CN111243811B - Neodymium-iron-boron material and preparation method and application thereof - Google Patents

Neodymium-iron-boron material and preparation method and application thereof Download PDF

Info

Publication number
CN111243811B
CN111243811B CN202010134686.9A CN202010134686A CN111243811B CN 111243811 B CN111243811 B CN 111243811B CN 202010134686 A CN202010134686 A CN 202010134686A CN 111243811 B CN111243811 B CN 111243811B
Authority
CN
China
Prior art keywords
percentage
mass
content
neodymium
raw material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010134686.9A
Other languages
Chinese (zh)
Other versions
CN111243811A (en
Inventor
付刚
刘少伟
黄佳莹
黄清芳
许德钦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujian Jinlong Rare Earth Co ltd
Original Assignee
Xiamen Tungsten Co Ltd
Fujian Changting Jinlong Rare Earth Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xiamen Tungsten Co Ltd, Fujian Changting Jinlong Rare Earth Co Ltd filed Critical Xiamen Tungsten Co Ltd
Priority to CN202010134686.9A priority Critical patent/CN111243811B/en
Publication of CN111243811A publication Critical patent/CN111243811A/en
Priority to PCT/CN2021/077199 priority patent/WO2021169905A1/en
Application granted granted Critical
Publication of CN111243811B publication Critical patent/CN111243811B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0575Alloys 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
    • H01F1/0577Alloys 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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
    • H01F41/0266Moulding; Pressing

Abstract

The invention discloses a neodymium iron boron material and a preparation method and application thereof. The raw material composition of the neodymium iron boron material comprises the following components in percentage by mass: r: 28.5 to 33.0 percent; r is a rare earth element at least containing Nd; cu: 0.45-2% but not 0.45%; b: 0.84-0.94%; al: 0.05-0.07%; co: less than or equal to 2.5 percent but not 0; fe: 62-70%; n: one or more of Ti, Zr and Nb; when N contains Ti, the content of Ti is 0.15-0.25%; when N contains Zr, the content of Zr is 0.2-0.35%; when the N contains Nb, the content of Nb is 0.2-0.5%; the percentage is the mass percentage of each component in the total mass of the raw material composition. The neodymium iron boron material has better magnetic property, and the magnetic property of products in the same batch is uniform.

Description

Neodymium-iron-boron material and preparation method and application thereof
Technical Field
The invention relates to a neodymium iron boron 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 increase the remanence of R-T-B-based sintered magnets, it is generally necessary to decrease the B content. However, when the content of B is at a low level, R is formed2T17And (4) phase(s). And R is2T17Has no room temperature uniaxial anisotropy, thereby making the magnetThe performance of the body deteriorates.
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, under the condition of not adding or adding a small amount of heavy rare earth, how to prepare the neodymium iron boron material with high coercivity and high remanence by adopting a low B system (B < 5.88 at%) is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to overcome the defect of poor magnet performance caused by a low B system (B is less than 5.88 at%) in the prior art, and provides a neodymium iron boron material and a preparation method and application thereof.
The invention discovers for the first time that in the prior art, the coercive force of an R-T-B series magnet product of a low B system is improved in a small test, but the magnet still has the defect of nonuniform performance in industrial production, such as the prior Chinese patent CN 110619984A. In order to make the R-T-B series magnet product suitable for large-scale industrial production, the inventor finds that the neodymium iron boron material with excellent magnet performance and uniform performance can be prepared by controlling the content of Al and properly matching Cu in a certain range with other elements through a large amount of research and experiments.
In order to achieve the purpose, the invention provides the following technical scheme:
one of the technical schemes provided by the invention is as follows:
a raw material composition of a neodymium iron boron material comprises the following components in percentage by mass:
r: 28.5 to 33.0 wt%; r is a rare earth element at least containing Nd;
cu: 0.45 to 2 wt% but not 0.45 wt%;
B:0.84~0.94wt%;
Al:0.05~0.07wt%;
co: less than or equal to 2.5 wt% but not 0;
Fe:62~70wt%;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.15-0.25 wt%;
when N contains Zr, the content of Zr is 0.2-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.5 wt%;
the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the present invention, in the raw material composition, the content of R is preferably 28.5 to 32.5 wt%, for example, 29 wt%, 29.5 wt%, 30.5 wt%, 31 wt%, 31.5 wt%, 32 wt% or 32.5 wt%, more preferably 30.5 to 32 wt%, which is a mass percentage based on the total mass of the raw material composition.
Wherein, in the raw material composition, the content of the Nd is preferably 19 to 24 wt%, such as 19 wt%, 20.8 wt%, 21.5 wt%, 22.2 wt%, 22.3 wt%, 22.5 wt%, 22.9 wt%, 23.3 wt%, 23.9 wt%; alternatively, the content of Nd is preferably 28 to 32 wt%, for example, 28.05 wt%, 28.07 wt%, 28.5 wt%, 28.57 wt%, 29.06 wt%, 29.07 wt%, 30.04 wt%, 30.54 wt%, 30.75 wt%, 31.25 wt%, in mass% based on the total mass of the raw material composition.
In the present invention, Ga is preferably not contained in the raw material composition.
In the invention, in the raw material composition, the R may further include Pr.
Wherein, when Pr is included in the R, the Pr content may be < 0.2 at% or > 8 at%; at% is the atomic percentage in the feedstock composition.
Wherein, when the R includes Pr, the content of Pr is preferably less than 1.0 wt% and not 0, more preferably 0.1 to 0.5 wt%, such as 0.25 wt%, 0.43 wt%, 0.44 wt%, 0.45 wt%, 0.46 wt%, 0.47 wt%, 0.49 wt%; or the Pr content is preferably 6 to 15 wt%, more preferably 7 to 12 wt%, such as 7.1 wt%, 7.2 wt%, 9.2 wt%, 9.3 wt%, 9.5 wt%, 9.6 wt%, 10.2 wt%, 10.5 wt%, 11.2 wt%; the percentage is the mass percentage of the total mass of the raw material composition.
In the present invention, the raw material composition may not contain heavy rare earth elements, and may also achieve a level of magnetic properties comparable to or even better than those of the prior art magnet materials. Alternatively, the raw material composition may further include RH, which is a heavy rare earth element.
When the raw material composition contains RH, the content of RH is preferably 1.5 to 6 wt%, more preferably 1 to 2.5 wt%, and the percentage is the mass percentage of the total mass of the raw material composition.
Wherein, the RH preferably includes one or more of Dy, Tb and Ho.
When the RH includes Dy, the content of Dy is preferably 1 to 2.5 wt%, for example, 2 wt%, in terms of mass percentage based on the total mass of the raw material composition.
When the RH includes Tb, the content of Tb is preferably 1 to 2.5 wt%, for example 2 wt%, and the percentage is the mass percentage of the total mass of the raw material composition.
In the present invention, the content of B in the raw material composition is preferably 0.85 to 0.94 wt%, for example, 0.85 wt%, 0.87 wt%, 0.88 wt%, 0.89 wt%, 0.9 wt%, 0.91 wt%, 0.92 wt%, 0.93 wt%, 0.94 wt%, which is a mass percentage based on the total mass of the raw material composition.
In the present invention, in the raw material composition, the atomic percentage of R and the atomic percentage of B preferably satisfy the following relationship: B/R is not less than 0.38, wherein B is the atomic percent of B in the raw material composition, and R is the atomic percent of R in the raw material composition.
In the present invention, in the raw material composition, when the R further includes Pr, it is preferable that the B and the Nd satisfy the following relational expression: B/(Pr + Nd) ≥ 0.405, wherein B refers to the atomic percentage of B in the raw material composition, Pr refers to the atomic percentage of Pr in the raw material composition, and Nd refers to the atomic percentage of Nd in the raw material composition.
In the present invention, the content of Cu in the raw material composition is preferably 0.6 wt% to 2 wt%, for example, 0.6 wt%, 0.75 wt%, 0.85 wt%, 0.91 wt%, 1.1 wt%, 1.15 wt%, 1.25 wt%, 1.45 wt%, 1.46 wt%, 1.6 wt%, 1.75 wt%, 1.8 wt%, 1.95 wt%, 2 wt%, more preferably 1 to 2 wt%, in percentage by mass based on the total mass of the raw material composition.
In the present invention, the content of Al in the raw material composition is preferably 0.06 to 0.07 wt%, for example, 0.06 wt%, 0.07 wt%, and more preferably 0.06 wt%, with the percentage being the mass percentage of the total mass of the raw material composition.
In the present invention, the content of Co in the raw material composition is preferably 0.5 to 2.5 wt%, for example, 0.5 wt%, 0.75 wt%, 0.8 wt%, 0.9 wt%, 1.00 wt%, 1.2 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, more preferably 1.00 to 2 wt%, and the percentage is a mass percentage based on the total mass of the raw material composition.
In the present invention, the content of Fe in the raw material composition is preferably 64 to 69 wt%, for example, 64.75 wt%, 64.91 wt%, 65.19 wt%, 65.47 wt%, 65.73 wt%, 65.85 wt%, 66.30 wt%, 66.54 wt%, 66.98 wt%, 67.35 wt%, 67.99 wt%, 68.91 wt%, which is a mass percentage of the total mass of the raw material composition.
In the present invention, when the N includes Ti in the raw material composition, the content of Ti is preferably 0.2 to 0.25 wt%, for example, 0.2 wt%, 0.25 wt%, and the percentage is a mass percentage based on the total mass of the raw material composition.
In the present invention, when the N includes Zr in the raw material composition, the Zr content is preferably 0.25 to 0.35 wt%, for example, 0.28 wt%, 0.30 wt%, 0.32 wt%, 0.35 wt%, and the percentage is a mass percentage based on the total mass of the raw material composition.
In the present invention, when the N contains Zr in the raw material composition, the Zr content is preferably 0.26 wt% or more and Zr < (3.48B-2.67) wt%, where B means a mass percentage of the B to the total mass of the raw material composition.
In the present invention, when the N includes Nb, the content of Nb in the raw material composition is preferably 0.2 to 0.3 wt%, for example, 0.25 wt%, 0.30 wt%, and the percentage is a mass percentage based on the total mass of the raw material composition.
In the present invention, when the N includes Ti and Nb in the raw material composition, the atomic percentage of Ti or Nb is preferably not less than 0.55 at%.
In the invention, the raw material composition of the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.06~0.07wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.2-0.25 wt%;
when N contains Zr, the content of Zr is 0.25-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.3 wt%;
the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the invention, the raw material composition of the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element comprising Nd and Pr;
pr: 0.1-0.5% or 6-15%;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.06~0.07wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.2-0.25 wt%;
when N contains Zr, the content of Zr is 0.25-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.3 wt%;
the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the invention, the raw material composition of the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.06~0.07wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
Ti:0.2~0.25wt%;
the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the invention, the raw material composition of the neodymium iron boron material preferably comprises the following components by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.06~0.07wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
Zr:0.25~0.35wt%;
the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the invention, the raw material composition of the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.06~0.07wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
Nb:0.2~0.3wt%;
the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 28.07 wt%; 0.43 wt% of Pr; 0.60 wt% of Cu; 0.06 wt% of Al; 0.50 wt% of Co; 0.15 wt% of Ti; b0.84 wt%; fe 69.35 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 28.57 wt%; 0.43 wt% of Pr; 0.85 wt% of Cu; 0.06 wt% of Al; 1.00 wt% of Co; 0.20 wt% of Ti; 0.90 wt% of B; fe 67.99 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 30.04 wt% of Nd; 0.46 wt% of Pr; cu 0.91 wt%; 0.07 wt% of Al; 1.50 wt% of Co; 0.25 wt% of Ti; b0.92 wt%; fe 65.85 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 30.75 wt% of Nd; 0.25 wt% of Pr; 1.10 wt% of Cu; 0.06 wt% of Al; 2.00 wt% of Co; 0.15 wt% of Ti; b0.94 wt%; fe 64.75 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 31.25 wt%; 0.25 wt% of Pr; 1.25 wt% of Cu; 0.06 wt% of Al; 2.50 wt% of Co; 0.25 wt% of Ti; b0.92 wt%; fe 63.52 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 20.80 wt% of Nd; pr 11.20 wt%; 1.46 wt% of Cu; 0.07 wt% of Al; 0.50 wt% of Co; 0.15 wt% of Ti; b0.91 wt%; fe 64.91 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 22.30 wt%; pr 10.20 wt%; 1.75 wt% of Cu; 0.06 wt% of Al; 1.00 wt% of Co; 0.20 wt% of Ti; b0.93 wt%; fe 63.56 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 19.00 wt%; pr 9.50 wt%; 1.80 wt% of Cu; 0.05 wt% of Al; 1.50 wt% of Co; 0.25 wt% of Ti; b0.92 wt%; fe 66.98 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 22.50 wt%; pr 10.50 wt%; 1.95 wt% of Cu; 0.06 wt% of Al; 1.50 wt% of Co; 0.15 wt% of Ti; b0.84 wt%; fe 62.5 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 22.20 wt%; pr 9.30 wt%; cu 2.00 wt%; 0.06 wt% of Al; 2.5 wt% of Co; 0.25 wt% of Ti; b0.88 wt%; fe 62.81 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 28.07 wt%; 0.43 wt% of Pr; 0.60 wt% of Cu; 0.07 wt% of Al; 0.80 wt% of Co; 0.20 wt% of Zr; b0.92 wt%; fe 68.91 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 29.06 wt%; 0.44 wt% of Pr; cu 2.00 wt%; 0.06 wt% of Al; 0.75 wt% of Co; 0.24 wt% of Zr; b0.91 wt%; fe 66.54 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 30.54 wt% of Nd; 0.47 wt% of Pr; 1.15 wt% of Cu; 0.06 wt% of Al; 0.90 wt% of Co; 0.30 wt% of Zr; 0.85 wt% of B; fe 65.73 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 22.90 wt%; pr 9.60 wt%; 1.25 wt% of Cu; 0.07 wt% of Al; 1.20 wt% of Co; 0.32 wt% of Zr; b0.87 wt%; fe 63.79 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 22.30 wt%; pr 9.20 wt%; 1.75 wt% of Cu; 0.06 wt% of Al; 1.50 wt% of Co; 0.28 wt% of Zr; b0.93 wt%; fe 63.98 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 21.50 wt%; pr 10.50 wt%; cu 2.00 wt%; 0.07 wt% of Al; 2.00 wt% of Co; 0.35 wt% of Zr; 0.89 wt% of B; fe 62.69 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 28.05 wt%; 0.45 wt% of Pr; tb 2.00 wt%; 0.75 wt% of Cu; 0.06 wt% of Al; 2.00 wt% of Co; 0.30 wt% of Nb; b0.92 wt%; fe 65.47 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 29.07 wt%; 0.43 wt% of Pr; dy 2.00 wt%; 1.60 wt% of Cu; 0.07 wt% of Al; 2.50 wt% of Co; 0.25 wt% of Nb; 0.90 wt% of B; fe 63.18 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 28.50 wt%; 1.45 wt% of Cu; 0.05 wt% of Al; 1.50 wt% of Co; 0.25 wt% of Ti; 0.90 wt% of B; fe 67.35 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 23.30 wt%; pr 7.20 wt%; cu 0.49 wt%; 0.07 wt% of Al; 1.50 wt% of Co; 0.20 wt% of Ti; b0.94 wt%; fe 66.30 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: nd 23.90 wt%; pr 7.10 wt%; cu 0.55 wt%; 0.07 wt% of Al; 2.00 wt% of Co; 0.25 wt% of Ti; b0.94 wt%; fe 65.19 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 30.75 wt% of Nd; 0.25 wt% of Pr; 1.10 wt% of Cu; 0.06 wt% of Al; 2.00 wt% of Co; 0.15 wt% of Ti; b0.94 wt%; fe 64.75 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 30.75 wt% of Nd; 0.25 wt% of Pr; 1.10 wt% of Cu; 0.06 wt% of Al; 2.00 wt% of Co; 0.15 wt% of Ti; b0.94 wt%; fe 64.75 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 30.75 wt% of Nd; 0.25 wt% of Pr; 1.10 wt% of Cu; 0.06 wt% of Al; 2.00 wt% of Co; 0.15 wt% of Ti; b0.94 wt%; fe 64.75 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron material preferably includes the following components by mass: 30.75 wt% of Nd; 0.25 wt% of Pr; 1.10 wt% of Cu; 0.06 wt% of Al; 2.00 wt% of Co; 0.15 wt% of Ti; b0.94 wt%; fe 64.75 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
The second technical scheme provided by the invention is as follows: a preparation method of a neodymium iron boron material comprises the following steps:
the melt of the raw material composition of the neodymium iron boron material is subjected to casting, powder making, forming, sintering and aging treatment;
the aging treatment comprises primary aging treatment and secondary aging treatment, wherein the temperature of the primary aging treatment is 830-870 ℃.
The melt of the raw material composition of the neodymium iron boron material can be prepared according to a conventional method in the field, for example: 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 ℃.
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) of the molten solution of the raw material composition of the neodymium iron boron material was passed through a rotating roller at 10 deg.f2DEG C/sec-104Cooling at a rate of DEG C/sec.
Wherein, 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 23.1 ℃, 23.4 ℃, 23.5 ℃, 23.6 ℃, 23.9 ℃, 24.2 ℃ or 24.5 ℃.
Wherein the roller can be a roller conventional in the art, such as a copper roller.
Wherein, the operation and the condition of the powder preparation can be the operation and the condition which are conventional in the field. The milling typically includes a hydrogen milling process and a jet milling process.
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 can be used for crushing for 3 hours.
After the pulverization, a lubricant, such as zinc stearate, may be added to the powder as is conventional in the art. The amount of the lubricant added may be 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 preheating temperature can 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 can be the conventional sintering temperature in the field, and is preferably 1050-1090 ℃, for example 1058-1088 ℃; more preferably 1060 to 1078 ℃.
The sintering time can be the sintering time conventional in the art, such as 7-9 h, and further such as 8 h.
Before cooling, Ar gas can be introduced to ensure that the gas pressure reaches 0.1 MPa.
Wherein the primary aging treatment temperature is preferably 840-860 ℃, such as 845 ℃, 850 ℃, and more preferably 850 ℃.
In the first-stage aging treatment, the temperature rise rate of the temperature rise to 830-870 ℃ is preferably 3-5 ℃/min. The starting point of the temperature increase may be 20 ℃.
The treatment time of the primary aging can be 3 hours.
The temperature of the secondary aging treatment can be the temperature of the conventional secondary aging treatment in the field, preferably 430-470 ℃, more preferably 440-460 ℃, such as 440 ℃, 445 ℃, 450 ℃, 455 ℃ and 460 ℃.
In the secondary aging treatment, the temperature rise rate of raising the temperature to 430-470 ℃ 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 third technical scheme of the invention is as follows: a neodymium iron boron material prepared by the method.
The fourth technical scheme of the invention is as follows: a neodymium iron boron material comprises the following components in percentage by mass:
r: 28.5 to 33.0 wt%; r is a rare earth element at least containing Nd;
cu: 0.45 to 2 wt% but not 0.45 wt%;
B:0.84~0.94wt%;
Al:0.08~0.12wt%;
co: less than or equal to 2.5 wt% but not 0;
Fe:62~70wt%;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.15-0.25 wt%;
when N contains Zr, the content of Zr is 0.2-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.5 wt%;
the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material;
the neodymium iron boron material contains R2T14A main phase B, a grain boundary phase and a rare earth-rich phase, wherein the grain boundary phase contains R6T13An M phase; the R is6T13The volume fraction of the M phase is more than or equal to 3.5 percent; percent means in the grain boundary phase, the R2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
Wherein the grain boundary phase refers to two or more R2T14B is a general term for grain boundary phases between grains.
Wherein, R is2T14In the B phase, R is a rare earth element, and T is Fe and/or Co.
Wherein, preferably, R is6T13The volume fraction of the M phase is 4-12%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In the inventionSaid R is6T13In the M phase, R is a rare earth element, T is Fe and/or Co, and M is Cu.
In the present invention, R is6T13The volume fraction of the M phase is preferably 4 to 11%, such as 5.1%, 5.6%, 6.7%, 7.6%, 7.8%, 8.4%, more preferably 5to 10%, the percentage being in the grain boundary phase, the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In the invention, in the neodymium iron boron material, the content of R is preferably 28.5 to 32.5 wt%, for example 29.500 wt%, 30.494 wt%, 30.504 wt%, 30.514 wt%, 30.9991 wt%, 30.9992 wt%, 30.995 wt%, 30.9997 wt%, 30.9999 wt%, 31.009 wt%, 31.491 wt%, 31.503 wt%, 31.504 wt%, 32.023 wt%, 32.398 wt%, more preferably 30.5 to 32 wt%, with the percentage being mass percent of the total mass of the neodymium iron boron material.
Wherein, in the raw material composition, the content of Nd is preferably 19 to 24 wt%, such as 19.012 wt%, 20.802 wt%, 21.503 wt%, 22.203 wt%, 22.301 wt%, 22.302 wt%, 22.502 wt%, 22.798 wt%, 23.302 wt%, 23.903 wt%; or, the content of Nd is preferably 28 to 32 wt%, for example 28.052 wt%, 28.071 wt%, 28.072 wt%, 28.502 wt%, 28.565 wt%, 29.057 wt%, 29.071 wt%, 30.042 wt%, 30.530 wt%, 30.748 wt%, 30.751 wt%, 30.754 wt%, 31.241 wt%, the percentage being mass percentage of the total mass of the neodymium iron boron material.
In the present invention, the neodymium iron boron material preferably does not contain Ga.
In the neodymium iron boron material, R can also comprise Pr.
Wherein, the content of Pr can be less than 0.2 at% or more than 8 at%; at% is the atomic percentage in the neodymium iron boron material.
Wherein, the content of Pr is preferably less than 1.0 wt% and not 0, more preferably 0.1 to 0.5 wt%, such as 0.241 wt%, 0.243 wt%, 0.248 wt%, 0.250 wt%, 0.424 wt%, 0.428 wt%, 0.434 wt%, 0.435 wt%, 0.443 wt%, 0.450 wt%, 0.452 wt%, 0.465 wt%; or the content of Pr is preferably 6 to 15 wt%, more preferably 7 to 12 wt%, such as 7.106 wt%, 7.202 wt%, 9.202 wt%, 9.300 wt%, 9.512 wt%, 9.600 wt%, 10.221 wt%, 10.496 wt%, 10.503 wt%, 11.221 wt%; the percentage is the mass percentage of the total mass of the neodymium iron boron material.
In the invention, the neodymium iron boron material does not contain heavy rare earth elements, and can also reach the level equivalent to or even better than the magnetic performance of the magnet material in the prior art. Or, the neodymium iron boron material can also comprise RH which is a heavy rare earth element.
When the neodymium iron boron material contains RH, the content of RH is preferably 1.5 to 6 wt%, more preferably 1 to 2.5 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material.
Wherein, the RH preferably includes one or more of Dy, Tb and Ho.
When the RH includes Dy, the content of Dy is preferably 1 to 2.5 wt%, for example, 1.985 wt%, which is a mass percentage of the total mass of the neodymium iron boron material.
When the RH includes Tb, the content of Tb is preferably 1 to 2.5 wt%, for example 2.012 wt%, which is the mass percentage of the total mass of the neodymium iron boron material.
In the present invention, in the neodymium iron boron material, the content of B is preferably 0.85 to 0.94 wt%, for example, 0.851 wt%, 0.872 wt%, 0.882 wt%, 0.891 wt%, 0.902 wt%, 0.912 wt%, 0.914 wt%, 0.922 wt%, 0.931 wt%, 0.932 wt%, which is the mass percentage of the total mass of the neodymium iron boron material.
In the neodymium iron boron material, the atomic percentage of R and the atomic percentage of B preferably satisfy the following relational expression: and B/R is not less than 0.38, wherein in the formula, B is the atomic percentage of B in the neodymium iron boron material, and R is the atomic percentage of R in the neodymium iron boron material.
In the present invention, in the neodymium iron boron material, when R further includes Pr, preferably, B and Nd satisfy the following relation: B/(Pr + Nd) is not less than 0.405, wherein B refers to the atomic percentage of B in the neodymium iron boron material, Pr refers to the atomic percentage of Pr in the neodymium iron boron material, and Nd refers to the atomic percentage of Nd in the neodymium iron boron material.
In the present invention, the content of Cu in the neodymium iron boron material is preferably 0.6 wt% to 2 wt%, such as 0.600 wt%, 0.602 wt%, 0.752 wt%, 0.852 wt%, 0.912 wt%, 1.102 wt%, 1.103 wt%, 1.104 wt%, 1.105 wt%, 1.152 wt%, 1.251 wt%, 1.252 wt%, 1.453 wt%, 1.461 wt%, 1.602 wt%, 1.752 wt%, 1.758 wt%, 1.802 wt%, 1.894 wt%, 1.952 wt%, 1.983 wt%, 1.997 wt%, more preferably 1 to 2 wt%, based on the total mass of the neodymium iron boron material.
In the invention, in the neodymium iron boron material, the content of Al is preferably 0.09-0.11 wt%, for example, 0.092 wt%, 0.102 wt%, 0.110 wt%, and the percentage is mass percentage of the total mass of the neodymium iron boron material.
In the present invention, in the neodymium iron boron material, the content of Co is preferably 0.5 to 2.5 wt%, for example, 0.502 wt%, 0.752 wt%, 0.802 wt%, 0.891 wt%, 1.002 wt%, 1.023 wt%, 1.202 wt%, 1.502 wt%, 1.981 wt%, 1.982 wt%, 1.985 wt%, 1.987 wt%, 2.005 wt%, 2.021 wt%, more preferably 1.00 to 2 wt%, with the percentage being mass percentage of the total mass of the neodymium iron boron material.
In the invention, in the neodymium iron boron material, the content of Fe is preferably 64 to 69 wt%, for example 64.706 wt%, 64.714 wt%, 64.715 wt%, 64.717 wt%, 64.719 wt%, 64.848 wt%, 65.143 wt%, 65.413 wt%, 65.703 wt%, 65.804 wt%, 66.237 wt%, 66.521 wt%, 66.916 wt%, 67.307 wt%, 67.931 wt%, 68.871 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material.
In the neodymium iron boron material, when the N includes Ti, the content of Ti is preferably 0.2 to 0.25 wt%, for example, 0.202 wt%, and the percentage is a mass percentage of the total mass of the neodymium iron boron material.
In the present invention, when the N in the neodymium iron boron material contains Zr, the content of Zr is preferably 0.25 to 0.35 wt%, for example, 0.202 wt%, 0.240 wt%, 0.281 wt%, 0.298 wt%, 0.322 wt%, and the percentage is mass percentage of the total mass of the neodymium iron boron material.
In the invention, when the N comprises Zr in the neodymium iron boron material, the Zr content is preferably 0.26 wt% or more and less than (3.48B-2.67 wt%), wherein B refers to the mass percentage of B in the total mass of the neodymium iron boron material.
In the neodymium iron boron material, when the N includes Nb, the content of Nb is preferably 0.2 to 0.3 wt%, for example, 0.252 wt%, and the percentage is a mass percentage of the total mass of the neodymium iron boron material.
In the invention, when the N in the neodymium iron boron material contains Ti and Nb, the atomic percentage of Ti or Nb is preferably greater than or equal to 0.55 at%.
In the invention, the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.09~0.11wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.2-0.25 wt%;
when N contains Zr, the content of Zr is 0.25-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.3 wt%;
the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material;
the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase, said R6T13The volume fraction of the M phase is 4-11%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In the invention, the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element comprising Nd and Pr;
pr: 0.1-0.5% or 6-15%;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.09~0.11wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.2-0.25 wt%;
when N contains Zr, the content of Zr is 0.25-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.3 wt%;
the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material;
the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase, said R6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In the invention, the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.09~0.11wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
Ti:0.2~0.25wt%;
the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material;
the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase, said R6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In the invention, the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.09~0.11wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
Zr:0.25~0.35wt%;
the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material;
the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase, said R6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In the invention, the neodymium iron boron material preferably comprises the following components by mass:
r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd;
Cu:0.6~2wt%;
B:0.85~0.94wt%;
Al:0.09~0.11wt%;
co: 0.5 to 2.5 wt% but not 0;
Fe:64~69wt%;
Nb:0.2~0.3wt%;
the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material;
the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase, said R6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 28.072 wt%; pr 0.424 wt%; 0.600 wt% of Cu; 0.092 wt% of Al; 0.502 wt% of Co; ti 0.152 wt%; b0.829 wt%; fe 69.329 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 6.7%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 28.565 wt%; pr 0.434 wt%; cu 0.852 wt%; 0.102 wt% of Al; 1.023 wt% of Co; 0.202 wt% of Ti; b0.891 wt%; fe 67.931 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 7.8%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 30.042 wt%; 0.452 wt% of Pr; cu 0.912 wt%; 0.122 wt% of Al; co 1.502 wt%; 0.252 wt% of Ti; b0.914 wt%; fe 65.804 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 5.6%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 30.751 wt%; pr 0.241 wt%; 1.102 wt% of Cu; 0.111 wt% of Al; co 1.985 wt%; 0.151 wt% of Ti; b0.942 wt%; fe 64.717 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 5.1%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 31.241 wt%; 0.250 wt% of Pr; 1.252 wt% of Cu; 0.092 wt% of Al; co 2.502 wt%; 0.252 wt% of Ti; b0.922 wt%; fe 63.489 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 7.6%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 20.802 wt%; pr 11.221 wt%; 1.461 wt% of Cu; 0.102 wt% of Al; 0.502 wt% of Co; ti 0.152 wt%; b0.912 wt%; fe 64.848 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 8.4%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 22.301 wt%; pr 10.221 wt%; cu 1.758 wt%; 0.112 wt% of Al; 1.002 wt% of Co; ti 0.202 wt%; b0.931 wt%; fe 63.473 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 6.7%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 19.012 wt%; pr 9.512 wt%; 1.802 wt% of Cu; 0.081 wt% of Al; co 1.502 wt%; 0.253 wt% of Ti; b0.922 wt%; fe 66.916 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 5.1%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 22.492 wt%; pr 10.496 wt%; 1.952 wt% of Cu; al 0.091 wt%; co 1.551 wt%; 0.151 wt% of Ti; 0.843 wt% of B; fe 62.424 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 7.6%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 22.203 wt%; pr 9.300 wt%; cu 1.894 wt%; 0.112 wt% of Al; co 2.502 wt%; 0.252 wt% of Ti; b0.882 wt%; fe 62.855 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 8.4%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the inventionThe neodymium iron boron material preferably comprises the following components in percentage by mass: nd 28.071 wt%; pr 0.428 wt%; cu 0.602 wt%; 0.102 wt% of Al; 0.802 wt% of Co; 0.202 wt% of Zr; b0.922 wt%; fe 68.871 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 6.7%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 29.057 wt%; pr 0.443 wt%; cu 1.983 wt%; 0.092 wt% of Al; 0.752 wt% of Co; 0.240 wt% of Zr; b0.912 wt%; fe 66.521 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 7.8%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 30.530 wt%; pr 0.465 wt%; cu 1.152 wt%; 0.110 wt% of Al; 0.891 wt% of Co; zr 0.298 wt%; b0.851 wt%; fe 65.703 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 6.7%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 22.798 wt%; pr 9.600 wt%; cu 1.251 wt%; 0.122 wt% of Al; 1.202 wt% of Co; 0.322 wt% of Zr; b0.872 wt%; fe 63.833 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 7.8%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 22.302 wt%; pr 9.202 wt%; 1.752 wt% of Cu; 0.092 wt% of Al; co 1.502 wt%; 0.281 wt% of Zr; b0.932 wt%; fe 63.937 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 5.6%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 21.503 wt%; pr 10.503 wt%; cu 1.997 wt%; 0.102 wt% of Al; co 1.987 wt%; 0.352 wt% of Zr; b0.891 wt%; fe 62.665 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 5.1%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 28.052 wt%; 0.450 wt% of Pr; tb 2.012 wt%; cu 0.752 wt%; 0.092 wt% of Al; 2.005 wt% of Co; 0.302 wt% of Nb; b0.922 wt%; fe 65.413 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 7.6%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 29.071 wt%; pr 0.435 wt%; dy 1.985 wt%; cu 1.602 wt%; 0.112 wt% of Al; co 2.503 wt%; nb 0.252 wt%; b0.902 wt%; fe 63.138 wt%; the above-mentionedThe percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 8.4%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 28.502 wt%; 1.453 wt% of Cu; al 0.082 wt%; co 1.502 wt%; 0.252 wt% of Ti; b0.902 wt%; fe 67.307 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 6.7%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 23.302 wt%; pr 7.202 wt%; cu 0.492 wt%; 0.121 wt% of Al; co 1.502 wt%; 0.202 wt% of Ti; b0.942 wt%; fe 66.237 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 5.1%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 23.903 wt%; pr 7.106 wt%; cu 0.551 wt%; 0.112 wt% of Al; co 1.987 wt%; 0.256 wt% of Ti; b0.942 wt%; fe 65.143 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 7.6%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium-iron-boron material preferably comprises the following components by mass: nd 30.748 wt%; 0.243 wt% of Pr; cu 1.105 wt%; 0.111 wt% of Al; co 1.985 wt%; 0.151 wt% of Ti; b0.942 wt%; fe 64.715 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 4.5%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 30.751 wt%; pr 0.248 wt%; 1.104 wt% of Cu; 0.113 wt% of Al; co 1.981 wt%; ti 0.152 wt%; b0.945 wt%; fe 64.706 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 4.3%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 30.754 wt%; 0.243 wt% of Pr; 1.102 wt% of Cu; 0.11 wt% of Al; co 1.985 wt%; 0.148 wt% of Ti; b0.944 wt%; fe 64.714 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 4.6%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
In a preferred embodiment of the present invention, the neodymium iron boron material preferably includes the following components by mass: nd 30.751 wt%; pr 0.241 wt%; cu 1.103 wt%; 0.111 wt% of Al; co 1.982 wt%; 0.151 wt% of Ti; b0.942 wt%; fe 64.719 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the R is6T13The volume fraction of the M phase is 4.7%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phaseThe percentage of the active ingredients is as follows.
The fifth technical scheme of the invention is as follows: an application of the neodymium iron boron 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) the elements with specific content in the neodymium iron boron material are matched with each other, and the prepared neodymium iron boron material contains R with specific content6T13And M. The neodymium iron boron material contains a small amount of boron element, and has better remanence, coercive force, squareness and temperature stability without adding heavy rare earth elements.
(2) The neodymium iron boron material has better magnetic property, and improves the consistency of the neodymium iron boron material, namely the magnetic property of products in the same batch is uniform.
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.
Examples 1 to 25 and comparative examples 1 to 9
The raw materials used for preparing the neodymium iron boron materials in the examples 1 to 25 and the comparative examples 1 to 9 are shown in table 1, and the preparation process is as follows:
(1) and (3) smelting: according to the 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 ensure that the air pressure reaches 5.5 ten thousand Pa, casting, and making the molten liquid into a rapid hardening alloy sheet with the thickness of 0.12-0.35mm by a copper roller with the rotation speed of 29 revolutions per minute, 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 ℃.
(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 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 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 10-3Keeping the temperature of the mixture at 300 ℃ and 600 ℃ for 1 hour respectively under the vacuum of Pa, sintering the mixture at 1050-1090 ℃ for 8 hours, introducing Ar gas to enable the pressure to reach 0.1MPa, and cooling the mixture to the room temperature.
(8) And (3) aging treatment process: heating the sintered body from 20 ℃ to the first-stage aging treatment temperature at a heating rate of 3-5 ℃/min in high-purity Ar gas, and performing first-stage aging treatment, wherein the method comprises the following specific steps: after heat treatment for 3 hours at the primary aging treatment temperature, the steel sheet is cooled to room temperature and taken out. Then, carrying out secondary aging treatment for 3h, wherein the temperature rise rate from room temperature to the secondary aging temperature is 3-5 ℃/min;
wherein the starting materials of examples 22-25 are the same as in example 1; the starting material of comparative example 7 was the same as in example 1; the raw material of comparative example 8 was the same as example 2; the starting material for comparative example 9 was the same as in example 3.
Wherein, the water inlet temperature of the copper roller in the casting process in the step (2), the sintering temperature in the step (7), the primary aging temperature in the step (8) and the secondary aging temperature in the step (8) are shown in the table 2.
TABLE 1 quality percentages of the raw materials in examples 1-25 and comparative examples 1-9
Figure BDA0002396106550000211
Figure BDA0002396106550000221
Figure BDA0002396106550000231
Note: TRE refers to the total rare earth content, including Nd, Pr, and heavy rare earths (Tb, Dy); "/" means that the element is not included.
The raw materials are prepared according to the formula shown in table 1, and the neodymium iron boron material is prepared under the same process conditions except the conditions shown in table 2.
TABLE 2
Figure BDA0002396106550000232
Figure BDA0002396106550000241
Effect example 1 ingredient measurement
The sintered magnets of examples 1 to 25 and comparative examples 1 to 9 were measured for specific components using a high-frequency inductively coupled plasma emission spectrometer (ICP-OES). The results of component detection are shown in Table 3.
TABLE 3
Figure BDA0002396106550000242
Figure BDA0002396106550000251
Figure BDA0002396106550000261
Note: TRE refers to the total rare earth content, including Nd, Pr, and heavy rare earths (Tb, Dy); the content of Al in the sintered magnets of examples 1 to 25 and comparative examples 1 to 9 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., crucible made of alumina during melting).
Effect example 2 magnetic Properties and consistency of magnetic Properties
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. Table 4 shows the results of magnetic property measurements. Wherein the content of the first and second substances,
(1) the detection method of the 6-13-1 phase comprises the following steps:
microstructure: the vertically oriented faces of the neodymium-iron-boron material were polished using FE-EPMA detection and detected using a field emission electron probe microanalyzer (FE-EPMA) (JEOL 8530F, Japan Electron Ltd.). Detection of R in grain boundaries6T13M phase, T Fe and/or Co, M Cu.
(2) Br, Hcj, 20-80 ℃ Br temperature coefficient, 20-80 ℃ Hcj temperature coefficient, 20-150 ℃ Hcj temperature coefficient, squareness degree and relative permeability are all mean values: the average value is calculated by testing the residual magnetism, the coercive force, the Br temperature coefficient at 20-80 ℃, the Hcj temperature coefficient at 20-150 ℃ and the squareness or the relative permeability of 5 parts of neodymium iron boron material samples in the same batch. Several ndfeb materials were prepared in each example and comparative example of the present invention, and the same batch refers to several ndfeb materials obtained in each example and comparative example, wherein the ndfeb material used for testing was a 10 x 10mm cylinder.
TABLE 4
Figure BDA0002396106550000271
Note: the magnetic performance of the neodymium iron boron material in the comparative examples 1-9 is the best performance which can be obtained by the formula of the comparative examples 1-9 after process optimization (water inlet temperature, sintering temperature and aging temperature).
Table 5 shows the results of the magnetic property uniformity measurement. Wherein the content of the first and second substances,
(1) squareness SQ ═ Hk/Hcj; wherein, Hk is the value of the corresponding external magnetic field H when B is 90% Br; hcj is the coercivity.
(2) The relative magnetic permeability is Br/Hcb; wherein Br is remanence, Hcb is magnetic induction coercive force, and when an inflection point exists in a B-H curve, the magnetic conductivity is taken before the inflection point.
(3) 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.
TABLE 5
Figure BDA0002396106550000281
Figure BDA0002396106550000291
As can be seen from Table 5, the coercivity difference of the same batch of the magnetic steel products in the comparative examples 4 and 6 is more than 1.5kOe, namely Max (Hcj) -Min (Hcj) > 1.5kOe, and the magnet performance consistency can be judged to be poor; the neodymium iron boron materials in the embodiments 1-25 are low in relative permeability and high in squareness, the coercive force difference of the magnetic steel products in the same batch is low, and the performance consistency of the magnet is good.

Claims (46)

1. The neodymium iron boron material is characterized by comprising the following components in percentage by mass:
r: 28.5 to 33.0 wt%; r is a rare earth element at least containing Nd and Pr; the content of Pr is less than 1.0 wt% and not 0, or 6-15 wt%;
cu: 0.45 to 2 wt% but not 0.45 wt%;
B:0.84~0.94 wt %;
Al:0.08~0.12 wt %;
co: less than or equal to 2.5 wt% but not 0;
Fe:62~70 wt %;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.15-0.25 wt%;
when N contains Zr, the content of Zr is 0.2-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.5 wt%;
the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material;
the neodymium iron boron material does not contain Ga;
the neodymium iron boron material contains R2T14A main phase B, a grain boundary phase and a rare earth-rich phase, wherein the grain boundary phase contains R6T13M phase, wherein M is Cu; the R is6T13The volume fraction of the M phase is more than or equal to 3.5 percent; percent means in the grain boundary phase, the R2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
2. The neodymium-iron-boron material of claim 1, wherein R is6T13The volume fraction of the M phase is 4-12%, and the percentage refers to the grain boundary phase and the R phase2T14The percentage of the sum of the volumes of the main phase B and the rare earth-rich phase;
and/or the content of R is 28.5-32.5 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or the content of Nd is 19-24 wt%, or 28-32 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or the content of Pr is less than 0.2 at% or more than 8 at%, the at% being the atomic percentage in the neodymium iron boron material;
and/or, the neodymium iron boron material comprises RH which is a heavy rare earth element;
and/or the content of B is 0.85-0.94 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or the atomic percent of R and the atomic percent of B in the neodymium iron boron material satisfy the following relational expression: B/R is more than or equal to 0.38, wherein B is the atomic percentage of B in the neodymium iron boron material, and R is the atomic percentage of R in the neodymium iron boron material;
and/or, when the R comprises Pr, the B and the Nd satisfy the following relational expression: B/(Pr + Nd) is not less than 0.405, wherein B is the atomic percentage of B in the neodymium iron boron material, Pr is the atomic percentage of Pr in the neodymium iron boron material, and Nd is the atomic percentage of Nd in the neodymium iron boron material;
and/or the Cu content is 0.6-2 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or the content of Al is 0.09-0.11 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or the content of Co is 0.5-2.5 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or the Fe content is 64-69 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or in the neodymium iron boron material, when the N contains Ti, the content of the Ti is 0.2-0.25 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or in the neodymium iron boron material, when the N contains Zr, the content of the Zr is 0.25-0.35 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material; or the Zr content is more than or equal to 0.26 wt% and less than (3.48B-2.67 wt%), wherein B is the mass percent of B in the total mass of the neodymium iron boron material;
and/or in the neodymium iron boron material, when the N contains Nb, the content of Nb is 0.2-0.3 wt%, and the percentage is the mass percentage of the total mass of the neodymium iron boron material;
and/or, when the N contains Ti and/or Nb, the atomic percent of the Ti or the Nb is more than or equal to 0.55at percent.
3. The neodymium-iron-boron material of claim 2, wherein R is6T13The volume fraction of the M phase is 4-11%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
4. The neodymium-iron-boron material of claim 3, wherein R is6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
5. The neodymium-iron-boron material as claimed in claim 2, wherein the content of R is 30.5-32 wt%, and the percentage is mass percentage of the total mass of the neodymium-iron-boron material.
6. The neodymium-iron-boron material of claim 2, wherein the content of Pr is 0.1-0.5 wt%, or 7-12 wt%; the percentage is the mass percentage of the total mass of the neodymium iron boron material.
7. The neodymium-iron-boron material of claim 2, wherein when the neodymium-iron-boron material contains RH, the content of the RH is 1.5-6 wt%, and the percentage is mass percentage of the total mass of the neodymium-iron-boron material.
8. The neodymium-iron-boron material of claim 2, wherein when the neodymium-iron-boron material contains RH, the content of the RH is 1-2.5 wt%, and the percentage is the mass percentage of the total mass of the neodymium-iron-boron material.
9. The ndfeb material of claim 2, wherein the RH species comprises one or more of Dy, Tb and Ho.
10. The ndfeb material of claim 9, wherein when the RH comprises Dy, the Dy is present in an amount of 1 to 2.5 wt% in mass percentage based on the total mass of the ndfeb material.
11. The ndfeb material of claim 9, wherein when the RH comprises Tb, the Tb content is 1 to 2.5 wt%, percentage being mass percentage of the total mass of the ndfeb material.
12. The neodymium-iron-boron material as claimed in claim 2, wherein the content of Cu is 1-2 wt%, and the percentage is mass percentage of the total mass of the neodymium-iron-boron material.
13. The neodymium-iron-boron material as claimed in claim 2, wherein the content of Co is 1-2 wt%, and the percentage is mass percentage of the total mass of the neodymium-iron-boron material.
14. The neodymium-iron-boron material as claimed in any one of claims 1 to 13, wherein the neodymium-iron-boron material comprises the following components in percentage by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.09-0.011 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; n: one or more of Ti, Zr and Nb; when N contains Ti, the content of Ti is 0.2-0.25wt%; when N contains Zr, the content of Zr is 0.25-0.35 wt%; when the N contains Nb, the content of Nb is 0.2-0.3 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the grain boundary phase of the neodymium iron boron material comprises R6T13M phase, said R6T13The volume fraction of the M phase is 4-11%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
15. The neodymium-iron-boron material as claimed in any one of claims 1 to 13, wherein the neodymium-iron-boron material comprises the following components in percentage by mass: r: 28.5-32.5 wt%; r is a rare earth element comprising Nd and Pr; pr: 0.1-0.5% or 6-15%; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.09-0.11 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; n: one or more of Ti, Zr and Nb; when N contains Ti, the content of Ti is 0.2-0.25 wt%; when N contains Zr, the content of Zr is 0.25-0.35 wt%; when the N contains Nb, the content of Nb is 0.2-0.3 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase, said R6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
16. The neodymium-iron-boron material as claimed in any one of claims 1 to 13, wherein the neodymium-iron-boron material comprises the following components in percentage by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.09-0.11 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; ti: 0.2-0.25 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase ofR6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
17. The neodymium-iron-boron material as claimed in any one of claims 1 to 13, wherein the neodymium-iron-boron material comprises the following components in percentage by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.09-0.11 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; zr: 0.25-0.35 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the grain boundary phase of the neodymium iron boron material also comprises R6T13M phase, said R6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
18. The neodymium-iron-boron material as claimed in any one of claims 1 to 13, wherein the neodymium-iron-boron material comprises the following components in percentage by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.09-0.11 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; nb: 0.2-0.3 wt%; the percentage is the mass percentage of each component in the total mass of the neodymium iron boron material; the grain boundary phase of the neodymium iron boron material comprises R6T13M phase, said R6T13The volume fraction of the M phase is 5-10%, and the percentage refers to the grain boundary phase and the R phase2T14The sum of the volumes of the B main phase and the rare earth-rich phase is a percentage.
19. A raw material composition for preparing the neodymium iron boron material as claimed in any one of claims 1 to 18, which is characterized by comprising the following components in percentage by mass:
r: 28.5 to 33.0 wt%; r is a rare earth element at least containing Nd and Pr; the content of Pr is less than 1.0 wt% and not 0, or 6-15 wt%;
cu: 0.45 to 2 wt% but not 0.45 wt%;
B:0.84~0.94 wt %;
Al:0.05~0.07 wt %;
co: less than or equal to 2.5 wt% but not 0;
Fe:62~70 wt %;
n: one or more of Ti, Zr and Nb;
when N contains Ti, the content of Ti is 0.15-0.25 wt%;
when N contains Zr, the content of Zr is 0.2-0.35 wt%;
when the N contains Nb, the content of Nb is 0.2-0.5 wt%;
the percentage is the mass percentage of each component in the total mass of the raw material composition;
the raw material composition does not contain Ga.
20. The raw material composition of claim 19, wherein the content of R in the raw material composition is 28.5 to 32.5 wt%, and the percentage is mass percentage based on the total mass of the raw material composition;
and/or the content of Nd is 19-24 wt%, or 28-32 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or, the content of Pr is < 0.2 at% or > 8 at%, at% being the atomic percentage in the raw material composition;
and/or the raw material composition comprises RH which is a heavy rare earth element;
and/or the content of B is 0.85-0.94 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or, in the raw material composition, the atomic percent of R and the atomic percent of B satisfy the following relational expression: B/R is more than or equal to 0.38, wherein B is the atomic percent of B in the raw material composition, and R is the atomic percent of R in the raw material composition;
and/or, when the R comprises Pr, the B and the Nd satisfy the following relational expression: B/(Pr + Nd) is not less than 0.405, wherein B is the atomic percent of B in the raw material composition, Pr is the atomic percent of Pr in the raw material composition, and Nd is the atomic percent of Nd in the raw material composition;
and/or the Cu content is 0.6-2 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or the Al content is 0.06-0.07 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or the Co content is 0.5-2.5 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or the Fe content is 64-69 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or when the N contains Ti, the content of the Ti is 0.2-0.25 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or when the N contains Zr, the content of the Zr is 0.25-0.35 wt%, and the percentage is the mass percentage of the total mass of the raw material composition; or the mass content of Zr is more than or equal to 0.26 wt% and less than (3.48B-2.67 wt%), wherein B is the mass percentage of B in the total mass of the raw material composition;
and/or when the N contains Nb, the content of Nb is 0.2-0.3 wt%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or, when the N contains Ti and/or Nb, the atomic percent of the Ti or the Nb is more than or equal to 0.55at percent.
21. A raw material composition according to claim 20, wherein the content of R in the raw material composition is 30.5 to 32 wt% in percentage by mass based on the total mass of the raw material composition.
22. The feed composition of claim 20, wherein the Pr content is 0.1 to 0.5 wt% or 7 to 12 wt%; the percentage is the mass percentage of the total mass of the raw material composition.
23. A raw material composition according to claim 20, wherein when RH is contained in the raw material composition, the content of RH is 1.5 to 6 wt% in percentage by mass based on the total mass of the raw material composition.
24. A raw material composition according to claim 20, wherein when RH is contained in the raw material composition, the content of RH is 1 to 2.5 wt%, and the percentage is a mass percentage based on the total mass of the raw material composition.
25. The raw material composition as claimed in claim 20, wherein the RH species includes one or more of Dy, Tb and Ho.
26. The raw material composition as claimed in claim 25, wherein, when the RH includes Dy, the Dy is contained in an amount of 1 to 2.5 wt% in percentage by mass based on the total mass of the raw material composition.
27. The raw material composition according to claim 25, wherein when the RH comprises Tb, the Tb content is 1 to 2.5 wt%, and the percentage is mass percentage based on the total mass of the raw material composition.
28. The raw material composition according to claim 20, wherein the content of Cu is 1 to 2 wt% in terms of mass percentage based on the total mass of the raw material composition.
29. The raw material composition according to claim 20, wherein the content of Al is 0.06 wt% in percentage by mass based on the total mass of the raw material composition.
30. The raw material composition according to claim 20, wherein the content of Co is 1 to 2 wt% in terms of mass percentage based on the total mass of the raw material composition.
31. The raw material composition of any one of claims 19 to 30, wherein the raw material composition of the neodymium iron boron material comprises the following components by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.06-0.07 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; n: one or more of Ti, Zr and Nb; when N contains Ti, the content of Ti is 0.2-0.25 wt%; when N contains Zr, the content of Zr is 0.25-0.35 wt%; when the N contains Nb, the content of Nb is 0.2-0.3 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition;
or, the raw material composition of the neodymium iron boron material comprises the following components by mass: r: 28.5-32.5 wt%; r is a rare earth element comprising Nd and Pr; pr: 0.1-0.5% or 6-15%; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.06-0.07 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; n: one or more of Ti, Zr and Nb; when N contains Ti, the content of Ti is 0.2-0.25 wt%; when N contains Zr, the content of Zr is 0.25-0.35 wt%; when the N contains Nb, the content of Nb is 0.2-0.3 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition;
or, the raw material composition of the neodymium iron boron material comprises the following components by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.06-0.07 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; ti: 0.2-0.25 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition;
or, the raw material composition of the neodymium iron boron material comprises the following components by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.06-0.07 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; zr: 0.25-0.35 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition;
or, the raw material composition of the neodymium iron boron material comprises the following components by mass: r: 28.5-32.5 wt%; r is a rare earth element at least containing Nd; cu: 0.6-2 wt%; b: 0.85-0.94 wt%; al: 0.06-0.07 wt%; co: 0.5 to 2.5 wt% but not 0; fe: 64 to 69 wt%; nb: 0.2-0.3 wt%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
32. The preparation method of the neodymium-iron-boron material as claimed in any one of claims 1 to 18, characterized by comprising the following steps: casting, pulverizing, forming, sintering and aging the melt of the raw material composition of the neodymium iron boron material according to any one of claims 19 to 31;
the aging treatment comprises primary aging treatment and secondary aging treatment, wherein the temperature of the primary aging treatment is 830-870 ℃.
33. The method of manufacturing a neodymium-iron-boron material of claim 32, wherein the casting further comprises smelting;
and/or said casting is at 102DEG C/sec-104Cooling at a speed of DEG C/second;
and/or the water inlet temperature of the roller in the casting process is less than or equal to 25 ℃;
and/or, the milling comprises a hydrogen crushing process and an airflow milling process;
wherein the hydrogen breaking process comprises hydrogen absorption, dehydrogenation and cooling treatment;
wherein the hydrogen absorption is carried out under the condition that the hydrogen pressure is 0.15 MPa;
wherein the jet mill pulverization is carried out in a nitrogen atmosphere having an oxidizing gas content of 120ppm or less;
wherein the pressure of a crushing chamber for crushing by the jet mill is 0.38 MPa;
wherein the jet mill is used for crushing for 3 hours;
after the crushing, adding a lubricant into the powder;
and/or the forming process is a magnetic field forming method or a hot-pressing hot-deformation method;
and/or, the sintering also comprises preheating;
and/or the sintering temperature is 1050-1090 ℃;
and/or the sintering time is 5-10 h;
and/or, the primary aging treatment is carried out under the condition of high-purity Ar;
and/or the temperature of the primary aging treatment is 840-860 ℃;
and/or in the primary aging treatment, the temperature rise rate of the temperature rise to 830-870 ℃ is 3-5 ℃/min;
and/or the treatment time of the primary aging is 3 h;
and/or the temperature of the secondary aging treatment is 430-470 ℃;
and/or in the secondary aging treatment, the temperature rise rate of raising the temperature to 430-470 ℃ is 3-5 ℃/min;
and/or the treatment time of the secondary aging is 3 h.
34. The method of manufacturing the neodymium-iron-boron material of claim 33, wherein the temperature of the melting is below 1500 ℃.
35. The method of preparing a neodymium iron boron material of claim 33, wherein the lubricant is zinc stearate.
36. The method for preparing a neodymium-iron-boron material according to claim 33, wherein the addition amount of the lubricant is 0.10-0.15% of the weight of the mixed powder.
37. The method for preparing neodymium-iron-boron material according to claim 33, wherein the preheating temperature is 300-600 ℃.
38. The method for preparing neodymium-iron-boron materials according to claim 33, wherein the preheating time is 1-2 hours.
39. The method for preparing neodymium-iron-boron material according to claim 33, wherein the preheating is performed at 300 ℃ and 600 ℃ for 1 hour respectively.
40. The method for preparing neodymium iron boron materials according to claim 33, wherein the sintering temperature is 1058-1088 ℃.
41. The method for preparing the neodymium-iron-boron material of claim 40, wherein the sintering temperature is 1060-1078 ℃.
42. The method of preparing a neodymium iron boron material of claim 33, wherein the sintering time is 8 hours.
43. The method for preparing a neodymium-iron-boron material according to claim 33, wherein the primary aging treatment temperature is 850 ℃.
44. The method for preparing the neodymium-iron-boron material of claim 33, wherein the temperature of the secondary aging treatment is 440-460 ℃.
45. A neodymium iron boron material prepared by the preparation method of the neodymium iron boron material as claimed in any one of claims 32-44.
46. Use of a neodymium iron boron material according to any one of claims 1 to 18 and 45 as an electronic component.
CN202010134686.9A 2020-02-29 2020-02-29 Neodymium-iron-boron material and preparation method and application thereof Active CN111243811B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202010134686.9A CN111243811B (en) 2020-02-29 2020-02-29 Neodymium-iron-boron material and preparation method and application thereof
PCT/CN2021/077199 WO2021169905A1 (en) 2020-02-29 2021-02-22 Neodymium iron boron material, preparation method therefor and use thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010134686.9A CN111243811B (en) 2020-02-29 2020-02-29 Neodymium-iron-boron material and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN111243811A CN111243811A (en) 2020-06-05
CN111243811B true CN111243811B (en) 2021-07-30

Family

ID=70875229

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010134686.9A Active CN111243811B (en) 2020-02-29 2020-02-29 Neodymium-iron-boron material and preparation method and application thereof

Country Status (2)

Country Link
CN (1) CN111243811B (en)
WO (1) WO2021169905A1 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111243811B (en) * 2020-02-29 2021-07-30 厦门钨业股份有限公司 Neodymium-iron-boron material and preparation method and application thereof
CN112111686A (en) * 2020-09-23 2020-12-22 赣州富尔特电子股份有限公司 Preparation method of magnetic steel special for grain boundary diffusion

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101315825A (en) * 2007-05-31 2008-12-03 北京中科三环高技术股份有限公司 Fire resistant permanent magnet alloy and manufacturing method thereof
JP2018160642A (en) * 2017-03-24 2018-10-11 日立金属株式会社 R-T-B based sintered magnet
CN109585151A (en) * 2017-09-28 2019-04-05 日立金属株式会社 The manufacturing method of R-T-B based sintered magnet and diffusion source
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

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1934283B (en) * 2004-06-22 2011-07-27 信越化学工业株式会社 R-Fe-B-based rare earth permanent magnet material
WO2016086397A1 (en) * 2014-12-04 2016-06-09 浙江大学 Method for improving coercive force of sintered neodymium iron boron magnet by adding dysprosium hydrogen compound and product
CN106024235B (en) * 2015-03-30 2020-01-17 日立金属株式会社 R-T-B sintered magnet
JP6798546B2 (en) * 2016-03-17 2020-12-09 日立金属株式会社 Manufacturing method of RTB-based sintered magnet
JP7276132B2 (en) * 2018-03-23 2023-05-18 株式会社プロテリアル Method for producing RTB based sintered magnet
CN111243811B (en) * 2020-02-29 2021-07-30 厦门钨业股份有限公司 Neodymium-iron-boron material and preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101315825A (en) * 2007-05-31 2008-12-03 北京中科三环高技术股份有限公司 Fire resistant permanent magnet alloy and manufacturing method thereof
JP2018160642A (en) * 2017-03-24 2018-10-11 日立金属株式会社 R-T-B based sintered magnet
CN109585151A (en) * 2017-09-28 2019-04-05 日立金属株式会社 The manufacturing method of R-T-B based sintered magnet and diffusion source
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

Also Published As

Publication number Publication date
CN111243811A (en) 2020-06-05
WO2021169905A1 (en) 2021-09-02

Similar Documents

Publication Publication Date Title
TW202121452A (en) Ndfeb magnet material, raw material composition, preparation method and application
CN110853855A (en) R-T-B series permanent magnetic material and preparation method and application thereof
KR102574303B1 (en) Neodymium iron boron magnetic material, raw material composition and manufacturing method and application
CN111243809B (en) Neodymium-iron-boron material and preparation method and application thereof
CN111326306B (en) R-T-B series permanent magnetic material and preparation method and application thereof
CN111326304B (en) Rare earth permanent magnetic material and preparation method and application thereof
CN111243812B (en) R-T-B series permanent magnetic material and preparation method and application thereof
CN111180159B (en) Neodymium-iron-boron permanent magnet material, preparation method and application
CN110428947B (en) Rare earth permanent magnetic material and raw material composition, preparation method and application thereof
KR102589802B1 (en) Neodymium iron boron magnetic material, raw material composition, manufacturing method and application
CN110323053B (en) R-Fe-B sintered magnet and preparation method thereof
CN111243811B (en) Neodymium-iron-boron material and preparation method and application thereof
CN111243808B (en) Neodymium-iron-boron material and preparation method and application thereof
CN111312463B (en) Rare earth permanent magnetic material and preparation method and application thereof
CN111312462B (en) Neodymium-iron-boron material and preparation method and application thereof
CN113674944A (en) Neodymium-iron-boron magnet material and preparation method and application thereof
CN111091945B (en) R-T-B series permanent magnetic material, raw material composition, preparation method and application
CN110853857B (en) Alloy containing Ho and/or Gd, rare earth permanent magnet, raw materials, preparation method and application
CN111261356B (en) R-T-B series permanent magnetic material and preparation method and application thereof
CN111048273A (en) R-T-B series permanent magnetic material, raw material composition, preparation method and application
CN111312464B (en) Rare earth permanent magnetic material and preparation method and application thereof
CN113593802A (en) Corrosion-resistant high-performance neodymium iron boron sintered magnet and preparation method and application thereof
CN117316565A (en) Regenerated NdFeB magnet and preparation method thereof
CN115662773A (en) High-density terbium-free sintered neodymium-iron-boron permanent magnet and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20220627

Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province

Patentee after: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd.

Address before: 361000 Ke Gang, Haicang District, Fujian, Xiamen

Patentee before: XIAMEN TUNGSTEN Co.,Ltd.

Patentee before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd.

CP01 Change in the name or title of a patent holder
CP01 Change in the name or title of a patent holder

Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province

Patentee after: Fujian Jinlong Rare Earth Co.,Ltd.

Address before: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province

Patentee before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd.