CN111627633B - R-T-B magnetic material and preparation method thereof - Google Patents

R-T-B magnetic material and preparation method thereof Download PDF

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Publication number
CN111627633B
CN111627633B CN202010599672.4A CN202010599672A CN111627633B CN 111627633 B CN111627633 B CN 111627633B CN 202010599672 A CN202010599672 A CN 202010599672A CN 111627633 B CN111627633 B CN 111627633B
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crushing
molding
sintering
hydrogen absorption
micro
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CN111627633A (en
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付刚
黄佳莹
黄清芳
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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    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/70—Wind energy
    • Y02E10/72—Wind turbines with rotation axis in wind direction

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  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses an R-T-B magnetic material, which is characterized by comprising the following components in percentage by weight: 27.42 wt.% to 33.00 wt.% R; r is rare earth element and contains Pr and RH(ii) a The Pr is more than or equal to 15.00 wt.%; said RHContaining Tb and/or Dy; 0.24 wt.% to 0.80 wt.% Cu; 0.19 wt.% to 0.30 wt.% Zr; 0 wt.% to 1.52 wt.% Al; 0.90 wt.% to 1.03 wt.% of B; and, 0.04 wt.% to 0.09 wt.% Ga or 0.28 wt.% to 1.50 wt.% Ga. The magnetic material has better remanence, coercive force, temperature coefficient and the like.

Description

R-T-B magnetic material and preparation method thereof
Technical Field
The invention relates to an R-T-B magnetic material and a preparation method thereof.
Background
By Nd2Fe14The neodymium iron boron (NdFeB) magnet material with the B as the main component has higher remanence, coercive force and maximum magnetic energy product, has excellent comprehensive magnetic performance, and is applied to the aspects of wind power generation, new energy automobiles, variable frequency household appliances and the like. At present, the rare earth component in the neodymium iron boron magnet material in the prior art is mainly neodymium, and only a small amount of praseodymium is contained. Although there are few reports in the prior art that a part of neodymium is replaced by praseodymium to improve the performance of the magnet material, the improvement degree is limited, and the improvement is not significant. On the other hand, the neodymium iron boron magnet material with better coercive force and remanence performance in the prior art also needs to depend on a large amount of addition of heavy rare earth elements, and has higher cost.
Disclosure of Invention
The invention aims to solve the technical problem that the existing R-T-B magnetic material is single in composition, and therefore, the invention provides the R-T-B magnetic material and the preparation method thereof.
The invention provides an R-T-B magnetic material, which is characterized by comprising the following components in percentage by weight:
27.42 wt.% to 33.00 wt.% R; r is rare earth element and contains Pr and RH(ii) a The Pr is more than or equal to 15.00 wt.%; said RHTb and/or Dy are contained;
0.24 wt.% to 0.80 wt.% Cu;
0.19 wt.% to 0.30 wt.% Zr;
0 wt.% to 1.52 wt.% Al;
0.90 wt.% to 1.03 wt.% of B;
and, 0.04 wt.% to 0.09 wt.% Ga, or, 0.28 wt.% to 1.50 wt.% Ga.
In one embodiment, the definitions, contents, and the like of some components in the magnetic material are as follows, and the definitions, contents, and the like of the components which are not referred to are as described in any of the preceding embodiments (hereinafter, referred to as "in one embodiment"): the content of R can be 29.50 wt.% to 31.00 wt.%, 30.77 wt.% to 30.88 wt.%, and 30.78 wt.%.
In one scheme, R consists of Pr and R HAnd (4) forming.
In a certain aspect, the R can further include Nd.
In one aspect, when R further comprises Nd, R is selected from Nd, Pr, and RHAnd (4) forming.
In a certain aspect, when R further comprises Nd, the amount of Nd can be 7.80 wt.% to 13.22 wt.%, or 9.20 wt.% to 12.68 wt.%, or 10.19 wt.%, 10.69 wt.%, or 11.56 wt.%.
In a certain embodiment, the content of Pr may be 15.00 wt.% to 22.29 wt.%, or 15.97 wt.% to 21.30 wt.%, or 18.68 wt.%, 19.22 wt.%, or 19.80 wt.%.
In a certain scheme, R isHThe content of (b) can be 0.50 wt.% to 1.10 wt.%, or 0.69 wt.% to 0.89 wt.%, or 0.85 wt.% to 0.86 wt.%.
In one embodiment, R isHThe mass ratio of R can be 0.016-0.033, 0.023-0.031, and 0.028-0.029.
Said RHAre conventional heavy rare earth elements in the art.
In one embodiment, R isHTb and/or Dy.
In one aspect, when R is saidHWhen Tb is contained, the content of Tb can be 0.20 wt.% to 0.85 wt.%, 0.28 wt.% to 0.69 wt.%, and 0.50 wt.% to 0.54 wt.%.
In one aspect, when R is saidHWhen Dy is contained, the content of Dy can be 0.20-1.10 wt.%, 0.32-0.57 wt.% or 0.49 wt.%.
In a certain embodiment, the content of Cu may be 0.35 wt.% to 0.68 wt.%, or 0.39 wt.% to 0.55 wt.%, or may be 0.50 wt.%.
In a certain embodiment, the content of Zr may be 0.25 wt.% to 0.28 wt.%, and may also be 0.26 wt.%.
In a certain embodiment, the Al content may be 0.15 wt.% to 0.80 wt.%, or 0.47 wt.% to 0.73 wt.%, or 0.66 wt.%.
In a certain scheme, the content of B may be 0.93 wt.% to 0.99 wt.%, or 0.95 wt.% to 0.98 wt.%.
In a certain embodiment, the Ga content may be 0.04 wt.% to 0.09 wt.%, and may be 0.05 wt.%.
In a certain embodiment, the Ga content may be 0.28 wt.% to 1.50 wt.%, or 0.31 wt.% to 0.45 wt.%.
In addition to the transition metals, T in the R-T-B magnetic material may also comprise other transition metals conventional in the art.
In one embodiment, the T may comprise Fe.
In a certain aspect, when T may include Fe, the Fe content may be 65.10 wt.% to 70.55 wt.%, 65.34 wt.% to 66.88 wt.%, 66.46 wt.%, 66.63 wt.%, or 66.64 wt.%.
In one embodiment, T may be comprised of Fe, Cu, and Zr.
In one embodiment, the R-T-B based magnetic material may be composed of the R, the Cu, the Zr, the Al, the B, the Ga, and the Fe.
The R-T-B magnetic material may contain inevitable impurities such as carbon.
In a certain scheme, the R-T-B series magnetic material comprises the following components in percentage by weight:
Figure BDA0002558134010000031
Figure BDA0002558134010000041
the numbers in the table are in wt.%.
The R-T-B magnetic material can be prepared according to the conventional method of the materials in the field.
In one embodiment, the R-T-B based magnetic material can be prepared according to a first method comprising the steps of: the raw materials are subjected to smelting, casting, powder making, molding, sintering and heat treatment to obtain the R-T-B magnetic material.
In the first method, a person skilled in the art can adjust the components of the target product R-T-B series magnetic material by combining losses, introduced impurities and the like during the preparation process to obtain the components of the raw materials.
In the first method, the smelting may be a smelting conventional in the art. The smelting temperature can be 1400-1500 ℃. The pressure of the smelting can be 5 x 10 -2Pa。
In the first method, the casting may be a casting conventional in the art. The casting may be performed in Ar gas. The casting pressure can be 5.5 ten thousandPa. The cooling rate of the casting may be 102DEG C/sec-104DEG C/sec.
In the first method, the powder preparation can be conventional powder preparation in the field. The powder preparation method comprises the steps of hydrogen absorption crushing and micro-crushing in sequence. The particle size of the D50 after pulverization can be 3.2-5.0 μm.
The hydrogen absorption fragmentation may be a hydrogen absorption fragmentation as is conventional in the art. The hydrogen absorption temperature for hydrogen absorption and crushing can be 20-25 ℃. The hydrogen absorption pressure of the hydrogen absorption crushing can be 0.15 MPa. The dehydrogenation temperature of hydrogen absorption and crushing can be 500-550 ℃.
The micronization may be any micronization conventional in the art. The micro-pulverization can be jet milling pulverization. The environment of the jet mill during the pulverization can be under nitrogen with oxygen content of below 150 ppm. The pressure of the jet mill during crushing can be 0.38 MPa.
Zinc stearate can also be added into the powder. The addition amount of the zinc stearate can be 0.12 percent of the weight of the mixed powder.
In the first method, the molding may be a molding conventionally used in the art. The molding method can be a magnetic field molding method.
When the molding method can be a magnetic field molding method, the magnetic field molding can be a two-time molding. When the magnetic field molding is carried out twice, the pressure at the time of primary molding may be 0.35ton/cm2The pressure during the second molding may be 1.3ton/cm2. When the magnetic field molding is twice molding, the magnetic field intensity during the primary molding can be 1.6T, and no magnetic field is generated during the secondary molding.
In the first method, the sintering may be sintering conventional in the art. The sintering can be three times. When the sintering is carried out for three times, the temperature during the primary sintering can be 300 ℃, the temperature during the secondary sintering can be 600 ℃, and the temperature during the third sintering can be 1060-1065 ℃. When the sintering is performed three times, the time for the first sintering may be 1 hour, the time for the second sintering may be 1 hour, and the time for the third sintering may be 6 hours.
In the first method, the heat treatment may be a heat treatment conventional in the art. The temperature of the heat treatment may be 460 to 480 ℃ (e.g., 470 ℃). The time for the heat treatment may be 3 hours. The heat treatment may be performed in Ar gas.
The invention also provides a preparation method of the R-T-B magnetic material, which comprises the following steps: smelting, casting, pulverizing, molding, sintering and heat treating the raw materials to obtain the R-T-B magnetic material;
the raw materials of the R-T-B series magnetic material comprise the following components in percentage by weight:
27.35 wt.% to 33.00 wt.% R; r is rare earth element and contains Pr and RH(ii) a The Pr is more than or equal to 15.00 wt.%; said RHContaining Tb and/or Dy;
0.24 wt.% to 0.80 wt.% Cu;
0.20 wt.% to 0.30 wt.% Zr;
0 wt.% to 1.52 wt.% Al;
0.90 wt.% to 1.03 wt.% of B;
and, 0.02 wt.% to 0.09 wt.% Ga, or, 0.28 wt.% to 1.50 wt.% Ga.
In the preparation method, the definitions, contents, preparation method parameters and the like of certain components in the raw materials are as follows, and the definitions, contents, preparation method parameters and the like of the components which are not referred to are as described in any of the previous schemes (hereinafter referred to as "in the preparation method"): the content of R can be 29.50 wt.% to 31.00 wt.%, 30.76 wt.% to 30.90 wt.%, and 30.80 wt.%.
In the preparation method, the R is formed by Pr and R HAnd (4) forming.
In the preparation method, R may further include Nd.
In the preparation method, when the R also contains Nd, the R is formed by Nd, Pr and RHAnd (4) forming.
In the preparation method, when R further includes Nd, the content of Nd may be 7.80 wt.% to 13.25 wt.%, or 9.20 wt.% to 12.70 wt.%, or may be 10.20 wt.%, 10.70 wt.%, or 11.50 wt.%.
In the preparation method, the content of Pr may be 15.00 wt.% to 22.30 wt.%, 15.95 wt.% to 21.30 wt.%, or 18.65 wt.%, 19.20 wt.%, or 19.80 wt.%.
In the preparation method, the RHThe content of (b) can be 0.50 wt.% to 1.10 wt.%, or 0.70 wt.% to 0.90 wt.%, or 0.85 wt.% to 0.86 wt.%.
In the preparation method, the RHThe mass ratio of R can be 0.016-0.033, 0.023-0.031, and 0.028-0.029.
Said RHAre conventional heavy rare earth elements in the art.
In the preparation method, the RHTb and/or Dy.
In the preparation method, when R isHWhen Tb is contained, the content of Tb can be 0.20 wt.% to 0.85 wt.%, 0.28 wt.% to 0.70 wt.%, and 0.50 wt.% to 0.54 wt.%.
In the preparation method, when R isHWhen Dy is contained, the content of Dy can be 0.20-1.10 wt.%, 0.32-0.57 wt.% or 0.50 wt.%.
In the preparation method, the content of Cu may be 0.35 wt.% to 0.68 wt.%, or 0.40 wt.% to 0.55 wt.%, or may be 0.50 wt.%.
In the preparation method, the content of Zr can be 0.25 wt.% to 0.28 wt.%, and can be 0.26 wt.%.
In the preparation method, the content of Al may be 0.15 wt.% to 0.80 wt.%, or 0.47 wt.% to 0.72 wt.%, or 0.66 wt.%.
In the preparation method, the content of B can be 0.93 wt.% to 0.99 wt.%, and can be 0.95 wt.% to 0.98 wt.%.
In the preparation method, the content of Ga can be 0.02 wt.% to 0.09 wt.%, and can be 0.05 wt.%.
In the preparation method, the content of Ga can be 0.28-1.50 wt.%, and can be 0.31-0.45 wt.%.
In addition to the transition metals, T in the R-T-B magnetic material may also comprise other transition metals conventional in the art.
In the preparation method, the T may comprise Fe.
In the preparation method, when T may include Fe, the content of Fe may be 65.11 wt.% to 70.61 wt.%, 65.33 wt.% to 66.88 wt.%, and may be 66.45 wt.%, 66.61 wt.% or 66.65 wt.%.
In the preparation method, the T can be composed of Fe, Cu and Zr.
In the above production method, the R-T-B based magnetic material may be composed of the R, the Cu, the Zr, the Al, the B, the Ga, and the Fe.
The raw material may contain inevitable impurities such as carbon element.
The R-T-B magnetic material may contain inevitable impurities such as carbon.
In the preparation method, the raw materials comprise the following components in percentage by weight:
numbering Nd Pr Dy Tb Ho Fe B Al Ga Cu Zr
1 9.2 21.3 0 0.5 0 66.65 0.93 0.8 0.02 0.4 0.2
2 10.2 19.8 0.2 0.7 0 66.61 0.99 0.47 0.28 0.5 0.25
3 7.8 22.3 0.5 0.2 0 66.45 0.98 0.72 0.45 0.35 0.25
4 12.70 15.95 0.57 0.28 0 66.88 0.98 1.52 0.31 0.55 0.26
5 11.50 15.00 0 0.85 0 70.61 0.95 0.15 0.05 0.68 0.20
6 13.25 18.65 1.10 0 0 65.33 1.03 0 0.09 0.24 0.30
7 10.70 19.20 0.32 0.54 0 65.11 0.90 0.66 1.50 0.80 0.28
The numbers in the table are in wt.%.
In the preparation method, the smelting can be the smelting conventional in the field. The smelting temperature can be 1400-1500 ℃. The pressure of the smelting can be 5 x 10-2Pa。
In the preparation method, the casting may be a casting conventional in the art. The casting may be performed in Ar gas. The casting pressure may be 5.5 ten thousand Pa. The cooling rate of the casting may be 10 2DEG C/sec-104DEG C/sec.
In the preparation method, the powder preparation can be conventional powder preparation in the field. The powder preparation method comprises the steps of hydrogen absorption crushing and micro-crushing in sequence. The particle size of the D50 after milling can be 3.2-5.0 μm.
The hydrogen absorption fragmentation may be a hydrogen absorption fragmentation as is conventional in the art. The hydrogen absorption temperature for hydrogen absorption and crushing can be 20-25 ℃. The hydrogen absorption pressure of the hydrogen absorption crushing can be 0.15 MPa. The dehydrogenation temperature of hydrogen absorption and crushing can be 500-550 ℃.
The micronization may be any micronization conventional in the art. The micro-pulverization can be jet milling pulverization. The environment of the jet mill during the pulverization can be under nitrogen with oxygen content of below 150 ppm. The pressure of the jet mill during crushing can be 0.38 MPa.
Zinc stearate can also be added into the powder. The addition amount of the zinc stearate can be 0.12 percent of the weight of the mixed powder.
In the preparation method, the molding may be a molding that is conventional in the art. The molding method can be a magnetic field molding method.
When the molding manner may be a magnetic field molding method, the magnetic field molding may be a two-time molding. When the magnetic field molding is carried out twice, the pressure at the time of primary molding may be 0.35ton/cm 2The pressure at the time of the second molding may be 1.3ton/cm2. When the magnetic field molding is twice molding, the magnetic field intensity during the primary molding can be 1.6T, and no magnetic field is generated during the secondary molding.
In the preparation method, the sintering may be sintering conventional in the art. The sintering can be three times. When the sintering is carried out for three times, the temperature during the primary sintering can be 300 ℃, the temperature during the secondary sintering can be 600 ℃, and the temperature during the third sintering can be 1060-1065 ℃. When the sintering is performed three times, the time for the first sintering may be 1 hour, the time for the second sintering may be 1 hour, and the time for the third sintering may be 6 hours.
In the preparation method, the heat treatment may be a heat treatment conventional in the art. The temperature of the heat treatment may be 460 to 480 ℃ (e.g., 470 ℃). The time for the heat treatment may be 3 hours. The heat treatment may be performed in Ar gas.
The invention also provides an R-T-B magnetic material which is prepared according to the preparation method of the R-T-B magnetic material.
Unless otherwise indicated, the wt.% in the claims and the description have the following meanings:
1. Wt.% in the raw material formulation refers to the percentage of an element relative to the sum of all raw materials;
2. the wt.% in the elemental analysis of the resulting material generally refers to the percentage of an element relative to the mass of the product to which the ICP-OES measured data (percentage of an element relative to the sum of all ICP-OES measured elements) is close.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the magnetic material of the invention has better remanence, coercive force, temperature coefficient and the like.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the invention thereto. 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.
Table 1 raw material formulation of example (number in wt.% in table)
Example numbering Nd Pr Dy Tb Ho Fe B Al Ga Cu Zr Nb Co
1 9.2 21.3 0 0.5 0 66.65 0.93 0.8 0.02 0.4 0.2 0 0
2 10.2 19.8 0.2 0.7 0 66.61 0.99 0.47 0.28 0.5 0.25 0 0
3 7.8 22.3 0.5 0.2 0 66.45 0.98 0.72 0.45 0.35 0.25 0 0
4 12.70 15.95 0.57 0.28 0 66.88 0.98 1.52 0.31 0.55 0.26 0 0
5 11.50 15.00 0 0.85 0 70.61 0.95 0.15 0.05 0.68 0.20 0 0
6 13.25 18.65 1.10 0 0 65.33 1.03 0 0.09 0.24 0.30 0 0
7 10.70 19.20 0.32 0.54 0 65.11 0.90 0.66 1.50 0.80 0.28 0 0
Example 1
(1) Smelting: according to the formulation shown in Table 1, 50-500kg of the prepared raw materials were put into an alumina crucible and heated in a high-frequency vacuum induction melting furnace at 5X 10 -2Vacuum melting is carried out in vacuum of Pa at the temperature of 1400 ℃ and 1500 ℃.
(2) The casting process comprises the following steps: ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen furnace for placing the quenched alloy at 20-25 ℃ by 5X 10-2Pa, introducing hydrogen with the purity of 99.9 percent into a hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, raising the temperature to 500-550 ℃ after fully absorbing hydrogen, fully dehydrogenating, cooling, and taking outHydrogen crushing the pulverized powder.
(4) A micro-grinding process: and (3) subjecting the powder obtained after the hydrogen crushing to jet milling for 3 hours under the condition that the pressure of a crushing chamber is 0.38MPa in a nitrogen atmosphere with the content of less than 150ppm to obtain fine powder, wherein D50 is 3.2-5.0 mu m.
(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 perpendicular orientation type, in an orientation magnetic field of 1.6T, at 0.35ton/cm2The zinc stearate-added powder 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 vacuum-sealed with a vacuum bag so as not to contact air, and then subjected to secondary molding (isostatic pressing) at 1.3ton/cm 2Secondary 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, sintering at 1060 deg.C for 6 hr, introducing Ar gas to make the pressure reach 0.1MPa, and cooling to room temperature.
(8) And (3) heat treatment process: the sintered body was heat-treated in high-purity Ar gas at 460 ℃ for 3 hours, cooled to room temperature, and taken out.
Example 2
(1) And (3) smelting: according to the formulation shown in Table 1, 50-500kg of the prepared raw materials are put into an alumina crucible and are smelted in a high-frequency vacuum induction smelting furnace at the temperature of 5 multiplied by 10-2Vacuum melting is carried out in vacuum of Pa at the temperature of 1400 ℃ and 1500 ℃.
(2) The casting process comprises the following steps: ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen furnace for placing the quenched alloy at 20-25 ℃ by 5X 10-2Pa, introducing hydrogen with the purity of 99.9 percent into a hydrogen breaking furnace, maintaining the pressure of the hydrogen at 0.15MPa, fully absorbing the hydrogen, raising the temperature to 500-550 ℃, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: and (3) subjecting the powder obtained after the hydrogen crushing to jet milling for 3 hours under the condition that the pressure of a crushing chamber is 0.38MPa in a nitrogen atmosphere with the content of less than 150ppm to obtain fine powder, wherein D50 is 3.2-5.0 mu m.
(5) Adding zinc stearate into the powder crushed by the jet mill, wherein the addition amount of the zinc stearate is 0.12 percent of the weight of the mixed powder, and 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 perpendicular 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 vacuum-sealed with a vacuum bag 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, sintering at 1065 deg.C for 6 hr, introducing Ar gas to make pressure reach 0.1MPa, and cooling to room temperature.
(8) And (3) heat treatment process: the sintered body was heat-treated in high-purity Ar gas at 470 ℃ for 3 hours, cooled to room temperature, and taken out.
Example 3
(1) And (3) smelting: according to the formulation shown in Table 1, 50-500kg of the prepared raw materials are put into an alumina crucible and are smelted in a high-frequency vacuum induction smelting furnace at the temperature of 5 multiplied by 10-2Vacuum melting is carried out in vacuum of Pa at the temperature of 1400 ℃ and 1500 ℃.
(2) The casting process comprises the following steps: ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen furnace for placing the quenched alloy at 20-25 ℃ by 5X 10-2Pa, introducing hydrogen with the purity of 99.9 percent into a hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, raising the temperature to 500-550 ℃, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: and (3) subjecting the powder obtained after the hydrogen crushing to jet milling for 3 hours under the condition that the pressure of a crushing chamber is 0.38MPa in a nitrogen atmosphere with the content of less than 150ppm to obtain fine powder, wherein D50 is 3.2-5.0 mu m.
(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 perpendicular 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 vacuum-sealed with a vacuum bag 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, sintering at 1060 deg.C for 6 hr, introducing Ar gas to make the pressure reach 0.1MPa, and cooling to room temperature.
(8) And (3) heat treatment process: the sintered body was heat-treated in high-purity Ar gas at 480 ℃ for 3 hours, cooled to room temperature, and taken out.
Example 4
(1) And (3) smelting: according to the formulation shown in Table 1, 50-500kg of the prepared raw materials are put into an alumina crucible and are smelted in a high-frequency vacuum induction smelting furnace at the temperature of 5 multiplied by 10-2Vacuum melting is carried out in vacuum of Pa at the temperature of 1400 ℃ and 1500 ℃.
(2) The casting process comprises the following steps: ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees 2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen furnace for placing the quenched alloy at 20-25 ℃ by 5X 10-2Pa, introducing hydrogen with the purity of 99.9 percent into a hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, raising the temperature to 500-550 ℃, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: and (3) subjecting the powder obtained after the hydrogen crushing to jet milling for 3 hours under the condition that the pressure of a crushing chamber is 0.38MPa in a nitrogen atmosphere with the content of less than 150ppm to obtain fine powder, wherein D50 is 3.2-5.0 mu m.
(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 perpendicular 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 vacuum-sealed with a vacuum bag so as not to contact air, and then subjected to secondary molding (isostatic pressing) at 1.3ton/cm 2Is subjected to secondary forming under pressure.
(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, sintering at 1060 deg.C for 6 hr, introducing Ar gas to make the pressure reach 0.1MPa, and cooling to room temperature.
(8) And (3) heat treatment process: the sintered body was heat-treated in high-purity Ar gas at 460 ℃ for 3 hours, cooled to room temperature, and taken out.
Example 5
(1) And (3) smelting: according to the formula shown in Table 1Putting 50-500kg of prepared raw materials into a crucible made of alumina, and performing high-frequency vacuum induction melting in a high-frequency vacuum induction melting furnace at a speed of 5 multiplied by 10-2Vacuum melting is carried out in vacuum of Pa at the temperature of 1400 ℃ and 1500 ℃.
(2) The casting process comprises the following steps: ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen furnace for placing the quenched alloy at 20-25 ℃ by 5X 10-2Pa, introducing hydrogen with the purity of 99.9 percent into a hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, raising the temperature to 500-550 ℃, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: and (3) in a nitrogen atmosphere with a content of 150ppm or less, pulverizing the powder after hydrogen decrepitation for 3 hours by jet milling under a condition that the pressure in the pulverizing chamber is 0.38MPa to obtain fine powder, wherein D50 is 3.2-5.0 μm.
(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 perpendicular 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 vacuum-sealed with a vacuum bag so as not to contact air, and then subjected to secondary molding (isostatic pressing) at 1.3ton/cm2Is subjected to secondary forming under pressure.
(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, sintering at 1060 deg.C for 6 hr, introducing Ar gas to make the pressure reach 0.1MPa, and cooling to room temperature.
(8) And (3) heat treatment process: the sintered body was heat-treated in high-purity Ar gas at 460 ℃ for 3 hours, cooled to room temperature, and taken out.
Example 6
(1) And (3) smelting: according to the formulation shown in Table 1, 50-500kg of the prepared raw materials are put into an alumina crucible and are smelted in a high-frequency vacuum induction smelting furnace at the temperature of 5 multiplied by 10-2Vacuum melting is carried out in vacuum of Pa at the temperature of 1400 ℃ and 1500 ℃.
(2) The casting process comprises the following steps: ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing: vacuumizing the hydrogen furnace for placing the quenched alloy at 20-25 ℃ by 5X 10-2Pa, introducing hydrogen with the purity of 99.9 percent into a hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, raising the temperature to 500-550 ℃, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: and (3) subjecting the powder obtained after the hydrogen crushing to jet milling for 3 hours under the condition that the pressure of a crushing chamber is 0.38MPa in a nitrogen atmosphere with the content of less than 150ppm to obtain fine powder, wherein D50 is 3.2-5.0 mu m.
(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 perpendicular 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 vacuum-sealed with a vacuum bag 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 ℃ and 600 ℃ for 1 hour, and then sintering at 1060 ℃ for 6 hoursThen Ar gas is introduced to make the air pressure reach 0.1MPa, and then the mixture is cooled to the room temperature.
(8) And (3) heat treatment process: the sintered body was heat-treated in high-purity Ar gas at 460 ℃ for 3 hours, cooled to room temperature, and taken out.
Example 7
(1) And (3) smelting: according to the formulation shown in Table 1, 50-500kg of the prepared raw materials are put into an alumina crucible and are smelted in a high-frequency vacuum induction smelting furnace at the temperature of 5 multiplied by 10-2Vacuum melting is carried out in vacuum of Pa at the temperature of 1400 ℃ and 1500 ℃.
(2) The casting process comprises the following steps: ar gas was introduced into the vacuum-melted melting furnace to make the gas pressure 5.5 ten thousand Pa, and then the casting was carried out at 10 degrees centigrade 2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen furnace for placing the quenched alloy at 20-25 ℃ by 5X 10-2Pa, introducing hydrogen with the purity of 99.9 percent into a hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, raising the temperature to 500-550 ℃, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: and (3) subjecting the powder obtained after the hydrogen crushing to jet milling for 3 hours under the condition that the pressure of a crushing chamber is 0.38MPa in a nitrogen atmosphere with the content of less than 150ppm to obtain fine powder, wherein D50 is 3.2-5.0 mu m.
(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 perpendicular 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 vacuum-sealed with a vacuum bag so as not to contact air, and then subjected to secondary molding (isostatic pressing) at 1.3ton/cm 2Is subjected to secondary forming under pressure.
(7) And (3) sintering: will be provided withThe 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, sintering at 1060 deg.C for 6 hr, introducing Ar gas to make the pressure reach 0.1MPa, and cooling to room temperature.
(8) And (3) heat treatment process: the sintered body was heat-treated in high-purity Ar gas at 460 ℃ for 3 hours, cooled to room temperature, and taken out.
Effect example 1
The R-T-B magnetic materials obtained in examples 1 to 7 were used to determine their components and magnetic properties.
(1) Component determination: each component was measured using a high-frequency inductively coupled plasma emission spectrometer (ICP-OES). The component detection results are shown in table 2:
TABLE 2 ICP test results (wt%)
Figure BDA0002558134010000161
(2) Evaluation of magnetic Properties: the material 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 results of the magnetic property measurements are shown in Table 3:
TABLE 3 results of magnetic properties
Figure BDA0002558134010000171
Description of the drawings: the temperature coefficient is an absolute value.

Claims (9)

1. An R-T-B magnetic material, characterized in that, in weight percent,
the R-T-B magnetic material comprises the following components:
Figure DEST_PATH_IMAGE002
wherein the units of numbers are wt.%;
Wherein, the magnetic performance of the magnetic materials with the numbers 1-7 is correspondingly the following magnetic performance effect;
Figure DEST_PATH_IMAGE004
2. the R-T-B based magnetic material according to claim 1, wherein said R-T-B based magnetic material is prepared according to a first method comprising the steps of: the raw materials are subjected to smelting, casting, powder making, molding, sintering and heat treatment to obtain the R-T-B magnetic material.
3. The R-T-B system magnetic material according to claim 2, wherein said R-T-B system magnetic material is composed of said R, said Cu, said Zr, said Al, said B, said Ga, and said Fe;
and/or the smelting temperature is 1400-1500 ℃;
and/or the pressure of the smelting is 5 x 10-2Pa；
And/or, said casting is carried out in Ar gas;
and/or the pressure of the casting is 5.5 ten thousand Pa;
and/or the cooling speed of the casting is 102DEG C/sec-104DEG C/sec;
and/or the powder preparation mode comprises hydrogen absorption crushing and micro crushing in sequence;
and/or the particle size of the D50 after powder preparation is 3.2-5.0 μm;
and/or the molding mode is a magnetic field molding method;
and/or, the sintering is three times;
And/or the temperature of the heat treatment is 460-480 ℃;
and/or, the time of the heat treatment is 3 hours;
and/or, the heat treatment is carried out in Ar gas.
4. The R-T-B magnetic material according to claim 3,
when the powder preparation mode sequentially comprises hydrogen absorption crushing and micro crushing, the hydrogen absorption temperature of the hydrogen absorption crushing is 20-25 ℃;
and/or when the powder preparation mode comprises hydrogen absorption crushing and micro crushing in sequence, the hydrogen absorption pressure of the hydrogen absorption crushing is 0.15 MPa;
and/or when the powder preparation mode comprises hydrogen absorption crushing and micro crushing in sequence, the dehydrogenation temperature of the hydrogen absorption crushing is 500-550 ℃;
and/or when the powder preparation mode sequentially comprises hydrogen absorption crushing and micro-crushing, the micro-crushing is jet mill crushing; the environment of the jet mill during crushing is under nitrogen with oxygen content of below 150 ppm; the pressure of the jet mill during crushing is 0.38 MPa;
and/or, when the powder preparation mode sequentially comprises hydrogen absorption crushing and micro-crushing, zinc stearate is added into the powder preparation; the addition amount of the zinc stearate is 0.12 percent of the weight of the mixed powder;
And/or, when the molding mode is a magnetic field molding method, the magnetic field molding is two-time molding: the pressure at the time of primary molding was 0.35ton/cm2The pressure at the time of the second molding was 1.3 ton/cm2；
And/or, when the molding mode is a magnetic field molding method, the magnetic field molding is a two-time molding: the magnetic field intensity during primary molding is 1.6T, and no magnetic field is generated during secondary molding;
and/or when the sintering is carried out for three times, the temperature during the primary sintering is 300 ℃, the temperature during the secondary sintering is 600 ℃, and the temperature during the third sintering is 1060-1065 ℃;
and/or, when the sintering is carried out for three times, the time for the primary sintering is 1 hour, the time for the secondary sintering is 1 hour, and the time for the third sintering is 6 hours;
and/or the temperature of the heat treatment is 470 ℃.
5. A preparation method of an R-T-B magnetic material comprises the following steps: smelting, casting, pulverizing, molding, sintering and heat treating the raw materials to obtain the R-T-B magnetic material;
in terms of weight percentage, the weight percentage of the active carbon is,
the R-T-B series magnetic material comprises the following raw materials:
Figure DEST_PATH_IMAGE006
wherein the units of numbers are wt.%;
Wherein, the magnetic performance of the magnetic materials with the numbers 1-7 is correspondingly the following magnetic performance effect;
Figure 10952DEST_PATH_IMAGE004
6. the method as claimed in claim 5, wherein the smelting temperature is 1400-1500 ℃;
and/or the pressure of the smelting is 5 x 10-2Pa；
And/or, said casting is carried out in Ar gas;
and/or the pressure of the casting is 5.5 ten thousand Pa;
and/or the cooling speed of the casting is 102DEG C/sec-104DEG C/sec;
and/or the powder preparation mode comprises hydrogen absorption crushing and micro crushing in sequence;
and/or the particle size of the D50 after powder preparation is 3.2-5.0 μm;
and/or the molding mode is a magnetic field molding method;
and/or, the sintering is three times;
and/or the temperature of the heat treatment is 460-480 ℃;
and/or, the time of the heat treatment is 3 hours;
and/or, the heat treatment is carried out in Ar gas.
7. The process according to claim 6, wherein when the pulverization is carried out by hydrogen absorption pulverization and micro pulverization in this order, the hydrogen absorption temperature of the hydrogen absorption pulverization is 20 to 25 ℃;
and/or when the powder preparation mode comprises hydrogen absorption crushing and micro crushing in sequence, the hydrogen absorption pressure of the hydrogen absorption crushing is 0.15 MPa;
And/or when the powder preparation mode comprises hydrogen absorption crushing and micro crushing in sequence, the dehydrogenation temperature of the hydrogen absorption crushing is 500-550 ℃;
and/or when the powder preparation mode sequentially comprises hydrogen absorption crushing and micro-crushing, the micro-crushing is jet mill crushing;
and/or, when the powder preparation mode sequentially comprises hydrogen absorption crushing and micro-crushing, zinc stearate is added into the powder preparation;
and/or, when the molding mode is a magnetic field molding method, the magnetic field molding is twice molding;
and/or when the sintering is carried out for three times, the temperature during the primary sintering is 300 ℃, the temperature during the secondary sintering is 600 ℃, and the temperature during the third sintering is 1060-1065 ℃;
and/or, when the sintering is carried out for three times, the time for the primary sintering is 1 hour, the time for the secondary sintering is 1 hour, and the time for the third sintering is 6 hours;
and/or the temperature of the heat treatment is 470 ℃.
8. The method according to claim 7, wherein when the pulverization is carried out by hydrogen-absorption pulverization and micro-pulverization in this order, the micro-pulverization is carried out by jet milling in an atmosphere of nitrogen gas containing oxygen in an amount of 150ppm or less;
And/or when the powder preparation mode sequentially comprises hydrogen absorption crushing and micro crushing, the micro crushing is jet mill crushing, and the pressure of the jet mill crushing is 0.38 MPa;
and/or, when the powder preparation mode comprises hydrogen absorption crushing and micro crushing in sequence, zinc stearate is also added into the powder preparation; the addition amount of the zinc stearate is 0.12 percent of the weight of the mixed powder;
and/or, when the molding mode is a magnetic field molding method, the magnetic field molding is a two-time molding: the pressure at the time of primary molding was 0.35ton/cm2And the pressure at the time of the second molding was 1.3 ton/cm2；
And/or, when the molding mode is a magnetic field molding method, the magnetic field molding is a two-time molding: the magnetic field intensity during primary molding is 1.6T, and no magnetic field is generated during secondary molding;
and/or when the sintering is carried out for three times, the temperature during the first sintering is 300 ℃, the temperature during the second sintering is 600 ℃, and the temperature during the third sintering is 1075 ℃.
9. An R-T-B magnetic material produced by the method for producing an R-T-B magnetic material according to any one of claims 5to 8.
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CN110957092A (en) * 2019-12-19 2020-04-03 厦门钨业股份有限公司 R-T-B series magnet material, raw material composition, preparation method and application

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DE102017222060A1 (en) * 2016-12-06 2018-06-07 Tdk Corporation Permanent magnet based on R-T-B
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CN110828089A (en) * 2019-11-21 2020-02-21 厦门钨业股份有限公司 Neodymium-iron-boron magnet material, raw material composition, preparation method and application
CN110853855A (en) * 2019-11-21 2020-02-28 厦门钨业股份有限公司 R-T-B series permanent magnetic material and preparation method and application thereof
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