CN108133798A - A kind of rare-earth permanent magnet and preparation method thereof - Google Patents

A kind of rare-earth permanent magnet and preparation method thereof Download PDF

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Publication number
CN108133798A
CN108133798A CN201711387056.7A CN201711387056A CN108133798A CN 108133798 A CN108133798 A CN 108133798A CN 201711387056 A CN201711387056 A CN 201711387056A CN 108133798 A CN108133798 A CN 108133798A
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Prior art keywords
ingredient
permanent magnet
rare
powder
earth permanent
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CN201711387056.7A
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Chinese (zh)
Inventor
朱小英
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Ningbo City Yinzhou Zhi Companion Mdt Infotech Ltd
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Ningbo City Yinzhou Zhi Companion Mdt Infotech Ltd
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Priority to CN201711387056.7A priority Critical patent/CN108133798A/en
Publication of CN108133798A publication Critical patent/CN108133798A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266Moulding; Pressing

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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 kind of rare-earth permanent magnet and preparation method thereof, component and weight ratio are as follows:Ingredient be 28.15 La, ingredient be 49.4 Ce, ingredient be 6 Pr, ingredient be 16 Nb, ingredient be 0.05 Dy, ingredient be 0.01 Sm, the raw material such as Gd and pure iron that ingredient is 0.03, ferro-boron, cathode copper, the electrolytic aluminium that boron mass fraction is 19.2%.The process of preparation:By (NdPr)18.2(MM)13.6Fe66.22B1.08Cu0.2Al0.7(mass fraction) carries out dispensing, and in pulverizing process, powder is 1280~1440A/m in magnetic field, and forming is orientated in the press that pressure is 5~10MPa;Forming green compact are kept 240 minutes or so under 10 3~10 2Pa vacuum conditions within the temperature range of 1060 DEG C, are then tempered 2h at 600 DEG C;Its magnetic property is measured with 10000 type magnetism testing instrument of NIM to be machined, coating;Impulse magnetization;The residual magnetic flux density (Br) of gained mischmetal permanent magnet is 1116~112T, and intrinsic coercivity (Hcj) is 960~1000kA/m, and magnetic energy product (BH) is 248~264kJ/m3.

Description

A kind of rare-earth permanent magnet and preparation method thereof
Technical field
The invention belongs to field of rare-earth permanent magnetic, more particularly to a kind of rare-earth permanent magnet and preparation method thereof.
Background technology
The magnet that can keep it magnetic for a long time claims permanent magnet.Such as natural magnetite (magnetic iron ore) and artificial magnet's (aluminium Nickel cobalt (alloy)) etc..In magnet in addition to permanent magnet, also there is the just magnetic electromagnet that need to be powered.Permanent magnet is also hard magnetic body, no Easy loss of excitation is not easy to be magnetized.But if permanent magnet is heated beyond Curie temperature or in the environment of reversed high magnetic field intensity In, magnetism also can be reduced or be disappeared.Some magnets enbrittle, and may rupture at high temperature.The highest of alnico magnet Temperature in use is more than 540 DEG C (1,000 °F), and samarium-cobalt magnet and ferrite are about 300 DEG C (570 °F), neodymium magnet and soft magnet About 140 DEG C (280 °F), but actual numerical value still can be different according to the crystal grain of material.And as magnetizer and the material of electromagnet Material is mostly soft magnetic bodies.Permanent magnet polarity will not change, and soft magnetic bodies polarity becomes with added polarity of the magnetic field.They can Attract irony object, we are this property magnetism.1967, Strnat of Dayton universities of the U.S. etc. used powder bonding SmCo5 permanent magnets are successfully made in method, indicate the arrival in rare earth permanent magnet epoch.So far, rare earth permanent magnet has undergone first Third generation Nd-Fe-B permanent-magnet materials are developed to for SmCo5, second generation precipitation hardenable Sm2Co17.In addition, in history by with That makees permanent-magnet material also has Cu-Ni-Fe, Fe-Co-Mo, Fe-Co-V, MnBi, A1MnC alloy etc..These alloys due to performance not Height, cost be not low, has seldom been used in most of occasions.And the alloys such as AlNiCo, FeCrCo, PtCo in some special occasions also It is applied.Ba, Sr ferrite are still the permanent-magnet material of dosage maximum at present, but its many application is gradually by Nd-Fe- B classes material replaces.Also, the output value of current rare-earth permanent magnetic material has substantially exceeded ferrite permanent-magnet materials, rare earth permanent magnet material The production of material has evolved into a big industry.When producing magnet from these materials, N33, the rare earth material that N35 neodymium iron boron magnetic bodies use Material is limited, will be lacked later using some, and it is applied in such as toy magnetic, packing fastener magnetic and magnetic salvaging The fields such as device.
In view of above defect in the prior art, it is necessary to be further improved, make it more for practicability, Actual use situation can be met.
Invention content
To overcome above-mentioned deficiency, the present invention provides a kind of rare-earth permanent magnet.
The present invention takes following technical scheme to realize:A kind of rare-earth permanent magnet, component and weight ratio are as follows:
Ingredient is 28.15 La, and ingredient is 49.4 Ce, and ingredient is 6 Pr, and ingredient is 16 Nb, and ingredient is 0.05 Dy, ingredient are 0.01 Sm, the ferro-boron, cathode copper, electricity that Gd and pure iron that ingredient is 0.03, boron mass fraction are 19.2% Solve the raw material such as aluminium.
A kind of preparation method of rare-earth permanent magnet, it is characterised in that:Include the following steps:
(1):By (NdPr)18.2(MM)13.6Fe66.22B1.08Cu0.2Al0.7(mass fraction) carries out dispensing;
(2):The raw material prepared is carried out to get rid of band melting, forms the alloy of thin ribbon shaped;
(3):Thin ribbon shaped alloy is crushed by hydrogen, then is milled into the alloy powder that average particle size is 4.0 μm with air-flow.Powder processed In the process, different amounts of antioxidant and aviation gasoline are added respectively, and the oxygen of powder is measured with IRO-I type determination of oxygen content instrument Content;
(4):Powder is 1280~1440A/m in magnetic field, and forming is orientated in the press that pressure is 5~10MPa;
(5):Shape green compact under 10-3~10-2Pa vacuum conditions in 700 DEG C or more less than 1000 DEG C within the temperature range of It is kept for less than 420 minutes 10 minutes or more being sintered, 10 points is then kept within the scope of the temperature below 1000 DEG C or more 1200 DEG C It is more than clock 420 minutes hereinafter, then 600 DEG C be tempered 2h;
(6):Its magnetic property is measured with NIM-10000 type magnetism testing instrument;
(7):Mechanical processing, coating;
(8):Impulse magnetization;
Further, in the sintering process by one or more, and extraneous factor activated sintering process is used, raising The activity of powder, reduces sintering temperature, and sintering process is accelerated, and reaches the method for improving material property and is known as activated sintering.It adopts There is method chemically or physically with method:Activator or addition strong reductant are added such as in atmosphere, applies external carbuncle etc..
Further, the element M is at least containing one or more in Pr, Nd, Sm.
Further, the antioxidant is a kind of substance (1%~3%) in Zr84Al16 and La, Ce, Pr, Nd.
The residual magnetic flux density (Br) of gained mischmetal permanent magnet is 1116~112T, and intrinsic coercivity (Hcj) is 960~1000kA/m, magnetic energy product (BH) are 248~264kJ/m3.
In technical scheme of the present invention, (NdPr) after the completion of dispensing18.2(MM)13.6Fe66.22B1.08Cu0.2Al0.7(quality Score), next, by slightly being got rid of with the size crushed as 0.1mm~5mm or so in alloy material absorbing hydrogen.Moreover, use spray Penetrate mill carry out it is finely divided so that grain size using the value measured by laser method be 0.1 μm~10 μm, preferably 3 μm~5 μm, from And obtain alloy powder.In addition, coarse crushing and it is finely divided when, can not also the lubricant of same amount be used as grinding aid. The powder lubricant of+0.3% aviation gasoline of 0.4% antioxidant is added in obtained alloy powder and is mixed, at this time Oxygen content reaches minimum value 0.22%, then oriented moulding in the press under the magnetic field of 1300A/m and 8MPa pressure, then will Molding green compact are kept for 240 minutes or so under 10-3~10-2Pa vacuum conditions within the temperature range of 1060 DEG C, then 600 DEG C tempering 2h.
In summary the invention has the advantages that:Part PrNd alloys are replaced with the mischmetal rich in La, Ce As raw material, by (NdPr)18.2(MM)13.6Fe66.22B1.08Cu0.2Al0.7(mass fraction) carry out dispensing, by get rid of band melting in a manner of Thin ribbon shaped alloy is formed, alloy is milled into powder after hydrogen crushes, with air-flow, and last repressed sintering obtains rare-earth permanent magnet. The residual magnetic flux density of the mischmetal permanent magnet of gained be 1116~112T, intrinsic coercivity be 960~1000kA/m, magnetic Energy product is 248~264kJ/m3.The performance and N33, N35 neodymium iron boron magnetic body performance are suitable, it can instead it is applied in toy magnetic The fields such as iron, packing fastener magnetic and hell raiser.
Specific embodiment
To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, with reference to Specific embodiment, the present invention is further explained.
Embodiment 1
A kind of foregoing process for preparing rare-earth permanent magnet, includes the following steps:
(1):By (NdPr)18.2(MM)13.6Fe66.22B1.08Cu0.2Al0.7(mass fraction) carries out dispensing;
(2):The raw material prepared is carried out to get rid of band melting, forms the alloy of thin ribbon shaped;
(3):Thin ribbon shaped alloy is crushed by hydrogen, then is milled into the alloy powder that average particle size is 4.0 μm with air-flow.Powder processed In the process, it does not add any room oxidant respectively to measure, in the antioxidant and aviation gasoline of addition, and with IRO-I types Determination of oxygen content instrument measures the oxygen content of powder;
(4):Powder is 1280~1440A/m in magnetic field, and forming is orientated in the press that pressure is 5~10MPa;
(5):Forming green compact keep 240 minutes left sides under 10-3~10-2Pa vacuum conditions within the temperature range of 1060 DEG C The right side is then tempered 2h at 600 DEG C;
(6):Its magnetic property is measured with NIM-10000 type magnetism testing instrument;
(7):Mechanical processing, coating;
(8):Impulse magnetization;
After testing, the oxygen content index in the present embodiment 1 after powder processed is shown in Table 1.
Table 1
In table 1, when having 0.4% antioxidant of addition, powder oxygen content obtained is less.
Embodiment 2
A kind of foregoing process for preparing rare-earth permanent magnet, includes the following steps:
(1):By (NdPr)18.2(MM)13.6Fe66.22B1.08Cu0.2Al0.7(mass fraction) carries out dispensing;
(2):The raw material prepared is carried out to get rid of band melting, forms the alloy of thin ribbon shaped;
(3):Thin ribbon shaped alloy is crushed by hydrogen, then is milled into the alloy powder that average particle size is 4.0 μm with air-flow.Powder processed In the process, 0.4% antioxidant is added respectively to measure, in addition+0.3% aviation gasoline of 0.4% antioxidant, be used in combination IRO-I type determination of oxygen content instrument measures the oxygen content of powder;
(4):Powder is 1280~1440A/m in magnetic field, and forming is orientated in the press that pressure is 5~10MPa;
(5):Forming green compact keep 240 minutes left sides under 10-3~10-2Pa vacuum conditions within the temperature range of 1060 DEG C The right side is then tempered 2h at 600 DEG C;
(6):Its magnetic property is measured with NIM-10000 type magnetism testing instrument;
(7):Mechanical processing, coating;
(8):Impulse magnetization;
After testing, oxygen, nitrogen content and feed ratio discharging detection size indicator are shown in Table 2 in the present embodiment.
Table 2
In table 2, when adding 0.4%+0.3% aviation gasoline of antioxidant, powder oxygen content obtained is less.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.

Claims (5)

1. a kind of preparation method of rare-earth permanent magnet, which is characterized in that include the following steps:
Step 1:By (NdPr)18.2(MM)13.6Fe66.22B1.08Cu0.2Al0.7(mass fraction) carries out dispensing;
Step 2:The raw material prepared is carried out to get rid of band melting, forms the alloy of thin ribbon shaped;
Step 3:Thin ribbon shaped alloy is crushed by hydrogen, then is milled into the alloy powder that average particle size is 4.0 μm with air-flow.Powder mistake processed Cheng Zhong adds different amounts of antioxidant and aviation gasoline, and is contained with the oxygen of IRO-I type determination of oxygen content instrument measurement powder respectively Amount;
Step 4:Powder is 1280~1440A/m in magnetic field, and forming is orientated in the press that pressure is 5~10MPa;
Step 5:Shape green compact under 10-3~10-2Pa vacuum conditions in 700 DEG C or more less than 1000 DEG C within the temperature range of protect It holds less than 420 minutes 10 minutes or more and is sintered, then kept for 10 minutes within the scope of the temperature below 1000 DEG C or more 1200 DEG C More than 420 minutes hereinafter, then 600 DEG C be tempered 2h;
Step 6:Its magnetic property is measured with NIM-10000 type magnetism testing instrument;
Step 7:Mechanical processing, coating;
Step 8:Impulse magnetization;
The residual magnetic flux density (Br) of gained mischmetal permanent magnet is 1116~112T, intrinsic coercivity (Hcj) for 960~ 1000kA/m, magnetic energy product (BH) are 248~264kJ/m3.
2. a kind of rare-earth permanent magnet according to claim 1, it is characterised in that:Its component and weight ratio are as follows:
Ingredient is 28.15 La, and ingredient is 49.4 Ce, and ingredient is 6 Pr, and ingredient is 16 Nb, and ingredient is 0.05 Dy, into It is divided into 0.01 Sm, Gd and pure iron that ingredient is 0.03, ferro-boron, cathode copper, the electrolytic aluminium that boron mass fraction is 19.2% etc. Raw material.
3. a kind of rare-earth permanent magnet according to claim 1-2, it is characterised in that:By one kind in the sintering process Or it is a variety of, and with extraneous factor activated sintering process, improve the activity of powder, reduce sintering temperature, sintering process is accelerated, and reaches It is known as activated sintering to the method for improving material property.There is method chemically or physically using method:It adds and lives such as in atmosphere Agent or addition strong reductant, apply external carbuncle etc..
4. a kind of rare-earth permanent magnet according to claim 1-3, it is characterised in that:The element M at least containing Pr, Nd, It is one or more in Sm.
5. a kind of rare-earth permanent magnet according to claim 2, it is characterised in that:The antioxidant for Zr84Al16 and A kind of substance (1%~3%) in La, Ce, Pr, Nd.
CN201711387056.7A 2017-12-20 2017-12-20 A kind of rare-earth permanent magnet and preparation method thereof Pending CN108133798A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109616308A (en) * 2018-11-07 2019-04-12 湖北第二师范学院 A kind of ball shaped nano yttrium oxide DNA extracts Magnaglo and its production method
CN113782331A (en) * 2021-09-18 2021-12-10 泮敏翔 Preparation method of high-performance double-hard-magnetic-phase nano composite magnet

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105869816A (en) * 2016-04-08 2016-08-17 龙岩紫荆创新研究院 Mischmetal-mixed neodymium iron boron hot-pressed and hot-deformed magnet and manufacturing method thereof
CN106128674A (en) * 2016-07-08 2016-11-16 钢铁研究总院 A kind of double Hard Magnetic principal phase mischmetal permanent magnet and preparation method thereof
CN106298133A (en) * 2015-06-12 2017-01-04 中国科学院物理研究所 Permanent magnet material based on the primary norium of common association and its preparation method and application
CN107123538A (en) * 2017-05-15 2017-09-01 江苏品和天磁科技有限公司 A kind of production method containing lanthanum, the low price rapidly quenched magnetic powder of cerium

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106298133A (en) * 2015-06-12 2017-01-04 中国科学院物理研究所 Permanent magnet material based on the primary norium of common association and its preparation method and application
CN105869816A (en) * 2016-04-08 2016-08-17 龙岩紫荆创新研究院 Mischmetal-mixed neodymium iron boron hot-pressed and hot-deformed magnet and manufacturing method thereof
CN106128674A (en) * 2016-07-08 2016-11-16 钢铁研究总院 A kind of double Hard Magnetic principal phase mischmetal permanent magnet and preparation method thereof
CN107123538A (en) * 2017-05-15 2017-09-01 江苏品和天磁科技有限公司 A kind of production method containing lanthanum, the low price rapidly quenched magnetic powder of cerium

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109616308A (en) * 2018-11-07 2019-04-12 湖北第二师范学院 A kind of ball shaped nano yttrium oxide DNA extracts Magnaglo and its production method
CN109616308B (en) * 2018-11-07 2020-09-04 湖北第二师范学院 Magnetic powder extracted from spherical nanometer iridium oxide DNA and production method thereof
CN113782331A (en) * 2021-09-18 2021-12-10 泮敏翔 Preparation method of high-performance double-hard-magnetic-phase nano composite magnet
CN113782331B (en) * 2021-09-18 2023-10-20 中国计量大学 Preparation method of high-performance double-hard-magnetic-phase nanocomposite magnet

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Application publication date: 20180608