EP0608188A1 - Verfahren zum Schutz von Magnetpudern und verdichte Dauermagneten, Typ Nd-Fe-B, gegen Oxydation und atmospherische Korrosion - Google Patents

Verfahren zum Schutz von Magnetpudern und verdichte Dauermagneten, Typ Nd-Fe-B, gegen Oxydation und atmospherische Korrosion Download PDF

Info

Publication number
EP0608188A1
EP0608188A1 EP94420016A EP94420016A EP0608188A1 EP 0608188 A1 EP0608188 A1 EP 0608188A1 EP 94420016 A EP94420016 A EP 94420016A EP 94420016 A EP94420016 A EP 94420016A EP 0608188 A1 EP0608188 A1 EP 0608188A1
Authority
EP
European Patent Office
Prior art keywords
powders
fluorine
ppm
atmospheric corrosion
magnets
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
EP94420016A
Other languages
English (en)
French (fr)
Other versions
EP0608188B1 (de
Inventor
Masato Sagawa
Fernand Vial
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.)
Ugimag SA
Original Assignee
Ugimag SA
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
Application filed by Ugimag SA filed Critical Ugimag SA
Publication of EP0608188A1 publication Critical patent/EP0608188A1/de
Application granted granted Critical
Publication of EP0608188B1 publication Critical patent/EP0608188B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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
    • H01F41/026Apparatus 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 protecting methods against environmental influences, e.g. oxygen, by surface treatment
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys 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
    • H01F1/0572Alloys 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 with a protective layer

Definitions

  • the present invention relates to a method of protecting magnetic powders and permanent magnets of the transition metal - rare earth metal type against oxidation and atmospheric corrosion by the introduction of gaseous fluorine during the grinding of the powders. It applies more particularly to powders and magnets of the transition metal - rare earth - boron family, where the metal is essentially iron, and the rare earth essentially of neodymium and / or praseodymium.
  • the process illustrated here by way of example, consists in introducing during the fine grinding step, for example, into a gas jet mill (jet mill) a mixture N 2 + F 2 , which can contain between 1 and 100 ppm in flight. of fluorine, and preferably between 1 and 10 ppm, with the usual carrier gas flow rates and grinding time for this operation (for example 100 Nm 3 / h of nitrogen under a relative pressure of 0.5 Pa, for 3 h ).
  • a gas jet mill jet mill
  • the optimum fluorine content of powders and sintered magnets is between 600 and 2000 ppm. Below 600 ppm, the resistance to powder oxidation and to corrosion in a humid atmosphere of the magnets is insufficient; beyond 2000 ppm, densification defects are noted during densification and weaker intrinsic coercive fields.
  • Powders treated with fluorine are more stable with respect to atmospheric oxidation.
  • the flow rate of the F 2 + N 2 gas mixture was controlled by a calibrated nozzle and by the pressure difference upstream and downstream of the nozzle.
  • the powders thus obtained were axially compressed under an axial field of 1.1 T, at a pressure of 1.6 t / cm 2 in cylindrical samples 15 mm in diameter and 12 mm high.
  • densification was obtained by sintering carried out under vacuum at temperatures between 1060 and 1090 ° C for 4 hours.
  • the blanks thus obtained underwent the usual heat treatments of magnetic hardening, adjusted according to the rare earth content.
  • Alloy powders of the initial composition given in Table V were prepared and ground in a gas mill with or without the introduction of fluorine, under conditions analogous to those of Example 1, the fluorine content in the grinding chamber being 1 ppm (in vol.) in nitrogen.
  • the present process has been illustrated in the production range of powders and magnets by sintering these powders of the TR 2 Fe 14 B type enriched with rare earth.
  • these fine powders are obtained from alloy ingots, but they can also be obtained from coarse powders obtained by the so-called reduction-diffusion process.
EP94420016A 1993-01-22 1994-01-19 Verfahren zum Schutz von Magnetpudern und verdichte Dauermagneten, Typ Nd-Fe-B, gegen Oxydation und atmospherische Korrosion Expired - Lifetime EP0608188B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9300840A FR2700720B1 (fr) 1993-01-22 1993-01-22 Procédé de protection de poudres magnétiques et aimants permanents densifiés type Fe Nd B contre l'oxydation et la corrosion atmosphérique.
FR9300840 1993-01-22

Publications (2)

Publication Number Publication Date
EP0608188A1 true EP0608188A1 (de) 1994-07-27
EP0608188B1 EP0608188B1 (de) 1996-10-02

Family

ID=9443427

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94420016A Expired - Lifetime EP0608188B1 (de) 1993-01-22 1994-01-19 Verfahren zum Schutz von Magnetpudern und verdichte Dauermagneten, Typ Nd-Fe-B, gegen Oxydation und atmospherische Korrosion

Country Status (10)

Country Link
US (1) US5411603A (de)
EP (1) EP0608188B1 (de)
JP (1) JP3400840B2 (de)
AT (1) ATE143745T1 (de)
CA (1) CA2112868A1 (de)
DE (1) DE69400618T2 (de)
FI (1) FI940318A (de)
FR (1) FR2700720B1 (de)
MX (1) MX9400180A (de)
SI (1) SI9400020A (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6580820B1 (en) 1999-06-09 2003-06-17 Xerox Corporation Digital imaging method and apparatus for detection of document security marks

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5437544B2 (ja) * 2001-06-11 2014-03-12 株式会社三徳 二次電池用負極の製造法
JP4747562B2 (ja) * 2004-06-25 2011-08-17 株式会社日立製作所 希土類磁石及びその製造方法、並びに磁石モータ
US8211327B2 (en) * 2004-10-19 2012-07-03 Shin-Etsu Chemical Co., Ltd. Preparation of rare earth permanent magnet material
TWI417906B (zh) * 2005-03-23 2013-12-01 Shinetsu Chemical Co 機能分級式稀土族永久磁鐵
MY141999A (en) 2005-03-23 2010-08-16 Shinetsu Chemical Co Functionally graded rare earth permanent magnet
TWI413136B (zh) * 2005-03-23 2013-10-21 Shinetsu Chemical Co 稀土族永久磁體
MY142024A (en) * 2005-03-23 2010-08-16 Shinetsu Chemical Co Rare earth permanent magnet
US7955443B2 (en) * 2006-04-14 2011-06-07 Shin-Etsu Chemical Co., Ltd. Method for preparing rare earth permanent magnet material
JP4656323B2 (ja) * 2006-04-14 2011-03-23 信越化学工業株式会社 希土類永久磁石材料の製造方法
JP4840606B2 (ja) 2006-11-17 2011-12-21 信越化学工業株式会社 希土類永久磁石の製造方法
DE102007032406B3 (de) * 2007-07-10 2008-10-23 Gkss-Forschungszentrum Geesthacht Gmbh Herstellung von Legierungen auf Basis von Titanaluminiden
JP2012039017A (ja) * 2010-08-11 2012-02-23 Hitachi Ltd 磁石材料,磁石成形品及び回転機
CN113444982A (zh) * 2020-03-25 2021-09-28 Neo新材料技术(新加坡)私人有限公司 合金粉末及其制备方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01205502A (ja) * 1988-02-12 1989-08-17 Seiko Epson Corp 希土類・鉄系樹脂結合型磁石

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61124502A (ja) * 1984-11-21 1986-06-12 Mitsui Mining & Smelting Co Ltd 安定性金属磁性粉末及びその製造方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01205502A (ja) * 1988-02-12 1989-08-17 Seiko Epson Corp 希土類・鉄系樹脂結合型磁石

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
J.H.SWISHER ET AL, JOURNAL OF THE ELECTROCHEMICAL SOCIETY, vol. 117, no. 4, April 1970 (1970-04-01), MANCHESTER, NEW HAMPSHIRE US, pages 537 - 540 *
PATENT ABSTRACTS OF JAPAN vol. 13, no. 509 (E - 846) 15 November 1989 (1989-11-15) *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6580820B1 (en) 1999-06-09 2003-06-17 Xerox Corporation Digital imaging method and apparatus for detection of document security marks

Also Published As

Publication number Publication date
MX9400180A (es) 1994-07-29
EP0608188B1 (de) 1996-10-02
ATE143745T1 (de) 1996-10-15
CA2112868A1 (fr) 1994-07-23
US5411603A (en) 1995-05-02
DE69400618D1 (de) 1996-11-07
FR2700720B1 (fr) 1995-05-05
FR2700720A1 (fr) 1994-07-29
JPH07320917A (ja) 1995-12-08
FI940318A0 (fi) 1994-01-21
SI9400020A (en) 1994-09-30
JP3400840B2 (ja) 2003-04-28
DE69400618T2 (de) 1997-02-27
FI940318A (fi) 1994-07-23

Similar Documents

Publication Publication Date Title
EP0608188A1 (de) Verfahren zum Schutz von Magnetpudern und verdichte Dauermagneten, Typ Nd-Fe-B, gegen Oxydation und atmospherische Korrosion
JP5561170B2 (ja) R−t−b系焼結磁石の製造方法
JP4831253B2 (ja) R−T−Cu−Mn−B系焼結磁石
JP5477282B2 (ja) R−t−b系焼結磁石およびその製造方法
JP2006210450A (ja) R−t−b系焼結磁石
JP2019012796A (ja) 希土類磁石の製造方法
JP2009224413A (ja) NdFeB焼結磁石の製造方法
JP6717230B2 (ja) R−t−b系焼結磁石の製造方法
EP0428718A1 (de) Verbesserte magnetische materialien und deren herstellungsverfahren
JPH06188113A (ja) NdFeBを主成分とする永久磁石の製造方法
CN113161094A (zh) 一种r-t-b磁体及其制备方法
WO2015182705A1 (ja) R-t-b系焼結磁石の製造方法
JP7315889B2 (ja) R-t-b系永久磁石用合金およびr-t-b系永久磁石の製造方法
CN111489874A (zh) R-t-b系烧结磁体的制造方法
EP0707739B1 (de) Ein seltener erd-cobalttyp fluorenthaltender magnetpuder und verdichtete dauermagneten daraus und deren herstellungsverfahren
EP0468903B1 (de) Herstellungsverfahren von Seltenerdübergangsmetall-Bortyp-Magnetpulver für korrosionsfeste Magnete
CN112086256B (zh) 一种R-Fe-B系稀土烧结磁铁及制备方法
JP7380369B2 (ja) R-t-b系焼結磁石の製造方法及び拡散用合金
JP7452159B2 (ja) R-t-b系焼結磁石の製造方法
US20220384072A1 (en) Rare earth sintered magnet and making method
US20230005646A1 (en) Rare-earth sintered magnet
JPH06200307A (ja) 稀土類磁石用原料合金粉末の製造方法
WO2023080169A1 (ja) R-t-b系永久磁石
SU710791A1 (ru) Способ изготовлени посто нных магнитов
JP2021057565A (ja) R−t−b系焼結磁石

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT CH DE ES GB IT LI NL SE

17P Request for examination filed

Effective date: 19940822

17Q First examination report despatched

Effective date: 19951002

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT CH DE ES GB IT LI NL SE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 19961002

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRE;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED.SCRIBED TIME-LIMIT

Effective date: 19961002

Ref country code: ES

Free format text: THE PATENT HAS BEEN ANNULLED BY A DECISION OF A NATIONAL AUTHORITY

Effective date: 19961002

Ref country code: AT

Effective date: 19961002

REF Corresponds to:

Ref document number: 143745

Country of ref document: AT

Date of ref document: 19961015

Kind code of ref document: T

REF Corresponds to:

Ref document number: 69400618

Country of ref document: DE

Date of ref document: 19961107

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 19961104

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Effective date: 19970102

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Effective date: 19970131

Ref country code: CH

Effective date: 19970131

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

26N No opposition filed
REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20060112

Year of fee payment: 13

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20060118

Year of fee payment: 13

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20070801

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20070119

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20070119