EP1032940A1 - Procede pour produire une poudre d'alliage magnetique - Google Patents

Procede pour produire une poudre d'alliage magnetique

Info

Publication number
EP1032940A1
EP1032940A1 EP98956933A EP98956933A EP1032940A1 EP 1032940 A1 EP1032940 A1 EP 1032940A1 EP 98956933 A EP98956933 A EP 98956933A EP 98956933 A EP98956933 A EP 98956933A EP 1032940 A1 EP1032940 A1 EP 1032940A1
Authority
EP
European Patent Office
Prior art keywords
alloy
powder
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.)
Granted
Application number
EP98956933A
Other languages
German (de)
English (en)
Other versions
EP1032940B1 (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
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE1997151366 external-priority patent/DE19751366C2/de
Priority claimed from DE19751367A external-priority patent/DE19751367C2/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
Application granted granted Critical
Publication of EP1032940B1 publication Critical patent/EP1032940B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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 for producing a magnetic alloy powder for hard magnetic applications.
  • the powder consists of a samanum-cobalt-based alloy.
  • the powder can be used to produce highly coercive permanent magnets by hot compaction or plastic binding. With the powder, however, such permanent magnets can also be produced by powder sintering by sintering.
  • Sm-Co-based permanent magnets have so far mainly been produced by powder metallurgy by sintering
  • CONFIRMATION HEADS Set microstructure that enables a high coercive force through the pinmng mechanism. However, these additives reduce the saturation magnetization.
  • the HD process (hydride decrepitation) has long been known in the field of the manufacture of magnetic powders based on alloys with elements from the rare earth element group (SE) (US Pat. No. 5,580,396, column 8, lines 30 to 41; Rare-earth Iron Permanent Magnets, ed.JMD Coey, Oxford 1996, pages 346 to 349 and pages 370 to 380).
  • SE rare earth element group
  • This process is used for crushing coarse, compact alloy bodies, and is therefore used for powder production.
  • the effect is used here that the hydrogen diffused into the intermediate grain phase or onto the intermediate lattice sites of the SE compound leads to an expansion of the intermediate grain phase or to a lattice extension of the SE compound.
  • HDDR hydrogenation-disproportionation-desorption-
  • This chemical reaction can be represented schematically (using the model substance A x B y mentioned above) as follows:
  • the hydrogenated alloy elements are then dehydrated again in a second process stage by means of a heat treatment under vacuum conditions, with simultaneous recombination of the alloy composition decomposed in stage 1 according to the following reaction equation:
  • HDDR stage 1 heating up to the temperatures of 500 ° C to 1000 ° C necessary for the above-described reaction often results in the hydrogen absorption typical of the HD process, as described above in the equation for the HD process is described, however, this is only an intermediate reaction, which is immediately followed by the desorption of the hydrogen.
  • the HDDR treatment can be carried out completely independently of the HD process, as has been shown, for example, with the “sol-HDDR” process, in which the hydrogen gas only reaches the peactor at the temperature m required for disproportionation (HDDR stage 1) is admitted and so there is no interstitial absorption of the hydrogen and thus no HD process (Gutyak et al., J. Alloys Compd. 215 (1994) 227).
  • the invention has for its object to provide a method which enables a technologically controllable and inexpensive production of a hard magnetic powder consisting of a samarium-cobalt-base alloy for highly coercive permanent magnets.
  • the process is based on an HDDR treatment in which a starting powder is subjected to hydrogenation with disproportionation of the alloy in a first process step under hydrogen and in a subsequent second process step to hydrogen desorption with recombination of the alloy under vacuum conditions.
  • a starting powder containing samarium and cobalt is used in the first process stage either at a high temperature in the range from 500 ° C. to 900 ° C. and with a high hydrogen pressure of> 0.5 MPa or using intensive fine grinding at a low temperature in the range from 50 ° C to 500 ° C and treated with a hydrogen pressure of> 0.15 MPa.
  • a hydrogen pressure in the range of 1.0 MPa to 5.0 MPa is preferably applied.
  • the intensive fine grinding is carried out for a period of 1 h to 100 h.
  • a starting powder can be a powder of an Sm-Co-based alloy or a powder mixture consisting of the individual elements of an S-Co-based alloy and / or consisting of one or more, for use in the case of intensive fine grinding a Sm-Co-based alloy suitable master alloys are used.
  • the starting powder should preferably be finely ground at a hydrogen pressure in the range from 0.5 MPa to 2.5 MPa.
  • the hydrogen desorption treatment is expediently carried out on the magnetic powder obtained by means of a heat treatment in the range from 500 ° C. to 1000 ° C.
  • starting powders which form magnetic alloy powders having the alloy composition Sm x Co ⁇ oo- x with 10 ⁇ x ⁇ 30 or the alloy composition Sm x C ⁇ oo- x - a - b - c Fe a CU b Zr c with 10 ⁇ x ⁇ 30, a ⁇ 45, b ⁇ 15 and c ⁇ 15.
  • the method according to the invention creates a new possibility for the magnetic hardening of Sm-Co base compounds.
  • the method opens up new approaches for optimizing the magnetic properties of Sm-Co magnets, which leads to an improvement in the properties and represents an inexpensive alternative for the production of such magnets.
  • a melted Sm 2 (Co, Fe, Cu, Zr) ⁇ 7 starting alloy as is usually used for the production of S-Co sintered magnets and whose coercive strengths are determined by the pinmng mechanism, is crushed down to particle sizes ⁇ 160 ⁇ 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, with a disproportionation of the alloy taking place.
  • the powder is then heated to 750 ° C. with constant pumping and is held at this temperature again for half an hour.
  • the powder produced in this way has a high coercive force H c of about 5 kA / cm and can be processed into powerful permanent magnets.
  • An SmCos base alloy is crushed to particle sizes ⁇ 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. Then the powder is under constant Pumping heated up to 750 ° C and held again at this temperature for half an hour.
  • the powder produced in this way has a high coercive force H c of about 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 is crushed down to particle sizes smaller than 160 ⁇ m and then, using a vibratory mill in a hydrogen atmosphere of 1 MPa, at a grinding bowl temperature of 350 ° C., intensively ground for a period of 20 hours. In addition to fine grinding, a disproportionation of the alloy takes place simultaneously due to the hydrogen present.
  • the powder is then heated to 750 ° C. while hydrogen is being pumped out, and is held at this temperature for half an hour in order to carry out hydrogen desorption.
  • the powder produced in this way has a high coercive force H c of about 10 kA / cm and can be processed into powerful permanent magnets.
  • An SmCos base alloy is crushed down to particle sizes smaller than 500 ⁇ m and then with the help of a
  • the powder produced in this way has a high coercive force H c of about 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)
  • Hard Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention a pour objet de créer un procédé économique et technologiquement maîtrisable pour produire une poudre magnétique dure constituée d'un alliage à base de samarium et de cobalt et destinée à des aimants permanents extrêmement coercitifs. Ce procédé se fonde sur un traitement HDDR (hydrogénation-disproportionation-désorption-recombinaison). Lors d'une première étape du procédé, une poudre initiale est soumise à une hydrogénation sous hydrogène avec disproportionation de l'alliage. Lors d'une deuxième étape subséquente, la poudre est soumise à une désorption d'hydrogène sous vide avec recombinaison de l'alliage. Selon l'invention, une poudre initiale contenant du samarium et du cobalt est traitée, lors d'une première étape du procédé, soit à une température élevée comprise entre 500 °C et 900 °C et avec une pression d'hydrogène élevée > 0,5 MPa, soit par trituration intensive à une basse température comprise entre 50 °C et 500 °C et avec une pression d'hydrogène > 0,15 MPa. Ce procédé permet donc de produire des poudres d'alliage magnétique à partir d'alliages à base de samarium et de cobalt. Ces poudres s'utilisent pour produire des aimants permanents extrêmement coercitifs, notamment par compactage à chaud ou liaison plastique.
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
DE1997151366 DE19751366C2 (de) 1997-11-20 1997-11-20 Verfahren zur Herstellung eines hartmagnetischen Samarium-Kobalt-Basis-Materials
DE19751367A DE19751367C2 (de) 1997-11-20 1997-11-20 Verfahren zur Herstellung eines hartmagnetischen, aus einer Samarium-Kobalt-Basis-Legierung bestehenden Pulvers
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 true EP1032940A1 (fr) 2000-09-06
EP1032940B1 EP1032940B1 (fr) 2001-09-12

Family

ID=26041753

Family Applications (1)

Application Number Title Priority Date Filing Date
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
CZ305703B6 (cs) * 2014-11-07 2016-02-10 Vysoká škola chemicko- technologická v Praze Výroba nanostrukturovaných prášků slitin kobaltu dvoustupňovým mechanickým legováním

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2011077969A1 (ja) * 2009-12-24 2013-05-02 コニカミノルタホールディングス株式会社 反応容器及びそれを用いた燃料電池システム
DE102012200850A1 (de) * 2012-01-20 2013-07-25 Robert Bosch Gmbh Verfahren zur Herstellung eines magnetischen Materials und Permanentmagnet
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
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
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

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* 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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9927544A1 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CZ305703B6 (cs) * 2014-11-07 2016-02-10 Vysoká škola chemicko- technologická v Praze Výroba nanostrukturovaných prášků slitin kobaltu dvoustupňovým mechanickým legováním

Also Published As

Publication number Publication date
JP2001524604A (ja) 2001-12-04
EP1032940B1 (fr) 2001-09-12
WO1999027544A1 (fr) 1999-06-03
DE59801474D1 (de) 2001-10-18
US6352597B1 (en) 2002-03-05

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