CN111312463A - Rare earth permanent magnetic material and preparation method and application thereof - Google Patents
Rare earth permanent magnetic material and preparation method and application thereof Download PDFInfo
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- CN111312463A CN111312463A CN202010132231.3A CN202010132231A CN111312463A CN 111312463 A CN111312463 A CN 111312463A CN 202010132231 A CN202010132231 A CN 202010132231A CN 111312463 A CN111312463 A CN 111312463A
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- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 239
- 239000000696 magnetic material Substances 0.000 title claims abstract description 118
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 115
- 239000002994 raw material Substances 0.000 claims abstract description 114
- 239000000463 material Substances 0.000 claims abstract description 109
- 230000005291 magnetic effect Effects 0.000 claims abstract description 34
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 34
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 28
- 229910052796 boron Inorganic materials 0.000 claims abstract description 24
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 22
- 230000032683 aging Effects 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 23
- 229910052779 Neodymium Inorganic materials 0.000 claims description 20
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 16
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 238000005266 casting Methods 0.000 claims description 12
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
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- 229910052689 Holmium Inorganic materials 0.000 claims description 4
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 5
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a rare earth permanent magnetic material and a preparation method and application thereof. The raw material composition of the rare earth permanent magnetic material comprises the following components: r: 28.5 to 33 percent; r is a rare earth element including Nd; b: 0.84-0.94%; ga: 0.6< Ga is less than or equal to 1.8 percent; co: less than or equal to 2.5 percent; fe: 61.6-69%; n comprises one or more of Ti, Zr and Nb; when N contains Ti, Ti is 0.15-0.25%; when N contains Zr, Zr is 0.2-0.35%; when N contains Nb, Nb is 0.2-0.5%; the percentage is the percentage of each component in the total mass of the rare earth permanent magnet material. The rare earth permanent magnet material adopts a low-boron aluminum-free system under the condition of not adding heavy rare earth elements, so that the magnetic properties such as remanence, coercive force, temperature stability, squareness and the like are still better, and the magnetic properties of the permanent magnet materials in the same batch are uniform.
Description
Technical Field
The invention particularly relates to a rare earth permanent magnet material and a preparation method and application thereof.
Background
Due to the excellent magnetic characteristics, the rare earth permanent magnet material is widely applied to the fields of electronic products, automobiles, wind power, household appliances, elevators, industrial robots and the like, for example, permanent magnet motors such as hard disks, mobile phones, earphones, elevator traction machines, generators and the like are used as energy sources, the demand of the rare earth permanent magnet material is gradually expanded, and the requirements of various manufacturers on magnet performances such as remanence, coercive force performance, temperature stability, magnet squareness and the like are gradually improved.
The rare-earth permanent magnetic material is mainly composed of R2T14The main phase of the B compound and a grain boundary phase located in a grain boundary portion of the main phase. The R is2T14The B compound is a ferromagnetic material having a high saturation magnetization and an anisotropic magnetic field. The coercive force of the rare earth permanent magnetic material is reduced at high temperature, so irreversible thermal demagnetization occurs. It is currently known that: replacement of R as the main phase by the heavy rare earth element RH2T14In the compound B, part of the light rare earth RL in R is increased in coercive force, and the coercive force is increased with the increase in substitution amount. On the other hand, however, the residual magnetic flux Br decreases. In addition, RH is a scarce resource and expensive resource. In order to increase the remanence of rare earth permanent magnetic materials, it is generally necessary to reduce 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 deteriorating the performance of the magnet.
The squareness of the magnet material is a ratio of a magnetic field value Hk (knee point coercive force) corresponding to a magnetic polarization strength J of 0.9Jr (Jr is remanent polarization, and is equal to a remanent induction strength Br, and both are collectively referred to as remanence) on the J-H demagnetization curve to a magnetic field value Hcj (intrinsic coercive force) corresponding to a magnetic polarization strength J of 0 on the J-H demagnetization curve, that is, Hk/Hcj. Having a higher squareness is a necessary condition for a high-quality magnet. So as to reduce the loss of magnetism during the use process, especially under the environment with higher relative use temperature, and ensure that the magnet still has high magnetic performance when used in the environment for a long time. Even though the coercive force and the remanence of the permanent magnet material in the prior art are high, the squareness of the permanent magnet material cannot be improved to a better level at the same time.
Therefore, under the condition of not adding or adding a small amount of heavy rare earth, how to prepare the rare earth permanent magnetic material with high coercivity, high remanence, squareness and better consistency by adopting a method of a low B and Al-free system is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to overcome the defects that a large amount of heavy rare earth elements are usually required to be added when the rare earth permanent magnetic material adopts a low B system to improve the magnetic property in the prior art, and the magnetic property (remanence, coercive force, temperature stability and squareness) can not be obviously improved even if the heavy rare earth elements are added, and provides a rare earth permanent magnetic material and a preparation method and application thereof. On the premise of not adding heavy rare earth elements, the rare earth permanent magnet material can still be prepared by adopting a low-boron aluminum-free system to obtain better magnetic properties (remanence, coercive force, temperature stability and squareness degree), and meanwhile, the permanent magnet materials in the same batch have uniform magnetic properties.
It should be noted that, in the prior art, a certain amount of Al is usually added to the rare earth permanent magnet material to obtain a magnet material with better performance, but the inventor finds out through verification of multiple experiments that: although the addition of Al improves the magnetic properties of the magnet material, the magnetic properties are not uniform in the production of the same batch of products, i.e., the difference between the maximum value and the minimum value of the coercive force in the same batch of products is greater than 1.5 kOe. And the uniformity of the rare earth permanent magnet material finally obtained is better through a specific formula.
The invention adopts the following technical scheme to solve the technical problems.
The invention provides a raw material composition of a rare earth permanent magnetic material, which comprises the following components in percentage by mass:
r: 28.5 to 33 percent; r is a rare earth element and at least comprises Nd;
B：0.84～0.94％；
Ga：0.6<Ga≤1.8％；
co: less than or equal to 2.5 percent and not 0;
Fe：61.6～69％；
n: one or more of Ti, Zr and Nb;
when the N contains Ti, the content of the Ti is 0.15-0.25%;
when the 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 rare earth permanent magnet material.
In the invention, all the components and corresponding contents in the raw material composition are actively added, and the components and/or contents introduced in the preparation process and/or impurities are not included.
In the present invention, in the raw material composition, the content of R is preferably 29.3 to 32%, for example, 29.3%, 29.5%, 30%, 30.5%, 31%, 31.3% or 32%, more preferably 29.4 to 31.5%, by mass, based on the total mass of the raw material composition.
In the invention, the content of Nd is preferably 8-13%, such as 8.5%, 9.5%, 12.3%, 12.5%; alternatively, the content of Nd is preferably 28 to 31%, for example 28.5%, 29%, 29.3%, 30.2%, or 31%, in mass% based on the total mass of the raw material composition.
In the present invention, the raw material composition preferably does not contain Cu.
In the present invention, the raw material composition preferably does not contain Al; it means that Al is not actively added, but a trace amount of Al (below 0.08%) may be introduced during the addition of other elements (e.g., Fe) or during the manufacturing process (e.g., alumina crucible preparation melt).
In the present invention, in the raw material composition, the R may generally further include Pr.
Wherein, the content of Pr is preferably less than 1.5% and not 0, more preferably 0.1-0.5%, such as 0.2% or 0.3%; or the content of Pr is preferably 17 to 25%, more preferably 18.5 to 21.5%, for example 18.5% or 21.5%, by mass, based on 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 to 2.5% by mass 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%, for example, 2%, in 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%, for example 2%, and the percentage is the mass percentage of the total mass of the raw material composition.
In the present invention, the content of B is preferably 0.86 to 0.94%, for example, 0.86%, 0.88%, 0.9%, 0.92% or 0.94%, in mass% based on the total mass of the raw material composition.
In the present invention, the atomic percentages of R and B in the raw material composition preferably satisfy the following relationship: B/R is more than or equal to 0.38, wherein in the formula, the atom percentage of B in the raw material composition is shown, and the atom percentage of R in the raw material composition is shown.
In the present invention, when Pr is included in the raw material composition, it is preferable that B and Nd satisfy the following relationship: 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 Ga content is preferably 0.65 to 1.8%, for example, 0.65%, 0.85%, 1%, 1.05%, 1.2%, 1.25%, 1.45%, 1.55%, or 1.8%, more preferably 0.65 to 1.25%, in mass% based on the total mass of the raw material composition.
In the present invention, the content of Co is preferably 0.5 to 2.5%, for example, 0.5%, 1.05%, 1.5%, 1.55%, 2%, 2.45%, or 2.5%, more preferably 1.05 to 2%, by mass, based on the total mass of the raw material composition.
In the present invention, the content of Fe is preferably 61.8 to 68.36%, for example, 61.88%, 63.31%, 63.93%, 64.01%, 64.41%, 64.98%, 65.56%, 65.58%, 66.34%, 66.95%, 67.06%, 67.16%, 67.69% or 68.36%, more preferably 63.3 to 68%, in percentage by mass based on the total mass of the raw material composition.
In the present invention, when the N includes Ti, the content of Ti is preferably 0.2 to 0.25%, for example, 0.2%, 0.22%, or 0.25%, in percentage by mass based on the total mass of the raw material composition.
In the present invention, when the N contains Zr, the content of Zr is preferably 0.25 to 0.35%, for example, 0.26%, 0.3%, or 0.35%, in percentage by mass based on the total mass of the raw material composition.
In the present invention, when the N contains Zr, the content of Zr preferably satisfies: zr is more than or equal to 0.20 percent and less than (3.48B-2.67 percent), wherein B refers to the mass percent of the B in the total mass of the raw material composition.
In the present invention, when the N includes Nb, the content of Nb is preferably 0.2 to 0.25% by mass of the total mass of the raw material composition.
In the present invention, when the N includes Ti and Nb, preferably, the Ti/Nb is greater than or equal to 1.5, where Ti is a mass percentage in the raw material composition, and Nb is a mass percentage in the raw material composition.
In the present invention, the raw material composition of the rare earth permanent magnetic material preferably includes the following components by mass: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 61.8-68.36%; n: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.25%; when the N contains Zr, the content of Zr is 0.25-0.35%; when the N contains Nb, the content of Nb is 0.2-0.35%; the raw material composition does not contain Cu and Al; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the present invention, the raw material composition of the rare earth permanent magnetic material preferably includes the following components by mass: r: 29.4-31.5%; the R is a rare earth element and comprises Nd and Pr; pr: 0.1-0.5% or 17-25%; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 63.3-68% N: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.25%; when the N contains Zr, the content of Zr is 0.25-0.35%; when the N contains Nb, the content of Nb is 0.2-0.35%; the raw material composition does not contain Cu and Al; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the present invention, the raw material composition of the rare earth permanent magnetic material preferably includes the following components by mass: r: 29.4-31.5%; r is a rare earth element and at least comprises Nd; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 63.3-68.5%; ti: 0.2-0.25%; the raw material composition does not contain Cu and Al; the percentage is the mass percentage of each component in the total mass of the raw material composition.
In the present invention, the raw material composition of the rare earth permanent magnetic material preferably includes the following components by mass: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 62-67.5%; zr: 0.25 to 0.35 percent; the raw material composition does not contain Cu and Al; 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 rare earth permanent magnetic material comprises the following components: 29.3 percent of Nd; 0.2 percent of Pr; ga 0.65%; 0.5 percent of Co; 0.15 percent of Ti; 0.84 percent of B; fe 68.36%; 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 rare earth permanent magnetic material comprises the following components: 30.2 percent of Nd; 0.3 percent of Pr; ga 0.85%; 1.05 percent of Co; 0.2 percent of Ti; 0.2 percent of Nb; b0.86%; fe68.34 percent; 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 rare earth permanent magnetic material comprises the following components: nd is 31 percent; 0.3 percent of Pr; ga 1.05 percent; 1.55 percent of Co; 0.22 percent of Ti; 0.9 percent of B; fe 64.98%; 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 rare earth permanent magnetic material comprises the following components: 12.5 percent of Nd; pr is 18.5 percent; ga 1.45 percent; 2% of Co; 0.22 percent of Ti; 0.92 percent of B; fe 64.41%; 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 rare earth permanent magnetic material comprises the following components: 9.5 percent of Nd; 21.5 percent of Pr; ga 1.8 percent; 2.45 percent of Co; 0.25 percent of Ti; 0.25 percent of Nb; 0.94 percent of B; fe63.31%; 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 rare earth permanent magnetic material comprises the following components: 30.2 percent of Nd; 0.3 percent of Pr; ga 1.05 percent; 1.5 percent of Co; 0.26 percent of Zr; 0.25 percent of Nb; b is 0.88; fe65.56%; 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 rare earth permanent magnetic material comprises the following components: 8.5 percent of Nd; 21.5 percent of Pr; ga 1.2 percent; 0.5 percent of Co; 0.3 percent of Zr; 0.94 percent of B; fe 67.06%; 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 materials of the rare earth permanent magnetic material comprise the following components by mass: 8.5 percent of Nd; 21.5 percent of Pr; ga 1.2 percent; 0.5 percent of Co; 0.2 percent of Zr; 0.94 percent of B; fe 67.16%; 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 rare earth permanent magnetic material comprises the following components: 29.3 percent of Nd; 0.2 percent of Pr; ga 1.25 percent; 0.5 percent of Co; 0.2 percent of Zr; b0.86%; fe 67.69%; 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 rare earth permanent magnetic material comprises the following components: 12.5 percent of Nd; pr is 18.5 percent; ga 1.55 percent; 0.5 percent of Co; 0.26 percent of Zr; 0.25 percent of Nb; b0.86%; fe65.58%; 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 rare earth permanent magnetic material comprises the following components: 9.5 percent of Nd; 21.5 percent of Pr; ga 1.8 percent; 2% of Co; 0.35 percent of Zr; 0.92 percent of B; fe 63.93%; 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 rare earth permanent magnetic material comprises the following components: nd29 percent; 0.3 percent of Pr; ga 0.65%; 2% of Co; 0.2 percent of Zr; 0.9 percent of B; fe 66.95%; 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 rare earth permanent magnetic material comprises the following components: 12.3 percent of Nd; pr 17%; ga 0.65%; 2% of Co; 0.2 percent of Zr; 0.9 percent of B; fe 66.95%; 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 rare earth permanent magnetic material comprises the following components: 28.5 percent of Nd; pr 1.5%; tb 2%; ga 0.85%; 2% of Co; 0.26 percent of Zr; 0.88 percent of B; fe 64.01 percent; 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 rare earth permanent magnetic material comprises the following components: 12.5 percent of Nd; pr is 18.5 percent; dy 2%; ga 1 percent; 2.5 percent of Co; 0.15 percent of Ti; 0.35 percent of Zr; 0.2 percent of Nb; 0.92 percent of B; fe 61.88%; the percentage is the mass percentage of each component in the total mass of the raw material composition.
The invention also provides a preparation method of the rare earth permanent magnetic material, which comprises the following steps:
the raw material composition of the rare earth permanent magnet material is subjected to casting, milling, forming, sintering and aging treatment.
In the present invention, the person skilled in the art knows that the casting usually also comprises smelting.
Wherein the smelting operations and conditions may be conventional in the art. The vacuum degree of the smelting can be 0.05 Pa. The temperature of the smelting can be below 1500 ℃. The smelting equipment can be a high-frequency vacuum induction smelting furnace.
In the present invention, the casting operation and conditions may be those conventional in the art. The casting is typically at 10 deg.f2DEG C/sec-104Cooling at a rate of DEG C/sec to prepare an alloy sheet. The atmosphere for the casting may typically be argon. The casting pressure may typically be 5.5 x 104Pa。
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 23.4 ℃, 22.5 ℃, 22.8 ℃, 23.1 ℃, 23.4 ℃, 23.6 ℃ or 23.8 ℃, and more preferably 23-23.8 ℃. The roller may be a copper roller.
In the present invention, the operation and conditions for milling can be those conventional in the art. 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 for example, the hydrogen breaking process 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, the jet milling process can be a jet milling process which is conventional in the field, and the jet milling process can be carried out under a nitrogen atmosphere with the content of the oxidizing gas of below 120 ppm. The oxidizing gas refers to oxygen or moisture content.
The pressure of the crushing chamber in the jet milling process can be 0.3-0.4 MPa, such as 0.38 MPa.
The duration of the jet milling process may be 2 to 4 hours, for example 3 hours.
After the jet milling process, 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.
In the present invention, the molding operation and conditions may be those conventional in the art. Including, for example, magnetic field forming or hot-press hot-deformation.
In the present invention, the sintering operation and conditions may be sintering operation conditions conventional in the art.
Wherein the sintering environment may be a vacuum. The vacuum may have a pressure of 5 x 10-3Pa。
Wherein, the sintering also comprises preheating before. The preheating temperature can be 300-600 ℃. The preheating time can be 1-2 h. The preheating is preferably at a temperature of 300 ℃ and 600 ℃ for 1 hour each.
Wherein the sintering temperature is preferably 1050 to 1095 ℃, such as 1063 ℃, 1065 ℃, 1073 ℃, 1075 ℃, 1080 ℃, 1090 ℃ or 1092 ℃, more preferably 1063 to 1090 ℃.
The sintering time is preferably 5-10 h, such as 8 h.
In the present invention, the aging treatment preferably includes a primary aging treatment and a secondary aging treatment.
Wherein, the temperature of the primary aging treatment is preferably 850-950 ℃, and more preferably 900 ℃.
The time of the primary aging treatment is preferably 2 to 4 hours, for example 3 hours, and the time refers to the time at the temperature of the primary aging treatment.
The temperature of the secondary aging treatment is preferably 455-470 ℃, such as 455 ℃, 460 ℃ or 470 ℃.
The time of the secondary aging treatment is preferably 2 to 4 hours, for example 3 hours, and the time refers to the time at the temperature of the secondary aging treatment.
Wherein the rate of raising the temperature to the temperature of the primary aging treatment or the secondary aging treatment can be conventional in the art, and is usually 3-5 ℃/min.
The invention also provides the rare earth permanent magnetic material prepared by the preparation method.
The invention also provides a rare earth permanent magnetic material which comprises the following components in percentage by mass:
r: 28.5 to 33 percent; r is a rare earth element and at least comprises Nd;
B：0.84～0.943％；
Ga：0.6<Ga≤1.804％；
co: less than or equal to 2.5 percent and not 0;
Al：<0.08％；
Fe：61.6～69％；
n: one or more of Ti, Zr and Nb;
when the N contains Ti, the content of the Ti is 0.15-0.252%;
when the N contains Zr, the content of Zr is 0.2-0.351%;
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 rare earth permanent magnet material.
In the present invention, the grain boundary phase of the rare earth permanent magnetic material preferably further includes R6T13And (4) an M phase. Wherein R is a rare earth element, T is Fe and/or Co, and M is Ga.
Wherein, R is6T13The volume of the M phase is preferably 2-12% of the total volume of the main phase, the grain boundary phase and the rare earth-rich phase; more preferably 2.5-11.5%, such as 2.5%, 3.6%, 3.7%, 4.8%, 5.2%, 5.7%, 6.5%, 10.2%, 10.5%, 11.3% or 11.5%, more preferably 5-11%.
In the present invention, the grain boundary phase refers to two or more Nd2T4B is a general term for grain boundary phases between grains. Wherein, the Nd2Tl4B grains refer to the main phase, and T refers to Fe and/or Co.
In the rare earth permanent magnet material, the content of R is preferably 29.3 to 32%, for example, 29.296%, 29.308%, 29.486%, 29.494%, 30.004%, 30.01%, 30.485%, 30.5028%, 30.994%, 30.996%, 30.999%, 31.194% or 31.986%, more preferably 29.4 to 31.5%, in percentage by mass based on the total mass of the rare earth permanent magnet material.
In the present invention, the content of Nd is preferably 8 to 13%, for example, 8.501%, 8.506%, 9.491%, 9.494%, 12.303%, 12.491%, 12.497% or 12.503%; or, the content of Nd is preferably 28 to 31%, for example, 28.497%, 29.002%, 29.291%, 29.302%, 30.194%, 30.202% or 30.891%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
In the present invention, the rare earth permanent magnetic material preferably does not contain Cu.
In the rare earth permanent magnetic material, the R may also include Pr.
Wherein, the content of Pr is preferably less than 1.5% and not 0, more preferably 0.1-0.5%, such as 0.192%, 0.195%, 0.291%, 0.294%, 0.301%, 0.303%, or 1.502%; or the content of Pr is preferably 17 to 25%, for example, 17.005%, 18.502%, 18.503%, 21.502%, 21.503%, 21.504% or 21.505%, more preferably 18.5 to 21.505%, by mass, based on the total mass of the rare earth permanent magnetic material.
In the invention, the rare earth permanent magnetic material does not contain heavy rare earth elements, and can reach the level equivalent to or even better than the magnetic performance of the magnet material in the prior art. Or, the rare earth permanent magnetic material can also comprise RH, wherein the RH is a heavy rare earth element.
When the rare earth permanent magnet material contains RH, the content of the RH is preferably 1-2.5%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet 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%, for example, 1.992%, in mass percentage based on the total mass of the rare earth permanent magnet material.
When the RH includes Tb, the content of Tb is preferably 1 to 2.5%, for example 1.987%, by mass, based on the total mass of the rare earth permanent magnet material.
In the present invention, the content of B is preferably 0.861 to 0.943%, for example, 0.861%, 0.862%, 0.864%, 0.878%, 0.882%, 0.895%, 0.897%, 0.902%, 0.918%, 0.921%, 0.922%, 0.942%, or 0.943%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
In the rare earth permanent magnet material, the atomic percentage of R and the atomic percentage of B preferably satisfy the following relational expression: B/R is more than or equal to 0.38, wherein B is the atomic percentage in the rare earth permanent magnet material, and R is the atomic percentage in the rare earth permanent magnet material.
In the present invention, when Pr is included in the rare earth permanent magnetic material, preferably, B and Nd satisfy the following relation: B/(Pr + Nd) is more than or equal to 0.405, wherein B refers to the atomic percent of B in the rare earth permanent magnet material, Pr refers to the atomic percent of Pr in the rare earth permanent magnet material, and Nd refers to the atomic percent of Nd in the rare earth permanent magnet material.
In the present invention, the Ga content is preferably 0.65 to 1.804%, for example, 0.651%, 0.652%, 0.655%, 0.851%, 0.853%, 1.005%, 1.052%, 1.201%, 1.203%, 1.252%, 1.452%, 1.552%, 1.802%, 1.804%, more preferably 0.65 to 1.25%, in mass% based on the total mass of the rare earth permanent magnet material.
In the present invention, the content of Co is preferably 0.5 to 2.5%, for example, 0.502%, 0.503%, 0.504%, 0.505%, 1.047%, 1.502%, 1.554%, 1.987%, 1.989%, 2.003%, 2.005%, 2.452%, or 2.502%, more preferably 1.05 to 2.005%, by mass based on the total mass of the rare earth permanent magnetic material.
In the present invention, the content of Al is preferably 0.02 to 0.06%, more preferably 0.025 to 0.053%, for example, 0.025%, 0.031%, 0.035%, 0.042%, 0.043%, 0.051%, 0.052%, or 0.053%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
In the present invention, the content of Fe is preferably 61.8 to 68.36%, for example, 61.826%, 63.253%, 63.891%, 63.973%, 64.361%, 65.039%, 65.517%, 65.521%, 66.292%, 66.912%, 66.923%, 67.017%, 67.1%, 67.647% or 68.323%, more preferably 63.3 to 68.36%, in percentage by mass based on the total mass of the rare earth permanent magnet material.
In the present invention, the content of Ti is preferably 0.151 to 0.252%, for example, 0.151%, 0.154%, 0.205%, 0.222%, 0.224%, or 0.252%, and more preferably 0.2 to 0.252%, by mass, based on the total mass of the rare earth permanent magnet material.
In the present invention, the content of Zr is preferably 0.25 to 0.351%, for example, 0.202%, 0.203%, 0.205%, 0.207%, 0.262%, 0.302%, or 0.351%, in percentage by mass based on the total mass of the rare earth permanent magnet material.
In the present invention, when Zr is contained in the rare earth permanent magnetic material, the content of Zr preferably satisfies: zr is more than or equal to 0.20 percent and less than (3.48B-2.67 percent), wherein B refers to the mass percent of B in the total mass of the rare earth permanent magnet material.
In the present invention, the content of Nb is preferably 0.2 to 0.25%, for example, 0.202%, 0.251%, or 0.252%, and the percentage is a mass percentage of the total mass of the rare earth permanent magnet material.
In the invention, when the rare earth permanent magnet material contains Ti and Nb, preferably, the Ti/Nb ratio is more than or equal to 1.5, wherein Ti is the mass percentage in the rare earth permanent magnet material, and Nb is the mass percentage in the rare earth permanent magnet material.
In the present invention, the rare earth permanent magnetic material preferably comprises the following components by mass: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.02-0.06%; fe: 61.8-68.36%; n: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.252%; when the N contains Zr, the content of Zr is 0.25-0.351%; when the N contains Nb, the content of Nb is 0.2-0.35%; the rare earth permanent magnetic material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13The ratio of the volume of the Ga phase to the total volume of the main phase, the grain boundary phase and the rare earth-rich phase is 2.5-11.5%.
In the present invention, the rare earth permanent magnetic material preferably comprises the following components by mass: r: 29.4-31.5%; the R is a rare earth element and comprises Nd and Pr; pr: 0.1-0.5% or 17-25%; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.025 to 0.053%; fe: 63.3 to 68.36 percent; n: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.252%; when the N contains Zr, the content of Zr is 0.25-0.351%; when the N contains Nb, the content of Nb is 0.2-0.35%; the rare earth permanent magnetic material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13The ratio of the volume of the Ga phase to the total volume of the main phase, the grain boundary phase and the rare earth-rich phase is 5-11%.
In the present invention, the rare earth permanent magnetic material preferably comprises the following components by mass: r: 29.4-31.5%; r is a rare earth element and at least comprises Nd; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.025 to 0.053%; fe: 63.3-68.5%; ti: 0.2-0.252%; the rare earth permanent magnetic material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13The ratio of the volume of the Ga phase to the total volume of the main phase, the grain boundary phase and the rare earth-rich phase is 5.7-11.3%.
In the present invention, the rare earth permanent magnetic material preferably comprises the following components by mass: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.025 to 0.053%; fe: 62-67.5%; zr: 0.25 to 0.351 percent; the rare earth permanent magnetic material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13The ratio of the volume of the Ga phase to the total volume of the main phase, the grain boundary phase and the rare earth-rich phase is 2.5-11.5%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd29.302 percent; pr is 0.192 percent; ga 0.651%; 0.505% of Co; 0.031% of Al; 0.151 percent of Ti; 0.845% of B; fe68.323 percent; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 5.7%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by mass: nd30.194 percent; pr 0.291%; ga 0.853%; 1.047% of Co; al (Al)0.052 percent; 0.205 percent of Ti; nb 0.202 percent; 0.864 percent of B; fe 66.292%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 5.2%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd30.891%; pr 0.303%; ga 1.052%; 1.554 percent of Co; 0.042% of Al; 0.222% of Ti; b0.897%; fe65.039%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 3.6%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd12.497%; pr 18.502%; ga 1.452 percent; 1.989% of Co; 0.053 percent of Al; 0.224 percent of Ti; b0.922%; fe64.361%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 11.3%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd 9.491%; pr 21.505%; ga 1.802%; 2.452% of Co; 0.051 percent of Al; 0.252 percent of Ti; nb 0.252%; b0.942%; fe 63.253%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 10.2%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd30.202 percent; pr 0.301%; ga 1.052%; 1.502% of Co; 0.035% of Al; 0.262 percent of Zr; nb 0.251%; 0.878% of B; fe 65.517%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the rare earth permanent magnet materialIn the material R6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 6.5%.
In a preferred embodiment of the invention, the rare earth permanent magnetic material comprises the following components of Nd 8.506%; pr 21.504%; ga 1.201%; 0.502% of Co; 0.025 percent of Al; 0.302 percent of Zr; 0.943 percent of B; fe67.017 percent; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 5.7%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd 8.501%; pr 21.503%; ga 1.203 percent; 0.503 percent of Co; 0.043 percent of Al; 0.205 percent of Zr; b0.942%; fe 67.1%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 5.2%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd29.291%; pr is 0.195 percent; ga 1.252%; 0.504% of Co; 0.042% of Al; 0.207% of Zr; b0.862%; fe67.647%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 3.6%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd12.491%; pr 18.503%; ga 1.552%; 0.505% of Co; 0.053 percent of Al; 0.262 percent of Zr; nb 0.252%; b0.861%; fe 65.521%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 11.3%.
In a preferred embodiment of the present invention, the rare earth element isThe magnetic material comprises the following components in percentage by weight: nd 9.494%; pr 21.502%; ga 1.804%; 1.989% of Co; 0.051 percent of Al; 0.351 percent of Zr; b0.918%; fe63.891%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 11.5%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd29.002%; pr 0.294%; ga 0.655%; 2.005% of Co; 0.035% of Al; 0.202 percent of Zr; 0.895% of B; fe66.912%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 3.7%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd12.303 percent; pr 17.005%; ga 0.652%; 1.987 percent of Co; 0.025 percent of Al; 0.203 percent of Zr; b0.902%; fe66.923 percent; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 4.8%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by mass: nd28.497%; pr 1.502%; tb 1.987%; ga 0.851%; 2.003 percent of Co; 0.043 percent of Al; 0.262 percent of Zr; b0.882%; fe 63.973%; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 2.5%.
In a preferred embodiment of the present invention, the rare earth permanent magnetic material comprises the following components by weight: nd12.503 percent; pr 18.502%; 1.992 percent of Dy; ga 1.005%; 2.502 percent of Co; 0.042% of Al; 0.154 percent of Ti; 0.351 percent of Zr; nb 0.202 percent; b0.921%; fe 61.826%;the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; r in the rare earth permanent magnetic material6T13The ratio of the volume of the Ga phase to the total volume of the "main phase, grain boundary phase and rare earth-rich phase" was 10.5%.
The invention also provides an application of the rare earth permanent magnetic material as an electronic component.
The application field can be the automobile driving field, the wind power field, the servo motor field and the household appliance field (such as an air conditioner).
In the present invention, the room temperature means 25 ℃. + -. 5 ℃.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
(1) the elements with specific content in the rare earth permanent magnet material are matched with each other, and the prepared rare earth permanent magnet material contains R with specific content6T13Ga. The rare earth permanent magnetic material contains a small amount (0.84-0.943%) of boron element, and can obtain better remanence, coercive force, squareness and temperature stability without adding heavy rare earth elements.
(2) The rare earth permanent magnet material not only can obtain a permanent magnet material with better magnetic property, but also improves the consistency of the rare earth permanent magnet material under the condition of not adding a proper amount of Al, namely the magnetic property of the same batch of products 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.
1. Example 1
The raw materials used for preparing the rare earth permanent magnet material in the example are shown in table 1, and the preparation process is as follows:
(1) and (3) smelting: according to the formulation shown in example 1 of Table 1, the prepared raw materials were placed in a crucible made of alumina and placed in a high-frequency vacuum induction melting furnace at 5X 10-2Vacuum melting is carried out at a temperature of 1500 ℃ or lower in a vacuum of Pa.
(2) The casting process comprises the following steps: introducing Ar gas into a smelting furnace after vacuum smelting to enable the air pressure to reach 5.5 ten thousand Pa, then casting, and enabling the molten liquid to pass through a copper roller with the rotation speed of 29 revolutions per minute to prepare a rapid hardening alloy sheet with the thickness of 0.12-0.35mm, wherein in the casting process, chilled water needs to be introduced into the copper roller, and the water inlet temperature is 23.4 ℃; at 102DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(3) Hydrogen crushing and crushing: vacuumizing the hydrogen breaking furnace in which the quenching alloy is placed at room temperature, introducing hydrogen with the purity of 99.9% into the hydrogen breaking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, vacuumizing while heating, fully dehydrogenating, cooling, and taking out the powder after hydrogen breaking and crushing.
(4) A micro-grinding process: the powder after hydrogen crushing was pulverized by jet milling for 3 hours under a nitrogen atmosphere having an oxidizing gas content of 120ppm or less and a pressure in the pulverization chamber of 0.38MPa to obtain a fine powder. The oxidizing gas refers to oxygen or moisture.
(5) Adding zinc stearate into the powder crushed by the jet mill, wherein the adding amount of the zinc stearate is 0.12 percent of the weight of the mixed powder, and then fully mixing the zinc stearate and the mixed powder by using a V-shaped mixer.
(6) Magnetic field forming process: using a magnetic field forming machine of a 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 10-3Pa at 300 deg.C and 600 deg.C for 1 hrThen, the mixture was sintered at 1090 ℃ for 8 hours, and then Ar gas was introduced so that the pressure became 0.1MPa, followed by cooling to room temperature.
(8) And (3) aging treatment process: and (3) heating the sintered body from 20 ℃ to 900 ℃ at the heating rate of 3-5 ℃/min in high-purity Ar gas, carrying out first-stage aging treatment at the temperature of 900 ℃ for 3 hours, cooling to room temperature, and taking out. And then heating from 20 ℃ to 470 ℃ at a heating rate of 3-5 ℃/min, and carrying out secondary aging at 470 ℃.
2. The raw material compositions of the rare earth permanent magnet materials of examples 1 to 13 and comparative examples 1 to 12, and the water inlet temperature, sintering temperature and secondary aging temperature of the copper roller in the preparation method are shown in the following table 1.
TABLE 1
Note: "/" means that the element is not included. The wt% is mass percent.
2. The formulations of the raw material compositions of the rare earth permanent magnet materials in examples 2 to 13 and comparative examples 1 to 12 are shown in table 1, and the parameters of the preparation methods are the same as those of example 1 except that the sintering temperature, the copper roll inlet water temperature and the secondary aging temperature are the same as those in table 1.
It should be noted that: the magnetic performance of the neodymium iron boron materials in the comparative examples 1-6 is the best performance obtained by the formula of the comparative examples 1-6 after process optimization (aging temperature, sintering temperature or water inlet temperature).
3. Component determination: the rare earth permanent magnetic materials in examples 1 to 13 and comparative examples 1 to 12 were measured by using a high-frequency inductively coupled plasma emission spectrometer (ICP-OES). The test results are shown in table 2 below.
TABLE 2 composition and content (wt%) of rare earth permanent magnet material
Note: "/" means that the element is not included. The wt% is mass percent.
Effect example 1 detection of magnetic Properties of rare-earth permanent magnet materials in examples 1 to 13 and comparative examples 1 to 6
1. Microstructure: the perpendicular orientation plane of the rare earth permanent magnetic material was polished by FE-EPMA detection, and detected by field emission electron probe microanalyzer (FE-EPMA) (JEOL 8530F, Japan Electron Ltd.). Detection of R in grain boundaries6T13Ga phase and R6T13Al phase, T refers to Fe and/or Co. The test results are shown in table 3 below.
Wherein R is6T13Ga phase and R6T13The ratio of Al phase content was measured as the average value of the ratios of 5 rare earth permanent magnetic materials in the same batch among the rare earth permanent magnetic materials in each example and comparative example, which were calculated.
2. Remanence and coercive force: the sintered magnet is detected by using an NIM-10000H type BH large rare earth permanent magnet nondestructive measurement system of China measurement institute. And the temperature coefficient of remanence and the temperature coefficient of coercive force are obtained by calculation. The test results are shown in table 3 below.
Wherein, the Br or Hcj mean value refers to: and (3) calculating an average value by testing the residual magnetism or the coercive force of 5 rare earth permanent magnetic materials in the same batch.
3. Consistency detection of magnetic properties of rare earth permanent magnetic materials
Squareness ═ Hk/Hcj; where Hk is the value of the external magnetic field H when Br is 90% Br, and Hcj is the coercive force.
The relative magnetic permeability is Br/Hcb; wherein Br is remanence, Hcb is magnetic induction coercive force, and when an inflection point exists in the J-H curve, the magnetic conductivity is taken before the inflection point.
Max (Max hcj) -Min (hcj): in the same example or the same comparative example, the coercivity minimum value is subtracted from the coercivity maximum value, and if it is more than 1.5kOe, the magnetic uniformity is poor. The test results are shown in table 3 below.
Several ndfeb materials were prepared in each example and comparative example of the present invention, and the same lot refers to several ndfeb materials obtained in each example and comparative example. For each test in table 3, each ndfeb material refers to a 10mm by 10mm cylinder cut according to the unit of performance test.
TABLE 3
Note: "X" means no R6T13Ga phase or R6T13The other parameters in table 3 are the average values of 5 nd fe-b materials measured in the same batch except max (Hcj) -min (Hcj). the data in table 3 for Br temperature coefficient α (Br)%/° c at 20-80 ℃, Hcj temperature coefficient β (Hcj)%/° c at 20-80 ℃, Br temperature coefficient β (Hcj)%/° c at 20-150 ℃, and Hcj temperature coefficient β (Hcj)%/° c at 20-150 ℃ are absolute values.
Claims (10)
1. The raw material composition of the rare earth permanent magnetic material is characterized by comprising the following components in percentage by mass:
r: 28.5 to 33 percent; r is a rare earth element and at least comprises Nd;
B：0.84～0.94％；
Ga：0.6<Ga≤1.8％；
co: less than or equal to 2.5 percent and not 0;
Fe：61.6～69％；
n: one or more of Ti, Zr and Nb;
when the N contains Ti, the content of the Ti is 0.15-0.25%;
when the 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 rare earth permanent magnet material.
2. The raw material composition according to claim 1, wherein the content of R in the raw material composition is 29.3 to 32%, preferably 29.4 to 31.5%, in percentage by mass based on the total mass of the raw material composition;
and/or the content of Nd is 8-13%, or 28-31%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or, the raw material composition does not contain Cu;
and/or, the raw material composition does not contain Al;
and/or, in the raw material composition, the R also comprises Pr;
wherein, the content of Pr is preferably less than 1.5% and not 0, or 17-25%; the content of Pr is more preferably 0.1-0.5%, or 18.5-21.5%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or, the raw material composition also comprises RH which is a heavy rare earth element;
wherein the RH preferably includes one or more of Dy, Tb and Ho;
when the RH comprises Dy, the content of Dy is preferably 1-2.5% by mass of the total mass of the raw material composition;
when the RH comprises Tb, the content of Tb is preferably 1-2.5%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or the content of B is 0.86-0.94%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or the atomic percent of R and the atomic percent of B in the raw material composition satisfy the following relational expression: B/R is more than or equal to 0.38, wherein B is the atomic percentage in the rare earth permanent magnet material, and R is the atomic percentage in the rare earth permanent magnet material;
and/or the content of Ga is 0.65-1.8%, preferably 0.65-1.25%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or the content of Co is 0.5-2.5%, preferably 1.05-2%, and the percentage is the mass percentage of the total mass of the raw material composition;
and/or the content of Fe is 61.8-68.36%, preferably 63.3-68.36%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or when the N contains Ti, the content of the Ti is 0.2-0.25 percent, 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 Zr is 0.25-0.35 percent, and the percentage is the mass percentage of the total mass of the raw material composition;
wherein, when the N contains Zr, the mass content of Zr preferably satisfies: zr is more than or equal to 0.20 percent and less than (3.48B-2.67 percent), wherein B refers to the mass percent of the B in the total mass of the raw material composition;
and/or when the N contains Nb, the content of Nb is 0.2-0.25%, and the percentage is the mass percentage of the total mass of the raw material composition.
3. The raw material composition of claim 1 or 2, wherein the raw material composition of the rare earth permanent magnetic material comprises the following components in percentage by mass: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 61.8-68.36%; n: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.25%; when the N contains Zr, the content of Zr is 0.25-0.35%; when the N contains Nb, the content of Nb is 0.2-0.35%; the raw material composition does not contain Cu and Al; 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 rare earth permanent magnetic material comprises the following components in percentage by mass: r: 29.4-31.5%; the R is a rare earth element and comprises Nd and Pr; pr: 0.1-0.5% or 17-25%; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 63.3-68%; n: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.25%; when the N contains Zr, the content of Zr is 0.25-0.35%; when the N contains Nb, the content of Nb is 0.2-0.35%; the raw material composition does not contain Cu and Al; 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 rare earth permanent magnetic material comprises the following components in percentage by mass: r: 29.4-31.5%; r is a rare earth element and at least comprises Nd; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 63.3-68.5%; ti: 0.2-0.25%; the raw material composition does not contain Cu and Al; the percentage is the mass percentage of each component in the total mass of the raw material composition;
or the raw material composition of the rare earth permanent magnetic material comprises the following components in percentage by mass: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.94%; ga: 0.65-1.8%; co: 0.5-2.5%; fe: 62-67.5%; zr: 0.25 to 0.35 percent; the raw material composition does not contain Cu and Al; the percentage is the mass percentage of each component in the total mass of the raw material composition.
4. The preparation method of the rare earth permanent magnetic material is characterized by comprising the following steps of: a raw material composition of the rare earth permanent magnet material as claimed in any one of claims 1 to 3 is subjected to casting, milling, forming, sintering and aging treatment.
5. The method of claim 4, wherein the casting further comprises melting;
wherein the smelting temperature is preferably below 1500 ℃;
and/or said casting is at 102DEG C/sec-104Cooling at a speed of DEG C/second;
wherein the cooling is preferably realized by introducing cooling water into the rollers;
the water inlet temperature of the roller is preferably less than or equal to 25 ℃, and more preferably 23-23.8 ℃;
and/or, the milling comprises a hydrogen crushing process and an airflow milling process;
wherein, the hydrogen breaking process preferably comprises hydrogen absorption, dehydrogenation and cooling treatment;
wherein the jet milling process is preferably carried out under a nitrogen atmosphere having an oxidizing gas content of 120ppm or less;
wherein, the pressure of the crushing chamber of the jet milling process is preferably 0.3-0.4 MPa;
wherein the time of the air flow milling process is preferably 2-3 hours;
after the jet milling process, a lubricant is preferably added into the powder; the addition amount of the lubricant is preferably 0.10-0.15% of the weight of the mixed powder;
and/or, the forming comprises a magnetic field forming method or a hot-pressing hot-deformation method;
and/or, the sintering also comprises preheating; the preheating temperature is preferably 300-600 ℃; the preheating time is preferably 1-2 h;
and/or the sintering temperature is 1050-1095 ℃, preferably 1063-1090 ℃;
and/or the sintering time is 5-10 h;
and/or the aging treatment comprises primary aging treatment and secondary aging treatment;
wherein, the temperature of the first-stage aging treatment is preferably 850-950 ℃, and more preferably 900 ℃;
wherein the time of the primary aging treatment is preferably 2-4 h;
wherein, the temperature of the secondary aging treatment is preferably 455-470 ℃, more preferably 455 ℃, 460 ℃ or 470 ℃;
wherein the time of the secondary aging treatment is preferably 2-4 h;
wherein the rate of raising the temperature to the temperature of the primary or secondary aging treatment is preferably 3to 5 ℃/min.
6. A rare earth permanent magnetic material obtained by the production method according to claim 4 or 5.
7. The rare earth permanent magnetic material is characterized by comprising the following components in percentage by mass:
r: 28.5 to 33 percent; r is a rare earth element and at least comprises Nd;
B：0.84～0.943％；
Ga：0.6<Ga≤1.804％；
co: less than or equal to 2.5 percent but not 0 percent;
Al：<0.08％；
Fe：61.6～69％；
n: one or more of Ti, Zr and Nb;
when the N contains Ti, the content of the Ti is 0.15-0.252%;
when the N contains Zr, the content of Zr is 0.2-0.351%;
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 rare earth permanent magnet material.
8. The rare earth permanent magnetic material as claimed in claim 7, further comprising R in the grain boundary phase of the rare earth permanent magnetic material6T13An M phase;
wherein, R is6T13The volume of the M phase is preferably 2-12% of the total volume of the main phase, the grain boundary phase and the rare earth-rich phase; more preferably 2.5 to 11.5%;
and/or in the rare earth permanent magnet material, the content of R is 29.3-32%, preferably 29.4-31.5%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the content of Nd is 8-13%, or 28-31%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the rare earth permanent magnetic material does not contain Cu;
and/or the content of Pr is less than 1.5% and not 0, or 17-25%; preferably 0.1-0.5%, or 18.5-21.505%, the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or, the rare earth permanent magnetic material also comprises RH which is a heavy rare earth element;
when the rare earth permanent magnet material contains RH, the content of the RH is preferably 1-2.5%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
wherein the RH preferably includes one or more of Dy, Tb and Ho;
when the RH contains Dy, the content of Dy is preferably 1-2.5%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
when the RH comprises Tb, the content of Tb is preferably 1-2.5%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the content of B is 0.861-0.943%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the atomic percent of R and the atomic percent of B in the rare earth permanent magnet material satisfy the following relational expression: B/R is more than or equal to 0.38, wherein B is the atomic percentage in the rare earth permanent magnet material, and R is the atomic percentage in the rare earth permanent magnet material;
and/or the Ga content is 0.65-1.804%, preferably 0.65-1.25%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the content of Co is 0.5-2.5%, preferably 1.05-2.005%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the Al content is 0.02-0.06%, preferably 0.025-0.053%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the content of Fe is 61.8-68.36%, preferably 63.3-68.36%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the content of Ti is 0.151-0.252%, preferably 0.2-0.252%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
and/or the Zr content is 0.25-0.351%, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material;
when Zr is contained in the rare earth permanent magnetic material, the content of Zr preferably satisfies: zr is more than or equal to 0.20 percent and less than (3.48B-2.67 percent), wherein B refers to the mass percent of B in the total mass of the rare earth permanent magnet material;
and/or the content of Nb is 0.2-0.25 percent, and the percentage is the mass percentage of the total mass of the rare earth permanent magnet material.
9. The rare earth permanent magnetic material according to claim 7 or 8, wherein the rare earth permanent magnetic material comprises the following components in percentage by weight: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.02-0.06%; fe: 61.88 to 68.36 percent; n: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.252%; when the N contains Zr, the content of Zr is 0.25-0.351%; when the N contains Nb, the content of Nb is 0.2-0.35%; the rare earth permanent magnetic material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13The ratio of the volume of the Ga phase to the total volume of the main phase, the grain boundary phase and the rare earth-rich phase is 2.5-11.5%;
or, the rare earth permanent magnetic material comprises the following components by mass: r: 29.4-31.5%; the R is a rare earth element and comprises Nd and Pr; pr: 0.1-0.5% or 17-25%; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.025 to 0.053%; fe: 63.3 to 68.36 percent; n: one or more of Ti, Zr and Nb; when the N contains Ti, the content of the Ti is 0.2-0.252%; when the N contains Zr, the content of Zr is 0.25-0.351%; when the N contains Nb, the content of Nb is 0.2-0.35%; the rare earth permanent magnetic material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13The ratio of the volume of the Ga phase to the total volume of the main phase, the grain boundary phase and the rare earth-rich phase is 5-11%;
or, the rare earth permanent magnetic material comprises the following components by mass: r: 29.4-31.5%; r is a rare earth element and at least comprises Nd; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.025 to 0.053%; fe: 63.3-68.5%; ti: 0.2-0.252%; the rare earth permanent magnetic material does not contain Cu; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13The ratio of the volume of the Ga phase to the total volume of the main phase, the grain boundary phase and the rare earth-rich phase is 5.7-11.3%;
or, the rare earth permanent magnetic material comprises the following components by mass: r: 29.3-32%; r is a rare earth element and at least comprises Nd; b: 0.86-0.943%; ga: 0.65-1.8%; co: 0.5-2.5%; al: 0.025 to 0.053%; fe: 62-67.5%; zr: 0.25 to 0.351 percent; the rare earth permanent magnetic material does not contain Cu and Al; the percentage is the mass percentage of each component in the total mass of the rare earth permanent magnet material; the grain boundary phase of the rare earth permanent magnetic material also comprises R6T13Ga phase, said R6T13Of Ga phaseThe volume ratio of the main phase, the grain boundary phase and the rare earth-rich phase is 2.5-11.5%.
10. Use of a rare earth permanent magnetic material according to any of claims 7 to 9 as an electronic component.
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| CN112992462A (en) * | 2021-03-17 | 2021-06-18 | 福建省长汀金龙稀土有限公司 | R-T-B magnet and preparation method thereof |
| WO2021169899A1 (en) * | 2020-02-29 | 2021-09-02 | 厦门钨业股份有限公司 | Rare earth permanent magnet material, preparation method therefor and application thereof |
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| CN112992462A (en) * | 2021-03-17 | 2021-06-18 | 福建省长汀金龙稀土有限公司 | R-T-B magnet and preparation method thereof |
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