WO2022191349A1 - Procédé de fabrication d'un aimant permanent déformé à chaud - Google Patents

Procédé de fabrication d'un aimant permanent déformé à chaud Download PDF

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Publication number
WO2022191349A1
WO2022191349A1 PCT/KR2021/003122 KR2021003122W WO2022191349A1 WO 2022191349 A1 WO2022191349 A1 WO 2022191349A1 KR 2021003122 W KR2021003122 W KR 2021003122W WO 2022191349 A1 WO2022191349 A1 WO 2022191349A1
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WO
WIPO (PCT)
Prior art keywords
hot
powder
permanent magnet
heat treatment
post
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PCT/KR2021/003122
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English (en)
Korean (ko)
Inventor
안종빈
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주식회사 디아이씨
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Priority to PCT/KR2021/003122 priority Critical patent/WO2022191349A1/fr
Publication of WO2022191349A1 publication Critical patent/WO2022191349A1/fr

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    • 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
    • B22F3/12—Both compacting and sintering
    • 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
    • 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
    • H01F1/06—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 in the form of particles, e.g. powder
    • H01F1/08—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 in the form of particles, e.g. powder pressed, sintered, or bound together
    • 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

Definitions

  • the present invention relates to a method for manufacturing a hot-deformed permanent magnet, by mixing NdFeB magnetic powder and ReF 3 powder to adhere ReF 3 powder to the surface of NdFeB magnetic powder, first hot pressing and second hot deformation ) and 1st and 2nd post-heat treatment to make the crystal grains of the columnar grains uniform, increase the c-axis orientation, and produce a magnet with high coercive force and high maximum energy or residual magnetic flux density.
  • Dy and Tb adhering to the magnet surface are sent to the inside of the sintered body through the grain boundaries of the sintered body, and diffuse from the grain boundary to the inside of each particle of the main phase R 2 Fe 14 B (R is a rare earth element) (grain boundary diffusion) ).
  • R 2 Fe 14 B R is a rare earth element
  • the diffusion rate of Dy or Tb in the grain boundary is much faster than the diffusion rate from the grain boundary to the inside of the columnar grains.
  • the method of manufacturing an anisotropic neodymium-based permanent magnet is usually produced by metal melting, rapid cooling, milling, magnetic powder is formed while applying a magnetic field, followed by sintering at a high temperature (1000 ° C. or higher) and post-heat treatment. manufactured through In this process, as another method of securing the high coercive force of the magnetic powder, there is a method of refining the size of the crystal grains to the size of a single sphere.
  • Patent Document 1 Korean Patent Publication No. 10-2015-0033423 (2015.04.01)
  • Patent Document 2 Japanese Patent Laid-Open No. 62-074048 (April 4, 1987)
  • Patent Document 3 Korean Patent No. 10-1447301 (2014.09.26)
  • the present invention relates to a method of manufacturing a hot deformable permanent magnet, by mixing NdFeB magnetic powder and ReF 3 powder to adhere ReF 3 powder to the surface of NdFeB magnetic powder, first hot pressing and second hot deformation ) and 1st and 2nd post-heat treatment to make the crystal grains of the columnar grains uniform, increase the degree of c-axis orientation, and produce a magnet with high coercive force and high maximum energy or residual magnetic flux density.
  • the method for manufacturing a hot-deformed permanent magnet comprises the steps of preparing NdFeB magnetic powder; mixing the NdFeB magnetic powder and ReF 3 (Re is other rare earth metals except for the rare earth included in NdFeB) powder; hot pressing the mixture in which the ReF3 powder is attached to the surface of the NdFeB magnetic powder; hot deformation of the isotropic permanent magnet formed by the hot pressing; first post-heating the hot-deformed anisotropic permanent magnet; Secondary post-heat treatment of the anisotropic permanent magnet subjected to the first post-heat treatment;
  • the NdFeB magnetic powder is a melt spun powder, and the particle size of the NdFeB magnetic powder is 100 to 300 ⁇ m.
  • the NdFeB magnetic powder is Nd 30.1 Fe bal. It is characterized in that it has a composition ratio of Co 5.0 Ga 0.6 B 0.9 .
  • the ReF 3 powder is DyF 3 and has a particle size of 50 to 150 nm.
  • the Nd 30.1 Fe bal. 1.0 to 2.0 parts by weight of the DyF 3 powder is mixed with 100 parts by weight of Co 5.0 Ga 0.6 B 0.9 magnetic powder.
  • the step of hot pressing in the method for manufacturing a hot deformable permanent magnet according to the present invention is performed at a temperature of 600 to 800 °C for 10 to 30 minutes, a pressure of 50 to 100 MPa, and a density of 95% or more.
  • the hot deformation is performed at a temperature of 700 to 850° C. for 5 to 20 minutes, a pressure of 50 to 200 MPa, and the height of the isotropic permanent magnet is 60 to It is characterized in that it deforms by 80%.
  • the step of hot deformation in the manufacturing method of the hot deformable permanent magnet according to the present invention After that, the first post-heat treatment at 600 to 700 ° C. for 1 to 2 hours to remove residual stress and homogenize the tissue Tea post-heat treatment step; characterized in that it is added.
  • the first post-heat treatment step in the method for manufacturing a hot-deformed permanent magnet according to the present invention Then, the second post-heat treatment at 600 to 800 ° C. for 1 to 2 hours to make magnetic homogenization, magnetic grain homogenization, sintering density maximization, magnetic phase /
  • a secondary heat treatment step for controlling the fraction of the non-magnetic phase characterized in that it is added.
  • the method for manufacturing a hot-deformed permanent magnet According to the method for manufacturing a hot-deformed permanent magnet according to the present invention, there is no need for a high-temperature sintering process through hot pressing and hot-deformation secondary pressurization, and the magnetization direction of crystal grains is aligned in one direction without applying a magnetic field due to hot deformation. Therefore, the magnetic field application process is unnecessary.
  • a magnet with a high coercive force and a high maximum energy or residual magnetic flux density by homogenizing the crystal grains of the columnar grains and increasing the c-axis orientation by performing primary and secondary heat treatment can be manufactured.
  • FIG. 1 is a flowchart of a manufacturing method according to the present invention.
  • Figure 2 is before mixing Nd 30.1 Fe bal. It is a photomicrograph of the powder of Co 5.0 Ga 0.6 B 0.9 composition.
  • Nd 30.1 Fe bal This is a photo of DyF3 powder attached to the surface of the powder having a composition of Co 5.0 Ga 0.6 B 0.9 .
  • 6 is a hot deformation process diagram at 70% deformation at the height of the permanent magnet, deformation rate 0.002 S -1 , deformation temperature 800° C., and deformation pressure 160 Mpa
  • FIG. 9 is a graph showing the thickness of the grain boundary after two-stage post-heat treatment of the anisotropic permanent magnet to which DyF 3 powder is added and the composition of the grain boundary after the second-stage post-heat treatment of the anisotropic permanent magnet to which DyF 3 powder is added.
  • NdFeB-based powder (Nd 30.1 Fe bal. Co 5.0 Ga 0.6 B 0.9 ) was melted, and the melt was injected into a cooling roll rotating at high speed to prepare a ribbon-shaped alloy.
  • the ribbon-shaped ingot produced by the rolling process is milled with a stamp mill and pulverized to a size of about 100 to 300 ⁇ m to prepare neodymium-based magnetic powder.
  • ReF 3 powder (Re is other rare earth metals except for the rare earth contained in NdFeB), and a particle size of 50 to 150 nm is prepared.
  • DyF 3 powder having an average particle diameter of 100 nm-300 nm is mixed with 100 parts by weight of NdFeB-based powder (Nd 30.1 Fe bal. Co 5.0 Ga 0.6 B 0.9 ), and kneaded in a 3D mixer for 1 hour.
  • a mixture having DyF 3 powder adhered to the surface of the NdFeB powder (Nd 30.1 Fe bal. Co 5.0 Ga 0.6 B 0.9 ) is hot-pressed at a temperature of 600 to 800° C. for 10 to 30 minutes, and a pressure of 50 to 100 MPa.
  • the hot pressing holding time is preferably 15 to 25 minutes, more preferably 20 minutes.
  • an isotropic permanent magnet having a density of 95% or more can be manufactured.
  • the isotropic permanent magnet manufactured by the hot pressing is performed at a temperature of 700 to 850° C. for 5 to 20 minutes, a pressure of 50 to 200 MPa, and the height of the anisotropic permanent magnet is deformed by 60 to 80%.
  • the hot deformation holding time is preferably 8 to 12 minutes, more preferably 10 minutes.
  • an anisotropic permanent magnet By the hot deformation, an anisotropic permanent magnet can be manufactured.
  • a primary post-heat treatment is performed to remove residual stress and align the grains of the anisotropic permanent magnet manufactured by the hot deformation.
  • the primary post-heat treatment is performed at 600 to 700° C. for 1 to 2 hours to remove residual stress and homogenize the tissue.
  • a second post-heat treatment is performed to equalize the magnetic structure, equalize the magnetic grain boundary, maximize the sintering density, and control the fraction of the non-magnetic phase.
  • the secondary post-heat treatment is maintained in a high vacuum at 600 to 800° C. for 1 to 2 hours.
  • Nd 30.1 Fe baL 1.6 parts by weight of DyF 3 powder having an average particle diameter of 100 nm-300 nm was mixed with a 200 ⁇ m average particle diameter powder having a composition of Co 5.0 Ga 0.6 B 0.9 and kneaded in a 3D mixer for 1 hour.
  • Figure 2 is Nd 30.1 Fe baL before mixing. It is a photomicrograph of the powder of Co 5.0 Ga 0.6 B 0.9 composition. 3 is a micrograph of DyF 3 powder before mixing. 4 is after mixing, Nd 30.1 Fe bal. This is a photograph of DyF 3 powder attached to the surface of the powder having a composition of Co 5.0 Ga 0.6 B 0.9 .
  • Nd 30.1 Fe bal By kneading, Nd 30.1 Fe bal.
  • An isotropic permanent magnet having a density of 95% or more was prepared by hot pressing a mixture having DyF 3 powder attached to the surface of the powder having a composition of Co 5.0 Ga 0.6 B 0.9 at 750° C. for 20 minutes at 70 Mpa pressure and in a high vacuum atmosphere.
  • FIG. 5 is crystal analysis data of an isotropic permanent magnet obtained by hot-pressing a mixture containing 1.6 parts by weight of DyF 3 at 750° C. and a pressure of 70 MPa for 20 minutes.
  • DyF 3 is added Nd 2 Fe 14 B 1 phase analysis results through X-ray diffraction analysis.
  • Table 1 is a table comparing the density according to the hot pressing temperature. It can be seen that when the hot pressing temperature is 700° C. or higher, the hot pressing density can be controlled to 96% or higher.
  • the isotropic permanent magnet manufactured by the hot pressing was hot deformed at 800° C. for 10 minutes at a pressure of 160 Mpa, in a high vacuum atmosphere at a deformation rate of 0.002 s ⁇ 1 .
  • a permanent magnet was manufactured.
  • FIG. 6 is a hot deformation process diagram at 70% deformation at the height of a permanent magnet, a deformation rate of 0.002 S -1 , a deformation temperature of 800° C., and a deformation pressure of 160 Mpa.
  • a primary post-heat treatment is performed to remove residual stress and align the grains of the anisotropic permanent magnet manufactured by the hot deformation.
  • the hot-deformed anisotropic permanent magnet was maintained in high vacuum at 600°C for 1 hour.
  • FIG. 8 is a pole figure data in the (006) direction after the primary heat treatment of the anisotropic permanent magnet.
  • FIG. 8 it can be seen that crystal anisotropy has occurred in the (006) direction after the first post-heat treatment.
  • the crystalline phase of a hot-deformed permanent magnet having a tetragonal (tetragonal structure) structure according to the primary post-heat treatment is added for the purpose of grain boundary diffusion during hot deformation. (001) direction), the grain alignment is increased, and it is determined that the residual magnetization value is improved.
  • a second post heat treatment is performed to equalize the magnetic structure, equalize the magnetic grain boundary, maximize the sintering density, and control the fraction of the non-magnetic phase.
  • the anisotropic permanent magnet subjected to the first post-heat treatment was maintained at 700° C. for 2 hours in a high vacuum.
  • FIG. 9 is a graph showing the thickness of the grain boundary after two-stage post-heat treatment of the anisotropic permanent magnet to which DyF 3 powder is added and the composition of the grain boundary after two-stage post-heat treatment of the anisotropic permanent magnet to which DyF 3 powder is added.
  • the grain boundary thickness was uniformly manufactured to a thickness of 2 nm, a stable crystal phase was formed, and a pinning force that inhibits the magnetic domain wall movement was generated due to an increase in the Nd-rich phase and a decrease in the Fe-rich phase, resulting in a high residual magnetization value. , the coercive force was improved.
  • Examples 2 and 3 were prepared in amounts of 0.2 parts by weight and 0.4 parts by weight of the added powder DyF 3 decreased by 0.2 parts by weight compared to Example 1, and the coercive force was 3 to 5 as compared to Example 1 as the amount decreased by 0.2 parts by weight. % tends to decrease, and the residual magnetization value tends to decrease by 0.5 to 1.2% as compared with Example Group 1 as the addition amount decreases by 0.2 parts by weight.
  • Table 2 shows the presence or absence of secondary post-heat treatment and post-heat treatment temperature for Comparative Groups 2 to 4.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'un aimant permanent déformé à chaud, comprenant les étapes consistant : à préparer une poudre magnétique NdFeB ; à mélanger la poudre magnétique NdFeB et la poudre ReF3 (Re est un métal des terres rares autre que les métaux des terres rares contenus dans le NdFeB) ; à former par pressage à chaud un mélange dans lequel la poudre ReF3 est fixée à la surface de la poudre magnétique NdFeB ; à déformer à chaud un produit formé par pressage à chaud ; à effectuer un traitement post-thermique primaire sur l'aimant permanent anisotrope déformé à chaud ; et à effectuer un traitement post-thermique secondaire sur l'aimant permanent anisotrope qui a été traité par post-chauffage primaire.
PCT/KR2021/003122 2021-03-12 2021-03-12 Procédé de fabrication d'un aimant permanent déformé à chaud WO2022191349A1 (fr)

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PCT/KR2021/003122 WO2022191349A1 (fr) 2021-03-12 2021-03-12 Procédé de fabrication d'un aimant permanent déformé à chaud

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PCT/KR2021/003122 WO2022191349A1 (fr) 2021-03-12 2021-03-12 Procédé de fabrication d'un aimant permanent déformé à chaud

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150033423A (ko) * 2013-09-24 2015-04-01 엘지전자 주식회사 열간가압성형 공정을 이용한 이방성 열간가압성형 자석의 제조방법 및 이 방법으로 제조된 열간가압성형 자석
US20150132174A1 (en) * 2009-09-04 2015-05-14 Electron Energy Corporation Rare Earth Composite Magnets with Increased Resistivity
JP2015126081A (ja) * 2013-12-26 2015-07-06 トヨタ自動車株式会社 希土類磁石とその製造方法
KR20180067760A (ko) * 2016-12-12 2018-06-21 현대자동차주식회사 희토류 영구자석 제조방법
KR101918975B1 (ko) * 2017-08-09 2018-11-16 한국기계연구원 Nd-Fe-B계 자석 및 그 제조방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150132174A1 (en) * 2009-09-04 2015-05-14 Electron Energy Corporation Rare Earth Composite Magnets with Increased Resistivity
KR20150033423A (ko) * 2013-09-24 2015-04-01 엘지전자 주식회사 열간가압성형 공정을 이용한 이방성 열간가압성형 자석의 제조방법 및 이 방법으로 제조된 열간가압성형 자석
JP2015126081A (ja) * 2013-12-26 2015-07-06 トヨタ自動車株式会社 希土類磁石とその製造方法
KR20180067760A (ko) * 2016-12-12 2018-06-21 현대자동차주식회사 희토류 영구자석 제조방법
KR101918975B1 (ko) * 2017-08-09 2018-11-16 한국기계연구원 Nd-Fe-B계 자석 및 그 제조방법

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