EP1032940B1 - Procede pour produire une poudre d'alliage magnetique - Google Patents

Procede pour produire une poudre d'alliage magnetique Download PDF

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Publication number
EP1032940B1
EP1032940B1 EP98956933A EP98956933A EP1032940B1 EP 1032940 B1 EP1032940 B1 EP 1032940B1 EP 98956933 A EP98956933 A EP 98956933A EP 98956933 A EP98956933 A EP 98956933A EP 1032940 B1 EP1032940 B1 EP 1032940B1
Authority
EP
European Patent Office
Prior art keywords
powder
alloy
mpa
hydrogen
range
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP98956933A
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German (de)
English (en)
Other versions
EP1032940A1 (fr
Inventor
Oliver Gutfleisch
Michael Kubis
Axel Handstein
Bernhard Gebel
Karl-Hartmut MÜLLER
Ivor Rex Harris
Ludwig Schultz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institut fuer Festkoerper und Werkstofforschung Dresden eV
Original Assignee
Institut fuer Festkoerper und Werkstofforschung Dresden eV
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Filing date
Publication date
Priority claimed from DE19751367A external-priority patent/DE19751367C2/de
Priority claimed from DE1997151366 external-priority patent/DE19751366C2/de
Application filed by Institut fuer Festkoerper und Werkstofforschung Dresden eV filed Critical Institut fuer Festkoerper und Werkstofforschung Dresden eV
Publication of EP1032940A1 publication Critical patent/EP1032940A1/fr
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Publication of EP1032940B1 publication Critical patent/EP1032940B1/fr
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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
    • H01F1/0553—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 obtained by reduction or by hydrogen decrepitation or embrittlement
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/023—Hydrogen absorption
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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

Definitions

  • the invention relates to the field of metallurgical Process engineering and relates to a method of manufacture a magnetic alloy powder for hard magnetic Applications.
  • the powder consists of a samarium-cobalt-based alloy.
  • the powder can be highly coercive Permanent magnets by hot compaction or Plastic binding can be made. With the powder you can such permanent magnets, however, also powder metallurgy by sintering.
  • Sm-Co-based permanent magnets have hitherto been produced primarily by powder metallurgy by sintering (K. Strnat and RMW Strnat, J. Magn. Magn. Mater. 100 (1991) 38).
  • To produce the Sm-Co powder required for this it is already known to first melt a corresponding alloy, to comminute it after solidification and to heat-treat it in a passivation gas below the phase transformation temperature of the alloy (US Pat. No. 5,122,203).
  • Such a production method has the disadvantage that an energy-consuming and time-consuming multi-stage heat treatment is necessary in order to set high coercive field strengths.
  • Such a production method has the disadvantage that additives such as Cu and Zr are necessary for magnets of the Sm 2 Co 17 type in order to set a microstructure which enables a high coercive field strength through the pinning mechanism.
  • additives such as Cu and Zr are necessary for magnets of the Sm 2 Co 17 type in order to set a microstructure which enables a high coercive field strength through the pinning mechanism.
  • these additives reduce the saturation magnetization.
  • the expansion or Stresses caused by the lattice strain lead to inter- and intergranular cracking and eventually to one regular bursting or atomization (Decrepit) the hydrogenated material.
  • This The pulverization process can also be affected of vibrations (DE 28 16 538) or by using a Vibratory mill (CH 560 955) are supported.
  • the hydrogen is then often removed / desorbed during the further processing of the powder produced into the end product in the course of the subsequent process steps, for example during sintering, in which the reaction A x B y H z ⁇ A x B y + z / 2 H 2 expires.
  • This chemical reaction can be represented schematically (using the model substance A x B y mentioned above) as follows: A x B y + z / 2 H 2 ⁇ A x H z + yB
  • the hydrogenated alloy elements are then dehydrated again in a second process stage by means of heat treatment under vacuum conditions, with simultaneous recombination of the alloy composition decomposed in stage 1 in accordance with the following reaction equation: A x H z + yB ⁇ A x B y + z / 2 H 2
  • the HDDR treatment achieves a crystallite size that is in the range of the single-domain particle size, which is approximately 300 nm for Nd 2 Fe 14 B and Sm 2 Fe 17 N 3, for example.
  • This grain refinement which leads to an improvement in the magnetic properties of the magnetic powder, is the main goal of the HDDR treatment and not - as in the HD process - the powder production.
  • the HD process is not identical to the first stage of HDDR treatment, as the first two letters of the abbreviation "HDDR" might suggest.
  • SE-Fe compounds The increasing stabilization of SE-Fe compounds is also known in the case of substitution of Fe by Co (A. Fujita and I.R. Harris, IEEE Trans. Magn. 30 (1994) 860).
  • the invention is based on the object of a method create a technologically manageable and inexpensive manufacture of a hard magnetic, from a Samarium-cobalt-based alloy for existing powder enables high-coercivity permanent magnets.
  • the procedure is based on HDDR treatment, in which a Starting powder in a first stage under Hydrogen hydrogenation with disproportionation of Alloy and in a subsequent second process stage under vacuum conditions with hydrogen desorption Recombination of the alloy is subjected.
  • a Starting powder in a first stage under Hydrogen hydrogenation with disproportionation of Alloy and in a subsequent second process stage under vacuum conditions with hydrogen desorption Recombination of the alloy is subjected.
  • According to the invention becomes a samarium and cobalt containing Starting powder in the first process stage either at a high temperature in the range of 500 ° C to 900 ° C and with a high hydrogen pressure of> 0.5 MPa or else using an intensive fine grinding at a low temperature in the range of 50 ° C to 500 ° C and with treated with a hydrogen pressure of> 0.15 MPa.
  • the intensive fine grinding for a period of 1 h to 100 h performed.
  • a intensive fine grinding according to the invention a powder of an Sm-Co-based alloy or a powder mixture consisting from the individual elements of an Sm-Co-based alloy and / or consisting of one or more, for the production a Sm-Co-based alloy suitable master alloys, be used.
  • the starting powder should be used in the case of a intensive fine grinding preferably with one Hydrogen pressure in the range of 0.5 MPa to 2.5 MPa be finely ground.
  • the hydrogen desorption treatment is expedient on the magnetic powder obtained by means of a heat treatment performed in the range of 500 ° C to 1000 ° C.
  • those starting powders are preferably used which form magnetic alloy powders with the alloy composition Sm x Co 100-x with 10 ⁇ x ⁇ 30 or the alloy composition Sm x Co 100-xabc Fe a Cu b Zr c with 10 ⁇ x ⁇ 30, a ⁇ 45, b ⁇ 15 and c ⁇ 15.
  • a melted Sm 2 (Co, Fe, Cu, Zr) 17 starting alloy as is usually used for the production of Sm-Co sintered magnets and whose coercive field strengths are determined by the pinning mechanism, is crushed down to particle sizes ⁇ 160 ⁇ m and then heated in a hydrogen atmosphere of 2 MPa to a temperature of 600 ° C and held at this temperature for half an hour.
  • the powder is hydrogenated by the hydrogen, whereby the alloy is disproportionated.
  • the powder is then heated up to 750 ° C with constant pumping and held again at this temperature for half an hour.
  • the powder produced in this way has a high coercive field strength H c of approximately 5 kA / cm and can be processed into powerful permanent magnets.
  • An SmCo 5 starting alloy is comminuted to particle sizes of ⁇ 500 ⁇ m and then heated in a hydrogen atmosphere of 2 MPa to a temperature of 600 ° C. and held at this temperature for half an hour. The powder is then heated up to 750 ° C with constant pumping and held again at this temperature for half an hour.
  • the powder produced in this way has a high coercive field strength H c of approximately 10 kA / cm and can be used for the production of powerful permanent magnets.
  • a melted Sm 2 (Co, Fe, Cu, Zr) 17 starting alloy as is usually used for the production of Sm-Co sintered magnets and whose coercive field strengths are determined by the pinning mechanism, is reduced to particle sizes smaller than 160 ⁇ m and then intensively ground with the help of a vibration mill in a hydrogen atmosphere of 1 MPa at a grinding bowl temperature of 350 ° C. for a period of 20 h. In addition to fine grinding, the alloy is disproportionated due to the presence of hydrogen. The powder is then heated to 750.degree. C. to carry out hydrogen desorption while continuously pumping out hydrogen and held at this temperature for half an hour.
  • the powder produced in this way has a high coercive field strength H c of approximately 10 kA / cm and can be processed into powerful permanent magnets.
  • An SmCo 5 starting alloy is ground down to particle sizes smaller than 500 ⁇ m and then ground with the aid of a vibration mill in a hydrogen atmosphere of 1 MPa at a temperature of the grinding bowl of 350 ° C. for a period of 20 h. In addition to fine grinding, the alloy is disproportionated due to the presence of hydrogen. The powder is then heated to 900 ° C. with the continuous pumping out of hydrogen and kept at this temperature for half an hour in order to carry out a hydrogen desorption.
  • the powder produced in this way has a high coercive field strength H c of approximately 30 kA / cm and can be used for the production of powerful permanent magnets.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Claims (8)

  1. Procédé de fabrication d'une poudre d'alliage magnétique pour des applications magnétiques dures, consistant à soumettre une poudre de départ à un traitement HDDR, lors duquel l'on effectue, dans une première étape de procédé, dans une atmosphère d'hydrogène, une hydrogénation avec dismutation de l'alliage et, dans une deuxième étape de procédé consécutive, dans des conditions de mise sous vide, une désorption de l'hydrogène avec recombinaison de l'alliage, caractérisé en ce que l'on traite une poudre de départ contenant du samarium et du cobalt dans la première étape de procédé, soit à une température élevée dans le domaine de 500°C à 900°C et à une pression élevée d'hydrogène > 0,5 MPa, soit, par contre, par utilisation d'une mouture fine intensive à une température basse dans le domaine de 50°C à 500°C et à une pression d'hydrogène > 0,15 MPa.
  2. Procédé selon la revendication 1, caractérisé en ce que, dans le cas de l'utilisation de la température élevée dans le domaine de 500°C à 900°C, l'on fait usage d'une pression d'hydrogène dans le domaine de 1,0 MPa à 5,0 MPa.
  3. Procédé selon la revendication 1, caractérisé en ce que la mouture fine intensive est effectuée pendant une durée de 1 à 100 heures.
  4. Procédé selon la revendication 1, caractérisé en ce que, dans le cas de l'utilisation d'une mouture fine intensive, l'on utilise, en tant que poudre de départ, une poudre d'un alliage à base Sm-Co ou un mélange de poudres, se composant des éléments individuels d'un alliage à base Sm-Co et/ou se composant d'un ou de plusieurs alliages préalables, appropriés à la fabrication d'un alliage à base Sm-Co.
  5. Procédé selon la revendication 1, caractérisé en ce que, dans le cas de l'utilisation d'une mouture fine intensive, la poudre de départ est moulue d'une manière fine à une pression d'hydrogène se situant dans le domaine de 0,5 MPa à 2,5 MPa.
  6. Procédé selon la revendication 1, caractérisé en ce que le traitement de désorption de l'hydrogène est effectué à l'aide d'un traitement thermique dans le domaine de 500°C à 1000°C.
  7. Procédé selon la revendication 1, caractérisé en ce que l'on fabrique une poudre d'alliage magnétique dans la composition d'alliage SmxCo100-x, avec 10 < x < 30.
  8. Procédé selon la revendication 1, caractérisé en ce que l'on fabrique une poudre d'alliage magnétique dans la composition d'alliage SmxCo100-x- a-b-cFeaCubZrc, avec 10 < x < 30, a < 45, b < 15 et c < 15.
EP98956933A 1997-11-20 1998-11-19 Procede pour produire une poudre d'alliage magnetique Expired - Lifetime EP1032940B1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE19751367 1997-11-20
DE19751367A DE19751367C2 (de) 1997-11-20 1997-11-20 Verfahren zur Herstellung eines hartmagnetischen, aus einer Samarium-Kobalt-Basis-Legierung bestehenden Pulvers
DE1997151366 DE19751366C2 (de) 1997-11-20 1997-11-20 Verfahren zur Herstellung eines hartmagnetischen Samarium-Kobalt-Basis-Materials
DE19751366 1997-11-20
PCT/EP1998/007418 WO1999027544A1 (fr) 1997-11-20 1998-11-19 Procede pour produire une poudre d'alliage magnetique

Publications (2)

Publication Number Publication Date
EP1032940A1 EP1032940A1 (fr) 2000-09-06
EP1032940B1 true EP1032940B1 (fr) 2001-09-12

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EP98956933A Expired - Lifetime EP1032940B1 (fr) 1997-11-20 1998-11-19 Procede pour produire une poudre d'alliage magnetique

Country Status (5)

Country Link
US (1) US6352597B1 (fr)
EP (1) EP1032940B1 (fr)
JP (1) JP2001524604A (fr)
DE (1) DE59801474D1 (fr)
WO (1) WO1999027544A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012200850A1 (de) * 2012-01-20 2013-07-25 Robert Bosch Gmbh Verfahren zur Herstellung eines magnetischen Materials und Permanentmagnet

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011077969A1 (fr) * 2009-12-24 2011-06-30 コニカミノルタホールディングス株式会社 Conteneur de réaction et système de pile à combustible comprenant ce conteneur
CN103050267B (zh) * 2012-12-31 2016-01-20 厦门钨业股份有限公司 一种基于细粉热处理的烧结Nd-Fe-B系磁铁制作方法
CN103050268B (zh) * 2012-12-31 2016-01-20 厦门钨业股份有限公司 基于细粉蒸着热处理的烧结Nd-Fe-B系磁铁制作方法
CZ305703B6 (cs) * 2014-11-07 2016-02-10 Vysoká škola chemicko- technologická v Praze Výroba nanostrukturovaných prášků slitin kobaltu dvoustupňovým mechanickým legováním
CN111180157B (zh) * 2019-12-24 2021-04-06 中国计量大学 一种2：17型SmCoCuFeZrB烧结永磁体及其制备方法
CN115938718B (zh) * 2023-03-09 2023-05-30 天通控股股份有限公司 一种直插式一体成型共烧电感及其制备方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1554384A (en) * 1977-04-15 1979-10-17 Magnetic Polymers Ltd Rare earth metal alloy magnets
US5143560A (en) * 1990-04-20 1992-09-01 Hitachi Metals, Inc., Ltd. Method for forming Fe-B-R-T alloy powder by hydrogen decrepitation of die-upset billets
US5474623A (en) * 1993-05-28 1995-12-12 Rhone-Poulenc Inc. Magnetically anisotropic spherical powder and method of making same
US5851312A (en) * 1996-02-26 1998-12-22 Aichi Steel Works, Ltd. Production method, production apparatus and heat treatment apparatus for anisotropic magnet powder
JP2881409B2 (ja) * 1996-10-28 1999-04-12 愛知製鋼株式会社 異方性磁石粉末の製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012200850A1 (de) * 2012-01-20 2013-07-25 Robert Bosch Gmbh Verfahren zur Herstellung eines magnetischen Materials und Permanentmagnet

Also Published As

Publication number Publication date
EP1032940A1 (fr) 2000-09-06
JP2001524604A (ja) 2001-12-04
WO1999027544A1 (fr) 1999-06-03
US6352597B1 (en) 2002-03-05
DE59801474D1 (de) 2001-10-18

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