EP2436016B1 - Matériau magnétique permanent nd-fe-b et son procédé de préparation - Google Patents

Matériau magnétique permanent nd-fe-b et son procédé de préparation Download PDF

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Publication number
EP2436016B1
EP2436016B1 EP10780039.3A EP10780039A EP2436016B1 EP 2436016 B1 EP2436016 B1 EP 2436016B1 EP 10780039 A EP10780039 A EP 10780039A EP 2436016 B1 EP2436016 B1 EP 2436016B1
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Prior art keywords
alloy
range
permanent magnetic
cobalt ferrite
magnetic material
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German (de)
English (en)
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EP2436016A4 (fr
EP2436016A1 (fr
Inventor
Qing Gong
Zhiqiang Zhang
Surong Zhang
Xin Du
Xiaofeng Cheng
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BYD Co Ltd
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BYD Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/087—Compacting only using high energy impulses, e.g. magnetic field impulses
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • H01F1/10—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 non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
    • H01F1/11—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 non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles

Definitions

  • the present invention relates to an Nd-Fe-B permanent magnetic material and a preparation method thereof.
  • Nd-Fe-B permanent magnetic materials are widely used in vehicles, computers, electronics, mechanical and medical devices, etc.
  • Nd-Fe-B materials have been the ideal materials to produce magnetic devices with high efficiency, small volume and light mass.
  • requirements for performance, operating temperature and corrosion resistance of permanent magnetic materials become higher and higher.
  • WO 2009/057742 A1 discloses a permanent magnet, comprising SmFeN type of magnetic material and Co ferrite, obtained by mixing those materials, orientating in a magnetic field, sintering and heat treating.
  • JP 2002 164205 A discloses a bonded composite magnet including R-T-B-type and magnetoplumbite ferrite powders.
  • JP 2005 159054 A discloses a sintered magnet including R-T-B-type and Ba/Sr ferrite powders.
  • the present invention is directed to provide an Nd-Fe-B permanent magnetic material, according to claim 1, with good high temperature and corrosion resistance properties, and further to provide a preparation method of the Nd-Fe-B permanent magnetic material, according to claim 5.
  • a permanent magnetic material with good high temperature and corrosion resistance properties comprises an Nd-Fe-B alloy and an additive comprising a cobalt ferrite.
  • a method of preparing the permanent magnetic material comprises the steps of mixing an Nd-Fe-B alloy and an additive including at least a cobalt ferrite to obtain a mixture; magnetically orienting and pressing the mixture in a magnetic filed; and sintering and tempering the mixture under protection of vacuum or an inert gas.
  • the cobalt ferrite is 0.5 wt % to 10 wt % of the Nd-Fe-B alloy.
  • An average particle diameter of the cobalt ferrite is in a range of 10 nanometers to 150 nanometers.
  • the cobalt ferrite is represented by a general formula of Co n Fe 3-n O 4 , and n is in a range of 0.1 ⁇ n ⁇ 2.0.
  • the Nd-Fe-B alloy is represented by a general formula of Nd a Re b Fe (100-a-b-c-d) B c M d , where: Re is at least one element selected from a group consisting of Pr, Dy, Tb, Ho, Gd, La, Ce and Y; M is at least one element selected from a group consisting of Co, Al, Cu, Zr, Ga, Nb and Mo; and a, b, c, and d are atomic weight ratios, in which a is in a range of 1 ⁇ a ⁇ 10, b is in a range of 5 ⁇ b ⁇ 12, c is in a range of 5 ⁇ c ⁇ 8, and d is in a range of 0 ⁇ d ⁇ 15.
  • a permanent magnetic material which comprises an Nd-Fe-B (neodymium-iron-boron) alloy and an additive including at least a cobalt ferrite.
  • the inventors of the present invention have found: by adding particles of a cobalt ferrite and distributing them uniformly along the grain boundary of the Nd-Fe-B alloy, the over-growth of the grain and magnetic domain size of the Nd-Fe-B alloy may be inhibited (i.e. pinning effect), thus improving the operating temperature effectively, and the cobalt element itself and neodymium can produce stable intergranular additional structure, thus improving the corrosion resistance property.
  • the content of the heavy metal cobalt may be reduced because of adding a nano-cobalt ferrite, thus lowering the cost.
  • An appropriate amount of oxygen in the cobalt ferrite may improve the high temperature resistance properties of the permanent magnetic material. Meanwhile, due to the presence of the cobalt ferrite, the corrosion resistance property of the permanent magnetic material may be improved greatly.
  • the cobalt ferrite is 0.5 wt % to 10 wt % of the Nd-Fe-B alloy.
  • the average particle diameter of the cobalt ferrite ranges from 20 nanometers to 60 nanometers.
  • the cobalt ferrite is represented by a general formula of Co n Fe 3-n O 4 , in which n is in a range of 0.1 ⁇ n ⁇ 2.0.
  • the particles of the cobalt ferrite are distributed uniformly along the grain boundary of the main phase of the Nd-Fe-B alloy, thus forming the pinning effect.
  • the content of cobalt may not exceed 20 wt % of the total weight of the Nd-Fe-B permanent magnetic material, otherwise the coercive force may be seriously reduced.
  • the Nd-Fe-B alloy is represented by a general formula of Nd a Re b Fe (100-a-b-c-d) B c M d , where Re is at least one element selected from the group consisting of Pr, Dy, Tb, Ho, Gd, La, Ce and Y; M is at least one element selected from the group consisting of Co, Al, Cu, Zr, Ga, Nb and Mo; and a, b, c, and d are atomic weight ratios, in which a is in a range of 1 ⁇ a ⁇ 10, b is in a range of 5 ⁇ b ⁇ 12, c is in a range of 5 ⁇ c ⁇ 8, and d is in a range of 0 ⁇ d ⁇ 15.
  • an embodiment of the present invention provides a method of preparing a permanent magnetic material, comprising steps of: mixing an Nd-Fe-B alloy and an additive including at least a cobalt ferrite to obtain a mixture; magnetically orienting and pressing the mixture in a magnetic filed; and sintering and tempering the mixture under protection of vacuum or an inert gas.
  • the sintering and tempering are performed under the protection of vacuum, alternatively under the protection of an inert gas.
  • the method of preparing a permanent magnetic material employing the sintering process may include without limitation one or more of the following steps: formulating, melting, crushing, milling, magnetically orienting and pressing in a magnetic field, sintering in vacuum, mechanical processing and electroplating.
  • the sintering and tempering process is known to those skilled in the art.
  • the sintering and tempering process are carried out under protection of vacuum or an inert gas.
  • the inert gas is any gas that does not participate in the reaction, for example, one selected from the group consisting of: nitrogen, helium, argon, neon, krypton and xenon.
  • the parison is sintered at a temperature of 1030 °C to 1120 °C for a period of 2 hours to 8 hours, then tempered in a first tempering step at a temperature of 800 °C to 920 °C for a period of 1 hour to 3 hours, and finally tempered in a second tempering step at a temperature of 500 °C to 650 °C for a period of 2 hours to 4 hours.
  • the second tempering step may further improve the coercive force. Because the cobalt ferrite has a melting point above 1120°C, when sintered at the above temperature, the cobalt ferrite may not be decomposed and melted.
  • the Nd-Fe-B permanent magnetic material obtained was labeled as CT1.
  • the process of this example was substantially similar to that of EXAMPLE 1, except that Co 2 Fe 1 O 4 was used as the additive in stead of CoFe 2 O 4 , and the amount of Co 2 Fe 1 O 4 was 5 wt % of the Nd-Fe-B alloy powder.
  • the Nd-Fe-B permanent magnetic material obtained was labeled as T2.
  • the process of this example was substantially similar to that of EXAMPLE 1, except that the average particle diameter of the CoFe 2 O 4 was 100 nanometers.
  • the Nd-Fe-B permanent magnetic material obtained was labeled as T3.
  • the process of this example was substantially similar to that of EXAMPLE 1, except that the amount of the CoFe 2 O 4 was 10 wt % of the Nd-Fe-B alloy.
  • the Nd-Fe-B permanent magnetic material obtained was labeled as T4.
  • the process of this example was substantially similar to that of EXAMPLE 1, except that Co was used as the additive instead of CoFe 2 O 4 , and an average particle diameter of the Co was 50 nanometers.
  • the Nd-Fe-B permanent magnetic material obtained was labeled as CT2.
  • Cylindrical samples with a diameter of 10 millimeters and a length of 7 millimeters were prepared from the permanent magnetic materials T1-T4, CT1 and CT2, and then tested on a HAS-70CP type Highly Accelerated Stress Tester commercially available from Terchy Environmental Technology Ltd, with a temperature of 130 °C, a humidity of 95%, a steam pressure of 2.7 bar, and a period of 10 days.
  • the mass loss (W loss ) of the permanent magnetic materials T1-T4, CT1 and CT2 were recorded in Table 1.
  • Cylindrical samples with a diameter of 10 millimeters and a length of 7 millimeters were prepared from the permanent magnetic materials T1-T4, CT1 and CT2 , and then heated using a curve measurement system NIM200C (National Institute of Metrology, P.R.C.) from a temperature of 60°C with a 2°C increment each time. When the line started to bend at a certain temperature, the permanent magnetic materials reached the maximum operating temperature.
  • NIM200C National Institute of Metrology, P.R.C.
  • T1 has a W loss of 2.1 mg/cm 2 and a inflection temperature 190°C and CT2 has a W loss of 2.7 mg/cm 2 and an inflection temperature 170°C, so that the permanent magnetic material according to the embodiments of the present disclosure exhibited a better corrosion resistance and higher temperature resistance properties.

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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)
  • Mechanical Engineering (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Claims (12)

  1. Matériau magnétique permanent, comprenant :
    un alliage de Nd-Fe-B ; et un additif comprenant au moins une ferrite de cobalt, caractérisé en ce que la ferrite de cobalt représente de 0,5 à 10 % en poids de l'alliage de Nd-Fe-B.
  2. Matériau magnétique permanent selon la revendication 1, dans lequel le diamètre de particule moyen de la ferrite de cobalt est compris dans la plage allant de 10 nanomètres à 150 nanomètres.
  3. Matériau magnétique permanent selon la revendication 1, dans lequel la ferrite de cobalt est représentée par la formule générale ConFe3-nO4, où n est compris dans la plage de 0,1 ≤ n ≤ 2,0.
  4. Matériau magnétique permanent selon la revendication 1, dans lequel l'alliage de Nd-Fe-B est représenté par la formule générale NdaRebFe(100-a-b-c-d)BcMd où :
    Re est au moins un élément choisi dans le groupe constitué par Pr, Dy, Tb, Ho, Gd, La, Ce et Y ;
    M est au moins un élément choisi dans le groupe constitué par Co, Al, Cu, Zr, Ga, Nb et Mo ; et
    a, b, c et d sont des rapports en poids atomique, où a est compris dans la plage de 1 ≤ a ≤ 10, b est compris dans la plage de 5 ≤ b ≤ 12, c est compris dans la plage de 5 ≤ c ≤ 8 et d est compris dans la plage de 0 ≤ d ≤ 15.
  5. Procédé de préparation d'un matériau magnétique permanent, comprenant les étapes consistant à :
    mélanger un alliage de Nd-Fe-B et un additif incluant au moins une ferrite de cobalt pour obtenir un mélange ;
    orienter magnétiquement et compresser le mélange dans un champ magnétique ; et
    fritter et réaliser une trempe du mélange sous la protection d'un vide ou d'un gaz inerte ;
    caractérisé en ce que la ferrite de cobalt représente de 0,5 à 10 % en poids de l'alliage de Nd-Fe-B.
  6. Procédé selon la revendication 5, dans lequel la ferrite de cobalt est représentée par la formule générale ConFe3-nO4, où n est compris dans la plage de 0,1 ≤ n ≤ 2,0.
  7. Procédé selon la revendication 5, dans lequel l'étape de mélange comprend le mélange de l'alliage de Nd-Fe-B et de l'additif en présence d'un antioxydant, dans lequel en fonction du poids de l'alliage de Nd-Fe-B, la quantité de l'antioxydant est d'environ 0,1 % en poids à environ 5 % en poids, et la quantité du lubrifiant est de 0 % en poids à 5 % en poids.
  8. Procédé selon la revendication 5, dans lequel l'étape de mélange comprend le mélange de l'alliage de Nd-Fe-B et de l'additif en présence d'un antioxydant et d'un lubrifiant, dans lequel en fonction du poids de l'alliage de Nd-Fe-B, la quantité de l'antioxydant est d'environ 0,1 % en poids à environ 5 % en poids, et la quantité du lubrifiant est de 0 % en poids à 5 % en poids.
  9. Procédé selon la revendication 5, dans lequel l'alliage de Nd-Fe-B est représenté par la formule générale NdaRebFe(100-a-b-c-d)BcMd où :
    Re est au moins un élément choisi dans le groupe constitué par Pr, Dy, Tb, Ho, Gd, La, Ce et Y ;
    M est au moins un élément choisi dans le groupe constitué par Co, Al, Cu, Zr, Ga, Nb et Mo ; et
    a, b, c et d sont des rapports en poids atomique, où a est compris dans la plage de 1 ≤ a ≤ 10, b est compris dans la plage de 5 ≤ b ≤ 12, c est compris dans la plage de 5 ≤ c ≤ 8 et d est compris dans la plage de 0 ≤ d ≤ 15.
  10. Procédé selon la revendication 5, dans lequel le diamètre de particule moyen de la ferrite de cobalt est compris dans la plage allant de 10 nanomètres à 150 nanomètres.
  11. Procédé selon la revendication 5, dans lequel le diamètre de particule moyen de l'alliage de Nd-Fe-B est compris dans la plage allant de 2 µm à 5 µm.
  12. Procédé selon la revendication 5, dans lequel l'orientation magnétique et la compression sont réalisées sous une intensité de champ magnétique de 1,2 T à 3,0 T et une pression de 10 MPa à 200 MPa pendant une période de 10 secondes à 60 secondes ; le frittage est réalisé à une température de 1030 °C à 1120 °C pendant une période de 2 heures à 8 heures ; et dans lequel les étapes de trempe comprennent une première étape de trempe et une seconde étape de trempe, la première étape de trempe étant réalisée à une température de 800 °C à 920 °C pendant une période de 1 heure à 3 heures, et la seconde étape de trempe étant réalisée à une température de 500 °C à 650 °C pendant une période de 2 heures à 4 heures.
EP10780039.3A 2009-05-27 2010-05-17 Matériau magnétique permanent nd-fe-b et son procédé de préparation Active EP2436016B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2009101076492A CN101901657B (zh) 2009-05-27 2009-05-27 一种烧结钕铁硼永磁材料及其制备方法
PCT/CN2010/072854 WO2010135958A1 (fr) 2009-05-27 2010-05-17 Matériau magnétique permanent nd-fe-b et son procédé de préparation

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EP2436016A1 EP2436016A1 (fr) 2012-04-04
EP2436016A4 EP2436016A4 (fr) 2012-10-31
EP2436016B1 true EP2436016B1 (fr) 2017-03-29

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CN102228760A (zh) * 2011-06-29 2011-11-02 无锡光旭新材料科技有限公司 一种永磁体过滤棒及其永磁材料体的制备方法
CN102510176B (zh) * 2011-11-04 2014-11-26 无锡天宝电机有限公司 一种电机用耐热钕铁硼永磁的制备方法
CN102361359B (zh) * 2011-11-04 2015-02-11 无锡天宝电机有限公司 一种耐腐蚀的电机用钕铁硼永磁
CN102969111B (zh) * 2012-11-30 2015-09-30 钢铁研究总院 低成本高电阻率铈磁体及其制备方法
CN102976738A (zh) * 2012-12-20 2013-03-20 南通万宝磁石制造有限公司 高抗压强度永磁铁氧体磁体的制造工艺
CN105499557A (zh) * 2016-01-28 2016-04-20 河南中硬合金有限公司 一种硬质合金大制品顶锤多元组分成型剂及制备方法
CN105957674B (zh) * 2016-05-13 2018-09-14 桂林电子科技大学 一种高矫顽力的Nd-Ce-Pr-Fe-B合金薄带永磁材料及其制备方法
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RU2642508C1 (ru) * 2016-11-21 2018-01-25 федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский ядерный университет "МИФИ" (НИЯУ МИФИ) СПОСОБ ПОЛУЧЕНИЯ ВЫСОКОКОЭРЦИТИВНЫХ МАГНИТОВ ИЗ СПЛАВОВ НА ОСНОВЕ Nd-Fe-B
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CN107931598A (zh) * 2017-11-16 2018-04-20 浙江中杭新材料科技有限公司 混合励磁同步电机磁钢的制备方法
RU2690867C1 (ru) * 2018-12-13 2019-06-06 Акционерное общество "Научно-производственное объединение "Магнетон" Шихта для получения термостабильных магнитных сплавов с редкоземельными металлами на основе системы Nd-Fe-B
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US6721144B2 (en) * 2001-01-04 2004-04-13 International Business Machines Corporation Spin valves with co-ferrite pinning layer
JP2005159054A (ja) * 2003-11-26 2005-06-16 Tdk Corp Ｒ−ｔ−ｂ系永久磁石の製造方法
US8465453B2 (en) * 2003-12-03 2013-06-18 Mayo Foundation For Medical Education And Research Kits, apparatus and methods for magnetically coating medical devices with living cells
CN100356487C (zh) * 2005-06-06 2007-12-19 浙江大学 一种烧结钕铁硼磁体的制备方法
WO2009057742A1 (fr) * 2007-11-02 2009-05-07 Asahi Kasei Kabushiki Kaisha Matériau magnétique composite pour aimant et procédé de fabrication de ce matériau

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EP2436016A4 (fr) 2012-10-31
WO2010135958A1 (fr) 2010-12-02
EP2436016A1 (fr) 2012-04-04
US20120058003A1 (en) 2012-03-08
CN101901657B (zh) 2012-06-20

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