CN108831653A - The neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force - Google Patents

The neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force Download PDF

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Publication number
CN108831653A
CN108831653A CN201810680775.6A CN201810680775A CN108831653A CN 108831653 A CN108831653 A CN 108831653A CN 201810680775 A CN201810680775 A CN 201810680775A CN 108831653 A CN108831653 A CN 108831653A
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rare earth
neodymium iron
iron boron
coercive force
heavy rare
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马驰
姜华
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Jingci Material Technology Co Ltd
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Jingci Material Technology Co Ltd
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    • 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
    • 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

Abstract

The invention discloses a kind of neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force, step includes：1) two kinds of NbFeB sintered alloys are chosen, one kind is main-phase alloy, and one kind is intergranular phase alloy, and wherein intergranular phase alloy forms by mass percentage includes：Pr-Nd：27%~30%, Dy：2~3%, Al：0.3~0.4%, B：0.85%~0.87%, Cu：0.1~0.3%, Co：0.5~0.8%, Ga：0.5~0.8%, surplus Fe；2) powder is respectively prepared in main-phase alloy and intergranular phase alloy, then mixes two kinds of alloy powders, the ratio of intergranular phase alloy powder and main-phase alloy powder is 0.1~10：100；3) mixed-powder is suppressed, then puts into sintering furnace and is sintered.The present invention starts with from the alloy formula and flouring technology of neodymium iron boron green compact, it is mixed with conventional Nd Fe B alloys in powder stage using special intergranular phase, and during the sintering process, element does not occur with conventional Nd Fe B alloys and mutually replaces for intergranular phase alloy, to improve coercivity, the magnet of the low heavy rare earth of high-residual magnetism high-coercive force can be obtained.

Description

The neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force
Technical field
The invention belongs to permanent magnet preparation technical field more particularly to a kind of neodymium iron of the low heavy rare earth of high-residual magnetism high-coercive force Boron preparation method.
Background technique
Permanent magnet, that is, hard magnetic body, the magnet that can keep it magnetic for a long time, is not easy loss of excitation, is also not easy to be magnetized.Thus, nothing By being in industrial production or in daily life one of most common muscle material of hard magnetic body.Neodymium iron boron magnetic body is also referred to as neodymium Magnet (Neodymium magnet), chemical formula Nd2Fe14B is a kind of artificial permanent magnet, is low by iron and price It is honest and clean, resourceful, can stable supplying neodymium and boron element be composed, can inexpensively manufacture, while the magnetic energy product of neodymium iron boron Can achieve ferritic 10 times or more, thus, neodymium iron boron magnetic body due to its cost performance is excellent, under volume, density is high, has excellent performance And it is widely used in the fields such as wind-powered electricity generation, motor, VCM, unmanned plane, and with the development of hybrid-electric car, have very in future Big development opportunity.Currently, high-performance Ne-Fe-B permanent magnet is mainly prepared by sintering process, wherein Zhou Shouzeng etc. exists《It is sintered neodymium iron Boron rare earth permanent-magnetic material and technology》In disclose the fabrication processing of sintered Nd-Fe-B permanent magnet, mainly melting, powder processed, Compression moulding, etc. static pressure and sintering five steps, specifically include ingredient, melting, hydrogen breaking, powder processed, powder orientation compression moulding, Equal static pressure, vacuum-sintering.
With the development of the related fieldss such as air-conditioning, electric car, the demand to neodymium iron boron is higher and higher, wants to magnetic property Ask also higher and higher, with the development of down-stream enterprise, traditional preparation method has been difficult to produce in the case where few heavy rare earth The magnet of high-residual magnetism high-coercive force out.
Summary of the invention
Technical problem solved by the invention is can to reduce about 1~3%wt while obtaining high-residual magnetism high-coercive force Heavy rare earth use, while excellent heat-resisting demagnetization performance can be obtained.
Aiming at the problem that being previously mentioned, the present invention provides a kind of neodymium iron boron preparation sides of the low heavy rare earth of high-residual magnetism high-coercive force Method, step include：
1) two kinds of NbFeB sintered alloys are chosen, one kind is main-phase alloy, and one kind is intergranular phase alloy, and wherein intergranular is harmonious Composition includes gold by mass percentage：Pr-Nd：27%~30%, Dy：2~3%, Al：0.3~0.4%, B：0.85%~ 0.87%, Cu：0.1~0.3%, Co：0.5~0.8%, Ga：0.5~0.8%, surplus Fe；
2) powder is respectively prepared in main-phase alloy and intergranular phase alloy, then mixes two kinds of alloy powders, intergranular is harmonious The ratio of bronze end and main-phase alloy powder is 0.1~10：100；
3) mixed-powder is suppressed, then puts into sintering furnace and is sintered.
Preferred embodiment is：Two kinds of alloys are subjected to the quick-fried processing of hydrogen respectively, obtain hydrogen breaking coarse powder, the coarse powder that then will be obtained Airflow milling is carried out respectively.
Preferred embodiment is：Airflow milling obtains the fine powder that granularity is 1~6 μm.
Preferred embodiment is：The coarse powder carries out airflow milling under the protection of inert gas.
Preferred embodiment is：Mixed powder is suppressed under the press that orientation field is 1.5T or more, is then put into Sintering furnace is sintered.
Preferred embodiment is：The green density of compression moulding is 3.5~5.5g/cm3。
Preferred embodiment is：The sintering furnace heating initial vacuum degree is 0.4~0.6Pa.
Preferred embodiment is：Sintering method in the sintering furnace is as follows：
1) after the sintering furnace being warming up to 200~400 DEG C, 1~3h is kept the temperature；
2) after the sintering furnace being warming up to 500~650 DEG C, 1~3h is kept the temperature；
3) after the sintering furnace being warming up to 700~850 DEG C, 3~4h is kept the temperature；
4) sintering furnace is warming up to 1000~1150 DEG C, keeps the temperature 10~12h.
Preferred embodiment is：The main-phase alloy forms by mass percentage：Pr-Nd：29%~31%, Dy：1.0~ 1.5%, Al：0.3~0.4%, B：0.95%~0.96%, Cu：0.1~0.2%, Co：0.5~0.7%, Zr：0.17~ 2.0%, surplus Fe.
Preferred embodiment is：Rapid casting is made in two kinds of alloys.
Multiple steps of the present invention in neodymium-iron-boron production procedure are analyzed, from the alloy formula of neodymium iron boron green compact Start with flouring technology, it is big or the case where need very high heavy rare earth content for high-residual magnetism high-coercive force difficulty is prepared now, Mix with conventional Nd Fe B alloys in powder stage using special intergranular phase, and during the sintering process, intergranular phase alloy with it is normal Element does not occur and mutually replaces for rule Nd Fe B alloys, thus guarantee the high remanent magnetism of conventional Nd Fe B alloys, after mutually being added by intergranular, Coercivity is improved, it is hereby achieved that the magnet of the low heavy rare earth of high-residual magnetism high-coercive force.
Specific embodiment
The present invention is described in further detail below, to enable those skilled in the art's refer to the instruction text being capable of evidence To implement.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more The presence or addition of a other elements or combinations thereof.
The present invention provides a kind of neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force, step includes：
1) two kinds of NbFeB sintered alloys are chosen, one kind is main-phase alloy, and one kind is intergranular phase alloy, and wherein intergranular is harmonious Composition includes gold by mass percentage：Pr-Nd：27%~30%, Dy：2~3%, Al：0.3~0.4%, B：0.85%~ 0.87%, Cu：0.1~0.3%, Co：0.5~0.8%, Ga：0.5~0.8%, surplus Fe；
2) powder is respectively prepared in main-phase alloy and intergranular phase alloy, then mixes two kinds of alloy powders, intergranular is harmonious The ratio of bronze end and main-phase alloy powder is 0.1~10：100；
3) mixed-powder is suppressed, then puts into sintering furnace and is sintered.
Preferred embodiment is：Two kinds of alloys are subjected to the quick-fried processing of hydrogen respectively, obtain hydrogen breaking coarse powder, the coarse powder that then will be obtained Airflow milling is carried out respectively.
Preferred embodiment is：Airflow milling obtains the fine powder that granularity is 1~6 μm.
Preferred embodiment is：The coarse powder carries out airflow milling under the protection of inert gas.
Preferred embodiment is：Mixed powder is suppressed under the press that orientation field is 1.5T or more, is then put into Sintering furnace is sintered.
Preferred embodiment is：The green density of compression moulding is 3.5~5.5g/cm3。
Preferred embodiment is：The sintering furnace heating initial vacuum degree is 0.4~0.6Pa.
Preferred embodiment is：Sintering method in the sintering furnace is as follows：
1) after the sintering furnace being warming up to 200~400 DEG C, 1~3h is kept the temperature；
2) after the sintering furnace being warming up to 500~650 DEG C, 1~3h is kept the temperature；
3) after the sintering furnace being warming up to 700~850 DEG C, 3~4h is kept the temperature；
4) sintering furnace is warming up to 1000~1150 DEG C, keeps the temperature 10~12h.
Preferred embodiment is：The main-phase alloy forms by mass percentage：Pr-Nd：29%~31%, Dy：1.0~ 1.5%, Al：0.3~0.4%, B：0.95%~0.96%, Cu：0.1~0.2%, Co：0.5~0.7%, Zr：0.17~ 2.0%, surplus Fe.
Preferred embodiment is：Rapid casting is made in two kinds of alloys.
Embodiment 1
A kind of neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force is present embodiments provided, step includes：
1) two kinds of NbFeB sintered alloys are chosen, one kind is main-phase alloy, and one kind is intergranular phase alloy, and wherein intergranular is harmonious Composition includes gold by mass percentage：Pr-Nd：27%, Dy：3%, Al：0.3%, B：0.85%, Cu：0.1%, Co：0.5%, Ga：0.5%, surplus Fe；The main-phase alloy forms by mass percentage：Pr-Nd：29%, Dy：1.5%, Al： 0.3%, B：0.95%, Cu：0.1%, Co：0.5%, Zr：0.17%, surplus Fe；
2) two kinds of alloys are subjected to hydrogen breaking respectively；
3) it carries out airflow milling powder respectively under the protection of inert gas, obtains the fine powder that granularity is 1um；
4) two kinds of alloy powders are mixed, the ratio of intergranular phase alloy powder and main-phase alloy powder is 0.1：100；
5) hybrid alloys powder is suppressed under the press that orientation field is 1.5T or more, it is 3.5g/cm that density, which is made,3 Green compact；
6) green compact is put into sintering furnace and is sintered, the heating initial vacuum degree of sintering furnace is 0.4Pa, the sintering furnace Interior sintering method is as follows：
A) after the sintering furnace being warming up to 200 DEG C, 1h is kept the temperature；
B) after the sintering furnace being warming up to 500 DEG C, 1h is kept the temperature；
C) after the sintering furnace being warming up to 700 DEG C, 3h is kept the temperature；
D) sintering furnace is warming up to 1000 DEG C, keeps the temperature 10h.
Magnetism testing is carried out to the neodymium iron boron magnetic body of above-mentioned steps preparation, as a result referring to table 1, table 1 is the system of the present embodiment 1 Standby neodymium iron boron magnetic body magnetic property, dysprosium content and terbium content balance data.
Table 1 is neodymium iron boron magnetic body magnetic property, density and crystallite dimension, sintering temperature correlation data prepared by the present embodiment 1
Table 1
Remarks：Terbium price is about three times of dysprosium, and the abundance of terbium is much smaller than dysprosium, although thus heavy rare earth content difference is not Greatly, but prior art has used terbium.
As can be seen from Table 1, the magnetic property of neodymium iron boron magnetic body manufactured in the present embodiment coercivity phase compared with the prior art When, but this method does not use terbium metal, and total heavy rare earth content reduces 1wt%.
Embodiment 2
A kind of neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force is present embodiments provided, step includes：
1) two kinds of NbFeB sintered alloys are chosen, one kind is main-phase alloy, and one kind is intergranular phase alloy, and wherein intergranular is harmonious Composition includes gold by mass percentage：Pr-Nd：30%, Dy：2%, Al：0.4%, B：0.87%, Cu：0.3%, Co：0.8%, Ga：0.8%, surplus Fe；The main-phase alloy forms by mass percentage：Pr-Nd：31%, Dy：1.0%, Al： 0.4%, B：0.96%, Cu：0.2%, Co：0.7%, Zr：2.0%, surplus Fe；
2) two kinds of alloys are subjected to hydrogen breaking respectively；
3) it carries out airflow milling powder respectively under the protection of inert gas, obtains the fine powder that granularity is 6um；
4) two kinds of alloy powders are mixed, the ratio of intergranular phase alloy powder and main-phase alloy powder is 1：10；
5) hybrid alloys powder is suppressed under the press that orientation field is 1.5T or more, it is 5.5g/cm that density, which is made,3 Green compact；
6) green compact is put into sintering furnace and is sintered, the heating initial vacuum degree of sintering furnace is 0.6Pa, the sintering furnace Interior sintering method is as follows：
A) after the sintering furnace being warming up to 400 DEG C, 3h is kept the temperature；
B) after the sintering furnace being warming up to 650 DEG C, 3h is kept the temperature；
C) after the sintering furnace being warming up to 850 DEG C, 4h is kept the temperature；
D) sintering furnace is warming up to 1150 DEG C, keeps the temperature 12h.
Magnetism testing is carried out to the neodymium iron boron magnetic body of above-mentioned steps preparation, as a result referring to table 2, table 2 is the system of the present embodiment 2 Standby neodymium iron boron magnetic body magnetic property, dysprosium content and terbium content balance data.
Neodymium iron boron magnetic body magnetic property, dysprosium content and the terbium content balance data of 2 the present embodiment 2 of table preparation
As shown in Table 2, the magnetic property of the neodymium iron boron magnetic body of this preparation method preparation coercivity and surplus compared with the prior art Magnetic is suitable, and heavy rare earth reduces 1.5wt%, and without using terbium.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details.

Claims (10)

1. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force, which is characterized in that step includes：
1) two kinds of NbFeB sintered alloys are chosen, one kind is main-phase alloy, and one kind is intergranular phase alloy, and wherein intergranular phase alloy is pressed Mass percentage composition includes：Pr-Nd：27%~30%, Dy：2~3%, Al：0.3~0.4%, B：0.85%~0.87%, Cu：0.1~0.3%, Co：0.5~0.8%, Ga：0.5~0.8%, surplus Fe；
2) powder is respectively prepared in main-phase alloy and intergranular phase alloy, then mixes two kinds of alloy powders, intergranular is harmonious bronze The ratio of end and main-phase alloy powder is 0.1~10：100；
3) mixed-powder is suppressed, then puts into sintering furnace and is sintered.
2. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 1, which is characterized in that will Two kinds of alloys carry out the quick-fried processing of hydrogen respectively, obtain hydrogen breaking coarse powder, and obtained coarse powder is then carried out airflow milling respectively.
3. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 2, which is characterized in that gas Stream mill obtains the fine powder that granularity is 1~6 μm.
4. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 2, which is characterized in that institute It states coarse powder and carries out airflow milling under the protection of inert gas.
5. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 1, which is characterized in that will Mixed powder is suppressed under the press that orientation field is 1.5T or more, is then put into sintering furnace and is sintered.
6. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 1, which is characterized in that pressure Making molding green density is 3.5~5.5g/cm3。
7. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 1, which is characterized in that institute Stating sintering furnace heating initial vacuum degree is 0.4~0.6Pa.
8. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 1, which is characterized in that institute The sintering method stated in sintering furnace is as follows：
1) after the sintering furnace being warming up to 200~400 DEG C, 1~3h is kept the temperature；
2) after the sintering furnace being warming up to 500~650 DEG C, 1~3h is kept the temperature；
3) after the sintering furnace being warming up to 700~850 DEG C, 3~4h is kept the temperature；
4) sintering furnace is warming up to 1000~1150 DEG C, keeps the temperature 10~12h.
9. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 1, which is characterized in that institute It states main-phase alloy and forms by mass percentage and include：Pr-Nd：29%~31%, Dy：1.0~1.5%, Al：0.3~0.4%, B：0.95%~0.96%, Cu：0.1~0.2%, Co：0.5~0.7%, Zr：0.17~2.0%, surplus Fe.
10. the neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force according to claim 1, which is characterized in that Rapid casting is made in two kinds of alloys.
CN201810680775.6A 2018-06-27 2018-06-27 The neodymium iron boron preparation method of the low heavy rare earth of high-residual magnetism high-coercive force Pending CN108831653A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111952032A (en) * 2020-08-15 2020-11-17 赣州嘉通新材料有限公司 Preparation method of low-boron low-weight rare earth high-coercivity sintered neodymium-iron-boron permanent magnet
CN112086255A (en) * 2020-09-18 2020-12-15 湖南奔朗新材料科技有限公司 High-coercivity and high-temperature-resistant sintered neodymium-iron-boron magnet and preparation method thereof
CN116313353A (en) * 2023-05-23 2023-06-23 包头天石稀土新材料有限责任公司 Neodymium-iron-boron magnet and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106920620A (en) * 2017-04-05 2017-07-04 北京京磁电工科技有限公司 Neodymium iron boron magnetic body and preparation method thereof
CN107316727A (en) * 2017-07-06 2017-11-03 京磁材料科技股份有限公司 A kind of sintered NdFeB preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106920620A (en) * 2017-04-05 2017-07-04 北京京磁电工科技有限公司 Neodymium iron boron magnetic body and preparation method thereof
CN107316727A (en) * 2017-07-06 2017-11-03 京磁材料科技股份有限公司 A kind of sintered NdFeB preparation method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111952032A (en) * 2020-08-15 2020-11-17 赣州嘉通新材料有限公司 Preparation method of low-boron low-weight rare earth high-coercivity sintered neodymium-iron-boron permanent magnet
CN112086255A (en) * 2020-09-18 2020-12-15 湖南奔朗新材料科技有限公司 High-coercivity and high-temperature-resistant sintered neodymium-iron-boron magnet and preparation method thereof
CN116313353A (en) * 2023-05-23 2023-06-23 包头天石稀土新材料有限责任公司 Neodymium-iron-boron magnet and preparation method thereof
CN116313353B (en) * 2023-05-23 2023-08-29 包头天石稀土新材料有限责任公司 Neodymium-iron-boron magnet and preparation method thereof

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