CN111312464B - Rare earth permanent magnetic material and preparation method and application thereof - Google Patents

Rare earth permanent magnetic material and preparation method and application thereof Download PDF

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CN111312464B
CN111312464B CN202010132232.8A CN202010132232A CN111312464B CN 111312464 B CN111312464 B CN 111312464B CN 202010132232 A CN202010132232 A CN 202010132232A CN 111312464 B CN111312464 B CN 111312464B
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permanent magnetic
magnetic material
content
percentage
series
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CN111312464A (en
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付刚
范宇峰
黄清芳
黄佳莹
许德钦
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Fujian Jinlong Rare Earth Co ltd
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Xiamen Tungsten Co Ltd
Fujian Changting Jinlong Rare Earth Co Ltd
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Priority to PCT/CN2021/077189 priority patent/WO2021169900A1/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • 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
    • H01F1/06—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 in the form of particles, e.g. powder
    • H01F1/08—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 in the form of particles, e.g. powder pressed, sintered, or bound together
    • 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
    • H01F1/06—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 in the form of particles, e.g. powder
    • H01F1/08—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 in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/086—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 in the form of particles, e.g. powder pressed, sintered, or bound 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

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The invention discloses a rare earth permanent magnetic material and a preparation method and application thereof. The permanent magnetic material comprises the following components: r: 28.45-33.1 wt%; ga: greater than 0.35 wt%; al: 0.08-0.125 wt%; b: 0.835-0.945 wt%; fe: 64.2-69.5 wt%; wherein: when the permanent magnetic material contains Ti, the content of Ti is 0.15-0.26 wt%; when the permanent magnetic material contains Zr, the content of Zr is 0.2-0.355 wt%; when the permanent magnetic material contains Nb, the content of Nb is 0.19-0.51 wt%; the R-T-B series permanent magnet material does not contain Co. The permanent magnetic material has excellent magnetic performance, smooth demagnetization curve, no step, low relative magnetic conductivity and good consistency of magnet performance.

Description

Rare earth permanent magnetic material and preparation method and application thereof
Technical Field
The invention relates to a rare earth permanent magnetic material and a preparation method and application thereof.
Background
Because of its excellent magnetic properties, R-T-B sintered magnets (R refers to rare earth elements, T refers to transition metal elements and group iii metal elements, and B refers to boron elements) are widely used in the fields of electronic products, automobiles, wind power, household appliances, elevators, industrial robots, and the like, for example, as energy sources in permanent magnet motors such as hard disks, mobile phones, earphones, elevator traction machines, generators, and the like, and the demand for the performance of magnets, such as remanence and coercive force, is increasing.
In order to lower the proportion of the B-rich phase and to raise the remanence of R-T-B sintered magnets, it is generally necessary to lower the B content, but when the B content is less than 5.88 at%, R is easily formed as seen from the Nd-Fe-B ternary phase diagram2T17And R is2T17Does not have room-temperature uniaxial anisotropy,thereby deteriorating the performance of the magnet.
In the prior art, heavy rare earth elements such as Dy, Tb, Gd and the like are generally added to improve the coercive force of the material and improve the temperature coefficient, but the heavy rare earth is high in price, and the method for improving the coercive force of the R-T-B sintered magnet product can increase the raw material cost and is not beneficial to the application of the R-T-B sintered magnet.
Therefore, how to prepare the R-T-B magnet with high coercivity and high remanence by adopting a low B system (B < 5.88 at%) under the condition of not adding or adding a small amount of heavy rare earth is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to overcome the defects that in the prior art, when B in an R-T-B series magnet is less than 5.88 at%, the performance of the magnet is deteriorated and the consistency is poor, and provides a rare earth permanent magnet material and a preparation method and application thereof.
The invention provides an R-T-B series permanent magnetic material, which comprises the following components: r, Ga, B, Al and Fe, and also comprises one or more of Ti, Zr and Nb, and the content is as follows in percentage by weight:
r: 28.45-33.1 wt%; r is a rare earth element at least containing Nd;
Ga：＞0.35wt％；
Al：0.08-0.125wt％；
B：0.835-0.945wt％；
fe: 64.2-69.5 wt%; wherein:
when the R-T-B series permanent magnet material contains Ti, the content of the Ti is 0.15-0.26 wt%;
when the R-T-B series permanent magnet material contains Zr, the content of Zr is 0.2-0.355 wt%;
when the R-T-B series permanent magnet material contains Nb, the content of Nb is 0.19-0.51 wt%;
the R-T-B series permanent magnet material does not contain Co.
In the invention, the R-T-B series permanent magnetic material comprises R2T14B main phase, grain boundary phase and rare earth-rich phase.
Wherein, theGrain boundary phases mean two or more R2Fel4B is a general term for grain boundary phases between grains.
Wherein, preferably, the grain boundary phase contains R6Fe13Ga phase, said R6Fe13The Ga phase has a volume fraction of 1.5-15%, e.g. 5.7%, 6.5%, 7.3%, 7.4%, 7.6%, 7.7%, 7.9%, 10.3%, 10.6%, 10.8%, 10.9%, 11.2%, 11.4%, 11.5% or 11.8%, the percentage referring to said R6Fe13The volume of Ga phase in the grain boundary phase and R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In the present invention, it is preferable that the R-T-B based permanent magnetic material does not contain Cu.
In the present invention, the content of said R is preferably 28.495-33.017 wt%, such as 28.495wt%, 29.494wt%, 29.992wt%, 29.999wt%, 30.008wt%, 30.02wt%, 30.495wt%, 30.496wt%, 30.497wt%, 30.498wt%, 30.501wt%, 30.502wt%, 30.503wt%, 31.0wt%, 31.002wt%, 31.003wt%, 31.004wt%, 31.005wt%, 31.007wt%, 31.966wt%, 31.968wt%, 31.979wt%, 31.984wt%, 31.987wt%, 33.003wt%, 33.004wt%, 33.005wt% or 33.017wt%, the percentage referring to the weight percentage in said R-T-B series permanent magnetic material.
In the present invention, the content of Nd is preferably 17.5 to 26.0 wt%, such as 21.372 to 24.753wt%, such as 21.372wt%, 21.987wt%, 22.122wt%, 22.496wt%, 22.497wt%, 22.505wt%, 22.752wt%, 22.872wt%, 22.873wt%, 22.874wt%, 22.877wt%, 23.248wt%, 23.249wt%, 23.251wt%, 23.252wt%, 23.253wt%, 23.255wt%, 23.976wt%, 23.987wt%, 23.989wt%, 24.751wt%, 24.752wt% or 24.753wt%, the percentage referring to the weight percentage in the R-T-B system permanent magnetic material.
In the invention, the R can also comprise Pr and/or heavy rare earth RH.
Wherein, the content of Pr can be less than 0.2 at% or more than 8 at%, and the percentage refers to the atomic percentage in the R-T-B series permanent magnetic material.
Wherein, the content of said Pr is preferably 7.0-8.5wt%, such as 7.123wt%, 7.372wt%, 7.496wt%, 7.503wt%, 7.523wt%, 7.622wt%, 7.623wt%, 7.624wt%, 7.628wt%, 7.629wt%, 7.748wt%, 7.750wt%, 7.752wt%, 7.753wt%, 7.992wt%, 7.995wt%, 8.000wt%, 8.252wt% or 8.253wt%, the percentage referring to the weight percentage in said R-T-B series permanent magnetic material.
Wherein, when said R further comprises Pr, the atomic percentage of B/(Pr + Nd) is preferably ≧ 0.405, such as 0.405, 0.408 or 0.410.
Wherein, the RH can be Tb or Dy.
Wherein the RH content may be 1.5-6.0wt%, such as 1.987wt% or 2.012wt%, the percentage referring to the weight percentage in the R-T-B series permanent magnetic material.
In the present invention, the content of Ga is preferably 0.396-2.0 wt%, for example 0.396-1.804 wt%, further for example 0.396 wt%, 0.552 wt%, 0.553 wt%, 0.596 wt%, 0.602 wt%, 0.652 wt%, 0.703 wt%, 0.793 wt%, 0.796 wt%, 0.802 wt%, 0.803 wt%, 0.903wt%, 0.905 wt%, 0.989 wt%, 1.052 wt%, 1.054 wt%, 1.104 wt%, 1.202 wt%, 1.203 wt%, 1.252 wt%, 1.253 wt%, 1.297 wt%, 1.352 wt%, 1.393 wt%, 1.403 wt%, 1.496 wt%, 1.597 wt%, 1.603 wt%, 1.697 wt%, 1.801 wt%, or 1.804 wt%, and the percentage means the weight percentage in the R-T-B system permanent magnetic material.
In the present invention, the content of Ga is preferably 1.05wt% or more, 0.35wt% or more and 0.55 wt% or less, 0.55 wt% or more and 1.05wt% or less, 1.05wt% or more and 1.25wt% or more, and Ga is 1.25wt% or more, and the percentage is the weight percentage in the R-T-B series permanent magnetic material.
In the present invention, the content of Al is preferably 0.081 to 0.123wt%, for example, 0.081wt%, 0.082wt%, 0.089wt%, 0.091wt%, 0.092wt%, 0.099wt%, 0.101wt%, 0.102wt%, 0.109wt%, 0.112wt%, 0.119wt%, 0.121wt%, or 0.123wt%, which is a weight percentage in the R-T-B system permanent magnetic material.
In the present invention, the content of B is preferably 0.839 to 0.944 wt%, for example, 0.839 wt%, 0.842 wt%, 0.843 wt%, 0.862 wt%, 0.863 wt%, 0.881 wt%, 0.882 wt%, 0.892 wt%, 0.894 wt%, 0.903wt%, 0.904 wt%, 0.913 wt%, 0.914 wt%, 0.916 wt%, 0.921 wt%, 0.922 wt%, 0.923 wt%, 0.942 wt%, or 0.944 wt%, the percentage referring to the weight percentage in the R-T-B series permanent magnetic material.
In the invention, the content of B is preferably not less than 0.915 wt% or not less than 5.55 at%; more preferably, the content of B is greater than 0.915 wt% and 5.55 at%; wt% means a weight percentage in the R-T-B system permanent magnetic material, and at% means an atomic percentage in the R-T-B system permanent magnetic material.
In the invention, preferably, the atomic percentage ratio of B to TRE is more than or equal to 0.38; wherein, TRE is total rare earth amount; for example, when Nd and Pr are included in the R, the TRE is the sum of the contents of the Nd and the Pr.
In the present invention, it is preferable that the atomic percentages of Ga and B satisfy the following condition: ga > 7.2941-1.24B.
In the present invention, the content of Fe is preferably 64.275 to 69.378wt%, for example 64.275wt%, 64.489wt%, 64.667wt%, 64.909wt%, 65.027wt%, 65.27wt%, 65.465wt%, 65.803wt%, 65.922wt%, 65.969wt%, 66.023wt%, 66.054wt%, 66.168wt%, 66.227wt%, 66.367wt%, 66.372wt%, 66.599wt%, 66.652wt%, 66.821wt%, 66.835wt%, 66.87wt%, 66.898wt%, 66.902wt%, 66.938wt%, 66.973wt%, 67.051wt%, 67.225wt%, 67.273wt%, 67.522wt%, 67.528wt%, 67.546wt%, 67.554wt%, 67.719wt%, 67.729wt%, 67.817wt%, 67.827wt%, 68.236wt%, or 69.378wt%, the percentage referring to the weight percentage in the R-T-B system permanent magnetic material.
In the present invention, when the R-T-B based permanent magnetic material contains Ti, the content of Ti is preferably 0.151 to 0.256wt%, for example, 0.151wt%, 0.152wt%, 0.200wt%, 0.201wt%, 0.203wt%, 0.204wt%, 0.205wt%, 0.251wt%, 0.252wt%, 0.253wt%, 0.254wt%, or 0.256wt%, which means the weight percentage in the R-T-B based permanent magnetic material.
In the present invention, when the R-T-B based permanent magnetic material contains Zr, the content of Zr is preferably 0.202 to 0.352wt%, for example, 0.202wt%, 0.203wt%, 0.261wt%, 0.262wt%, 0.302wt%, 0.303wt%, or 0.352wt%, which means the weight percentage in the R-T-B based permanent magnetic material.
In the present invention, when the R-T-B based permanent magnetic material contains Nb, the content of Nb is preferably 0.192 to 0.503wt%, for example, 0.192wt%, 0.201wt%, 0.202wt%, 0.298wt%, 0.301wt%, 0.302wt%, 0.392wt%, 0.401wt%, 0.492wt%, or 0.503wt%, which is a weight percentage in the R-T-B based permanent magnetic material.
In the present invention, when the R-T-B series permanent magnetic material contains Zr, the Zr content is preferably 0.20wt% to Zr < 3.48B-2.67 wt% or Zr < 0.26wt%, for example 0.26wt% to Zr < 3.48B-2.67 wt%, wherein B is the weight percentage of B in the R-T-B series permanent magnetic material; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, Ga more than or equal to 1.05wt%, Al: 0.08-0.125 wt%, B: 0.835-0.945 wt%, Fe: 64.2-69.5 wt%, Ti: 0.15-0.26 wt%, the percentage refers to the weight percentage in the R-T-B series permanent magnetic material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, 0.55 wt% or more and less than 1.05wt% of Ga, Al: 0.08-0.125 wt%, B: 0.835-0.945 wt%, Fe: 64.2-69.5 wt%, Ti: 0.15-0.26 wt%, the percentage refers to the weight percentage in the R-T-B series permanent magnetic material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, 0.35wt% < Ga < 0.55 wt%, Al: 0.08-0.125 wt%, B: 0.835-0.945 wt%, Fe: 64.2-69.5 wt%, Ti: 0.15-0.26 wt% or Zr: 0.2-0.355 wt%, the percentage refers to the weight percentage in the R-T-B series permanent magnetic material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, 1.05wt% or more and less than 1.25wt% of Ga, Al: 0.08-0.125 wt%, B: 0.835-0.945 wt%, Fe: 64.2 to 69.5wt%, Zr: 0.2-0.355 wt%; wherein, preferably, the Zr content is more than or equal to 0.26 percent and less than (3.48B-2.67 percent) by weight; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, Ga not less than 1.25wt%, Al: 0.08-0.125 wt%, B: 0.835-0.945 wt%, Fe: 64.2 to 69.5wt%, Zr: 0.2-0.355 wt%; wherein, the Zr content is preferably that Zr is more than or equal to 0.26 wt%; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, 0.55 wt% or more and less than 1.05wt% of Ga, Al: 0.08-0.125 wt%, B: 0.835-0.945 wt%, Fe: 64.2 to 69.5wt%, Zr: 0.2-0.355 wt%; wherein, preferably, the Zr content is more than or equal to 0.26 percent and less than (3.48B-2.67 percent) by weight; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
The invention provides a raw material composition of an R-T-B series permanent magnetic material, which comprises the following components: r, Ga, B, Al and Fe, and also comprises one or more of Ti, Zr and Nb, and the content is as follows in percentage by weight:
r: 28.5-33.0 wt%; r is a rare earth element at least containing Nd;
Ga：＞0.35wt％；
Al：0.05-0.07wt％；
B：0.84-0.94wt％；
fe: 64.0 to 69.5 weight percent; wherein:
when the R-T-B series permanent magnet material contains Ti, the content of the Ti is 0.15-0.25 wt%;
when the R-T-B series permanent magnet material contains Zr, the content of Zr is 0.2-0.35 wt%;
when the R-T-B series permanent magnet material contains Nb, the content of Nb is 0.2-0.5 wt%;
the R-T-B series permanent magnet material does not contain Co.
As known to those skilled in the art, the raw material composition of the R-T-B series permanent magnetic material generally refers to raw materials actively added in the preparation process of the permanent magnetic material, and does not include components and/or contents introduced in the preparation process or impurities.
In the present invention, the content of R is preferably 29.5 to 33.0wt%, for example 29.5wt%, 30.0wt%, 30.5wt%, 31.0wt%, 32.0wt% or 33.0wt%, which is a weight percentage in the raw material composition of the R-T-B-based permanent magnetic material.
In the present invention, the content of Nd is preferably 21.0 to 25.0wt%, for example 21.375wt%, 22.0wt%, 22.125wt%, 22.5wt%, 22.75wt%, 22.875wt%, 23.25wt%, 24.0wt%, or 24.75wt%, which is a weight percentage in the raw material composition of the R-T-B-based permanent magnetic material.
In the invention, the R can also comprise Pr and/or heavy rare earth RH.
Wherein, the content of Pr can be less than 0.2 at% or more than 8 at%, and the percentage refers to the atomic percentage in the raw material composition of the R-T-B series permanent magnetic material.
Wherein, the content of Pr is preferably 2.5-12.0wt%, such as 7.125wt%, 7.375wt%, 7.5wt%, 7.625wt%, 7.75wt%, 8.00wt% or 8.25wt%, which is the weight percentage in the raw material composition of the R-T-B series permanent magnetic material.
Wherein, when the R also comprises Pr, the atomic percentage of B/(Pr + Nd) is preferably more than or equal to 0.405.
Wherein, the RH can be Tb or Dy.
Wherein the RH may be present in an amount of 1.5-6.0 wt.%, for example 2.0 wt.%, percentages referring to weight percentages in the raw material composition of the R-T-B based permanent magnetic material.
In the present invention, the content of Ga is preferably 0.4 to 2.0wt%, for example, 0.4wt%, 0.55 wt%, 0.6 wt%, 0.65 wt%, 0.7 wt%, 0.8 wt%, 0.9wt%, 1.0wt%, 1.05wt%, 1.1wt%, 1.2wt%, 1.25wt%, 1.3wt%, 1.35wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt%, or 1.8wt%, which is a weight percentage in the raw material composition of the R-T-B-based permanent magnetic material.
In the present invention, the content of Ga is preferably 1.05wt% or more, 0.55 wt% or more and 1.05wt% or less, 0.35wt% or more and 0.55 wt% or less, 1.05wt% or more and 1.25wt% or more, and the percentage means the weight percentage in the raw material composition of the R-T-B-based permanent magnetic material.
In the present invention, the content of Al is preferably 0.06 to 0.07wt%, for example, 0.06 wt% or 0.07wt%, which is a weight percentage in the raw material composition of the R-T-B based permanent magnetic material.
In the present invention, it is preferable that the raw material composition of the R-T-B based permanent magnetic material does not contain Cu.
In the present invention, the content of B is preferably 0.86 to 0.94 wt%, for example, 0.86wt%, 0.88wt%, 0.90 wt%, 0.915 wt%, 0.92 wt%, or 0.94 wt%, which is a weight percentage in the raw material composition of the R-T-B-based permanent magnetic material.
In the invention, the content of B is preferably not less than 0.915 wt% or not less than 5.55 at%; more preferably, the content of B is greater than 0.915 wt% and 5.55 at%; wt% means a weight percentage in the raw material composition of the R-T-B based permanent magnetic material, and at% means an atomic percentage in the raw material composition of the R-T-B based permanent magnetic material.
In the invention, preferably, the atomic percentage ratio of B to TRE is more than or equal to 0.38; wherein, TRE is total rare earth amount; for example, when Nd and Pr are included in the R, the TRE is the sum of the contents of the Nd and the Pr.
In the present invention, it is preferable that the atomic percentages of Ga and B satisfy the following condition Ga > 7.2941-1.24B, and the atomic percentages refer to atomic percentages in the raw material composition of the R-T-B-based permanent magnetic material.
In the present invention, the content of Fe is preferably 64.32 to 69.41wt%, for example 64.32wt%, 64.555wt%, 64.715wt%, 64.93wt%, 65.08wt%, 65.3wt%, 65.5wt%, 65.82wt%, 65.96wt%, 65.99wt%, 66.065 wt%, 66.11 wt%, 66.2wt%, 66.24wt%, 66.4wt%, 66.42wt%, 66.625wt%, 66.685wt%, 66.86wt%, 66.9wt%, 66.915 wt%, 66.935wt%, 66.94wt%, 66.98wt%, 67.01wt%, 67.08 wt%, 67.275wt%, 67.33wt%, 67.58 wt%, 67.585wt%, 67.6wt%, 67.76wt%, 67.86 wt%, 67.87wt%, 68.28wt%, or 69.41wt%, the percentage referring to the weight percentage in the raw material composition of the R-T-B system permanent magnetic material.
In the present invention, when the R-T-B based permanent magnetic material contains Ti, the content of Ti is preferably 0.20 to 0.25wt%, for example, 0.20wt% or 0.25wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B based permanent magnetic material.
In the present invention, when the R-T-B based permanent magnetic material contains Zr, the Zr content is preferably 0.26 to 0.35wt%, for example, 0.26wt%, 0.3wt%, or 0.35wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B based permanent magnetic material.
In the present invention, when the R-T-B based permanent magnetic material contains Nb, the content of Nb is preferably 0.3 to 0.5wt%, for example, 0.3wt%, 0.4wt%, or 0.5wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B based permanent magnetic material.
In the present invention, when Zr is contained in the raw material composition of the R-T-B series permanent magnetic material, the Zr content is preferably 0.20wt% or more and less Zr < (3.48B-2.67) wt% or more and less Zr than or equal to 0.26wt%, for example 0.26wt% or less and less Zr < (3.48B-2.67) wt%, wherein B is the weight percentage of B in the raw material composition of the R-T-B series permanent magnetic material; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.5-33.0wt%, Ga more than or equal to 1.05wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.94 wt%, Fe: 64.0-69.5wt%, Ti: 0.15-0.25wt%, the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.5-33.0wt%, 0.55 wt% or more and Ga less than 1.05wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.94 wt%, Fe: 64.0-69.5wt%, Ti: 0.15-0.25wt%, the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.5-33.0wt%, 0.35wt% < Ga < 0.55 wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.94 wt%, Fe: 64.0-69.5wt%, Ti: 0.15-0.25wt% or Zr: 0.2-0.35wt%, the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.5-33.0wt%, Ga is more than or equal to 1.05wt% and less than 1.25wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.94 wt%, Fe: 64.0 to 69.5wt%, Zr: 0.2-0.35 wt%; wherein, preferably, the Zr content is more than or equal to 0.26 percent and less than (3.48B-2.67 percent) by weight; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.5-33.0wt%, Ga not less than 1.25wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.94 wt%, Fe: 64.0 to 69.5wt%, Zr: 0.2-0.35 wt%; wherein, preferably, the content of Zr is more than or equal to 0.26 wt%; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
In a preferred embodiment of the present invention, the R-T-B based permanent magnetic material comprises the following components: r: 28.5-33.0wt%, 0.55 wt% or more and Ga less than 1.05wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.94 wt%, Fe: 64.0 to 69.5wt%, Zr: 0.2-0.35 wt%; wherein, preferably, the Zr content is more than or equal to 0.26 percent and less than (3.48B-2.67 percent) by weight; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
The invention also provides a preparation method of the R-T-B series permanent magnetic material, which comprises the following steps:
and (3) carrying out casting, hydrogen fracturing, forming, sintering and aging treatment on the molten liquid of the raw material composition of the R-T-B series permanent magnet material.
Wherein, the melting liquid of the raw material composition of the R-T-B series permanent magnetic material can be prepared by the conventional method in the field, such as: smelting in a high-frequency vacuum induction smelting furnace.
The vacuum degree of the smelting furnace can be 5 multiplied by 10-2Pa。
The temperature of the smelting can be below 1500 ℃.
The melting is generally carried out in a crucible of alumina. The alumina crucible introduces a portion of Al into the R-T-B based permanent magnet material.
Wherein the casting process may be a casting process conventional in the art, such as: in an Ar atmosphere (e.g. 5.5X 10)4Pa Ar atmosphere), passing the melt of the raw material composition of the R-T-B permanent magnetic material through a rotating roller at 10 deg.C2DEG C/sec-104Cooling at a rate of DEG C/sec.
The cooling can be realized by introducing cooling water into the roller. Preferably, the water inlet temperature of the roller is less than or equal to 25 ℃, such as 23.2 ℃, 23.4 ℃, 23.5 ℃, 23.6 ℃ or 23.7 ℃. The roller may be a copper roller.
The hydrogen breaking process can be a hydrogen breaking process conventional in the art, and can be performed through hydrogen absorption, dehydrogenation and cooling treatment.
The hydrogen absorption can be carried out under the condition that the hydrogen pressure is 0.15 MPa.
The dehydrogenation can be carried out under the condition of vacuum pumping and temperature rise.
Wherein, after the hydrogen is broken, the raw materials can be crushed by the conventional method in the field. The comminution process may be a comminution process conventional in the art, such as jet milling.
The jet mill pulverization may be performed in a nitrogen atmosphere having an oxidizing gas content of 120ppm or less. The oxidizing gas refers to oxygen or moisture content.
The pressure of the crushing chamber for crushing by the jet mill can be 0.38 MPa.
The jet mill pulverizing time may be 3 hours.
After the pulverization, a lubricant, such as zinc stearate, may be added to the powder as is conventional in the art. The lubricant may be added in an amount of 0.10 to 0.15%, for example 0.12% by weight of the mixed powder.
The forming process may be a forming process conventional in the art, such as magnetic field forming or hot press hot deformation.
Wherein the sintering process may be a sintering process conventional in the art, for example, under vacuum conditions (e.g., at 5 × 10)-3Pa, vacuum), preheating, sintering and cooling.
The temperature of the preheating may be 300-600 ℃. The preheating time can be 1-2 h. Preferably, the preheating is for 1h each at a temperature of 300 ℃ and 600 ℃.
The sintering temperature may be a sintering temperature conventional in the art, such as 1040-.
The sintering time may be a sintering time as conventional in the art, such as 5-10h, for example, further 8 h.
Before cooling, Ar gas can be introduced to ensure that the gas pressure reaches 0.1 MPa.
Wherein the aging treatment comprises primary aging treatment and secondary aging treatment.
The temperature of the primary ageing treatment is preferably 860 ℃ and 960 ℃, for example 900 ℃.
In the first-stage aging treatment, the temperature rise rate of rising the temperature to 860 ℃ and 960 ℃ is preferably 3-5 ℃/min. The starting point of the warming may be room temperature.
The time of the primary aging treatment can be 3 hours.
The temperature of the secondary aging treatment is preferably 430-560 ℃, such as 450-490 ℃, and further such as 460 ℃, 470 ℃, 475 ℃, 477 ℃ or 480 ℃.
In the secondary aging, the heating rate of heating to 430-560 ℃ is preferably 3-5 ℃/min. The starting point of the warming may be room temperature.
The treatment time of the secondary ageing can be 3 hours.
The invention also provides the R-T-B series permanent magnetic material prepared by the method.
The invention also provides application of the R-T-B series permanent magnetic material as an electronic component.
The application field can be the automobile driving field, the wind power field, the servo motor field and the household appliance field (such as an air conditioner).
In the present invention, the room temperature means 25 ℃. + -. 5 ℃.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
(1) excellent magnetic performance: the R-T-B series permanent magnetic material Br is more than or equal to 11.77kGs, Hcj is more than or equal to 19.25kOe, and after heavy rare earth elements are added, the Hcj can reach 27.91kOe (Tb) and 28.01kOe (Dy); the magnet has good temperature stability, and the absolute value of the Br temperature coefficient alpha%/DEG C at 20-80 ℃ is less than 0.105.
(2) The demagnetization curve is smooth, no step exists, the relative magnetic conductivity is low, the same-batch range of the coercive force is less than or equal to 1.5kOe, and the consistency of the magnet performance is good.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example 1
The raw materials used for preparing the R-T-B series permanent magnetic material in this example are shown in table 1, and the preparation process is as follows:
(1) and (3) smelting: push buttonThe formulation shown in Table 1, the prepared raw materials were put into a crucible made of alumina, and placed in a high-frequency vacuum induction melting furnace at 5X 10-2Vacuum melting is carried out in vacuum of Pa at the temperature of below 1500 ℃ to obtain molten liquid.
(2) The casting process comprises the following steps: introducing Ar gas into a smelting furnace after vacuum smelting to enable the air pressure to reach 5.5 ten thousand Pa, then casting, and enabling the molten liquid to pass through a copper roller with the rotation speed of 29 revolutions per minute to prepare a rapid hardening alloy sheet with the thickness of 0.12-0.35mm, wherein in the casting process, chilled water needs to be introduced into the copper roller, and the water inlet temperature is less than or equal to 25 ℃; at 102DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen breaking furnace in which the quenching alloy is placed at room temperature, introducing hydrogen with the purity of 99.9% into the hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, vacuumizing while heating, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: the powder after hydrogen crushing was pulverized by jet milling for 3 hours under a nitrogen atmosphere having an oxidizing gas content of 120ppm or less and a pressure in the pulverization chamber of 0.38MPa to obtain a fine powder. The oxidizing gas refers to oxygen or moisture.
(5) Adding zinc stearate into the powder crushed by the jet mill, wherein the adding amount of the zinc stearate is 0.12 percent of the weight of the mixed powder, and then fully mixing the zinc stearate and the mixed powder by using a V-shaped mixer.
(6) Magnetic field forming process: using a magnetic field forming machine of a right angle orientation type, in an orientation magnetic field of 1.6T, at 0.35ton/cm2The powder added with zinc stearate was once formed into a cube with a side length of 25mm under the molding pressure of (1), and demagnetized in a magnetic field of 0.2T after the primary molding. The molded article after the primary molding was sealed so as not to contact air, and then subjected to secondary molding (isostatic pressing) at 1.3ton/cm2Secondary forming is performed under pressure of (1).
(7) And (3) sintering: the molded bodies were transferred to a sintering furnace and sintered at 5X 10-3Pa at 300 deg.C and 600 deg.C for 1 hr, and sintering at 1090 deg.CAfter 8 hours, Ar gas was introduced to make the pressure 0.1MPa, and then the mixture was cooled to room temperature.
(8) And (3) aging treatment process: in high-purity Ar gas, the sintered body is heated from 20 ℃ to 900 ℃ at the heating rate of 3-5 ℃/min for first-stage aging treatment, and the method comprises the following specific steps: after heat treatment at 900 ℃ for 3 hours, the mixture was cooled to room temperature and taken out. After that, secondary aging treatment was performed for 3 hours at a temperature as shown in Table 2.
TABLE 1 weight percentages of raw materials in each example and comparative example
Figure BDA0002396105540000141
Figure BDA0002396105540000151
Example 2-example 39, comparative examples 1-8
Raw materials were prepared according to the formulation shown in Table 1, and the process conditions were the same as in example 1 except for the conditions shown in Table 2, to obtain R-T-B sintered magnets.
TABLE 2
Figure BDA0002396105540000152
Figure BDA0002396105540000161
Figure BDA0002396105540000171
Effects of the embodiment
(1) Component determination
The sintered magnets of examples 1 to 39 and comparative examples 1 to 8 were measured for specific components using a high frequency inductively coupled plasma emission spectrometer (ICP-OES). The following table shows the results of the component detection.
TABLE 3
Figure BDA0002396105540000172
Figure BDA0002396105540000181
Figure BDA0002396105540000191
Note: the content of Al in the sintered magnets of examples 1 to 39 and comparative examples 1 to 8 is the sum of the content of Al in the raw material and the content of Al introduced in other raw materials and processes (e.g., a crucible made of alumina during melting).
(2) Detection of magnetic Properties
The microstructure is as follows: the perpendicular orientation plane of the R-T-B system permanent magnetic material was polished by FE-EPMA detection, and detected by field emission electron probe microanalyzer (FE-EPMA) (JEOL 8530F, Japan Electron Ltd.). Detection of R in grain boundary phase6T13M phase, T denotes Fe, M denotes Ga. The test results are shown in table 4 below.
Magnetic performance evaluation: the sintered magnet is subjected to magnetic property detection by using an NIM-10000H type BH bulk rare earth permanent magnet nondestructive measurement system of China measurement institute. The following Table 4 shows the results of magnetic property measurements.
Wherein, Br or Hcj both mean values: calculating an average value by testing the remanence or coercive force of 5 parts of rare earth permanent magnetic material samples (10 mm x 10mm cylinders) in the same batch; the volume ratio of the 6-13-1 phase to the bulk phase and the temperature coefficient are also average values obtained by measuring the properties of 5 samples (10 mm cylinders 10mm) of the R-T-B-based permanent magnetic material in the same batch. The same batch refers to the product obtained in the same period of time according to the starting materials and processes shown in the examples or comparative examples.
TABLE 4
Figure BDA0002396105540000192
Figure BDA0002396105540000201
Figure BDA0002396105540000211
Note: in Table 4, the 6-13-1 phase means RE6Fe13Ga phase, wherein: the volume ratio of the 6-13-1 phase to the overall phase is referred to as RE6Fe13The volume ratio of Ga phase in the bulk phase, the bulk phase including grain boundary phase and R2T14A main phase B and a rare earth-rich phase. The magnetic properties of the R-T-B series permanent magnet materials in the comparative examples 1-8 are the best properties obtained by the formula of the comparative examples 1-8 after process optimization (water inlet temperature, sintering temperature and aging temperature).
(3) Magnetic property uniformity detection
Squareness: the formula is Hk/Hcj (Hk is the value of the external magnetic field H when B is 90% Br, Hcj is the coercive force).
Relative magnetic permeability: the calculation formula is Br/Hcb (Br is remanence, Hcb is magnetic coercive force).
Squareness and relative permeability are averages obtained by measuring the properties of 5 samples (10 mm cylinders by 10mm) of R-T-B series permanent magnetic material in the same batch.
Max (Max hcj) -Min (hcj): and subtracting the minimum value of the coercive force from the maximum value of the coercive force in the same batch of products, wherein if the minimum value of the coercive force is more than 1.5kOe, the consistency of the magnetic performance is poor. The same batch refers to the product obtained in the same period of time according to the starting materials and processes shown in the examples or comparative examples.
The following table shows the results of the magnetic property uniformity measurements.
TABLE 5
Figure BDA0002396105540000221
Figure BDA0002396105540000231

Claims (55)

1. An R-T-B series permanent magnetic material, comprising: r, Ga, B, Al and Fe, and also comprises one or more of Ti, Zr and Nb, and the content is as follows in percentage by weight:
r: 28.45-33.1 wt%; r is a rare earth element at least containing Nd;
Ga：0.903-2wt%；
Al：0.08-0.125 wt%；
B：0.835-0.894 wt%；
fe: 64.2-69.5 wt%; wherein:
when the R-T-B series permanent magnet material contains Ti, the content of the Ti is 0.15-0.26 wt%;
when the R-T-B series permanent magnet material contains Zr, the content of Zr is 0.2-0.355 wt%;
when the R-T-B series permanent magnet material contains Nb, the content of Nb is 0.19-0.51 wt%;
the R-T-B series permanent magnet material does not contain Co;
the R-T-B series permanent magnetic material comprises R2T14A main phase B, a grain boundary phase and a rare earth-rich phase, wherein the grain boundary phase contains R6Fe13Ga phase, said R6Fe13The volume fraction of Ga phase is 1.5-15%, the percentage referring to said R6Fe13The volume of Ga phase in the grain boundary phase and R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
2. The R-T-B series permanent magnetic material according to claim 1, wherein R is6Fe13A volume fraction of Ga phase of 5.7%, 6.5%, 7.3%, 7.4%, 7.6%, 7.7%, 7.9%, 10.3%, 10.6%, 10.8%, 10.9%, 11.2%, 11.4%, 11.5% or 11.8%;
and/or the R-T-B series permanent magnetic material does not contain Cu;
and/or the content of R is 28.495-33.017 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnetic material;
and/or, the content of Nd is 17.5-26.0 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnetic material;
and/or, the R also comprises Pr and/or heavy rare earth RH;
and/or the Ga content is 0.905 wt%, 0.989 wt%, 1.052 wt%, 1.054 wt%, 1.104 wt%, 1.202 wt%, 1.203 wt%, 1.252 wt%, 1.253 wt%, 1.297 wt%, 1.352 wt%, 1.393 wt%, 1.403 wt%, 1.496 wt%, 1.597 wt%, 1.603 wt%, 1.697 wt%, 1.801 wt% or 1.804 wt%, the percentages referring to the weight percentage in the R-T-B series permanent magnetic material;
or the content of Ga is 1.05-2 wt%, Ga is more than or equal to 0.903wt% and less than 1.05wt%, Ga is more than or equal to 1.05wt% and less than 1.25wt%, or, 1.25-2 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnetic material;
and/or the content of the Al is 0.081-0.123 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnet material;
and/or the content of B is 0.839 wt%, 0.842 wt%, 0.843 wt%, 0.862 wt%, 0.863 wt%, 0.881 wt%, 0.882 wt% or 0.892 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnetic material;
and/or the content of the Fe is 64.275-69.378 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnet material;
and/or, when the R-T-B series permanent magnet material contains Ti, the content of the Ti is 0.151-0.256 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnet material;
and/or, when the R-T-B series permanent magnetic material contains Zr, the content of the Zr is 0.202-0.352 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnetic material;
and/or, when the R-T-B series permanent magnet material contains Nb, the content of Nb is 0.192-0.503 wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnet material;
or, when the R-T-B series permanent magnetic material contains Zr, the Zr content is more than or equal to 0.20wt% and less than (3.48B-2.67 wt%), and the percentage refers to the weight percentage in the R-T-B series permanent magnetic material.
3. The R-T-B based permanent magnetic material according to claim 2, wherein the content of R is 28.495wt%, 29.494wt%, 29.992wt%, 29.999wt%, 30.008wt%, 30.02wt%, 30.495wt%, 30.496wt%, 30.497wt%, 30.498wt%, 30.501wt%, 30.502wt%, 30.503wt%, 31.0wt%, 31.002wt%, 31.003wt%, 31.004wt%, 31.005wt%, 31.007wt%, 31.966wt%, 31.968wt%, 31.979wt%, 31.984wt%, 31.987wt%, 33.003wt%, 33.004wt%, 33.005wt%, or 33.017wt%, and the percentage refers to the weight percentage in the R-T-B based permanent magnetic material.
4. The R-T-B based permanent magnetic material according to claim 2, wherein the content of Nd is 21.372-24.753wt%, percentage being weight percentage in the R-T-B based permanent magnetic material.
5. The R-T-B system permanent magnetic material according to claim 4, wherein the content of Nd is 21.372wt%, 21.987wt%, 22.122wt%, 22.496wt%, 22.497wt%, 22.505wt%, 22.752wt%, 22.872wt%, 22.873wt%, 22.874wt%, 22.877wt%, 23.248wt%, 23.249wt%, 23.251wt%, 23.252wt%, 23.253wt%, 23.255wt%, 23.976wt%, 23.987wt%, 23.989wt%, 24.751wt%, 24.752wt% or 24.753wt%, percentages being percentages by weight in the R-T-B system permanent magnetic material.
6. The R-T-B series permanent magnetic material according to claim 2, wherein the content of Pr is 7.0 to 8.5wt%, which is the weight percentage in the R-T-B series permanent magnetic material.
7. The R-T-B system permanent magnetic material according to claim 6, wherein the Pr content is 7.123wt%, 7.372wt%, 7.496wt%, 7.503wt%, 7.523wt%, 7.622wt%, 7.623wt%, 7.624wt%, 7.628wt%, 7.629wt%, 7.748wt%, 7.750wt%, 7.752wt%, 7.753wt%, 7.992wt%, 7.995wt%, 8.000wt%, 8.252wt% or 8.253wt%, and percentages refer to weight percentages in the R-T-B system permanent magnetic material.
8. The R-T-B based permanent magnetic material according to claim 2, wherein the RH is Tb or Dy; the RH content is 1.5-6.0wt%, and the percentage refers to the weight percentage in the R-T-B series permanent magnetic material.
9. The R-T-B series permanent magnetic material according to claim 8, wherein the RH content is 1.987wt% or 2.012wt%, which is the weight percentage in the R-T-B series permanent magnetic material.
10. The R-T-B based permanent magnetic material according to claim 9, wherein when said R further includes Pr, the atomic percentage of B/(Pr + Nd) is 0.405 or more.
11. The R-T-B based permanent magnetic material according to claim 10, wherein when Pr is further included in R, the atomic percentage of B/(Pr + Nd) is 0.408 or 0.410.
12. The R-T-B system permanent magnetic material according to claim 2, wherein the Al content is 0.081wt%, 0.082wt%, 0.089wt%, 0.091wt%, 0.092wt%, 0.099wt%, 0.101wt%, 0.102wt%, 0.109wt%, 0.112wt%, 0.119wt%, 0.121wt%, or 0.123wt%, and percentages refer to weight percentages in the R-T-B system permanent magnetic material.
13. The R-T-B system permanent magnetic material of claim 2, wherein the content of Fe is 64.275wt%, 64.489wt%, 64.667wt%, 64.909wt%, 65.027wt%, 65.27wt%, 65.465wt%, 65.803wt%, 65.922wt%, 65.969wt%, 66.023wt%, 66.054wt%, 66.168wt%, 66.227wt%, 66.367wt%, 66.372wt%, 66.599wt%, 66.652wt%, 66.821wt%, 66.835wt%, 66.87wt%, 66.898wt%, 66.902wt%, 66.938wt%, 66.973wt%, 67.051wt%, 67.225wt%, 67.273wt%, 67.522wt%, 67.528wt%, 67.546wt%, 67.554wt%, 67.719wt%, 67.729wt%, 67.817wt%, 67.827wt%, 68.236wt% or 69.378wt%, and the percentage refers to a weight percentage in the R-T-B system permanent magnetic material.
14. The R-T-B based permanent magnetic material according to claim 2, wherein when the R-T-B based permanent magnetic material contains Ti, the content of Ti is 0.151wt%, 0.152wt%, 0.200wt%, 0.201wt%, 0.203wt%, 0.204wt%, 0.205wt%, 0.251wt%, 0.252wt%, 0.253wt%, 0.254wt%, or 0.256wt%, with percentages being weight percentages in the R-T-B based permanent magnetic material.
15. The R-T-B based permanent magnetic material according to claim 2, wherein when the R-T-B based permanent magnetic material contains Zr, the content of Zr is 0.202wt%, 0.203wt%, 0.261wt%, 0.262wt%, 0.302wt%, 0.303wt%, or 0.352wt%, and the percentage refers to the weight percentage in the R-T-B based permanent magnetic material.
16. The R-T-B based permanent magnetic material according to claim 2, wherein when the R-T-B based permanent magnetic material contains Nb, the content of Nb is 0.192wt%, 0.201wt%, 0.202wt%, 0.298wt%, 0.301wt%, 0.302wt%, 0.392wt%, 0.401wt%, 0.492wt%, or 0.503wt%, percentage being the weight percentage in the R-T-B based permanent magnetic material.
17. The R-T-B based permanent magnetic material according to claim 2, wherein when said R-T-B based permanent magnetic material contains Zr, said Zr content is 0.26wt% Zr ≦ Zr < (3.48B-2.67) wt%, the percentage referring to the weight percentage in said R-T-B based permanent magnetic material.
18. The R-T-B series permanent magnetic material according to any one of claims 1 to 17, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.45 to 33.1 wt%, Ga: 1.05-2 wt% wt%, Al: 0.08-0.125 wt%, B: 0.835-0.894 wt%, Fe: 64.2-69.5 wt%, Ti: 0.15-0.26 wt%, the percentage refers to the weight percentage in the R-T-B series permanent magnetic material;
or, the R-T-B series permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, 0.903wt% or more and less than 1.05wt% of Ga, Al: 0.08-0.125 wt%, B: 0.835-0.894 wt%, Fe: 64.2-69.5 wt%, Ti: 0.15-0.26 wt%, the percentage refers to the weight percentage in the R-T-B series permanent magnetic material.
19. The R-T-B series permanent magnetic material according to any one of claims 1 to 17, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, 1.05wt% or more and less than 1.25wt% of Ga, Al: 0.08-0.125 wt%, B: 0.835-0.894 wt%, Fe: 64.2 to 69.5wt%, Zr: 0.2-0.355 wt%; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
20. The R-T-B based permanent magnetic material of claim 19, wherein Zr content is 0.26wt% Zr ≦ Zr < (3.48B-2.67) wt%, percentage referring to weight percentage in said R-T-B based permanent magnetic material.
21. The R-T-B series permanent magnetic material according to any one of claims 1 to 17, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.45 to 33.1 wt%, Ga: 1.25-2 wt%, Al: 0.08-0.125 wt%, B: 0.835-0.894 wt%, Fe: 64.2 to 69.5wt%, Zr: 0.2-0.355 wt%; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
22. The R-T-B-based permanent magnetic material according to claim 21, wherein the Zr content is Zr ≥ 0.26 wt%; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
23. The R-T-B series permanent magnetic material according to any one of claims 1 to 17, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.45-33.1 wt%, 0.903wt% or more and less than 1.05wt% of Ga, Al: 0.08-0.125 wt%, B: 0.835-0.894 wt%, Fe: 64.2 to 69.5wt%, Zr: 0.2-0.355 wt%; the percentage refers to the weight percentage in the R-T-B series permanent magnet material.
24. The R-T-B based permanent magnetic material of claim 23, wherein Zr content is 0.26wt% Zr ≦ Zr < (3.48B-2.67) wt%, percentage referring to weight percentage in said R-T-B based permanent magnetic material.
25. A method for preparing the R-T-B series permanent magnetic material according to any one of claims 1 to 24, which comprises the following steps:
the melting liquid of the raw material composition of the R-T-B series permanent magnet material is subjected to casting, hydrogen crushing, forming, sintering and aging treatment; the melting liquid of the raw material composition of the R-T-B series permanent magnet material is prepared by melting in an alumina crucible;
the raw material composition of the R-T-B series permanent magnetic material comprises: r, Ga, B, Al and Fe, and also comprises one or more of Ti, Zr and Nb, and the content is as follows in percentage by weight:
r: 28.5-33.0 wt%; r is a rare earth element at least containing Nd;
Ga：0.9-2wt%；
Al：0.05-0.07wt%；
B：0.84-0.9wt%；
fe: 64.0 to 69.5 weight percent; wherein: when the raw material composition of the R-T-B series permanent magnet material contains Ti, the content of the Ti is 0.15-0.25 wt%; when the raw material composition of the R-T-B series permanent magnet material contains Zr, the content of Zr is 0.2-0.35 wt%; when the raw material composition of the R-T-B series permanent magnet material contains Nb, the content of the Nb is 0.2-0.5 wt%; the raw material composition of the R-T-B series permanent magnet material does not contain Co.
26. The method for preparing R-T-B based permanent magnetic material according to claim 25, wherein the content of R is 29.5 to 33.0wt%, the percentage being in weight percentage in the raw material composition of the R-T-B based permanent magnetic material;
and/or, the content of Nd is 21.0-25.0wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material;
and/or, the R also comprises Pr and/or heavy rare earth RH; and/or the content of Ga is 1.0wt%, 1.05wt%, 1.1wt%, 1.2wt%, 1.25wt%, 1.3wt%, 1.35wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt% or 1.8wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material;
or the content of Ga is 1.05-2 wt%, Ga is more than or equal to 0.9wt% and less than 1.05wt%, Ga is more than or equal to 1.05wt% and less than 1.25wt%, or, 1.25-2 wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material;
and/or, the content of Al is 0.06-0.07wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material;
and/or the raw material composition of the R-T-B series permanent magnetic material does not contain Cu;
and/or the content of B is 0.86wt% or 0.88wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material;
and/or the content of the Fe is 64.32-69.41wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material;
and/or, when the raw material composition of the R-T-B series permanent magnet material contains Ti, the content of the Ti is 0.20-0.25wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material;
and/or, when the raw material composition of the R-T-B series permanent magnetic material contains Zr, the content of Zr is 0.26-0.35wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material;
and/or, when the raw material composition of the R-T-B series permanent magnetic material contains Nb, the content of Nb is 0.3-0.5wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material;
or, when Zr is contained in the raw material composition of the R-T-B series permanent magnetic material, the content of Zr is more than or equal to 0.20wt% and less than (3.48B-2.67) wt%.
27. The method for preparing an R-T-B based permanent magnetic material according to claim 26, wherein the content of R is 29.5wt%, 30.0wt%, 30.5wt%, 31.0wt%, 32.0wt%, or 33.0wt%, which is a weight percentage in a raw material composition of the R-T-B based permanent magnetic material.
28. The method of claim 26, wherein the Nd is 21.375wt%, 22.0wt%, 22.125wt%, 22.5wt%, 22.75wt%, 22.875wt%, 23.25wt%, 24.0wt%, or 24.75wt%, which is a weight percentage in a raw material composition of the R-T-B system permanent magnetic material.
29. The method of claim 26, wherein the content of Pr is 2.5 to 12.0wt% in the raw material composition of the R-T-B system permanent magnetic material.
30. The method of claim 29, wherein the Pr content is 7.125wt%, 7.375wt%, 7.5wt%, 7.625wt%, 7.75wt%, 8.00wt%, or 8.25wt%, and the percentage is a weight percentage of the raw material composition of the R-T-B-based permanent magnetic material.
31. The method for producing an R-T-B based permanent magnetic material according to claim 26, wherein the RH is Tb or Dy; the RH content is 1.5-6.0wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
32. The method for preparing an R-T-B based permanent magnetic material according to claim 31, wherein the RH content is 2.0wt%, and the percentage is a weight percentage in a raw material composition of the R-T-B based permanent magnetic material.
33. The method of manufacturing an R-T-B based permanent magnetic material according to claim 32, wherein when R further includes Pr, the atomic percentage of B/(Pr + Nd) is not less than 0.405.
34. The method of manufacturing an R-T-B system permanent magnetic material of claim 26, wherein the content of Fe is 64.32wt%, 64.555wt%, 64.715wt%, 64.93wt%, 65.08wt%, 65.3wt%, 65.5wt%, 65.82wt%, 65.96wt%, 65.99wt%, 66.065 wt%, 66.11 wt%, 66.2wt%, 66.24wt%, 66.4wt%, 66.42wt%, 66.625wt%, 66.685wt%, 66.86wt%, 66.9wt%, 66.915 wt%, 66.935wt%, 66.94wt%, 66.98wt%, 67.01wt%, 67.08 wt%, 67.275wt%, 67.33wt%, 67.58 wt%, 67.585wt%, 67.6wt%, 67.76wt%, 67.86 wt%, 67.87wt%, 68.28wt%, or 69.41wt%, which is a weight percentage in a raw material composition of the R-T-B system permanent magnetic material.
35. The method of manufacturing an R-T-B-based permanent magnetic material according to claim 26, wherein when the raw material composition of the R-T-B-based permanent magnetic material contains Zr, the content of Zr is 0.26wt%, 0.3wt%, or 0.35wt%, and the percentage refers to a weight percentage in the raw material composition of the R-T-B-based permanent magnetic material.
36. The method of manufacturing an R-T-B based permanent magnetic material according to claim 26, wherein when the raw material composition of the R-T-B based permanent magnetic material contains Nb, the content of Nb is 0.3wt%, 0.4wt%, or 0.5wt%, and the percentage refers to the weight percentage in the raw material composition of the R-T-B based permanent magnetic material.
37. The method for producing an R-T-B based permanent magnetic material according to claim 26, wherein when Zr is contained in the raw material composition of the R-T-B based permanent magnetic material, the content of Zr is 0.20wt% Zr ≦ Zr < (3.48B-2.67) wt%.
38. The method for preparing an R-T-B series permanent magnetic material according to any one of claims 25 to 37, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.5 to 33.0wt%, Ga: 0.9-1.05 wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.9wt%, Fe: 64.0-69.5wt%, Ti: 0.15-0.25wt%, the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnetic material.
39. The method for preparing an R-T-B series permanent magnetic material according to any one of claims 25 to 37, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.5-33.0wt%, Ga is more than or equal to 1.05wt% and less than 1.25wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.9wt%, Fe: 64.0 to 69.5wt%, Zr: 0.2-0.35 wt%; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
40. The method for producing an R-T-B based permanent magnetic material according to claim 39, wherein Zr content is 0.26wt% or more and Zr < 3.48B-2.67 wt%; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
41. The method for preparing an R-T-B series permanent magnetic material according to any one of claims 25 to 37, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.5 to 33.0wt%, Ga: 1.25-2 wt%, Al: 0.05 to 0.07wt%, B: 0.84-0.9wt%, Fe: 64.0 to 69.5wt%, Zr: 0.2-0.35 wt%; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
42. The method for preparing R-T-B series permanent magnetic material according to claim 41, wherein the Zr content is more than or equal to 0.26 wt%; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
43. The method for preparing an R-T-B series permanent magnetic material according to any one of claims 25 to 37, wherein the R-T-B series permanent magnetic material comprises the following components: r: 28.5-33.0wt%, 0.9wt% or more and less than 1.05wt% of Ga, Al: 0.05 to 0.07wt%, B: 0.84-0.9wt%, Fe: 64.0 to 69.5wt%, Zr: 0.2-0.35 wt%; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
44. The method for producing an R-T-B based permanent magnetic material according to claim 43, wherein Zr content is 0.26wt% or more and Zr < 3.48B-2.67 wt%; the percentage refers to the weight percentage in the raw material composition of the R-T-B series permanent magnet material.
45. The method for producing an R-T-B based permanent magnetic material according to claim 25, wherein the melt of the raw material composition of the R-T-B based permanent magnetic material is produced by: smelting in a high-frequency vacuum induction smelting furnace; the vacuum degree of the smelting furnace is 5 multiplied by 10-2Pa; the smelting temperature is below 1500 ℃;
and/or the casting process is carried out according to the following steps: in Ar atmosphere, at 102DEG C/sec-104Cooling at the speed of DEG C/second; the cooling is realized by introducing cooling water into the roller;
and/or the hydrogen cracking process is carried out according to the following steps: performing hydrogen absorption, dehydrogenation and cooling treatment;
and/or, crushing after the hydrogen is broken;
and/or the forming method is a magnetic field forming method or a hot-pressing hot-deformation method;
and/or the sintering process is carried out according to the following steps: preheating, sintering and cooling under a vacuum condition to obtain the product; the preheating temperature is 300-600 ℃, and the preheating time is 1-2 h; the sintering temperature is 1040-1090 ℃; the sintering time is 5-10 h;
and/or the ageing treatment comprises primary ageing treatment and secondary ageing treatment.
46. The method for preparing R-T-B series permanent magnetic material as claimed in claim 45, wherein the water inlet temperature of the roller is less than or equal to 25 ℃.
47. The method of claim 46, wherein the temperature of the water supplied to the roller is 23.2 ℃, 23.4 ℃, 23.5 ℃, 23.6 ℃ or 23.7 ℃.
48. The method for producing an R-T-B based permanent magnetic material according to claim 45, wherein the pulverization process is jet mill pulverization; the jet mill pulverization is carried out under the nitrogen atmosphere with the content of oxidizing gas below 120 ppm; the pressure of a crushing chamber for crushing by the jet mill is 0.38 MPa; the jet mill pulverizing time is 3 hours.
49. The method for preparing an R-T-B series permanent magnetic material according to claim 45, wherein the preheating is carried out at 300 ℃ and 600 ℃ for 1 hour respectively.
50. The method of claim 45, wherein the sintering temperature is 1055 ℃, 1057 ℃, 1058 ℃, 1065 ℃, 1067 ℃, 1068 ℃, 1070 ℃, 1072 ℃, 1073 ℃, 1075 ℃, 1076 ℃, 1079 ℃, 1080 ℃, 1083 ℃, 1085 ℃ or 1090 ℃; the sintering time is 8 h.
51. The method for preparing R-T-B series permanent magnetic material as claimed in claim 45, wherein the temperature of the primary aging treatment is 860-960 ℃;
the temperature of the secondary aging treatment is 430-560 ℃.
52. The method for preparing R-T-B series permanent magnetic material as claimed in claim 51, wherein in the first-stage aging treatment, the temperature-raising rate of raising the temperature to 860 ℃ and 960 ℃ is 3-5 ℃/min; the time of the primary aging treatment is 3 hours;
the temperature of the secondary aging treatment is 450-490 ℃; in the secondary aging, the temperature is increased to the temperature of 430-560 ℃ at the temperature increase rate of 3-5 ℃/min; the treatment time of the secondary aging is 3 h.
53. The method for preparing R-T-B series permanent magnet material according to claim 52, wherein the temperature of the primary aging treatment is 900 ℃;
the temperature of the secondary aging treatment is 460 ℃, 470 ℃, 475 ℃, 477 ℃ or 480 ℃.
54. An R-T-B series permanent magnetic material prepared by the method for preparing the R-T-B series permanent magnetic material as claimed in any one of claims 25 to 53.
55. Use of a R-T-B series permanent magnetic material according to any one of claims 1 to 24 and 54 as an electronic component.
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