the present invention adopts the following technical solutions to solve the above technical problems.
- the present invention provides a raw material composition of a rare earth permanent magnet material, which includes the following components in mass content:
- R 28.5-33%; the R is a rare earth element, and the R includes at least Nd;
- Ga 0.6 ⁇ Ga ⁇ 1.8%
- N contains one or more of Ti, Zr and Nb;
- N contains Zr
- the content of Zr is 0.2-0.35%
- Nb When N contains Nb, the content of Nb is 0.2-0.5%;
- the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material.
- the components and corresponding contents in the raw material composition are all actively added, and do not include the components and/or contents introduced in the preparation process and/or impurities.
- the content of R in the raw material composition is preferably 29.3 to 32%, such as 29.3%, 29.5%, 30%, 30.5%, 31%, 31.3% or 32%, more preferably It is 29.4 to 31.5%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the Nd content is preferably 8-13%, such as 8.5%, 9.5%, 12.3%, 12.5%; or the Nd content is preferably 28-31%, such as 28.5% , 29%, 29.3%, 30.2% or 31%, the percentage is the mass percentage of the total mass of the raw material composition.
- the raw material composition preferably does not contain Cu.
- the raw material composition preferably does not contain Al; it means that Al is not actively added, but it may be added during the addition of other elements (for example, Fe) or during the preparation process (for example, alumina crucible to prepare molten liquid) A small amount of Al (less than 0.08%) will be introduced.
- the R in the raw material composition, the R may also include Pr.
- the content of Pr is preferably less than 1.5% and not 0, more preferably 0.1 to 0.5%, such as 0.2% or 0.3%; or the content of Pr is preferably 17 to 25%, More preferably, it is 18.5% to 21.5%, such as 18.5% or 21.5%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the raw material composition may not contain heavy rare earth elements, and may also reach a level equivalent or even better than the magnetic properties of the prior art magnet materials.
- the raw material composition may further include RH, which is a heavy rare earth element.
- the content of the RH is preferably 1 to 2.5%, and the percentage is a mass percentage of the total mass of the raw material composition.
- the type of RH preferably includes one or more of Dy, Tb and Ho.
- the content of Dy is preferably 1 to 2.5%, for example 2%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the content of Tb is preferably 1 to 2.5%, for example 2%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the content of B is preferably 0.86-0.94%, such as 0.86%, 0.88%, 0.9%, 0.92% or 0.94%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the atomic percentage of R and the atomic percentage of B in the raw material composition preferably satisfy the following relationship: B/R ⁇ 0.38, where the B is in the raw material composition The atomic percentage of R in the raw material composition.
- the B and Nd satisfy the following relational formula: B/(Pr+Nd) ⁇ 0.405, where B refers to the B In the atomic percentage in the raw material composition, Pr refers to the atomic percentage of the Pr in the raw material composition, and Nd refers to the atomic percentage of the Nd in the raw material composition.
- the content of Ga is preferably 0.65% to 1.8%, for example 0.65%, 0.85%, 1%, 1.05%, 1.2%, 1.25%, 1.45%, 1.55% or 1.8%, more preferably It is 0.65 to 1.25%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the content of Co is preferably 0.5 to 2.5%, such as 0.5%, 1.05%, 1.5%, 1.55%, 2%, 2.45% or 2.5%, more preferably 1.05 to 2%, in percentage It is the mass percentage of the total mass of the raw material composition.
- the content of Fe is preferably 61.8-68.36%, such as 61.88%, 63.31%, 63.93%, 64.01%, 64.41%, 64.98%, 65.56%, 65.58%, 66.34%, 66.95%, 67.06 %, 67.16%, 67.69% or 68.36%, more preferably 63.3-68%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the content of Ti is preferably 0.2-0.25%, such as 0.2%, 0.22% or 0.25%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the content of Zr is preferably 0.25-0.35%, such as 0.26%, 0.3% or 0.35%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the content of the Zr preferably satisfies: 0.20% ⁇ Zr ⁇ (3.48B-2.67)%, where B means that the B accounts for the raw material composition The mass percentage of the total mass.
- the content of Nb is preferably 0.2-0.25%, and the percentage is the mass percentage of the total mass of the raw material composition.
- the N contains Ti and Nb, preferably the Ti/Nb ⁇ 1.5, where the Ti is the mass percentage in the raw material composition, and the Nb is the The mass percentage in the raw material composition.
- the raw material composition of the rare earth permanent magnet material preferably includes the following components by mass content: R: 29.3 to 32%; the R is a rare earth element, and the R includes at least Nd; B: 0.86 ⁇ 0.94%; Ga: 0.65 ⁇ 1.8%; Co: 0.5 ⁇ 2.5%; Fe: 61.8 ⁇ 68.36%; N: contains one or more of Ti, Zr and Nb; when N contains Ti, the The content of Ti is 0.2 to 0.25%; when N contains Zr, the content of Zr is 0.25 to 0.35%; when N contains Nb, the content of Nb is 0.2 to 0.35%; Contains Cu and Al; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material preferably includes the following components by mass content: R: 29.4 to 31.5%; the R is a rare earth element, and the R includes Nd and Pr; Pr: 0.1 to 0.5% or 17 to 25%; B: 0.86 to 0.94%; Ga: 0.65 to 1.8%; Co: 0.5 to 2.5%; Fe: 63.3 to 68% N: containing one of Ti, Zr and Nb or When N contains Ti, the content of Ti is 0.2-0.25%; when N contains Zr, the content of Zr is 0.25-0.35%; when N contains Nb, the content of Nb The content is 0.2-0.35%; the raw material composition does not contain Cu and Al; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material preferably includes the following components by mass content: R: 29.4 to 31.5%; the R is a rare earth element, and the R includes at least Nd; B: 0.86 ⁇ 0.94%; Ga: 0.65 ⁇ 1.8%; Co: 0.5 ⁇ 2.5%; Fe: 63.3 ⁇ 68.5%; Ti: 0.2 ⁇ 0.25%; the raw material composition does not contain Cu and Al; the percentage is the mass of each component It accounts for the mass percentage of the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material preferably includes the following components by mass content: R: 29.3 to 32%; the R is a rare earth element, and the R includes at least Nd; B: 0.86 ⁇ 0.94%; Ga: 0.65 ⁇ 1.8%; Co: 0.5 ⁇ 2.5%; Fe: 62 ⁇ 67.5%; Zr: 0.25 ⁇ 0.35%; the raw material composition does not contain Cu and Al; the percentage is the mass of each component It accounts for the mass percentage of the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 29.3%; Pr 0.2%; Ga 0.65%; Co 0.5%; Ti 0.15%; B 0.84% Fe 68.36%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 30.2%; Pr 0.3%; Ga 0.85%; Co 1.05%; Ti 0.2%; Nb 0.2% B 0.86%; Fe 68.34%; The percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 31%; Pr 0.3%; Ga 1.05%; Co 1.55%; Ti 0.22%; B 0.9% ; Fe 64.98%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 12.5%; Pr 18.5%; Ga 1.45%; Co 2%; Ti 0.22%; B 0.92% Fe 64.41%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 9.5%; Pr 21.5%; Ga 1.8%; Co 2.45%; Ti 0.25%; Nb 0.25% B 0.94%; Fe 63.31%; The percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 30.2%; Pr 0.3%; Ga 1.05%; Co 1.5%; Zr 0.26%; Nb 0.25% B 0.88; Fe 65.56%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 8.5%; Pr 21.5%; Ga 1.2%; Co 0.5%; Zr 0.3%; B 0.94% Fe 67.06%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material of the rare earth permanent magnet material includes the following components by mass content: Nd 8.5%; Pr 21.5%; Ga 1.2%; Co 0.5%; Zr 0.2%; B 0.94 %; Fe 67.16%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 29.3%; Pr 0.2%; Ga 1.25%; Co 0.5%; Zr 0.2%; B 0.86% Fe 67.69%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 12.5%; Pr 18.5%; Ga 1.55%; Co 0.5%; Zr 0.26%; Nb 0.25% B 0.86%; Fe 65.58%; The percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 9.5%; Pr 21.5%; Ga 1.8%; Co 2%; Zr 0.35%; B 0.92% ; Fe 63.93%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 29%; Pr 0.3%; Ga 0.65%; Co 2%; Zr 0.2%; B 0.9% Fe 66.95%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 12.3%; Pr 17%; Ga 0.65%; Co 2%; Zr 0.2%; B 0.9% Fe 66.95%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 28.5%; Pr 1.5%; Tb 2%; Ga 0.85%; Co 2%; Zr 0.26% B 0.88%; Fe 64.01%; The percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the raw material composition of the rare earth permanent magnet material includes the following components: Nd 12.5%; Pr 18.5%; Dy 2%; Ga 1%; Co 2.5%; Ti 0.15% Zr 0.35%; Nb 0.2%; B 0.92%; Fe 61.88%; the percentage is the mass percentage of the mass of each component to the total mass of the raw material composition.
- the present invention also provides a method for preparing rare earth permanent magnet material, which includes the following steps:
- the raw material composition of the rare earth permanent magnet material can be cast, powdered, shaped, sintered and aging treated.
- the operation and conditions of the smelting can be conventional in the art.
- the vacuum degree of the smelting may be 0.05 Pa.
- the melting temperature may be 1500°C or less.
- the melting equipment may be a high-frequency vacuum induction melting furnace.
- the casting operations and conditions may be conventional casting operations and conditions in the field.
- the casting is typically 10 2 °C / sec ⁇ 10 4 °C / sec cooling rate of the alloy to prepare a sheet.
- the atmosphere of the casting may generally be argon.
- the casting pressure may generally be 5.5 ⁇ 10 4 Pa.
- the cooling can be achieved by passing cooling water into the rollers.
- the water inlet temperature of the roller is ⁇ 25°C, for example 23.4°C, 22.5°C, 22.8°C, 23.1°C, 23.4°C, 23.6°C or 23.8°C, more preferably 23-23.8°C.
- the roller may be a copper roller.
- the operations and conditions of the powder milling can be conventional operations and conditions in the art.
- the pulverization usually includes a hydrogen cracking process and a jet milling process.
- the hydrogen breaking process may be a conventional hydrogen breaking process in the field, such as hydrogen absorption, dehydrogenation, and cooling treatment.
- the hydrogen absorption can be performed under the condition of a hydrogen pressure of 0.15 MPa.
- the dehydrogenation can be carried out under the conditions of raising the temperature while drawing a vacuum.
- the jet milling process can be a conventional jet milling process in the art, and the jet milling process can be performed in a nitrogen atmosphere with an oxidizing gas content of 120 ppm or less.
- the oxidizing gas refers to oxygen or moisture content.
- the pressure of the crushing chamber of the jet mill process can be 0.3-0.4 MPa, for example 0.38 MPa.
- the time of the jet milling process may be 2 to 4 hours, for example, 3 hours.
- a lubricant such as zinc stearate
- the added amount of the lubricant may be 0.10-0.15% of the weight of the powder after mixing, for example 0.12%.
- the molding operation and conditions can be conventional molding operations in the art.
- it includes a magnetic field forming method or a hot pressing and thermal deformation method.
- the sintering operation and conditions can be conventional sintering operation conditions in the art.
- the sintering environment may be a vacuum.
- the pressure of the vacuum may be 5 ⁇ 10 -3 Pa.
- preheating is usually included before the sintering.
- the preheating temperature may be 300-600°C.
- the preheating time may be 1 to 2 hours.
- the preheating is preferably at a temperature of 300°C and 600°C for 1 hour each.
- the sintering temperature is preferably 1050-1095°C, such as 1063°C, 1065°C, 1073°C, 1075°C, 1080°C, 1090°C or 1092°C, more preferably 1063°C to 1090°C.
- the sintering time is preferably 5-10h, for example 8h.
- the aging treatment preferably includes a primary aging treatment and a secondary aging treatment.
- the temperature of the primary aging treatment is preferably 850-950°C, more preferably 900°C.
- the time of the primary aging treatment is preferably 2 to 4 hours, such as 3 hours, and the time refers to the time at the temperature of the primary aging treatment.
- the temperature of the secondary aging treatment is preferably 455-470°C, such as 455°C, 460°C, or 470°C.
- the time of the secondary aging treatment is preferably 2 to 4 hours, such as 3 hours, and the time refers to the time at the temperature of the secondary aging treatment.
- the rate of heating up to the temperature of the primary aging treatment or secondary aging treatment may be conventional, and is usually 3 to 5° C./min.
- the invention also provides a rare earth permanent magnet material prepared by the above preparation method.
- the present invention also provides a rare earth permanent magnet material, which includes the following components in mass content:
- R 28.5-33%; the R is a rare earth element, and the R includes at least Nd;
- Ga 0.6 ⁇ Ga ⁇ 1.804%
- N contains one or more of Ti, Zr and Nb;
- N contains Nb
- the content of Nb is 0.2-0.5%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material.
- the grain boundary phase of the rare earth permanent magnetic material preferably further includes R 6 T 13 M phase.
- R refers to rare earth elements
- T refers to Fe and/or Co
- M refers to Ga.
- the volume of the R 6 T 13 M phase and the total volume of the "main phase, grain boundary phase, and rare earth-rich phase” are preferably 2-12%; more preferably 2.5-11.5%, such as 2.5%, 3.6%, 3.7%, 4.8%, 5.2%, 5.7%, 6.5%, 10.2%, 10.5%, 11.3% or 11.5%, more preferably 5-11%.
- the grain boundary phase refers to the general term for the grain boundary phase between two or more Nd 2 T 4 B crystal grains.
- the Nd 2 T 14 B crystal grains refer to the main phase
- T refers to Fe and/or Co.
- the content of R is preferably 29.3% to 32%, for example, 29.296%, 29.308%, 29.486%, 29.494%, 30.004%, 30.01%, 30.485%, 30.5028% , 30.994%, 30.996%, 30.999%, 31.194% or 31.986%, more preferably 29.4-31.5%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the Nd content is preferably 8-13%, such as 8.501%, 8.506%, 9.491%, 9.494%, 12.303%, 12.491%, 12.497% or 12.503%; or, the Nd content Preferably it is 28-31%, such as 28.497%, 29.002%, 29.291%, 29.302%, 30.194%, 30.202% or 30.891%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the rare earth permanent magnet material preferably does not contain Cu.
- the R in the rare earth permanent magnet material, the R may also include Pr.
- the content of Pr is preferably less than 1.5% and not 0, more preferably 0.1 to 0.5%, such as 0.192%, 0.195%, 0.291%, 0.294%, 0.301%, 0.303% or 1.502%; Or the content of Pr is preferably 17-25%, such as 17.005%, 18.502%, 18.503%, 21.502%, 21.503%, 21.504% or 21.505%, more preferably 18.5-21.505%, the percentage is The mass percentage of the total mass of the rare earth permanent magnet material.
- the rare earth permanent magnet material may not contain heavy rare earth elements, and may also reach a level equivalent to or even better than the magnetic properties of the prior art magnet materials.
- the rare earth permanent magnet material may further include RH, and the RH is a heavy rare earth element.
- the content of the RH is preferably 1 to 2.5%, and the percentage is a mass percentage of the total mass of the rare earth permanent magnet material.
- the type of RH preferably includes one or more of Dy, Tb and Ho.
- the content of Dy is preferably 1 to 2.5%, for example, 1.992%, and the percentage is a mass percentage of the total mass of the rare earth permanent magnet material.
- the content of Tb is preferably 1 to 2.5%, for example, 1.987%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the content of B is preferably 0.861% to 0.943%, such as 0.861%, 0.862%, 0.864%, 0.878%, 0.882%, 0.895%, 0.897%, 0.902%, 0.918%, 0.921%, 0.922 %, 0.942% or 0.943%, the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the atomic percentage of R and the atomic percentage of B in the rare earth permanent magnetic material preferably satisfy the following relational formula: B/R ⁇ 0.38, where B is in the rare earth permanent magnet The atomic percentage in the magnetic material, and the R is the atomic percentage in the rare earth permanent magnetic material.
- the rare earth permanent magnet material contains Pr
- the B and Nd satisfy the following relational formula: B/(Pr+Nd) ⁇ 0.405, where B refers to the The atomic percentage of B in the rare earth permanent magnetic material, Pr refers to the atomic percentage of the Pr in the rare earth permanent magnetic material, and Nd refers to the atomic percentage of the Nd in the rare earth permanent magnetic material.
- the Ga content is preferably 0.65 to 1.804%, for example, 0.651%, 0.652%, 0.655%, 0.851%, 0.853%, 1.005%, 1.052%, 1.201%, 1.203%, 1.252%, 1.452%, 1.552%, 1.802%, 1.804%, more preferably 0.65-1.25%, the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the content of Co is preferably 0.5 to 2.5%, such as 0.502%, 0.503%, 0.504%, 0.505%, 1.047%, 1.502%, 1.554%, 1.987%, 1.989%, 2.003%, 2.005 %, 2.452% or 2.502%, more preferably 1.05-2.005%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the content of Al is preferably 0.02-0.06%, more preferably 0.025-0.053%, such as 0.025%, 0.031%, 0.035%, 0.042%, 0.043%, 0.051%, 0.052% or 0.053 %, the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the content of Fe is preferably 61.8-68.36%, such as 61.826%, 63.253%, 63.891%, 63.973%, 64.361%, 65.039%, 65.517%, 65.521%, 66.292%, 66.912%, 66.923 %, 67.017%, 67.1%, 67.647% or 68.323%, more preferably 63.3-68.36%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the content of Ti is preferably 0.151 to 0.252%, such as 0.151%, 0.154%, 0.205%, 0.222%, 0.224% or 0.252%, more preferably 0.2 to 0.252%, and the percentage is The mass percentage of the total mass of the rare earth permanent magnet material.
- the content of Zr is preferably 0.25 to 0.351%, such as 0.202%, 0.203%, 0.205%, 0.207%, 0.262%, 0.302% or 0.351%, and the percentage is based on the total rare earth permanent magnetic material The mass percentage of mass.
- the content of Zr when Zr is contained in the rare earth permanent magnetic material, preferably satisfies: 0.20% ⁇ Zr ⁇ (3.48B-2.67)%, where B refers to the proportion of B occupies The mass percentage of the total mass of the rare earth permanent magnet material.
- the Nb content is preferably 0.2-0.25%, such as 0.202%, 0.251% or 0.252%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
- the rare earth permanent magnet material contains Ti and Nb, preferably, the Ti/Nb ⁇ 1.5, where the Ti is the mass percentage in the rare earth permanent magnet material, so The Nb is the mass percentage in the rare earth permanent magnetic material.
- the rare earth permanent magnet material preferably includes the following components by mass content: R: 29.3-32%; said R is a rare earth element, and said R includes at least Nd; B: 0.86-0.943%; Ga : 0.65 ⁇ 1.8%; Co: 0.5 ⁇ 2.5%; Al: 0.02 ⁇ 0.06%; Fe: 61.8 ⁇ 68.36%; N: contains one or more of Ti, Zr and Nb; when N contains Ti, The content of Ti is 0.2 to 0.252%; when N contains Zr, the content of Zr is 0.25 to 0.351%; when N contains Nb, the content of Nb is 0.2 to 0.35%; the rare earth The permanent magnet material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnet material also includes the R 6 T 13 Ga phase, and the R The ratio of the volume of the 6 T 13 Ga phase to the total volume of the "main phase, grain boundary phase, and rare earth-rich phase" is 2.5 to 11.
- the rare earth permanent magnetic material preferably includes the following components by mass: R: 29.4 to 31.5%; the R is a rare earth element, and the R includes Nd and Pr; Pr: 0.1 to 0.5% or 17 to 25%; B: 0.86 to 0.943%; Ga: 0.65 to 1.8%; Co: 0.5 to 2.5%; Al: 0.025 to 0.053%; Fe: 63.3 to 68.36%; N: including Ti, Zr and Nb One or more; when N contains Ti, the content of Ti is 0.2 to 0.252%; when N contains Zr, the content of Zr is 0.25 to 0.351%; when N contains Nb, the content of Ti is 0.2 to 0.252%; The Nb content is 0.2-0.35%; the rare earth permanent magnet material does not contain Cu; the percentage is the mass percentage of the mass of each component to the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnet material It also includes the R 6 T 13 Ga phase, and the ratio of the volume of the R 6 T 13 Ga
- the rare earth permanent magnet material preferably includes the following components by mass: R: 29.4-31.5 %; the R is a rare earth element, and the R includes at least Nd; B: 0.86-0.943%; Ga :0.65 ⁇ 1.8%; Co: 0.5 ⁇ 2.5%; Al: 0.025 ⁇ 0.053%; Fe: 63.3 ⁇ 68.5%; Ti: 0.2 ⁇ 0.252%; the rare earth permanent magnet material does not contain Cu; the percentage is each component mass percentage of the mass of the total mass of the rare earth permanent magnet material; grain boundary phase, rare earth permanent magnet material further comprises R 6 T 13 Ga phase, the volume of the R 6 T 13 Ga with the "main phase, crystal The ratio of the total volume of the "boundary phase and the rare earth-rich phase" is 5.7 to 11.3%.
- the rare earth permanent magnet material preferably includes the following components by mass content: R: 29.3-32%; said R is a rare earth element, and said R includes at least Nd; B: 0.86-0.943%; Ga :0.65 ⁇ 1.8%; Co: 0.5 ⁇ 2.5%; Al: 0.025 ⁇ 0.053%; Fe: 62 ⁇ 67.5%; Zr: 0.25 ⁇ 0.351%; the rare earth permanent magnet material does not contain Cu; the percentage is each component mass percentage of the mass of the total mass of the rare earth permanent magnet material; grain boundary phase, rare earth permanent magnet material further comprises R 6 T 13 Ga phase, the volume of the R 6 T 13 Ga with the "main phase, crystal The ratio of the total volume of the "boundary phase and the rare earth-rich phase" is 2.5 to 11.5%.
- the rare earth permanent magnet material includes the following components: Nd 29.302%; Pr 0.192%; Ga 0.651%; Co 0.505%; Al 0.031%; Ti 0.151%; B0.845 %; Fe 68.323%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material is related to the "main phase, grain boundary phase and rich The ratio of the total volume of the "rare earth phase" is 5.7%.
- the rare earth permanent magnet material includes the following components by mass content: Nd 30.194%; Pr 0.291%; Ga 0.853%; Co 1.047%; Al 0.052%; Ti 0.205%; Nb 0.202 %; B 0.864%; Fe 66.292%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnet The ratio of the total volume of the "boundary phase and the rare earth-rich phase" is 5.2%.
- the rare earth permanent magnet material includes the following components: Nd 30.891%; Pr 0.303%; Ga 1.052%; Co 1.554%; Al 0.042%; Ti 0.222%; B 0.897% Fe 65.039%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material is related to the "main phase, grain boundary phase and The ratio of the total volume of the "rare earth-rich phase" is 3.6%.
- the rare earth permanent magnet material includes the following components: Nd 12.497%; Pr 18.502%; Ga 1.452%; Co 1.989%; Al 0.053%; Ti 0.224%; B 0.922% Fe 64.361%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material is related to the "main phase, grain boundary phase and The ratio of the total volume of the "rare earth-rich phase" is 11.3%.
- the rare earth permanent magnet material includes the following components: Nd 9.491%; Pr 21.505%; Ga 1.802%; Co 2.452%; Al 0.051%; Ti 0.252%; Nb 0.252% B 0.942%; Fe 63.253%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material and the "main phase, grain boundary The ratio of the total volume of the "phase to the rare earth-rich phase" is 10.2%.
- the rare earth permanent magnet material includes the following components: Nd 30.202%; Pr 0.301%; Ga 1.052%; Co 1.502%; Al 0.035%; Zr 0.262%; Nb 0.251% B 0.878%; Fe 65.517%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material and the "main phase, grain boundary The ratio of the total volume of the phase and the rare earth-rich phase is 6.5%.
- the rare earth permanent magnet material includes the following components: Nd 8.506%; Pr 21.504%; Ga 1.201%; Co 0.502%; Al 0.025%; Zr 0.302%; B 0.943%; Fe 67.017%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material is related to the main phase, grain boundary phase and rare earth-rich phase "The ratio of the total volume is 5.7%.
- the rare earth permanent magnet material includes the following components: Nd 8.501%; Pr 21.503%; Ga 1.203%; Co 0.503%; Al 0.043%; Zr 0.205%; B 0.942% Fe 67.1%; The percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnet material and the "main phase, grain boundary phase and rare earth-rich The ratio of the total volume of "phase" is 5.2%.
- the rare earth permanent magnet material includes the following components: Nd 29.291%; Pr 0.195%; Ga 1.252%; Co 0.504%; Al 0.042%; Zr 0.207%; B 0.862% Fe 67.647%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnet material is related to the main phase, grain boundary phase and rare earth-rich The ratio of the total volume of "phase" is 3.6%.
- the rare earth permanent magnetic material includes the following components: Nd 12.491%; Pr 18.503%; Ga 1.552%; Co 0.505%; Al 0.053%; Zr 0.262%; Nb 0.252% B 0.861%; Fe 65.521%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material and the "main phase, grain boundary The ratio of the total volume of the phase and the rare earth-rich phase is 11.3%.
- the rare earth permanent magnet material includes the following components: Nd 9.494%; Pr 21.502%; Ga 1.804%; Co 1.989%; Al 0.051%; Zr 0.351%; B 0.918% Fe 63.891%; The percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnet material is related to the main phase, grain boundary phase and rare earth-rich The ratio of the total volume of "phase" is 11.5%.
- the rare earth permanent magnet material includes the following components: Nd 29.002%; Pr 0.294%; Ga 0.655%; Co 2.005%; Al 0.035%; Zr 0.202%; B 0.895% Fe 66.912%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnet material is related to the main phase, grain boundary phase and rare earth-rich The ratio of the total volume of "phase" is 3.7%.
- the rare earth permanent magnet material includes the following components: Nd 12.303%; Pr 17.005%; Ga 0.652%; Co 1.987%; Al 0.025%; Zr 0.203%; B 0.902% Fe 66.923%; The percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnetic material is related to the main phase, grain boundary phase and rare earth-rich The ratio of the total volume of "phase" is 4.8%.
- the rare earth permanent magnet material includes the following components by mass content: Nd 28.497%; Pr 1.502%; Tb 1.987%; Ga 0.851%; Co 2.003%; Al 0.043%; Zr 0.262 %; B 0.882%; Fe 63.973%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnetic material; the volume of the R 6 T 13 Ga phase in the rare earth permanent magnet The ratio of the total volume of the boundary phase to the rare earth-rich phase is 2.5%.
- the rare earth permanent magnet material includes the following components: Nd 12.503%; Pr 18.502%; Dy 1.992%; Ga 1.005%; Co 2.502%; Al 0.042%; Ti 0.154% Zr 0.351%; Nb 0.202%; B 0.921%; Fe 61.826%; The percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; R 6 T 13 Ga in the rare earth permanent magnet material.
- the ratio of the volume of the phase to the total volume of the "main phase, grain boundary phase, and rare earth-rich phase" is 10.5%.
- the invention also provides an application of the rare earth permanent magnet material as an electronic component.
- the application fields can be the automotive drive field, wind power field, servo motor and home appliance field (for example, air conditioner).
- the room temperature refers to 25°C ⁇ 5°C.
- the reagents and raw materials used in the present invention are all commercially available.
- the elements with a specific content are coordinated with each other, and the prepared rare earth permanent magnetic material contains a specific content of R 6 T 13 Ga.
- the rare earth permanent magnetic material of the present invention contains a small amount (0.84-0.943%) of boron element, and can obtain good remanence, coercivity, squareness, and temperature stability without adding heavy rare earth elements.
- the rare earth permanent magnetic material of the present invention not only obtains a permanent magnet material with better magnetic properties without adding an appropriate amount of Al, but also improves the consistency of the rare earth permanent magnet material, that is, the magnetic properties of the same batch of products Uniform.
- the raw materials used in the preparation of the rare earth permanent magnet material in this embodiment are shown in Table 1, and the preparation process is as follows:
- Example 1 (1) Melting process: According to the formula shown in Example 1 in Table 1, take the prepared raw materials and put them in a crucible made of alumina, and place them in a high-frequency vacuum induction melting furnace in a vacuum of 5 ⁇ 10 -2 Pa. Vacuum melting is performed at a temperature below 1500°C.
- Hydrogen breaking and pulverizing process Vacuum the hydrogen breaking furnace containing the quench alloy at room temperature, and then pass hydrogen with a purity of 99.9% into the hydrogen breaking furnace, maintain the hydrogen pressure at 0.15MPa, and fully absorb hydrogen. The temperature is raised while vacuuming, and the hydrogen is fully dehydrogenated, and then it is cooled, and the powder after the hydrogen cracking and pulverization is taken out.
- Fine pulverization process Under the nitrogen atmosphere with an oxidizing gas content of 120 ppm or less, the powder after hydrogen pulverization is pulverized by jet milling for 3 hours under the condition of a pulverizing chamber pressure of 0.38 MPa to obtain a fine powder.
- Oxidizing gas refers to oxygen or moisture.
- Magnetic field molding process using a right-angle orientation magnetic field molding machine, in a 1.6T orientation magnetic field, under a molding pressure of 0.35ton/cm 2 , the above-mentioned zinc stearate-added powder is formed into a side length at a time It is a 25mm cube, which is demagnetized in a 0.2T magnetic field after a single forming.
- a secondary molding machine isostatic press
- each molded body is moved to a sintering furnace for sintering, sintered in a vacuum of 5 ⁇ 10 -3 Pa, kept at a temperature of 300°C and 600°C for 1 hour, and then sintered at a temperature of 1090°C After 8 hours, Ar gas was introduced to bring the pressure to 0.1 MPa, and then cooled to room temperature.
- the sintered body is heated from 20°C to 900°C at a heating rate of 3 to 5°C/min in high-purity Ar gas, and then subjected to primary aging treatment at 900°C for 3 hours, and then cooled to room temperature After removing. Then, the temperature is increased from 20°C to 470°C at a heating rate of 3 to 5°C/min, and the secondary aging temperature is performed at a temperature of 470°C.
- the magnetic properties of the neodymium-iron-boron materials in Comparative Examples 1 to 6 are the best properties that can be obtained after the formulations of Comparative Examples 1 to 6 are optimized by process (aging temperature, sintering temperature or water inlet temperature).
- Example 2 30.194 0.291 / / 0.853 1.047 0.052 0.205 / 0.202 0.864 66.292
- Example 3 30.891 0.303 / / 1.052 1.554 0.042 0.222 / / 0.897 65.039
- Example 4 12.497 18.502 / / 1.452 1.989 0.053 0.224 / / 0.922 64.361
- Example 5 9.491 21.505 / / 1.802 2.452 0.051 0.252 / 0.252 0.942 63.253
- Example 6 30.202 0.301 / / 1.052 1.502 0.035 / 0.262 0.251 0.878 65.517
- Example 7 8.506 21.504 / / 1.201 0.502 0.025 / 0.302 / 0.943 67.017
- Example 7.1 8.501 21.503 / / 1.203 0.503 0.043 / 0.205 / 0.942 67.100
- Example 8 29.291 0.195
- Effect Example 1 The magnetic properties of rare-earth permanent magnet materials in Examples 1-13 and Comparative Examples 1-6 1.
- Microstructure FE-EPMA inspection is used to polish the vertical orientation surface of rare earth permanent magnetic materials, and field emission is used Electron probe microanalyzer (FE-EPMA) (JEOL, 8530F). The R 6 T 13 Ga phase and the R 6 T 13 Al phase in the grain boundary are detected, and T refers to Fe and/or Co. The test results are shown in Table 3 below.
- the proportion of R 6 T 13 Ga phase and R 6 T 13 Al phase content is measured by the proportion of 5 rare earth permanent magnetic materials in the same batch of rare earth permanent magnetic materials in each example and comparative example, and calculated average of.
- the average value of Br or Hcj refers to the average value calculated by testing the remanence or coercivity of 5 rare earth permanent magnetic materials in the same batch.
- the relative permeability is Br/Hcb; among them, Br is the remanence and Hcb is the magnetic coercivity.
- Br is the remanence
- Hcb is the magnetic coercivity.
- Max(Hcj)-Min(Hcj) The maximum value of the coercive force minus the minimum value of the coercive force in the same embodiment or the same comparative example. If it is greater than 1.5kOe, the magnetic performance consistency is poor. The test results are shown in Table 3 below.
- each neodymium iron boron material refers to a cylinder of 10mm*10mm cut out according to the unit of the performance test.
- ⁇ refers to the absence of R 6 T 13 Ga phase or R 6 T 13 Al phase. Except Max(Hcj)-Min(Hcj), the remaining parameters in Table 3 are the average values of 5 neodymium iron boron materials in the same batch.
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Abstract
Description
编号/wt% | Nd | Pr | Tb | Dy | Ga | Co | Al | Ti | Zr | Nb | B | Fe |
实施例1 | 29.302 | 0.192 | / | / | 0.651 | 0.505 | 0.031 | 0.151 | / | / | 0.845 | 68.323 |
实施例2 | 30.194 | 0.291 | / | / | 0.853 | 1.047 | 0.052 | 0.205 | / | 0.202 | 0.864 | 66.292 |
实施例3 | 30.891 | 0.303 | / | / | 1.052 | 1.554 | 0.042 | 0.222 | / | / | 0.897 | 65.039 |
实施例4 | 12.497 | 18.502 | / | / | 1.452 | 1.989 | 0.053 | 0.224 | / | / | 0.922 | 64.361 |
实施例5 | 9.491 | 21.505 | / | / | 1.802 | 2.452 | 0.051 | 0.252 | / | 0.252 | 0.942 | 63.253 |
实施例6 | 30.202 | 0.301 | / | / | 1.052 | 1.502 | 0.035 | / | 0.262 | 0.251 | 0.878 | 65.517 |
实施例7 | 8.506 | 21.504 | / | / | 1.201 | 0.502 | 0.025 | / | 0.302 | / | 0.943 | 67.017 |
实施例7.1 | 8.501 | 21.503 | / | / | 1.203 | 0.503 | 0.043 | / | 0.205 | / | 0.942 | 67.100 |
实施例8 | 29.291 | 0.195 | / | / | 1.252 | 0.504 | 0.042 | / | 0.207 | / | 0.862 | 67.647 |
实施例9 | 12.491 | 18.503 | / | / | 1.552 | 0.505 | 0.053 | / | 0.262 | 0.252 | 0.861 | 65.521 |
实施例10 | 9.494 | 21.502 | / | / | 1.804 | 1.989 | 0.051 | / | 0.351 | / | 0.918 | 63.891 |
实施例11 | 29.002 | 0.294 | / | / | 0.655 | 2.005 | 0.035 | / | 0.202 | / | 0.895 | 66.912 |
实施例11.1 | 12.303 | 17.005 | / | / | 0.652 | 1.987 | 0.025 | / | 0.203 | / | 0.902 | 66.923 |
实施例12 | 28.497 | 1.502 | 1.987 | / | 0.851 | 2.003 | 0.043 | / | 0.262 | / | 0.882 | 63.973 |
实施例13 | 12.503 | 18.502 | / | 1.992 | 1.005 | 2.502 | 0.042 | 0.154 | 0.351 | 0.202 | 0.921 | 61.826 |
对比例1 | 30.987 | 0.303 | / | / | 0.552 | 1.552 | 0.053 | 0.222 | / | / | 0.905 | 65.426 |
对比例2 | 8.502 | 21.491 | / | / | 1.902 | 0.504 | 0.051 | / | 0.305 | / | 0.942 | 66.303 |
对比例3 | 30.988 | 0.194 | / | / | 1.052 | 1.552 | 0.035 | 0.105 | / | / | 0.897 | 65.177 |
对比例4 | 31.012 | 0.291 | / | / | 1.051 | 1.552 | 0.025 | 0.348 | / | / | 0.905 | 64.816 |
对比例5 | 8.502 | 21.506 | / | / | 1.202 | 0.492 | 0.043 | / | 0.394 | / | 0.942 | 66.919 |
对比例6 | 8.493 | 21.504 | / | / | 1.205 | 0.498 | 0.192 | / | 0.297 | / | 0.941 | 66.870 |
Claims (10)
- 一种稀土永磁材料的原料组合物,其特征在于,其包括如下质量含量的组分:R:28.5~33%;所述R为稀土元素,所述R至少包括Nd;B:0.84~0.94%;Ga:0.6<Ga≤1.8%;Co:≤2.5%且不为0;Fe:61.6~69%;N:包含Ti、Zr和Nb中的一种或多种;当N中包含Ti时,所述Ti的含量为0.15~0.25%;当N中包含Zr时,所述Zr的含量为0.2~0.35%;当N中包含Nb时,所述Nb的含量为0.2~0.5%;百分比为各组分质量占所述稀土永磁材料总质量的质量百分比。
- 如权利要求1所述的原料组合物,其特征在于,所述原料组合物中,所述R的含量为29.3~32%,较佳地为29.4~31.5%,百分比为占所述原料组合物总质量的质量百分比;和/或,所述Nd的含量为8~13%,或者为28~31%,百分比为占所述原料组合物总质量的质量百分比;和/或,所述原料组合物中不含Cu;和/或,所述原料组合物中不含Al;和/或,所述原料组合物中,所述R还包括Pr;其中,所述Pr的含量较佳地在1.5%以下且不为0,或者为17~25%;所述Pr的含量更佳地为0.1~0.5%,或18.5~21.5%,百分比为占所述原料组合物总质量的质量百分比;和/或,所述原料组合物中还包括RH,所述RH为重稀土元素;其中,所述RH的种类较佳地包括Dy、Tb和Ho中的一种或多种;当所述RH包含Dy时,所述Dy的含量较佳地为1~2.5%,百分比为占所述原料组合物总质量的质量百分比;当所述RH包含Tb时,所述Tb的含量较佳地为1~2.5%,百分比为占所述原料组合物总质量的质量百分比;和/或,所述B的含量为0.86~0.94%,百分比为占所述原料组合物总质量的质量百分比;和/或,所述原料组合物中所述R的原子百分比和所述B的原子百分比满足如下关系式:B/R≥0.38,式中,所述B为在所述稀土永磁材料中的原子百分比,所述R为在所述稀土永磁材料中的原子百分比;和/或,所述Ga的含量为0.65~1.8%,较佳地为0.65~1.25%,百分比为占所述原料组合物总质量的质量百分比;和/或,所述Co的含量为0.5~2.5%,较佳地为1.05~2%,百分比为占所述原料组合物总质量的质量百分比;和/或,所述Fe的含量为61.8~68.36%,较佳地为63.3~68.36%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,当所述N包含Ti时,所述Ti的含量为0.2~0.25%,百分比为占所述原料组合物总质量的质量百分比;和/或,当所述N包含Zr时,所述Zr的含量为0.25~0.35%,百分比为占所述原料组合物总质量的质量百分比;其中,当所述N包含Zr时,所述Zr的质量含量较佳地满足:0.20%≤Zr<(3.48B-2.67)%,式中B指的是所述B占所述原料组合物总质量的质量百分比;和/或,当所述N包含Nb时,所述Nb的含量为0.2~0.25%,百分比为占所述原料组合物总质量的质量百分比。
- 如权利要求1或2所述的原料组合物,其特征在于,所述稀土永磁材料的原料组合物,包括如下质量含量的组分:R:29.3~32%;所述R为稀土元素,所述R至少包括Nd;B:0.86~0.94%;Ga:0.65~1.8%;Co:0.5~2.5%;Fe:61.8~68.36%;N:包含Ti、Zr和Nb中的一种或多种;当N中包含Ti时,所述Ti的含量为0.2~0.25%;当N中包含Zr时,所述Zr的含量为 0.25~0.35%;当N中包含Nb时,所述Nb的含量为0.2~0.35%;所述原料组合物中不含Cu和Al;百分比为各组分质量占所述原料组合物总质量的质量百分比;或者,所述稀土永磁材料的原料组合物,包括如下质量含量的组分:R:29.4~31.5%;所述R为稀土元素,所述R包括Nd和Pr;Pr:0.1~0.5%或者17~25%;B:0.86~0.94%;Ga:0.65~1.8%;Co:0.5~2.5%;Fe:63.3~68%;N:包含Ti、Zr和Nb中的一种或多种;当N中包含Ti时,所述Ti的含量为0.2~0.25%;当N中包含Zr时,所述Zr的含量为0.25~0.35%;当N中包含Nb时,所述Nb的含量为0.2~0.35%;所述原料组合物中不含Cu和Al;百分比为各组分质量占所述原料组合物总质量的质量百分比;或者,所述稀土永磁材料的原料组合物,包括如下质量含量的组分:R:29.4~31.5%;所述R为稀土元素,所述R至少包括Nd;B:0.86~0.94%;Ga:0.65~1.8%;Co:0.5~2.5%;Fe:63.3~68.5%;Ti:0.2~0.25%;所述原料组合物中不含Cu和Al;百分比为各组分质量占所述原料组合物总质量的质量百分比;或者,所述稀土永磁材料的原料组合物,包括如下质量含量的组分:R:29.3~32%;所述R为稀土元素,所述R至少包括Nd;B:0.86~0.94%;Ga:0.65~1.8%;Co:0.5~2.5%;Fe:62~67.5%;Zr:0.25~0.35%;所述原料组合物中不含Cu和Al;百分比为各组分质量占所述原料组合物总质量的质量百分比。
- 一种稀土永磁材料的制备方法,其特征在于,其包括下述步骤:将如权利要求1~3中任一项所述稀土永磁材料的原料组合物经铸造、制粉、成型、烧结和时效处理即可。
- 如权利要求4所述的制备方法,其特征在于,所述铸造之前还包括熔炼;其中,所述熔炼的温度较佳地在1500℃以下;和/或,所述铸造是以10 2℃/秒~10 4℃/秒的速度冷却;其中,所述冷却较佳地通过辊轮中通入冷却水实现;所述辊轮的进水温度较佳地≤25℃,更佳地为23~23.8℃;和/或,所述制粉包括氢破工艺和气流磨工艺;其中,所述氢破工艺较佳地包括吸氢、脱氢和冷却处理;其中,所述气流磨工艺较佳地在在氧化气体含量120ppm以下的氮气气氛下进行;其中,所述气流磨工艺的粉碎室压力较佳地为0.3~0.4MPa;其中,所述气流磨工艺的时间较佳地为2~3小时;其中,所述气流磨工艺后,较佳地在粉体中添加润滑剂;所述润滑剂的添加量较佳地为混合后粉末重量的0.10~0.15%;和/或,所述成型包括磁场成形法或热压热变形法;和/或,所述烧结之前还包括预热;所述预热的温度较佳地为300~600℃;所述预热的时间较佳地为1~2h;和/或,所述烧结的温度为1050~1095℃,较佳地为1063~1090℃;和/或,所述烧结的时间为5~10h;和/或,所述时效处理包括一级时效处理和二级时效处理;其中,所述一级时效处理的温度较佳地为850~950℃,更佳地为900℃;其中,所述一级时效处理的时间较佳地为2~4h;其中,所述二级时效处理的温度较佳地为455~470℃,更佳地为455℃、460℃或470℃;其中,所述二级时效处理的时间较佳地为2~4h;其中,升温至所述一级时效处理或二级时效处理的温度的速率较佳地为3~5℃/min。
- 一种如权利要求4或5所述的制备方法制得的稀土永磁材料。
- 一种稀土永磁材料,其特征在于,其包括如下质量含量的组分:R:28.5~33%;所述R为稀土元素,所述R至少包括Nd;B:0.84~0.943%;Ga:0.6<Ga≤1.804%;Co:≤2.5%、但不为0;Al:<0.08%;Fe:61.6~69%;N:包含Ti、Zr和Nb中的一种或多种;当N中包含Ti时,所述Ti的含量为0.15~0.252%;当N中包含Zr时,所述Zr的含量为0.2~0.351%;当N中包含Nb时,所述Nb的含量为0.2~0.5%;百分比为各组分质量占所述稀土永磁材料总质量的质量百分比。
- 如权利要求7所述的稀土永磁材料,其特征在于,所述稀土永磁材料的晶界相中还包括R 6T 13M相;其中,所述R 6T 13M相的体积与“主相、晶界相和富稀土相”总体积的比较佳地为2~12%;更佳地为2.5~11.5%;和/或,所述稀土永磁材料中,所述R的含量为29.3~32%,较佳地为29.4~31.5%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述Nd的含量为8~13%,或者,为28~31%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述稀土永磁材料中不含Cu;和/或,所述Pr的含量在1.5%以下且不为0,或者为17~25%;较佳地为0.1~0.5%,或者为18.5~21.505%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述稀土永磁材料中还包括RH,所述RH为重稀土元素;其中,当所述稀土永磁材料中包含RH时,所述RH的含量较佳地为1~2.5%,百分比为占所述稀土永磁材料总质量的质量百分比;其中,所述RH的种类较佳地包括Dy、Tb和Ho中的一种或多种;当所述RH包含Dy时,所述Dy的含量较佳地为1~2.5%,百分比为占所述稀土永磁材料总质量的质量百分比;当所述RH包含Tb时,所述Tb的含量较佳地为1~2.5%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述B的含量为0.861~0.943%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述稀土永磁材料中的所述R的原子百分比和所述B的原子百分比满足如下关系式:B/R≥0.38,式中,所述B为在所述稀土永磁材料中的原子百分比,所述R为在所述稀土永磁材料中的原子百分比;和/或,所述Ga的含量为0.65~1.804%,较佳地为0.65~1.25%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述Co的含量为0.5~2.5%,较佳地为1.05~2.005%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述Al的含量为0.02~0.06%,较佳地为0.025~0.053%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述Fe的含量为61.8~68.36%,较佳地为63.3~68.36%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述Ti的含量为0.151~0.252%,较佳地为0.2~0.252%,百分比为占所述稀土永磁材料总质量的质量百分比;和/或,所述Zr的含量为0.25~0.351%,百分比为占所述稀土永磁材料总质量的质量百分比;当所述稀土永磁材料中包含Zr时,所述Zr的含量较佳地满足:0.20%≤Zr<(3.48B-2.67)%,式中B指的是所述B占所述稀土永磁材料总质量的质量百分比;和/或,所述Nb的含量为0.2~0.25%,百分比为占所述稀土永磁材料总质量的质量百分比。
- 如权利要求7或8所述的稀土永磁材料,其特征在于,所述稀土永磁材料包括如下含量的组分:R:29.3~32%;所述R为稀土元素,所述R至少包括Nd;B:0.86~0.943%;Ga:0.65~1.8%;Co:0.5~2.5%;Al:0.02~0.06%; Fe:61.88~68.36%;N:包含Ti、Zr和Nb中的一种或多种;当N中包含Ti时,所述Ti的含量为0.2~0.252%;当N中包含Zr时,所述Zr的含量为0.25~0.351%;当N中包含Nb时,所述Nb的含量为0.2~0.35%;所述稀土永磁材料中不含Cu;百分比为各组分质量占所述稀土永磁材料总质量的质量百分比;所述稀土永磁材料的晶界相中还包括R 6T 13Ga相,所述R 6T 13Ga相的体积与“主相、晶界相和富稀土相”总体积的比为2.5~11.5%;或者,所述稀土永磁材料包括如下质量含量的组分:R:29.4~31.5%;所述R为稀土元素,所述R包括Nd和Pr;Pr:0.1~0.5%或者17~25%;B:0.86~0.943%;Ga:0.65~1.8%;Co:0.5~2.5%;Al:0.025~0.053%;Fe:63.3~68.36%;N:包含Ti、Zr和Nb中的一种或多种;当N中包含Ti时,所述Ti的含量为0.2~0.252%;当N中包含Zr时,所述Zr的含量为0.25~0.351%;当N中包含Nb时,所述Nb的含量为0.2~0.35%;所述稀土永磁材料中不含Cu;百分比为各组分质量占所述稀土永磁材料总质量的质量百分比;所述稀土永磁材料的晶界相中还包括R 6T 13Ga相,所述R 6T 13Ga相的体积与“主相、晶界相和富稀土相”总体积的比为5~11%;或者,所述稀土永磁材料包括如下质量含量的组分:R:29.4~31.5%;所述R为稀土元素,所述R至少包括Nd;B:0.86~0.943%;Ga:0.65~1.8%;Co:0.5~2.5%;Al:0.025~0.053%;Fe:63.3~68.5%;Ti:0.2~0.252%;所述稀土永磁材料中不含Cu;百分比为各组分质量占所述稀土永磁材料总质量的质量百分比;所述稀土永磁材料的晶界相中还包括R 6T 13Ga相,所述R 6T 13Ga相的体积与“主相、晶界相和富稀土相”总体积的比为5.7~11.3%;或者,所述稀土永磁材料,包括如下质量含量的组分:R:29.3~32%;所述R为稀土元素,所述R至少包括Nd;B:0.86~0.943%;Ga:0.65~1.8%;Co:0.5~2.5%;Al:0.025~0.053%;Fe:62~67.5%;Zr:0.25~0.351%;所述稀土永磁材料中不含Cu和Al;百分比为各组分质量占所述稀土永磁材料总质量的质量百分比;所述稀土永磁材料的晶界相中还包括R 6T 13Ga相,所述R 6T 13Ga相的体积与“主相、晶界相和富稀土相”总体积的比为2.5~11.5%。
- 如权利要求7~9中任一项所述的稀土永磁材料在作为电子元器件的应用。
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