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EP0775363A1 - Procede de fabrication de parties magnetiques dures - Google Patents

Procede de fabrication de parties magnetiques dures

Info

Publication number
EP0775363A1
EP0775363A1 EP96918658A EP96918658A EP0775363A1 EP 0775363 A1 EP0775363 A1 EP 0775363A1 EP 96918658 A EP96918658 A EP 96918658A EP 96918658 A EP96918658 A EP 96918658A EP 0775363 A1 EP0775363 A1 EP 0775363A1
Authority
EP
European Patent Office
Prior art keywords
powder
alloy
temperature range
mixture
samarium
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.)
Withdrawn
Application number
EP96918658A
Other languages
German (de)
English (en)
Inventor
Lei Cao
Axel Handstein
Karl-Hartmut MÜLLER
Ludwig Schultz
Volker Neu
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.)
Leibniz Institut fuer Festkorper und Werkstofforschung Dresden eV
Original Assignee
Leibniz Institut fuer Festkorper 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 DE19521221A external-priority patent/DE19521221C1/de
Priority claimed from DE19521218A external-priority patent/DE19521218C1/de
Application filed by Leibniz Institut fuer Festkorper und Werkstofforschung Dresden eV filed Critical Leibniz Institut fuer Festkorper und Werkstofforschung Dresden eV
Publication of EP0775363A1 publication Critical patent/EP0775363A1/fr
Withdrawn legal-status Critical Current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
    • H01F1/058—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C

Definitions

  • the method can be used, for example, for the production of hard magnetic parts based on interstitial Sm 2 Fe 17 C y compounds.
  • Sm 2 Fe 17 X y compounds with interstitial inclusions X carbon or nitrogen have very good preconditions for use as permanent magnet materials (JMCoey and H.Sun, J. Magn Magn. Mater. 87 (1990) L 251).
  • the Sm 2 Fe ⁇ 7 C y carbon compounds are unstable at y> 1.
  • the carbon content of Sm 2 Fe 17 C y can be increased by substitution of iron by gallium to y> 1 as a prerequisite for the improvement of the intrinsic properties, since the addition of gallium has the rhombohedral 2:17 structure necessary for good magnetic properties Compound stabilized (B.-G. Shen, L.-S. Kong, F.-W. Wang and L. Cao, Appl. Phys. Letters 63 (1993) 2288).
  • the finely ground mixture is heat-treated in the temperature range from 650 ° C. to 900 ° C. for partial or complete recrystallization and
  • the magnetic bodies obtained in this way have an isotropic magnetic behavior and, according to the invention, can subsequently be provided with a preferred magnetic direction by a process of hot forming in the temperature range from 650 ° C. to 900 ° C. and at a pressure above 200 MPa.
  • samarium with iron, M and carbon or samarium with an iron-carbon alloy and M in finely divided form in a ratio which corresponds to the composition of Sm2Fe 17 _ x M x Cy with x> 0.1 and 3>y> 0 corresponds to be mixed.
  • At least one element from the group formed by the elements aluminum, molybdenum, niobium, tantalum, titanium and zircon can be mixed in for M instead of or together with gallium.
  • the starting mixture is produced with an amount of samarium which in the end product of the process results in a samarium content below 10 to 3 at%, if starting from this starting mixture in stage b) by selecting the grinding intensity and duration, a grain size ⁇ 200 nm is generated and if in the subsequent stages c) and d) and in the case of subsequent hot forming of the magnetic bodies by selection of the heat treatment parameters, the grain growth to a value
  • a second embodiment of the process according to the invention can also be used in a melt-metallurgical way, by first melting an Sm2Fe 17 _ x M x Cy alloy with x> 0.1 and 3>y> 0 , after solidification, subjected to a homogenization annealing in the temperature range from 900 ° C to 1200 ° C and then crushed the alloy into a powder.
  • At least one element consisting of the elements aluminum, molybdenum,
  • Niobium, tantalum, titanium and zircon formed group are alloyed.
  • a Sm2Fe ] _ 7 _ x Ga x Cy alloy with x> 0.1 and 2>y> 0 can also be produced by the melt metallurgical route. After solidification, this alloy is subjected to a homogenization annealing in the temperature range from 900 ° C to 1200 ° C and then comminuted to a powder. The powder is first subjected to an annealing treatment at temperatures of 600 ° C to 900 ° C in hydrogen gas and then in a vacuum.
  • the powdered alloy is subjected to heat treatment in the Temperature range from 400 ° C to 600 ° C in a carbon-containing gas to a Sm2Fe ⁇ 7 _ x Ga x Cy alloy with y ⁇ 3 alloyed.
  • CH4 or C2H2 can be used to alloy the powder.
  • the prerequisites are created in order to produce compacted magnets from the interstitial compound Sm 2 (Fe, M) 17 C y in a rational and cost-effective manner. It is also advantageous that the method can be carried out with the conventional metallurgical plants used in permanent magnet production and is easy to use.
  • the Sm2 (Fe, M) 17 Cy materials processed in the manner according to the invention are up to temperatures of stable at about 1000 ° C.
  • Samarium, iron gallium and carbon are mixed in finely divided form to form a metal powder with the composition Sm 2 Fe ls Ga 2 C 2 and ground intensively in a ball mill.
  • the magnetically isotropic fine powder obtained afterwards with a coercive field strength of approximately 1000 kA / m is subjected to a heat treatment for recrystallization at 700 ° C. to 750 ° C. under vacuum or an inert gas atmosphere.
  • this powder is compressed in a hot press at 700 ° C to 750 ° C under vacuum or an inert gas atmosphere at a pressure of 300 MPa to 500 MPa for a period of 2 to 5 minutes. 5
  • compact permanent magnets are obtained with a coercive field strength that corresponds to that of the ground powder.
  • Example 1 The powder ground according to Example 1 but not yet heat-treated is placed in a hot press and compacted at 700 ° C. to 750 ° C. under vacuum or in an inert gas atmosphere at a pressure of 300 MPa to 500 MPa over a period of 10 to 60 minutes .
  • the heat treatment which is carried out in Example 1 as a separate process step before hot pressing, takes place according to Example 2 during the hot pressing process. With this procedure, compact permanent magnets are obtained which have a coercive field strength of approximately 1000 kA / m.
  • the magnets obtained in the result of Examples 1 and 2 which are characterized by an isotropic magnetic behavior, are subjected to hot deformation in the temperature range between 750 ° C and 800 ° C at a pressure of 300 MPa to 500 MPa under vacuum or an inert gas atmosphere. As a result, magnets with a preferred magnetic direction are obtained.
  • An alloy of the composition Sm 2 Fe 15 Ga 2 C 2 is homogenized after solidification, crushed and subjected to an intensive grinding process.
  • the magnetically isotropic fine powder obtained afterwards with a coercive field strength of approximately 1000 kA / m is subjected to a heat treatment for recrystallization at 700 ° C. to 750 ° C. under vacuum or an inert gas atmosphere.
  • this powder is compressed in a hot press at 700 ° C. to 750 ° C. under vacuum or an inert gas atmosphere at a pressure of 300 MPa to 500 MPa for a period of 2 to 5 minutes.
  • Example 4 The powder ground according to Example 4, but not yet heat-treated, is placed in a hot press and compacted at 700 ° C. to 750 ° C. under vacuum or in an inert gas atmosphere at a pressure of 300 MPa to 500 MPa over a period of 10 to 60 minutes .
  • the heat treatment which is carried out in Example 4 as a separate process step before hot pressing, takes place according to Example 5 during the hot pressing process. With this procedure, compact permanent magnets are obtained which have a coercive field strength of approximately 1000 kA / m.
  • An alloy with the composition Sm2Fe --_ gGa --_ is homogenized and comminuted after solidification at 1100 ° C.
  • the powder is heated to 750 ° C. in a hydrogen atmosphere and kept at this temperature for 60 min.
  • the powder is then heated in vacuo to 800 ° C. for 100 minutes and then cooled.
  • a very fine-grained S ⁇ r * 2Fe --_ 5Ga --_ powder is formed, which is then subjected to annealing in a methane atmosphere at 500 ° C. for a period of 6 hours in order to store the carbon.
  • the resulting Sir ⁇ FeigGa - ⁇ .4 powder in a hot press at 700 ° C to 750 ° C under vacuum or inert gas atmosphere at a pressure of 300 MPa to 500 MPa for a period of 2 to 5 min condensed.
  • the magnets obtained in the result of Examples 4, 5 and 6, which are characterized by an isotropic magnetic behavior, are subjected to a hot deformation in the temperature range between 750 ° C and 800 ° C at a pressure of 300 MPa to 500 MPa under vacuum or an inert gas atmosphere. As a result, magnets with a preferred magnetic direction are obtained.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Power Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

L'invention a pour objet un procédé permettant la fabrication de parties magnétiques dures, dont la technologie soit maîtrisable et économique, à partir de matières à base de Sm2-(Fe,M)17-Cy- avec inclusions interstitielles, où M = gallium et/ou au moins un élément métallique doit servir à la stabilisation d'une structure 2:17 rhomboédrique. Le procédé est caractérisé en ce que a) l'on produit un mélange en poudre Sm2Fe17-xMxCy où x > 0,1 et 3 >/= y >/= 0; b) l'on soumet ce mélange à un procédé de pulvérisation intensif dans un triturateur à boulets; c) l'on procède au traitement thermique du mélange pulvérisé dans une plage de températures comprise entre 650 DEG C et 900 DEG C pour une recristallisation partielle ou complète et; d) l'on comprime la poudre magnétique Sm2Fe17-xMxCy à grains ultrafins ainsi obtenue par un procédé thermique dans une plage de températures comprise entre 650 DEG C et 900 DEG C pour former des corps magnétiques. Ce procédé peut servir, par exemple, pour fabriquer des parties magnétiques dures à base de composés Sm2Fe17Cy interstitiels.
EP96918658A 1995-06-14 1996-06-01 Procede de fabrication de parties magnetiques dures Withdrawn EP0775363A1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE19521218 1995-06-14
DE19521221A DE19521221C1 (de) 1995-06-14 1995-06-14 Verfahren zur Herstellung hartmagnetischer Teile aus Sm¶2¶-(Fe, M)¶1¶¶7¶-C¶Y¶-Basis-Legierungen
DE19521221 1995-06-14
DE19521218A DE19521218C1 (de) 1995-06-14 1995-06-14 Verfahren zur Herstellung hartmagnetischer Teile aus Sm¶2¶-(Fe, M)¶1¶¶7¶-C¶Y¶-Basis-Werkstoffen
PCT/EP1996/002379 WO1997000524A1 (fr) 1995-06-14 1996-06-01 Procede de fabrication de parties magnetiques dures

Publications (1)

Publication Number Publication Date
EP0775363A1 true EP0775363A1 (fr) 1997-05-28

Family

ID=26015888

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96918658A Withdrawn EP0775363A1 (fr) 1995-06-14 1996-06-01 Procede de fabrication de parties magnetiques dures

Country Status (4)

Country Link
US (1) US5733384A (fr)
EP (1) EP0775363A1 (fr)
JP (1) JPH10504141A (fr)
WO (1) WO1997000524A1 (fr)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1717290B (zh) * 2003-05-27 2010-08-11 日立金属株式会社 稀土类合金造粒粉的制造方法及制造装置以及稀土类合金烧结体的制造方法
EP2258812A4 (fr) 2008-03-14 2014-01-22 Nippon Steel Eng Co Ltd Système réactionnel pour la synthèse d'un composé hydrocarboné et procédé d'élimination de particules finement divisées
JP5055345B2 (ja) * 2009-11-30 2012-10-24 株式会社日立製作所 強磁性化合物磁石
US9444105B2 (en) 2011-11-04 2016-09-13 Fluidic, Inc. Immersible gaseous oxidant cathode for electrochemical cell system
CN103123862B (zh) * 2011-11-21 2015-09-09 中国科学院宁波材料技术与工程研究所 提高热压/热变形辐射取向钕铁硼永磁环性能及其轴向均匀性的方法
WO2018075870A1 (fr) 2016-10-21 2018-04-26 Fluidic Inc. Électrode à combustible ondulée
CN107219105B (zh) * 2017-05-22 2020-02-07 西北有色金属研究院 一种对az31镁合金内部剪切带的观察方法
US11611115B2 (en) 2017-12-29 2023-03-21 Form Energy, Inc. Long life sealed alkaline secondary batteries
CN120049075A (zh) 2018-07-27 2025-05-27 福恩能源公司 用于电化学电池的负电极
US12294086B2 (en) 2019-07-26 2025-05-06 Form Energy, Inc. Low cost metal electrodes
JP7449538B2 (ja) * 2020-09-10 2024-03-14 国立大学法人東北大学 希土類鉄炭素系磁性粉末及びその製造方法
JP7751852B2 (ja) * 2022-03-02 2025-10-09 国立大学法人東北大学 希土類鉄炭素硼素系磁性粉末及びその製造方法

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4192696A (en) * 1975-12-02 1980-03-11 Bbc Brown Boveri & Company Limited Permanent-magnet alloy
DE3621905C1 (de) * 1986-06-30 1987-07-09 Voith Turbo Kg Hydrodynamische Kupplung
JPS63308904A (ja) * 1987-06-11 1988-12-16 Fuji Elelctrochem Co Ltd ボンド磁石の製造方法
US5007972A (en) * 1988-06-09 1991-04-16 The Charles Stark Draper Laboratory, Inc. Samarium-transition metal magnet formation
NL8901168A (nl) * 1989-05-10 1990-12-03 Philips Nv Hardmagnetisch materiaal en magneet vervaardigd uit dit hardmagnetische materiaal.
JPH04176805A (ja) * 1990-11-08 1992-06-24 Tokin Corp 希土類コバルト系ボンド磁石粉末の製造方法
DE4134245C2 (de) * 1991-10-16 1995-10-19 Siemens Ag Verfahren zur Herstellung von Magnetmaterial auf Basis des Stoffsystems Sm-Fe-C
DE4243048A1 (de) * 1992-12-18 1994-06-23 Siemens Ag Verfahren zur Herstellung eines hartmagnetischen Materials auf Basis des Stoffsystems Sm-Fe-C

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9700524A1 *

Also Published As

Publication number Publication date
JPH10504141A (ja) 1998-04-14
WO1997000524A1 (fr) 1997-01-03
US5733384A (en) 1998-03-31

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