CN111180158A - R-T-B series sintered permanent magnet and preparation method thereof - Google Patents

R-T-B series sintered permanent magnet and preparation method thereof Download PDF

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CN111180158A
CN111180158A CN201911391029.6A CN201911391029A CN111180158A CN 111180158 A CN111180158 A CN 111180158A CN 201911391029 A CN201911391029 A CN 201911391029A CN 111180158 A CN111180158 A CN 111180158A
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permanent magnet
equal
low
cost
content
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王少勃
张民
吕向科
刘小浪
竺晓东
毛应才
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Ningbo Yunsheng Magnet Devices Technology Co Ltd
Ningbo Yunsheng Co Ltd
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Ningbo Yunsheng Magnet Devices Technology Co Ltd
Ningbo Yunsheng Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets

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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 low-cost R-T-B series sintered permanent magnet and a preparation method thereof1And R2Composition R1One or a combination of at least two of Gd element, Ce element, La element and Y element, R2Is selected from any one or the combination of at least two of Nd element, Pr element and Ho element, the T component consists of Fe element and Al element or one or more of Fe element, Al element and other transition metal elements except Fe element, and R is1Has a content of x, R2The content of the element is recorded as y, the content of the element B is z, the content of the component T is recorded as w, x + y + z + w is 1, x + y is more than or equal to 30 wt% and less than or equal to 35 wt%, z is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and z/y is more than or equal to 0.1 and less than or equal to 0.9; has the advantages that one or more of high-abundance rare earth metals Gd, Ce, La and Y are used for replacing at least one of low-abundance Pr, Nd or Ho, and rare earth is used for replacingThe amount of the rare earth exceeds 70 percent of the total amount of the rare earth, and the production cost of the sintered permanent magnet is obviously reduced.

Description

R-T-B series sintered permanent magnet and preparation method thereof
Technical Field
The invention relates to an R-T-B sintered permanent magnet, in particular to an R-T-B sintered permanent magnet and a preparation method thereof.
Background
The Nd-Fe-B permanent magnet is the magnet with the highest commercial performance found at present and is called as 'Magang'. The Nd-Fe-B permanent magnet has extremely high magnetic performance and the maximum energy product (BH)maxThe temperature is over 10 times higher than Ferrite (Ferrite), the working temperature can reach 200 ℃ at most, and the Ferrite can be widely applied to the fields of aerospace, electronics, electric machinery, medical instruments, toys, packaging, hardware machinery and the like at present.
The Nd-Fe-B permanent magnet is an intermetallic compound Nd2Fe14The main components of the permanent magnetic material based on B are rare earth elements, Fe and B, and the rare earth elements are mainly Pr and Nd. In order to obtain different performances of the neodymium iron boron permanent magnet, other rare earth metals such as Dy, Tb and Ho can be used for partially replacing Pr and Nd, and other metals such as cobalt (Co) and aluminum (Al) can be used for partially replacing iron. Although the content of boron in the neodymium-iron-boron permanent magnet is low, boron plays an important role in forming an intermetallic compound with a tetragonal crystal structure, so that the compound has high saturation magnetization, high uniaxial anisotropy and high Curie temperature. The third generation rare earth neodymium iron boron permanent magnet is a permanent magnet with the strongest performance in the current generation magnet, and comprises the following main raw materials: 29-32.5 wt% of Nd, 63.95-68.65 wt% of Fe, 1.1-1.2 wt% of B, 0.6-8 wt% of Dy, 0.3-0.5 wt% of Al and 0.05-0.15 wt% of Cu.
The contents of rare earth elements in the earth crust are sequentially Ce, Y, La, Nd, Pr, Sm, Gd, Dy and Tb …, and the use of a large amount of rare earth permanent magnets ensures that Pr, Nd, Dy and Tb are rapidly consumed, so that a large amount of abundant rare earth such as La, Ce, Gd and Y is accumulated, and the utilization of rare earth resources is unbalanced. Taking bayu jaw rare earth ore as an example, the Nd: 18.5 wt%, Pr 6.2 wt%, Ce 50.0 wt%, La 23.0 wt%, other metals: 2.3 wt%. At present, light rare earth elements Nd and Pr and heavy rare earth elements Dy and Tb are still used in mass preparation of the neodymium iron boron permanent magnet. According to statistics, the use condition of the rare earth metal in the neodymium iron boron permanent magnet industry is as follows: nd: 64.44 wt%, Pr 20.02 wt%, Ce 5.41 wt%, La 3.57 wt%, other metals: 6.56 wt%. The low storage and high dosage lead to high price of light rare earth elements Nd and Pr and heavy rare earth elements Dy and Tb, and further lead to high price of the neodymium iron boron permanent magnet; meanwhile, a large amount of metal such as La, Ce and the like is accumulated, and rare earth resources and consumption are contradictory.
At present, research on high-abundance rare earth permanent magnets mainly focuses on the preparation of rare earth permanent magnets by replacing Nd with Ce. In the technique disclosed in chinese patent publication No. CN1035737A, Ce was used instead of part of Nd by direct smelting, and it was found that as the Ce content increased, both the coercive force and remanence of the magnet decreased. This is because of Ce2Fe14Intrinsic Property of B (H)A26kOe, 4 pi Ms 11.7kGs) is much lower than Nd2Fe14Intrinsic Property of B (H)A73kOe, 4 pi Ms 16.0 kGs); meanwhile, the microstructure of the permanent magnet is remarkably deteriorated after Ce replaces Nd, which is also a reason for greatly reducing the coercive force and remanence.
Magnet properties of conventional sintered permanent magnets: b isr≥11.7kGs，HcJNot less than 12kOe, the performance of the ferrite is as follows: b isr＜5kGs，HcJLess than 5kOe, and for customers needing performance between the two, only sintered neodymium iron boron with excellent performance can be selected, so that the production cost of the customers is high.
Disclosure of Invention
One of the technical problems to be solved by the present invention is to provide a low-cost R-T-B sintered permanent magnet. The sintered permanent magnet uses one or more of high-abundance rare earth metals Gd, Ce, La and Y to replace at least one of low-abundance Pr, Nd or Ho, the substitution amount of the rare earth exceeds 70 percent of the total content of the rare earth, and the production cost of the sintered permanent magnet is obviously reduced on the basis of having better magnetic performance.
The technical scheme adopted by the invention for solving one of the technical problems is as follows: aThe low-cost R-T-B sintered permanent magnet includes R component, T component and B element1And R2Composition R1One or a combination of at least two of Gd element, Ce element, La element and Y element, R2One or two of Nd, Pr and Ho, the T component is composed of Fe and Al or one or more of Fe, Al and other transition metal elements except Fe, and R is1The content of the low-cost R-T-B sintered permanent magnet is marked as x and R2The content of the B element in the low-cost R-T-B series sintered permanent magnet is recorded as y, the content of the B element in the low-cost R-T-B series sintered permanent magnet is recorded as z, the content of the T component in the low-cost R-T-B series sintered permanent magnet is recorded as w, and x, y, z and w simultaneously satisfy the following four relational expressions: x + y + z + w is 1, x + y is more than or equal to 30 wt% and less than or equal to 35 wt%, z is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and z/y is more than or equal to 0.1 and less than or equal to 0.9.
The T component is composed of one or more of Fe element, Al element and other transition metal elements except Fe element, and the content of Al element in the T component is 1.5 wt% -5 wt%. In the product, by adding a proper amount of metallic Al element, Al atoms enter the Nd-rich phase, and the Nd-rich liquid phase and Re are improved2Fe14The wettability of B solid phase enables Nd-rich to be distributed more uniformly along the boundary, improves the grain boundary structure, and further improves the H of the magnetcJ. The content of metallic Al element is reasonably controlled, and the excessive 8j occupied by Al atoms can be avoided2The crystal position causes the Br of the magnet to be reduced too much, so that the HcJ of the magnet can be obviously improved on the basis of avoiding the Br of the magnet to be reduced too much.
When R is1When Ce is contained in the compound, in R1Wherein the content of Ce element is more than or equal to 15 wt% and less than or equal to 50 wt%. In the product, Ce element is rare earth element with most abundant content in earth crust, the price is low, the metal Ce element is adopted to replace Pr element, Nd element or Ho element and the like, the production cost can be reduced, but the element Ce is H elementAIs far smaller than metal Pr element, Nd element or Ho element, and element Ce is suitable for ensuring the performance of R-T-B sintered permanent magnetThe amount of the element substitutes Pr element, Nd element or Ho element.
When R is1When containing Y element, at R1In the above formula, the content of Y element is not more than 15 wt%. In the product, the Y element is rare earth metal with the content of the earth crust being second to that of the Ce element, and the production cost of the magnet can be reduced by replacing the Pr element, the Nd element or the Ho element with the Y element, but the H element of the Y elementAIs far smaller than metal Pr element, Nd element or Ho element, and element Y is used to replace Pr element, Nd element or Ho element in proper amount to ensure the performance of R-T-B sintered permanent magnet.
Compared with the prior art, the R-T-B sintered permanent magnet has the advantages that the low-cost R-T-B sintered permanent magnet is designed through the R component, the T component and the B element, and the R component is formed by R1And R2Composition R1Selected from any one or combination of at least two of Gd element, Ce element, La element and Y element, R2Is selected from any one or the combination of at least two of Nd element, Pr element or Ho element, the T component consists of Fe element and Al element or one or more of Fe element, Al element and other transition metal elements except Fe element, and R is1The content of the sintered permanent magnet is x, R in the low-cost R-T-B series2The content of the B element in the low-cost R-T-B series sintered permanent magnet is recorded as y, the content of the B element in the low-cost R-T-B series sintered permanent magnet is recorded as z, the content of the T component in the low-cost R-T-B series sintered permanent magnet is recorded as w, and x, y, z and w simultaneously satisfy the following four relational expressions: the x + Y + z + w is 1, x + Y is more than or equal to 30 wt% and less than or equal to 35 wt%, z is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and z/Y is more than or equal to 0.1 and less than or equal to 0.9 wt%.
The second technical problem to be solved by the invention is to provide a preparation method of the R-T-B sintered permanent magnet, wherein the sintered permanent magnet prepared by the method is used for replacing at least one of low-abundance Pr, Nd or Ho by one or more of high-abundance rare earth metals Gd, Ce, La and Y, the substitution amount of the rare earth exceeds 70% of the total amount of the rare earth, and the production cost of the sintered permanent magnet is obviously reduced.
The second technical solution adopted by the present invention to solve the above technical problems is: a preparation method of a low-cost R-T-B series sintered permanent magnet comprises the following specific steps: firstly, proportioning according to the proportion, and then smelting, pulverizing, orientation forming and isostatic pressing to obtain the material with the density of 4.0-5.0 g/cm3The green body is sintered finally, and the sintering specific process comprises the following steps: firstly, high-temperature sintering is carried out at the temperature of 1010-1050 ℃ for 4-8 h, then primary aging treatment is carried out at the temperature of 850-950 ℃ for 2.5-4 h, and finally secondary aging treatment is carried out at the temperature of 500-600 ℃ for 4.5 h.
The T component consists of one or more of Fe element, Al element and other transition metal elements except Fe element, and the content of the Al element in the T component is 1.5 wt% -5 wt%.
When R is1When containing Y element, at R1In the above formula, the content of Y element is not more than 15 wt%.
When R is1When Ce is contained in the compound, in R1Wherein the content of Ce element is more than or equal to 15 wt% and less than or equal to 50 wt%.
Compared with the prior art, the preparation method of the R-T-B sintered permanent magnet has the advantages that the low-cost R-T-B sintered permanent magnet is prepared from the R component, the T component and the B element1And R2Composition R1Selected from any one or combination of at least two of Gd element, Ce element, La element and Y element, R2Is selected from any one or the combination of at least two of Nd element, Pr element or Ho element, and the T component consists of Fe element and Al element or one or more of Fe element, Al element and other transition metal elements except Fe elementTo form R1The content of the sintered permanent magnet is x, R in the low-cost R-T-B series2The content of the B element in the low-cost R-T-B series sintered permanent magnet is recorded as y, the content of the B element in the low-cost R-T-B series sintered permanent magnet is recorded as z, the content of the T component in the low-cost R-T-B series sintered permanent magnet is recorded as w, and x, y, z and w simultaneously satisfy the following four relational expressions: x + Y + z + w is 1, x + Y is more than or equal to 30 wt% and less than or equal to 35 wt%, z is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and z/Y is more than or equal to 0.1 and less than 0.9. in the preparation method of the R-T-B system sintered permanent magnet, rare earth metals Gd, Ce, La or Y with high abundance and low price are adopted to replace rare earth metals with low abundance and high price such as Pr, Nd or Ho, the substitution amount of the rare earth exceeds 70% of the total amount of the rare earth, the formula cost of the magnet is reduced, and a specific sintering process is adopted, so that the interior of the magnet has an excellent grain boundary structure, a low-cost R-T-B system sintered permanent magnet with the performance between that of a sintered neodymium-iron-boron magnet and that of ferrite and the working temperature of 80-120 ℃ is produced, on the basis of having better magnetic property, the production cost of the sintered permanent magnet is obviously reduced, the vacancy of the magnetic property is filled, and a new magnet market is opened.
Detailed Description
The invention discloses a low-cost R-T-B series sintered permanent magnet, which is further described in detail by combining the embodiment.
Example (b): a low-cost R-T-B sintered permanent magnet comprises R component, T component and B element1And R2Composition R1One or a combination of at least two of Gd element, Ce element, La element and Y element, R2Is selected from one or the combination of two of Nd element, Pr element and Ho element, the T component consists of Fe element and Al element or one or more of Fe element, Al element and other transition metal elements except Fe element, R is1The content of the sintered permanent magnet is x, R in the low-cost R-T-B series2The content of the element B in the low-cost R-T-B sintered permanent magnet is recorded as y, the content of the element B in the low-cost R-T-B sintered permanent magnet is recorded as z, and the content of the component T in the low-cost R-T-B sintered permanent magnet is recorded as zw, x, y, z, w satisfy the following four relations at the same time: x + y + z + w is 1, x + y is more than or equal to 30 wt% and less than or equal to 35 wt%, z is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and z/y is more than or equal to 0.1 and less than or equal to 0.9.
In this embodiment, the T component is composed of one or more of Fe, Al, and other transition metal elements except Fe, and the content of Al in the T component is 1.5 wt% to 5 wt%.
In this example, when R is1When containing Y element, at R1In the above formula, the content of Y element is not more than 15 wt%.
In this example, when R is1When Ce is contained in the compound, in R1Wherein the content of Ce element is more than or equal to 15 wt% and less than or equal to 50 wt%.
The invention also discloses a preparation method of the low-cost R-T-B series sintered permanent magnet, which is further described in detail by combining the embodiment.
Example (b): a preparation method of a low-cost R-T-B series sintered permanent magnet comprises the following specific steps: firstly, proportioning according to the proportion, and then smelting, pulverizing, orientation forming and isostatic pressing to obtain the material with the density of 4.0-5.0 g/cm3The green body is sintered at last, and the specific sintering process is as follows: firstly, high-temperature sintering is carried out at the temperature of 1010-1050 ℃ for 4-8 h, then primary aging treatment is carried out at the temperature of 850-950 ℃ for 2.5-4 h, and finally secondary aging treatment is carried out at the temperature of 500-600 ℃ for 4.5 h.
In this embodiment, the T component is composed of one or more of Fe, Al, and other transition metal elements except Fe, and the content of Al in the T component is 1.5 wt% to 5 wt%.
In this embodiment, when R is1When containing Y element, at R1In the above formula, the content of Y element is not more than 17 wt%.
In this embodiment, when R is1When Ce is contained in the compound, in R1Wherein the content of Ce element is more than or equal to 14 wt% and less than or equal to 50 wt%.
In order to verify the magnetic performance of the low-cost R-T-B series sintered permanent magnet, nine low-cost R-T-B series sintered permanent magnets with different components and proportions are prepared by the preparation method of the low-cost R-T-B series sintered permanent magnet, and the nine low-cost R-T-B series sintered permanent magnets are respectively named as cases one to nine. The performances of the nine low-cost R-T-B series sintered permanent magnets are detected by using a MIN-15000H rare earth permanent magnet tester, and the specific cases are as follows:
embodiment 1
(1) Raw materials are mixed according to the proportion of 8 wt% of Pr-Nd; 5 wt% of Ce; 18 wt% of Gd; 1.2 wt% of Al; 0.97 wt% of B; 0.2 wt% of Co; 0.1 wt% of Cu; 0.15 wt% of Zr and the balance of Fe are mixed together in proportion for batching.
(2) And (2) putting the mixed raw material prepared in the step (1) into a vacuum induction smelting furnace, vacuumizing to below 1Pa, filling Ar to 28kPa, heating, melting, measuring the temperature of the tested molten steel to 1480 ℃, and casting to obtain the rapid-hardening casting sheet with the thickness of 0.2-0.5 mm.
(3) And (3) carrying out hydrogen crushing and dehydrogenation on the quick-setting casting piece obtained in the step (2) to obtain coarse crushed magnetic powder, and carrying out airflow milling on the obtained coarse powder under the protection of inert gas to obtain fine powder with the SMD of 2.7 microns.
(4) Carrying out orientation molding and isostatic pressing on the fine powder obtained in the step (3) in a magnetic field with the magnetic field intensity of 1.5T to obtain the fine powder with the density of 4.5g/cm3The green compact of (1).
(5) Putting the green body obtained in the step (4) into a vacuum sintering furnace, and preserving heat for 5 hours at 1030 ℃, wherein the primary tempering temperature is 900 ℃, the secondary tempering temperature is 550 ℃, and the time is 4.5 hours
(6) And (3) detecting, namely detecting the performance of the magnet by using a MIN-15000H rare earth permanent magnet tester, wherein the result is shown in table 1.
Table 1: implementation case one test result
Br(kGs) HcJ(kOe) (BH)max(MGOe) Hk/HcJ
9.5 10.6 20.1 0.94
Example II
(1) 5 wt% of raw materials according to the Pr-Nd; 10 wt% of Ce; 12.6 wt% of Gd; 2 wt% of Al; 0.98 wt% of B; 0.2 wt% of Co; 0.1 wt% of Cu; 3 wt% of Y; 0.15 wt% of Zr and the balance of Fe are mixed together in proportion for batching.
(2) And (2) putting the mixed raw material prepared in the step (1) into a vacuum induction smelting furnace, vacuumizing to below 1Pa, filling Ar to 28kPa, heating, melting, measuring the temperature of the test molten steel at 1460 ℃, and casting to obtain a rapid-hardening casting sheet with the thickness of 0.2-0.5 mm.
(3) And (3) carrying out hydrogen crushing and dehydrogenation on the quick-setting casting piece obtained in the step (2) to obtain coarse crushed magnetic powder, and carrying out airflow milling on the obtained coarse powder under the protection of inert gas to obtain fine powder with the SMD of 2.6 microns.
(4) Carrying out orientation molding and isostatic pressing on the fine powder obtained in the step (3) in a magnetic field with the magnetic field intensity of 1.5T to obtain the fine powder with the density of 4.5g/cm3The green compact of (1).
(5) And (4) putting the green body obtained in the step (4) into a vacuum sintering furnace, and preserving heat for 5 hours at 1045 ℃, wherein the primary tempering temperature is 900 ℃ and 2.5 hours, the secondary tempering temperature is 575 ℃ and the time is 4.5 hours.
(6) Detecting, namely detecting the performance of the magnet by using a MIN-15000H rare earth permanent magnet tester, wherein the result is shown in a table 2: test results of example two
Br(kGs) HcJ(kOe) (BH)max(MGOe) Hk/HcJ
8.32 6.2 16.13 0.95
Example three
(1) 1.2 wt% of raw materials according to the Pr-Nd ratio; 13 wt% of Ce; 18 wt% of Gd; 3 wt% of Al; b, 1 wt%; 0.2 wt% of Co; 0.1 wt% of Cu; 0.15 wt% of Zr and the balance of Fe are mixed together in proportion for batching.
(2) And (2) putting the mixed raw material prepared in the step (1) into a vacuum induction smelting furnace, vacuumizing to below 1Pa, filling Ar to 28kPa, heating, melting, measuring the temperature, and casting to obtain a rapid-hardening casting sheet with the thickness of 0.2-0.5 mm, wherein the test molten steel temperature is 1490 ℃.
(3) And (3) carrying out hydrogen crushing and dehydrogenation on the quick-setting casting piece obtained in the step (2) to obtain coarse crushed magnetic powder, and carrying out airflow milling on the obtained coarse powder under the protection of inert gas to obtain fine powder with the SMD of 2.7 microns.
(4) Carrying out orientation molding and isostatic pressing on the fine powder obtained in the step (3) in a magnetic field with the magnetic field intensity of 1.5T to obtain the fine powder with the density of 4.5g/cm3The green compact of (1).
(5) And (4) putting the green body obtained in the step (4) into a vacuum sintering furnace, and preserving heat for 5 hours at 1030 ℃, wherein the primary tempering temperature is 900 ℃ and 2.5 hours, the secondary tempering temperature is 575 ℃ and the time is 4.5 hours.
(6) Detecting, namely detecting the performance of the magnet by using a MIN-15000H rare earth permanent magnet tester, wherein the result is shown in a table 3: results of the three tests of the example
Br(kGs) HcJ(kOe) (BH)max(MGOe) Hk/HcJ
6.7 4.1 10.7 0.97
Example four
(1) 3.5 wt% of raw materials according to the Pr-Nd; 11 wt% of Ce; 20 wt% of Gd; 2.5 wt% of Al; 0.96 wt% of B; 0.2 wt% of Co; 0.1 wt% of Cu; 0.15 wt% of Zr and the balance of Fe are mixed together in proportion for batching.
(2) And (2) putting the mixed raw material prepared in the step (1) into a vacuum induction smelting furnace, vacuumizing to below 1Pa, filling Ar to 28kPa, heating, melting, measuring the temperature, and casting at a test molten steel temperature of 1483 ℃ to obtain a rapid-hardening casting sheet with the thickness of 0.2-0.5 mm.
(3) And (3) carrying out hydrogen crushing and dehydrogenation on the quick-setting casting piece obtained in the step (2) to obtain coarse crushed magnetic powder, and carrying out airflow milling on the obtained coarse powder under the protection of inert gas to obtain fine powder with the SMD of 2.8 microns.
(4) Orienting the fine powder obtained in the step (3) in a magnetic field with the magnetic field intensity of 1.5T to obtainMolding, isostatic pressing to obtain a density of 4.6g/cm3The green compact of (1).
(5) And (4) putting the green body obtained in the step (4) into a vacuum sintering furnace, and preserving heat for 5 hours at 1030 ℃, wherein the primary tempering temperature is 900 ℃, the secondary tempering temperature is 500 ℃, and the time is 4.5 hours.
(6) Detecting, namely detecting the performance of the magnet by using a MIN-15000H rare earth permanent magnet tester, wherein the result is shown in a table 4: results of the four tests of the example
Br(kGs) HcJ(kOe) (BH)max(MGOe) Hk/HcJ
7.3 6.2 11.2 0.87
Other embodiments
(1) Raw materials are mixed together according to the proportion of 5 wt% of Pr-Nd, 10 wt% of Ce, 18 wt% of Gd, 1 wt% of Al, 0.97 wt% of B, 0.2 wt% of Co, 0.1 wt% of Cu, 0.15 wt% of Zr and the balance of Fe for batching.
And (2) putting the mixed raw material prepared in the step (1) into a vacuum induction melting furnace, vacuumizing to below 1Pa, filling Ar to 28kPa, heating, melting, measuring the temperature, and obtaining the rapid-hardening casting sheet with the thickness of 0.2-0.5 mm, wherein the casting temperature is 1488 ℃.
(3) And (3) carrying out hydrogen crushing and dehydrogenation on the quick-setting casting piece obtained in the step (2) to obtain coarse crushed magnetic powder, and carrying out airflow milling on the obtained coarse powder under the protection of inert gas to obtain fine powder with the SMD of 2.67 microns.
(4) And (4) carrying out orientation forming and isostatic pressing on the fine powder obtained in the step (3) in a magnetic field with the magnetic field intensity of 1.5T to obtain a magnet green body.
(5) And (4) putting the green body obtained in the step (4) into a vacuum sintering furnace, and preserving heat for 5 hours at 1030 ℃, wherein the primary tempering temperature is 900 ℃ and 2.5 hours, the secondary tempering temperature is 500-600 ℃ and the time is 4.5 hours.
(6) Detecting, namely detecting the performance of the magnet by using a MIN-15000H rare earth permanent magnet tester, wherein the result is shown in a table 5 as follows: other embodiments and test results
Figure BDA0002344947020000081
Figure BDA0002344947020000091
Analyzing the data in Table 5 shows that: with the increase of the secondary aging temperature of the R-T-B sintered permanent magnet, the Br of the R-T-B sintered permanent magnet does not change obviously, and the H of the R-T-B sintered permanent magnetcJThe method has the advantages of remarkable improvement, optimal effect at 575 ℃, and optimal performance of the R-T-B sintered permanent magnet.

Claims (8)

1. A low-cost R-T-B sintered permanent magnet is characterized by comprising an R component, a T component and an element B, wherein the R component is formed by R1And R2Composition R1Selected from any one or combination of at least two of Gd element, Ce element, La element and Y element, R2Selected from any one or the combination of at least two of Nd element, Pr element or Ho element, the T component consists of Fe element and Al element or one or more of Al element, Fe element and other transition metal elements except Fe element, R is1The content of the low-cost R-T-B sintered permanent magnet is marked as x and R2The content of the element B in the low-cost R-T-B sintered permanent magnet is marked as yThe content of the T component in the low-cost R-T-B series sintered permanent magnet is recorded as z, the content of the T component in the low-cost R-T-B series sintered permanent magnet is recorded as w, and x, y, z and w simultaneously satisfy the following four relational expressions: x + y + z + w is 1, x + y is more than or equal to 30 wt% and less than or equal to 35 wt%, z is more than or equal to 0.9 wt% and less than or equal to 1 wt%, and z/y is more than or equal to 0.1 and less than or equal to 0.9.
2. The low-cost R-T-B sintered permanent magnet according to claim 1, wherein the T component is composed of one or more of Fe element, Al element and transition metal element other than Fe element, and the content of Al element in the T component is 1.5 wt% to 5 wt%.
3. The low-cost R-T-B sintered permanent magnet according to claim 1, wherein when R is1When containing Y element, at R1In the above formula, the content of Y element is not more than 15 wt%.
4. The low-cost R-T-B sintered permanent magnet according to claim 1, wherein when R is1When Ce is contained in the compound, in R1Wherein the content of Ce element is more than or equal to 15 wt% and less than or equal to 50 wt%.
5. A method for preparing the low-cost R-T-B sintered permanent magnet according to claim 1, comprising the following steps: firstly, proportioning according to the proportion, and then smelting, pulverizing, orientation forming and isostatic pressing to obtain the material with the density of 4.0-5.0 g/cm3The green body is finally sintered to obtain the ceramic material, and the sintering specific process is as follows: firstly, high-temperature sintering is carried out at the temperature of 1010-1050 ℃ for 4-8 h, then primary aging treatment is carried out at the temperature of 850-950 ℃ for 2.5-4 h, and finally secondary aging treatment is carried out at the temperature of 500-600 ℃ for 4.5 h.
6. The method for preparing a low-cost R-T-B sintered permanent magnet according to claim 5, wherein the T component is composed of one or more of Fe element, Al element and transition metal elements other than Fe element, and the content of Al element in the T component is 1.5 wt% to 5 wt%.
7. The method for preparing a low-cost R-T-B sintered permanent magnet according to claim 5, wherein R is measured when R is greater than a predetermined value1When containing Y element, at R1In the above formula, the content of Y element is not more than 15 wt%.
8. The method for preparing a low-cost R-T-B sintered permanent magnet according to claim 5, wherein R is measured when R is greater than a predetermined value1When Ce is contained in the compound, in R1Wherein the content of Ce element is more than or equal to 15 wt% and less than or equal to 50 wt%.
CN201911391029.6A 2019-12-30 2019-12-30 R-T-B series sintered permanent magnet and preparation method thereof Pending CN111180158A (en)

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Application publication date: 20200519