CN110957093B - R-T-B series magnet material, raw material composition, preparation method and application - Google Patents
R-T-B series magnet material, raw material composition, preparation method and application Download PDFInfo
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- 239000007789 gas Substances 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 5
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- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
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- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 101100065878 Caenorhabditis elegans sec-10 gene Proteins 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical group [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
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- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical group [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical group [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
-
- 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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
Landscapes
- 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 an R-T-B series magnet material, a raw material composition, a preparation method and application. The raw material composition of the R-T-B series magnet material comprises the following components in percentage by mass: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: more than or equal to 17.15 percent; cu: 1.3 percent; b: 0.9-1.2%; fe: 61-68% by mass of the total mass of the raw material composition of the R-T-B magnet material. The R-T-B series magnet material provided by the invention uses a formula of combining higher content of Pr with higher content of Cu, so that the coercive force of the R-T-B series magnet material can be obviously improved, and meanwhile, higher remanence can be maintained.
Description
Technical Field
The invention relates to an R-T-B series magnet material, a raw material composition, a preparation method and application.
Background
By Nd2Fe14The R-T-B system (NdFeB) magnet material with B as the main component has higher remanence, coercive force and maximum magnetic energy product, has excellent comprehensive magnetic performance, and is applied to the aspects of wind power generation, new energy automobiles, variable frequency household appliances and the like. At present, the rare earth component of the R-T-B magnet material in the prior art is mainly neodymium, only a small amount of Pr exists, and the performance of the magnet material can be improved by replacing a part of the Pr with the neodymium, but the improvement degree is limited. For example, the formula of the R-T-B magnet material disclosed in the currently reported Chinese patent document CN104979062A is as follows: 25-31 wt% of praseodymium, 0-5 wt% of neodymium, 0.12 wt% of gallium, 0.97E1% boron and other additive elements. The formula is added with a high content of praseodymium, but the coercive force can only reach 18kOe at most.
Disclosure of Invention
The invention aims to overcome the defect that the coercive force is improved to a limited extent after neodymium is replaced by partial Pr in an R-T-B series magnet material in the prior art, and provides the R-T-B series magnet material, a raw material composition, a preparation method and application. The R-T-B series magnet material provided by the invention uses higher content of Pr and higher content of Cu, so that the R-T-B series magnet material can maintain higher remanence while the coercive force is obviously improved.
The invention solves the technical problems through the following technical scheme.
The invention provides a raw material composition of an R-T-B series magnet material, which comprises the following components in percentage by mass:
r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: more than or equal to 17.15 percent;
Cu：>1.3％；
B：0.9～1.2％；
fe: 61-68% by mass of the total mass of the raw material composition of the R-T-B magnet material.
In the present invention, the content of R' is preferably 29.65 to 31.65%, for example, 29.65%, 30.15%, 30.3%, 30.35%, 30.65%, 31.15%, 31.35%, or 31.65%, and the percentage means a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
In the present invention, the content of Pr is preferably 17.15 to 28.15%, for example, 17.15%, 18.15%, 19.15%, 20.15%, 20.85%, 21.15%, 22.15%, 22.85%, 23.15%, 24.15%, 25.15%, 25.85%, 26.15%, or 28.15%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
In the present invention, the R' may further include Nd.
Wherein the mass ratio of Nd to R' is preferably less than 0.5, more preferably 0.08 to 0.45, for example, 9.5/31.65, 9.5/31.15, 9.5/30.65, 9.5/29.65, 8.5/31.35, 8.5/30.65, 7.5/30.65, 6.5/31.65, 6.5/30.65, 6.5/29.65, 5.5/31.65, 5.5/31.15, 5.5/30.65, 4.5/31.15, 4.5/30.65, 4.5/30.35, 4.5/29.65, 3.5/30.65, 3.5/30.15, 3.5/29.65, 2.5/30.65, 14/31.15, 13/31.15, 13.5/31.65, 13.5/30.65, 12/31.65, 12/31.15, 12/30.65, 12.5/30.65, 10.5/30.15/10.65, 10.5/30.10.10/30.15, 10.5/30.65, 10/10.10.10/10.5/30.15, 10.10.10/10.10.10.10.10.10/30.15, 10.10.10.10.10.10.10.15, 10.15, 10.10.5/30.15, 10.65.
The content of Nd is preferably 15% or less, more preferably 2.5 to 14.5%, for example, 2.5%, 3.5%, 4.5%, 5.5%, 6.5%, 7.5%, 8.5%, 9.5%, 10%, 10.15%, 10.5%, 11.5%, 12%, 12.5%, 13%, 13.5%, or 14%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
Wherein, said R' may also include Y.
In the present invention, the R' preferably further includes RH, which is a heavy rare earth element.
Wherein, the RH may be a heavy rare earth element conventional in the art, such as one or more of Dy, Tb and Ho, preferably Dy and/or Tb.
Wherein, the mass ratio of the RH to the R' can be the conventional mass ratio in the field, preferably less than 0.253, more preferably 0.1-1, such as 0, 1/31.65, 1.5/31.65, 2/31.65, 1.5/31.15, 1/30.65, 1/30.15, 2/31.35, 1/31.15, 0.5/30.15 or 1.5/30.15.
The RH content is preferably 2.5% or less, more preferably 0.5 to 2.5%, for example, 0.5%, 1%, 1.5% or 2%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
When Tb is contained in the RH, the content of Tb is preferably 0.5 to 2%, for example, 0.5%, 1%, 1.5%, or 2%, and the percentage means the mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
When Dy is contained in the RH, the content of Dy is preferably 0.5 to 2%, for example, 0.5%, 1%, or 1.5%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
In the present invention, the Cu content is preferably 1.3to 2.5%, for example, 1.31%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, 2%, 2.1%, 2.2%, 2.3%, 2.4%, or 2.5%, and the percentage means a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
In the present invention, the content of B is preferably 0.92 to 1.2%, and for example, may be 0.905%, 0.955%, or 1.195%, and the percentage means a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
In the present invention, the content of Fe is preferably 61.8 to 68%, for example, 61.895%, 62.595%, 62.995%, 63.095%, 63.195%, 63.395%, 3.895%, 63.995%, 63.995%, 64.045%, 64.095%, 64.195%, 64.225%, 64.295%, 64.595%, 64.695%, 64.815%, 64.825%, 64.945%, 64.995%, 65.025%, 65.095%, 65.195%, 65.295%, 65.545%, 65.635%, 65.655%, 65.795%, 65.895%, 65.945%, 65.965%, 65.985%, 66.055%, 66.095%, 66.115%, 66.195%, 66.345%, 66.445%, 66.495%, 66.545%, 66.585%, 66.595%, 66.675%, 66.695%, 66.755%, 66.785%, 66.835%, 66.945%, 67.065%, 67.375%, 67.495%, 67.525% or 67.695%, and the percentage is a mass percentage of the total mass of the raw material composition of the R-T-B system magnet material.
In the present invention, the raw material composition of the R-T-B-based magnet material may further include one or more of Al, Ga, Co, Mn, Ni, Zn, Ag, In, Sn, Bi, V, Cr, Ta, and W.
Wherein, the content of Al can be the content conventional in the field, and is preferably 0-3% but not 0; for example, 0 to 0.03% but not 0, or 0.1 to 0.5%, or 0.5 to 3%; for another example, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.1%, 0.2%, 0.3%, 0.35%, 0.5%, 0.8%, 1%, 1.2%, 1.5%, 1.8%, 2%, 2.3%, 2.6%, or 2.9%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
Wherein, the content of Ga may be a content conventionally used in the art, preferably less than 1%, more preferably 0.1 to 1%, for example, 0.1%, 0.2%, 0.25%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1%, and the percentage means a mass percentage based on the total mass of the raw material composition of the R-T-B based magnet material.
The content of Co may be a content conventionally used in the art, and is preferably 2% or less, more preferably 0.5 to 1.5%, for example, 0.5 or 1%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
The content of Mn may be a content conventionally used in the art, and is preferably 0.05% or less, for example, 0.02% or 0.05%, and the percentage means a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
The content of Zn may be a content conventionally used in the art, and is preferably 0.05% or less, for example, 0.02% or 0.05%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
In the present invention, the raw material composition of the R-T-B based magnet material may further include N, which generally refers to a high melting point metal in the art. The N species typically include Zr, Ti or Nb.
Wherein the content of N is a content which is conventional in the art, and is preferably 2.5% or less but not 0, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material.
When the kind of the N is Zr, the content of Zr is preferably 0.25 to 1%, for example, 0.25%, 0.3%, 0.5%, 0.8% or 1%, and the percentage means a mass percentage based on the total mass of the raw material composition of the R-T-B based magnet material.
When the N is Ti, the content of Ti is preferably 0.3 to 2.5%, for example, 0.3%, 0.6%, 1%, 1.5%, 2%, or 2.5%, and the percentage means the mass percentage based on the total mass of the raw material composition of the R-T-B based magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material comprises the following components in parts by weight: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: more than or equal to 17.15 percent; cu: 1.3-2.5%; al: 0 to 3% but not 0; b: 0.9-1.2%; fe: 61-68%, wherein the content of Al is preferably 0.5-3%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.15 to 28.15 percent; cu: 1.3-2.5%; al: 0.1-0.5%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.5-14.5%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.15 to 28.15 percent; cu: 1.3-2.5%; al: 0.5-3%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.5-14.5%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: more than or equal to 17.15 percent; cu: 1.3-2.5%; al: 0 to 0.03% but not 0; ga: 0.25-1%; b: 0.9-1.2%; fe: 61-68%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.15 to 28.15 percent; cu: 1.3-2.5%; al: 0 to 0.03% but not 0; ga: 0.25-1%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.5-14.5%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: more than or equal to 17.15 percent; cu: 1.3-2.5%; al: 0.1-0.5%; ti: 0.3-2.5%; b: 0.9-1.2%; fe: 61-68%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.15 to 28.15 percent; cu: 1.3-2.5%; al: 0.1-0.5%; ti: 0.3-2.5%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.5-14.5%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
In a preferred embodiment of the present invention, the raw material composition of the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: more than or equal to 17.15 percent; cu: 1.3-2.5%; al: 0.1-0.5%; ga: 0 to 0.25% but not 0; b: 0.9-1.2%; fe: 61-68%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material. Wherein, the content of Pr is preferably 17.15-28.15%; r' preferably further comprises Nd; the content of Nd is preferably 2.5-14.5%.
The invention provides a preparation method of an R-T-B series magnet material, wherein the raw material of the R-T-B series magnet material in the preparation method is the raw material composition adopting the R-T-B series magnet material.
In the present invention, the production method may be a method conventionally used in the art, for example, a melt of the raw material composition of the above-described R-T-B-based magnet material is subjected to casting, hydrogen fracturing, forming, sintering, and aging treatment.
In the present invention, the melt of the raw material composition of the R-T-B based magnet material can be prepared by a method conventional in the art, 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 ℃.
In the present invention, the operation and conditions for the casting may be those conventional in the art, for example, in an Ar atmosphere (e.g., 5.5X 10)4Pa in Ar atmosphere) at 10 deg.f2DEG C/sec-104Cooling at a rate of DEG C/sec.
In the present invention, the hydrogen decrepitation may be performed under conventional conditions. For example, the treatment of hydrogen absorption, dehydrogenation and cooling is carried out.
Wherein the hydrogen absorption can be carried out under the condition that the hydrogen pressure is 0.15 MPa.
Wherein the dehydrogenation is carried out under a condition of raising the temperature while evacuating.
In the present invention, the hydrogen may be broken and then pulverized by a conventional method in the art. The comminution process may be a comminution process conventional in the art, such as jet milling. The jet milling is preferably carried out under a nitrogen atmosphere having an oxidizing gas content of 150ppm or less. The oxidizing gas refers to oxygen or moisture content. The pressure of a crushing chamber for crushing by the jet mill is preferably 0.38 MPa; the jet mill pulverizing time is preferably 3 h.
After the pulverization, a lubricant such as zinc stearate may be added to the powder by a conventional method 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 operation and conditions of the forming may be those conventional in the art, such as a magnetic field forming method or a hot press hot deformation method.
In the present invention, the operation and conditions of the sintering may be those conventional in the art. For example, under vacuum conditions (e.g. at 5X 10)-3Pa, vacuum), preheating, sintering and cooling.
Wherein the preheating temperature is usually 300-600 ℃. The preheating time is usually 1-2 h. Preferably the preheating is for 1h at a temperature of 300 ℃ and 600 ℃ each.
Wherein, the sintering temperature is preferably 1030-1080 ℃, for example 1040 ℃.
The sintering time can be conventional in the art, and is usually 4 to 10 hours, for example 6 hours.
Wherein Ar gas can be introduced before cooling to ensure that the gas pressure reaches 0.1 MPa.
In the present invention, after the sintering and before the aging treatment, a grain boundary diffusion treatment is preferably further performed.
The operation and conditions for grain boundary diffusion can be those conventional in the art. For example, a Tb-containing substance and/or Dy-containing substance may be deposited on the surface of the R-T-B magnet material by vapor deposition, coating, or sputtering, and then subjected to diffusion heat treatment.
The Tb containing substance may be Tb metal, a Tb containing compound, such as a Tb containing fluoride or an alloy.
The Dy-containing substance may be Dy metal, a Dy-containing compound, such as a fluoride containing Dy, or an alloy.
The temperature of the diffusion heat treatment can be 800-900 ℃, for example 850 ℃.
The diffusion heat treatment time may be 12-48h, for example 24 h.
In the invention, in the aging treatment, the temperature of the secondary aging treatment is preferably 520-650 ℃, for example 550 ℃.
In the present invention, in the secondary aging treatment, the heating rate of heating to 520 to 650 ℃ is preferably 3to 5 ℃/min. The starting point of the warming may be room temperature.
The invention also provides an R-T-B series magnet material which is prepared by adopting the preparation method.
The invention also provides an R-T-B series magnet material, which comprises a grain boundary Fe-rich phase; the grain boundary Fe-rich phase comprises the following components in percentage by mass: r': 49-60%, wherein R 'is a rare earth element, and R' comprises Pr; t: 39-50%, wherein T comprises Fe; m: 1.5-4%, wherein M comprises Cu; the percentage is the mass percentage of each component in the total mass of the grain boundary Fe-rich phase.
In the invention, the grain boundary Fe-rich phase refers to R in atomic percentage6T13M1And (4) phase(s).
Wherein, R is6T13M1Preferably, the amount of the metal oxide is 2 to 25%, for example, 15% by volume based on the total volume of the R-T-B based magnet material.
In the grain boundary Fe-rich phase, the content of R' is preferably 49%, 51%, 52.3%, 53.4%, 54%, 54.5%, 55.5%, 56% or 57.1%, and the percentage is the mass percentage of each component in the total mass of the grain boundary Fe-rich phase.
In the grain boundary Fe-rich, R' can also comprise Nd.
In the grain boundary Fe-rich phase, the T can also comprise one or more of Co, Al and Ti.
In the grain boundary Fe-rich phase, the T content is preferably 39.5-46%, such as 39.55%, 40.65%, 40.74%, 41.45%, 41.68%, 42.22%, 42.31%, 42.32%, 42.85%, 43.3%, 43.89%, 44.22%, 45.45% or 47.67%, by mass, based on the total mass of the grain boundary Fe-rich phase.
In the grain boundary Fe-rich phase, the Cu content is preferably 1.5 to 3.8%, for example, 1.52%, 1.68%, 1.72%, 1.76%, 1.85%, 3.55%, 3.68%, 3.75%, 3.78%, 3.81%, 3.82%, or 3.85%, in percentage by mass based on the total mass of the grain boundary Fe-rich phase.
In the grain boundary Fe-rich phase, M may further include Ga.
When the M contains Ga, the content of the Ga is preferably 1.51%, 1.53%, 1.58%, 1.59%, 1.61% or 1.63% by mass based on the total mass of the grain boundary Fe-rich phase.
In the present invention, the R-T-B magnet material generally contains a main phase.
Wherein, the main phase preferably comprises the following components in percentage by mass: r': 26-28%, wherein R 'is a rare earth element, and R' comprises Pr; b: 0.9-1.2%; t: 70-72%, wherein the T comprises Fe, and the percentage is the mass percentage of each component in the total mass of the main phase.
In the main phase, the content of R' is preferably 26.5 to 28%, for example 26.2%, 26.9%, 27.2%, 27.3%, 27.4%, 27.5% or 27.8%, by mass, based on the total mass of the main phase.
In the main phase, the R' may further include Nd.
In the main phase, the content of B is preferably 0.95 to 1.2%, for example, 0.98%, 1.01%, 1.06%, or 1.17%, in mass% based on the total mass of the main phase.
In the main phase, the content of T is preferably 71 to 72%, for example, 71.14%, 71.33%, 71.53%, 1.62%, 71.64%, 71.69%, 71.72%, 71.74%, 71.82%, 71.93%, 72.09% or 72.79%, by mass, based on the total mass of the main phase.
In the main phase, the kind of T may further include one or more of Co, Al, and N. Wherein said N comprises Ti or Zr.
In the present invention, the R-T-B-based magnet material usually further includes a grain boundary R 'rich phase, and R' is a rare earth element.
The grain boundary R' -rich phase preferably comprises the following components in percentage by mass: r': 84-87%, O: 13-16%, wherein R 'comprises Pr, and the percentage is the mass percentage of each component in the total mass of the crystal boundary R' rich phase.
The grain boundary is rich in R 'phase, and the R' also comprises Nd.
In the grain boundary R ' rich phase, the content of R ' is preferably 84.5 to 86.5%, for example, 84.7%, 85.2%, or 86.3%, and the percentage is the mass percentage of each component in the total mass of the grain boundary R ' rich phase.
In the grain boundary R 'rich phase, the content of O is preferably 13.5 to 16%, for example, 13.7%, 14.8% or 15.7%, and the percentages are mass percentages of the components in the total mass of the grain boundary R' rich phase.
The invention also provides an R-T-B series magnet material which comprises the following components in percentage by mass:
r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: not less than 17.14%;
Cu：>1.3％；
B：0.9～1.2％；
fe: 61-68% by mass of the total mass of the R-T-B magnet material.
In the present invention, the content of R' is preferably 29.6 to 31.7%, for example, 29.638%, 29.639%, 29.652%, 30.118%, 30.139%, 30.158%, 30.171%, 30.188%, 30.289%, 30.356%, 30.628%, 30.629%, 30.639%, 30.65%, 30.652%, 30.654%, 30.658%, 30.659%, 30.661%, 30.669%, 30.671%, 30.673%, 30.689%, 31.131%, 31.14%, 31.167%, 31.168%, 31.172%, 31.199%, 31.332%, 31.378%, 31.628%, 31.629%, 31.641%, 31.651%, 31.652%, 31.658%, 31.661%, 31.672%, 31.68%, 31.682% or 31.697%, where the percentage is a mass percentage of the total mass of the R-T-B magnet material.
In the present invention, the content of Pr is preferably 17.14 to 28.15%, for example, 17.148%, 17.149%, 17.151%, 17.152%, 18.148%, 18.149%, 18.151%, 19.148%, 19.151%, 20.147%, 20.148%, 20.149%, 20.151%, 20.847%, 21.149%, 21.151%, 22.148%, 22.149%, 22.152%, 22.852%, 23.149%, 23.151%, 24.148%, 24.151%, 25.147%, 25.148%, 25.149%, 25.15%, 25.151%, 25.851%, 26.148%, 26.149%, 26.151%, 28.148% or 28.149%, where the percentage is a mass percentage of the total mass of the R-T-B magnet material.
In the present invention, the R' may further include Nd.
Wherein the mass ratio of Nd to R' is preferably less than 0.5, more preferably 0.08 to 0.45, such as 0.081, 0.082, 0.114, 0.115, 0.116, 0.118, 0.144, 0.147, 0.148, 0.151, 0.174, 0.176, 0.180, 0.205, 0.206, 0.213, 0.219, 0.245, 0.271, 0.277, 0.278, 0.300, 0.304, 0.310, 0.320, 0.332, 0.335, 0.343, 0.348, 0.363, 0.364, 0.375, 0.380, 0.385, 0.395, 0.398, 0.408, 0.417, 0.426, 0.440, 0.441 or 0.450.
The Nd content is preferably 15% or less, more preferably 2.4 to 14.5%, for example, 2.48%, 2.51%, 3.48%, 3.49%, 3.501%, 3.502%, 3.51%, 4.49%, 4.505%, 4.52%, 5.49%, 5.501%, 5.51%, 6.47%, 6.501%, 6.51%, 6.52%, 7.52%, 8.48%, 8.49%, 8.501%, 8.502%, 8.51%, 9.49%, 9.501%, 9.51%, 9.52%, 10.02%, 10.14%, 10.48%, 10.501%, 10.52%, 11.48%, 11.51%, 12.02%, 12.51%, 12.98%, 13.47%, 13.48%, 13.49%, 13.501%, 13.502%, 13.51%, 13.52% or 14.02%, by mass percentage, based on the total mass of the R-T-B magnet material.
Wherein, said R' may also include Y.
In the present invention, it is known to those skilled in the art that the R' preferably further includes RH, which is a heavy rare earth element.
Wherein, the RH may be a heavy rare earth element conventional in the art, such as one or more of Dy, Tb and Ho, preferably Dy and/or Tb.
In the present invention, the mass ratio of RH to R' may be a conventional mass ratio in the art, and is preferably less than 0.253, and more preferably 0.1 to 1, such as 0.017, 0.032, 0.033, 0.047, 0.048, 0.050, 0.063, or 0.064.
The RH content is preferably 2.5% or less, preferably 0.4 to 2.5%, for example, 0.49%, 0.99%, 1.02%, 1.03%, 1.501%, 1.502%, 1.51%, 1.53%, 2.01%, or 2.03%, and the percentage is a mass percentage based on the total mass of the R-T-B-based magnet material.
When Tb is contained in the RH, the content of Tb is preferably 0.45 to 2%, for example, 0.49%, 0.51%, 1.02%, 1.03%, 1.502%, 1.51%, 2.01%, or 2.03%, and the percentage means a mass percentage based on the total mass of the R-T-B-based magnet material.
When Dy is contained in the RH, the content of Dy is preferably 0.45 to 2%, for example, 0.45%, 0.51%, 0.52%, 0.99%, 1.02%, 1.03%, or 1.501%, and the percentage means a mass percentage based on the total mass of the R-T-B-based magnet material.
In the present invention, the Cu content is preferably 1.3to 2.52%, for example, 1.3%, 1.309%, 1.31%, 1.311%, 1.32%, 1.39%, 1.403%, 1.41%, 1.42%, 1.49%, 1.501%, 1.51%, 1.601%, 1.602%, 1.68%, 1.701%, 1.71%, 1.79%, 1.802%, 1.81%, 1.88%, 1.901%, 1.91%, 2.02%, 2.08%, 2.101%, 2.11%, 2.19%, 2.201%, 2.21%, 2.22%, 2.29%, 2.301%, 2.31%, 2.32%, 2.403%, 2.41%, 2.49%, 2.498%, 2.503%, 2.51%, or 2.52%, and the percentage is a mass percentage of the total mass of the R-T-B magnet material.
In the present invention, the content of B is preferably 0.92 to 1.2%, and may be, for example, 0.904%, 0.952%, 0.953%, 0.954%, 0.955%, or 1.194%, and the percentage means a mass percentage based on the total mass of the R-T-B-based magnet material.
In the present invention, the content of Fe is preferably 61.8 to 68%, for example, 61.878%, 62.595%, 62.963%, 63.089%, 63.107%, 63.166%, 63.359%, 63.838%, 63.948%, 63.966%, 63.969%, 64.024%, 64.183%, 64.239%, 64.244%, 64.595%, 64.686%, 64.717%, 64.7842%, 64.797%, 64.905%, 64.971%, 64.985%, 65.063%, 65.161%, 65.193%, 65.277%, 65.522%, 65.646%, 65.65%, 65.815%, 65.865%, 65.884%, 65.907%, 65.955%, 65.967%, 66.044%, 66.055% or 66.055% by mass of the total magnet material in the T-T system.
In the present invention, the R-T-B-based magnet material may further include one or more of Al, Ga, Co, Mn, Ni, Zn, Ag, In, Sn, Bi, V, Cr, Ta, and W.
Wherein, the content of Al can be the content conventional in the field, and is preferably 0-3% but not 0. For example, 0 to 0.03% but not 0, or 0.1 to 0.5%, or 0.5 to 3%; specifically, for example, 0.01%, 0.019%, 0.031%, 0.039%, 0.049%, 0.059%, 0.06%, 0.071%, 0.102%, 0.11%, 0.111%, 0.19%, 0.29%, 0.349%, 0.482%, 0.5%, 0.51%, 0.791%, 0.8%, 1.02%, 1.03%, 1.2%, 1.21%, 1.51%, 1.52%, 1.8%, 1.81%, 2.02%, 2.3%, 2.6%, or 2.9% is defined as a mass percentage based on the total mass of the R-T-B magnet material.
Wherein, the content of Ga may be a content conventionally used in the art, preferably less than 1%, more preferably 0.1 to 1%, such as 0.101%, 0.102%, 0.21%, 0.251%, 0.31%, 0.402%, 0.41%, 0.49%, 0.501%, 0.503%, 0.59%, 0.602%, 0.71%, 0.801%, 0.88%, 1.02%, or 1.03%, by mass, based on the total mass of the R-T-B based magnet material.
The content of Co is a conventional content in the art, and is preferably 2% or less, more preferably 0.5 to 1.5%, for example, 0.51% or 1.02%, and the percentage is a mass percentage based on the total mass of the R-T-B-based magnet material.
Wherein the content of Mn may be a content conventional in the art, preferably 0.052% or less, for example, 0.018% or 0.051%, the percentage referring to the mass percentage based on the total mass of the R-T-B based magnet material.
Wherein the Zn content may be a content conventional in the art, preferably 0.05% or less, for example, 0.019% or 0.0548%, and the percentage means a mass percentage based on the total mass of the R-T-B based magnet material.
In the present invention, the R-T-B based magnet material may further include N, which generally refers to a refractory metal in the art. The N species typically include Zr, Ti or Nb.
Wherein, the content of N can be the content conventional in the field, preferably below 2.5%, and the percentage refers to the mass percentage of the total mass of the R-T-B series magnet material.
When the kind of the N is Zr, the Zr content is preferably 0.25 to 1.05%, for example, 0.251%, 0.302%, 0.501%, 0.503%, 0.51%, 0.802%, or 1.03%, and the percentage means a mass percentage based on the total mass of the R-T-B based magnet material.
When the kind of the N is Ti, the content of the Ti is preferably 0.3 to 2.5%, for example, 0.32%, 0.61%, 1.02%, 1.49%, 2.02%, or 2.48%, and the percentage means a mass percentage based on the total mass of the R-T-B based magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material comprises the following components in parts by weight: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: not less than 17.14%; cu: 1.3-2.52%; al: 0 to 3% but not 0; b: 0.9-1.2%; fe: 61-68%, wherein the content of Al is preferably 0.5-3%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.14 to 28.15 percent; cu: 1.3-2.52%; al: 0.1-0.5%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.4-14.5%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.14 to 28.15 percent; cu: 1.3-2.52%; al: 0.5-3%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.4-14.5%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: not less than 17.14%; cu: 1.3-2.52%; al: 0 to 0.03% but not 0; ga: 0.25 to 1% but not 0; b: 0.9-1.2%; fe: 61-68%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.14 to 28.15 percent; cu: 1.3-2.52%; al: 0 to 0.03% but not 0; ga: 0.25-1%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.4-14.5%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: not less than 17.14%; cu: 1.3-2.52%; al: 0.1-0.5%; ti: 0.3-2.5%; b: 0.9-1.2%; fe: 61-68%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R' is a rare earth element and comprises Pr and Nd; wherein, the Pr: 17.14 to 28.15 percent; cu: 1.3-2.52%; al: 0.1-0.5%; ti: 0.3-2.5%; b: 0.9-1.2%; fe: 61-68%; wherein, the content of Nd is preferably 2.4-14.5%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
In a preferred embodiment of the present invention, the R-T-B based magnet material includes the following components in amounts: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr; wherein, the Pr: not less than 17.14%; cu: 1.3-2.52%; al: 0.1-0.5%; ga: 0 to 0.25% but not 0; b: 0.9-1.2%; fe: 61-68%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material. Wherein, the content of Pr is preferably 17.14 to 28.15 percent; r' preferably further comprises Nd; the content of Nd is preferably 2.5-14.5%.
In the present invention, the R-T-B system magnet material preferably contains a grain boundary Fe-rich phase having the composition and content described above.
In the present invention, the R-T-B magnet material generally further contains a main phase. Wherein the components and contents of the main phase are preferably as described above.
In the present invention, the R-T-B magnet material generally contains a grain boundary rare earth-rich phase. Wherein the composition and content of the grain boundary rare earth-rich phase are preferably as described above.
The invention also provides an application of the R-T-B series magnet material as an electronic element.
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.
In the invention, Pr is praseodymium, Nd is neodymium, Cu is copper, B is boron, Fe is iron, Al is aluminum, Ga is gallium, Co is cobalt, Zr is zirconium, Ti is titanium, Zn is zinc, Dy is dysprosium, Tb is terbium, Ni is nickel, Ag is silver, In is indium, Sn is tin, Bi is bismuth, V is vanadium, Cr is chromium, Ta is tungsten, and O is oxygen.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the R-T-B series magnet material provided by the invention uses higher content of Pr and higher content of Cu, so that the R-T-B series magnet material can maintain higher remanence while the coercive force is obviously improved; in a further preferred embodiment of the present invention, R-T-B magnet material may be R6T13M1The coercive force of the magnet material can be further improved.
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.
The raw material compositions of the R-T-B system magnet materials in the respective examples and comparative examples are shown in Table 1 below.
TABLE 1
Note: the numbers 1 to 60 in Table 1 refer to examples 1 to 60, and the numbers 61 to 64 refer to comparative examples 61 to 64.
The preparation process of the R-T-B series magnet material of example 1 is as follows:
(1) and (3) casting: according to the formulation shown in Table 1, the raw materials prepared in example 1 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. Ar gas is introduced into a melting furnace after vacuum melting to make the gas pressure reach 5.5 ten thousand Pa, and then casting is carried out at 10 degrees2DEG C/sec-104The cooling rate of DEG C/second obtains the quenched alloy.
(2) Hydrogen crushing and crushing: vacuumizing the smelting furnace in which the quenching alloy is placed at room temperature, introducing hydrogen with the purity of 99.9% into the hydrogen cracking furnace, maintaining the hydrogen pressure at 0.15MPa, fully absorbing hydrogen, vacuumizing while heating, fully dehydrogenating, cooling, and taking out the powder after hydrogen cracking and crushing.
(3) 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 150ppm or less at a pressure in the pulverization chamber of 0.38MPa to obtain a fine powder. The oxidizing gas refers to oxygen or moisture.
(4) 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.
(5) 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).
(6) And (3) sintering: the molded bodies were transferred to a sintering furnace and sintered at 5X 10-3Keeping at 300 deg.C and 600 deg.C under Pa for 1 hr, sintering at 1040 deg.C for 6 hr, and introducing Ar gas to make the pressure reachAfter 0.1MPa, cool to room temperature.
(7) And (3) aging treatment process: the sintered body was heat-treated in high-purity Ar gas at 550 ℃ for 3 hours, cooled to room temperature, and taken out.
The R-T-B magnet materials of examples 2 to 60 and comparative examples 61 to 64 were prepared according to the formulation of the raw material composition shown in Table 1 by the same preparation process as in example 1.
Example 1.1 Dy grain boundary diffusion method
The raw material composition formulation of example 1 in table 1 was prepared by the preparation method of example 1, first, obtaining a sintered body, followed by grain boundary diffusion and then aging treatment. The aging treatment process is the same as that of the example 1, and the treatment process of grain boundary diffusion is as follows:
processing the sintered body into a magnet with the diameter of 20mm and the sheet thickness of less than 3mm, wherein the thickness direction is the magnetic field orientation direction, cleaning the surface, using a raw material prepared by Dy fluoride, spraying and coating the whole surface on the magnet, drying the coated magnet, sputtering metal attached with Dy element on the surface of the magnet in a high-purity Ar gas atmosphere, performing diffusion heat treatment at the temperature of 850 ℃ for 24 hours, and then cooling to the room temperature.
EXAMPLE 1.2 Tb grain boundary diffusion method was used
Example 1 in table 1 a sintered body was first prepared according to the preparation of the sintered body of example 1, and grain boundary diffusion was first performed, followed by aging treatment. The aging treatment process is the same as that of the example 1, and the treatment process of grain boundary diffusion is as follows:
processing the sintered body into a magnet with the diameter of 20mm and the sheet thickness of less than 7mm, wherein the thickness direction is the magnetic field orientation direction, cleaning the surface, using a raw material prepared from Tb fluoride, spraying and coating the whole surface of the raw material on the magnet, drying the coated magnet, sputtering metal attached with Tb on the surface of the magnet in a high-purity Ar gas atmosphere, and performing diffusion heat treatment at the temperature of 850 ℃ for 24 hours. And cooling to room temperature.
Effect example 1
The magnetic properties and components of the R-T-B magnet materials prepared in the examples and comparative examples were measured.
(1) Evaluation 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. The following table 2 shows the results of magnetic property measurements.
TABLE 2
(2) Component determination: the R-T-B magnet materials of the numbers 1 to 64 were measured by using a high-frequency inductively coupled plasma emission spectrometer (ICP-OES). The following table 3 shows the results of component detection.
TABLE 3
Note: 6:13:1 phases mean R 'in R-T-B based magnet material'6T13M1And phase R ' is a rare earth element, T is one or more of Fe, Co, Al and N, M is Cu and/or Ga, and O in the table represents R ' formed in the R-T-B magnet material '6T13M1X in the table represents R 'not formed in the R-T-B magnet material'6T13M1And (4) phase(s).
(3) FE-EPMA detection: R-T-B magnet materials 1, 2, 3, 11, 12, 23, 25, 28, 29, 31, 33, 35, 36, 41, 45, 61, 62, 63, 64, which were prepared in Table 3, were used. The vertical orientation surface of the sintered magnet was polished and examined by a field emission electron probe microanalyzer (FE-EPMA) (JEOL 8530F). The test results are shown in table 4 below. In table 4, the grain boundary Fe-rich phase is converted to atomic percent, wherein R': t: the atomic ratio of M is close to 6:13:1, wherein R 'is a rare earth element and R' comprises Pr; the kind of T includes one or more of Fe, Co, Al and N, but at least includes Fe; m comprises Cu and/or Ga.
TABLE 4
Claims (25)
1. A preparation method of R-T-B series magnet material is characterized in that the R-T-B series magnet material is prepared by melting and casting a melt of a raw material composition of the R-T-B series magnet material, breaking with hydrogen, forming, sintering and aging;
the raw material composition of the R-T-B series magnet material comprises the following components in percentage by mass: r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr;
wherein, the Pr: 17.15 to 28.15 percent;
1.3<Cu≤2.5%；
B：0.9~1.2%；
fe: 61-68%, the percentage being mass percentage of the total mass of the raw material composition of the R-T-B series magnet material;
the R-T-B series magnet material comprises a grain boundary Fe-rich phase; the grain boundary Fe-rich phase comprises the following components in percentage by mass: r': 49-60%, wherein R 'is a rare earth element, and R' comprises Pr; t: 39-50%, wherein T comprises Fe; m: 1.5-4%, wherein M comprises Cu; the percentage is the mass percentage of each component in the total mass of the grain boundary Fe-rich phase.
2. The production method according to claim 1, wherein in the raw material composition of the R-T-B-based magnet material, the content of R' is 29.65 to 31.65%, and the percentage is a mass percentage based on the total mass of the raw material composition of the R-T-B-based magnet material;
and/or, in the raw material composition of the R-T-B magnet material, the content of the Pr is 17.15%, 18.15%, 19.15%, 20.15%, 20.85%, 21.15%, 22.15%, 22.85%, 23.15%, 24.15%, 25.15%, 25.85%, 26.15% or 28.15%, and the percentage refers to the mass percentage of the total mass of the raw material composition of the R-T-B magnet material;
and/or, in the raw material composition of the R-T-B series magnet material, the R' further comprises Nd;
and/or, in the raw material composition of the R-T-B magnet material, the R' also comprises RH which is a heavy rare earth element;
and/or the content of Cu in the raw material composition of the R-T-B magnet material is 1.31%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, 2%, 2.1%, 2.2%, 2.3%, 2.4% or 2.5%, and the percentage refers to the mass percentage of the total mass of the raw material composition of the R-T-B magnet material;
and/or, in the raw material composition of the R-T-B series magnet material, the content of B is 0.92-1.2%;
and/or the content of Fe in the raw material composition of the R-T-B series magnet material is 61.8-68%;
and/or the raw material composition of the R-T-B magnet material further comprises one or more of Al, Ga, Co, Mn, Ni, Zn, Ag, In, Sn, Bi, V, Cr, Ta and W;
and/or the raw material composition of the R-T-B magnet material also comprises N, and the type of the N comprises Zr, Ti or Nb.
3. The production method according to claim 2, wherein in the raw material composition of the R-T-B based magnet material, the content of R' is 29.65%, 30.15%, 30.3%, 30.35%, 30.65%, 31.15%, 31.35%, or 31.65%;
and/or, in the raw material composition of the R-T-B series magnet material, the mass ratio of the Nd to the R' is less than 0.5; the content of Nd is less than 15%, and the percentage is the mass percentage of the total mass of the raw material composition of the R-T-B series magnet material;
and/or, in the raw material composition of the R-T-B series magnet material, the type of the RH includes one or more of Dy, Tb and Ho; the mass ratio of the RH to the R' is less than 0.253.
4. The production method according to claim 2, wherein in the raw material composition of the R-T-B based magnet material, a mass ratio of the Nd to the R' is 0.08 to 0.45; the content of Nd is 2.5-14.5%;
and/or, in the raw material composition of the R-T-B magnet material, the type of the RH includes Dy and/or Tb; the mass ratio of the RH to the R' is 0.1-1.
5. The production method according to claim 2, wherein the content of Nd in the raw material composition of the R-T-B-based magnet material is 2.5%, 3.5%, 4.5%, 5.5%, 6.5%, 7.5%, 8.5%, 9.5%, 10%, 10.15%, 10.5%, 11.5%, 12%, 12.5%, 13%, 13.5%, or 14%;
and/or the raw material composition of the R-T-B magnet material has an RH content of 2.5% or less.
6. The production method according to claim 2, wherein the raw material composition of the R-T-B magnet material contains 0.5 to 2.5% of RH; when the RH contains Tb, the content of Tb is 0.5-2%; when Dy is contained in the RH, the content of Dy is 0.5-2%.
7. The production method according to claim 2, wherein in the raw material composition of the R-T-B based magnet material, the content of Al is 0 to 3% but not 0; the percentage is the mass percentage of the total mass of the raw material composition of the R-T-B series magnet material;
and/or, in the raw material composition of the R-T-B series magnet material, the content of Ga is less than 1 percent, and the percentage is the mass percentage of the total mass of the raw material composition of the R-T-B series magnet material;
and/or, in the raw material composition of the R-T-B magnet material, the content of Co is less than 2 percent, and the percentage is the mass percentage of the total mass of the raw material composition of the R-T-B magnet material;
and/or, in the raw material composition of the R-T-B magnet material, the content of Mn is less than 0.05%, and the percentage is the mass percentage of the total mass of the raw material composition of the R-T-B magnet material;
and/or, in the raw material composition of the R-T-B magnet material, the Zn content is below 0.05 percent, and the percentage is the mass percentage of the total mass of the raw material composition of the R-T-B magnet material;
and/or, in the raw material composition of the R-T-B magnet material, the content of N is less than 2.5%, and the percentage is the mass percentage of the total mass of the raw material composition of the R-T-B magnet material.
8. The production method according to claim 7, wherein the content of Al in the raw material composition of the R-T-B based magnet material is 0 to 0.03% but not 0, or 0.1 to 0.5%, or 0.5 to 3%;
and/or, in the raw material composition of the R-T-B series magnet material, the content of Ga is 0.1-1%;
and/or, in the raw material composition of the R-T-B series magnet material, the content of Co is 0.5-1.5%;
and/or, in the raw material composition of the R-T-B series magnet material, the content of Mn is 0.02% or 0.05%;
and/or, in the raw material composition of the R-T-B series magnet material, the content of Zn is 0.02% or 0.05%;
and/or, in the raw material composition of the R-T-B magnet material, when the type of the N is Zr, the Zr content is 0.25-1%; when the type of the N is Ti, the content of the Ti is 0.3-2.5%; the percentages are mass percentages based on the total mass of the raw material composition of the R-T-B magnet material.
9. The production method according to any one of claims 1 to 8, wherein a temperature of melting in the melt-casting is 1500 ℃ or less.
10. The method according to any one of claims 1 to 8, wherein the sintering temperature is 1030 to 1080 ℃; the sintering time is 4-10 h.
11. The production method according to any one of claims 1 to 8, wherein after the sintering and before the aging treatment, a grain boundary diffusion treatment is further performed;
the temperature of diffusion heat treatment in the crystal boundary diffusion treatment is 800-900 ℃;
the time of diffusion heat treatment in the grain boundary diffusion treatment is 12-48 h.
12. The method according to any one of claims 1 to 8, wherein the secondary aging treatment is performed at a temperature of 520 to 650 ℃.
13. The method according to any one of claims 1 to 8, wherein the temperature of secondary aging in the aging treatment is 550 ℃.
14. The method according to claim 1, wherein the grain boundary Fe-rich phase accounts for 2 to 25% of the total volume of the R-T-B based magnet material.
15. The production method according to claim 1, wherein the R-T-B based magnet material further contains a main phase; the main phase comprises the following components in percentage by mass: r': 26-28%, wherein R 'is a rare earth element, and R' comprises Pr; b: 0.9-1.2%; t: 70-72%, wherein the T comprises Fe, and the percentage is the mass percentage of each component in the total mass of the main phase.
16. The production method according to claim 1, wherein the R-T-B-based magnet material further includes a grain boundary R 'rich phase, wherein R' is a rare earth element; the grain boundary R' -rich phase comprises the following components in percentage by mass: r': 84-87%, O: 13-16%, wherein R 'comprises Pr, and the percentage is the mass percentage of each component in the total mass of the crystal boundary R' rich phase.
17. An R-T-B series magnet material, characterized in that it is prepared by the preparation method as claimed in any one of claims 1 to 16.
18. An R-T-B series magnet material is characterized by comprising the following components in percentage by mass:
r': 29.5-32%, wherein R 'is a rare earth element, and R' comprises Pr;
wherein, the Pr: not less than 17.14%;
1.3<Cu≤2.52%；
B：0.9~1.2%；
fe: 61-68% by mass of the total mass of the R-T-B magnet material;
the R-T-B series magnet material comprises a grain boundary Fe-rich phase; the grain boundary Fe-rich phase comprises the following components in percentage by mass: r': 49-60%, wherein R 'is a rare earth element, and R' comprises Pr; t: 39-50%, wherein T comprises Fe; m: 1.5-4%, wherein M comprises Cu; the percentage is the mass percentage of each component in the total mass of the grain boundary Fe-rich phase.
19. The R-T-B magnet material according to claim 18, wherein the content of R' is 29.6 to 31.7% by mass based on the total mass of the R-T-B magnet material;
and/or the content of Pr is 17.14-28.15%, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or, said R' further comprises Nd;
and/or, said R' further comprises Y;
and/or, the R' also comprises RH which is a heavy rare earth element;
and/or the Cu content is 1.309-2.52%, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or the content of B is 0.92-1.2%, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or the content of Fe is 61.8-68%, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or, the R-T-B series magnet material further comprises one or more of Al, Ga, Co, Mn, Ni, Zn, Ag, In, Sn, Bi, V, Cr, Ta and W;
and/or the R-T-B series magnet material also comprises N, and the type of the N comprises Zr, Ti or Nb;
and/or, the R-T-B series magnet material also contains a main phase; the main phase comprises the following components in percentage by mass: r': 26-28%, wherein R 'is a rare earth element, and R' comprises Pr; b: 0.9-1.2%; t: 70-72%, wherein the T comprises Fe, and the percentage is the mass percentage of each component in the total mass of the main phase;
and/or the R-T-B series magnet material also comprises a grain boundary R 'rich phase, wherein R' is a rare earth element; the grain boundary R' rich phase comprises the following components in percentage by mass: r': 84-87%, O: 13-16%, wherein R 'comprises Pr, and the percentage is the mass percentage of each component in the total mass of the crystal boundary R' rich phase.
20. The R-T-B based magnet material according to claim 19, wherein a mass ratio of the Nd to the R' is less than 0.5; the content of Nd is below 15%;
and/or, the RH species comprises one or more of Dy, Tb and Ho, preferably comprises; the mass ratio of the RH to the R' is less than 0.253;
and/or the Al content is 0-3% but not 0, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or the content of Ga is less than 1 percent, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or the content of Co is less than 2 percent, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or the Mn content is less than 0.052%, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or the Zn content is less than 0.05 percent, and the percentage is the mass percentage of the total mass of the R-T-B series magnet material;
and/or the content of N is below 2.5 percent.
21. The R-T-B based magnet material according to claim 19, wherein a mass ratio of Nd to R' is 0.08 to 0.45; the content of Nd is 2.4-14.5%;
and/or, the RH species includes Dy and/or Tb; the mass ratio of the RH to the R' is 0.1-1;
and/or the content of Al is 0-0.03% but not 0, or 0.1-0.5%, or 0.5-3%;
and/or the content of Ga is 0.1-1%;
and/or the content of Co is 0.5-1.5%;
and/or when the type of the N is Zr, the Zr content is 0.25-1.05%; when the N is Ti, the content of Ti is 0.3-2.5%.
22. The R-T-B based magnet material according to claim 19, wherein the RH content is 2.5% or less.
23. The R-T-B magnet material according to claim 19, wherein the RH is 0.4 to 2.5%; when the RH contains Tb, the content of Tb is 0.45-2%; when Dy is contained in the RH, the content of Dy is 0.45-2%; the percentage is the mass percentage of the total mass of the R-T-B series magnet material.
24. The R-T-B magnet material according to claim 18, wherein the grain boundary Fe-rich phase accounts for 2 to 25% of the total volume of the R-T-B magnet material.
25. Use of the R-T-B based magnet material according to any one of claims 17 to 24 as an electronic component.
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