EP0538320B1 - Behandlung von magnetpulvermaterialien und so erhaltene gegenstände - Google Patents

Behandlung von magnetpulvermaterialien und so erhaltene gegenstände Download PDF

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EP0538320B1
EP0538320B1 EP91912597A EP91912597A EP0538320B1 EP 0538320 B1 EP0538320 B1 EP 0538320B1 EP 91912597 A EP91912597 A EP 91912597A EP 91912597 A EP91912597 A EP 91912597A EP 0538320 B1 EP0538320 B1 EP 0538320B1
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temperature
magnetic
magnetic properties
precursor
oriented
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French (fr)
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EP0538320A1 (de
Inventor
Daniel Fruchart
Salvatore Miraglia
Paul Mollar
René Perrier De la Bathie
Robert Fruchart
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Centre National de la Recherche Scientifique CNRS
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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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/023—Hydrogen absorption
    • 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
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys 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
    • H01F1/0573—Alloys 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 obtained by reduction or by hydrogen decrepitation or embrittlement
    • 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
    • H01F1/065—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 obtained by a reduction

Definitions

  • the invention relates to an improved method for optimizing the magnetic properties of a material with permanent magnet properties, in order to obtain a product with high magnetic performance and in finely divided form. More specifically, it relates to a process capable of increasing the internal magnetic energy of such a material, of the rare earth / iron / boron alloy type, obtained after decrepitation by the hydriding-dehydriding procedure. Finally, it also relates to the products obtained by this process.
  • the production of bonded magnets is basically carried out by introducing a large amount of magnetic material in the most divided form possible, into an organic continuous matrix, generally made of a synthetic polymer. This step is carried out in the traditional way by means of a twin screw, at the melting point of the polymer. In this way, in order to obtain high performance bonded magnets, it is sought to introduce into the matrix the greatest possible quantity of magnetic material. As part of an optimization of such magnets, the aim is to minimize the size of the "particles" constituting the magnetic material, while increasing the magnetic properties, and in particular the coercivity of said "particles". In addition, it is important that the size distribution of these "particles" be as tight as possible, in particular in order to optimize the magnetic properties (coercivity, induction) of the bonded magnet.
  • This property is particularly important in the context of the production of magnets linked to strong anisotropy. Indeed, on this small distribution, and on the effective size of the "particles" obtained, depend on the one hand, the dispersibility of the powders, namely, their ability to disperse homogeneously, for example in the matrix or resin d coating, and on the other hand their orientability, namely, their ability to orient themselves under magnetic field, and more precisely to align their direction of easy magnetization with the direction of the applied magnetic field, and this by mechanical rotation.
  • One of the aims of the present invention is to propose a process capable of manufacturing such powders, having a high coercivity.
  • the object of the invention consists, starting from materials having qualities of permanent magnets - either intrinsically or potentially (example amorphous product) - to obtain powders having the same magnetic properties as their precursors by applying heat treatments corresponding to particular conditions.
  • the invention also aims to obtain powders of small homogeneous particle size, endowed with these magnetic properties.
  • a second heat treatment is applied to a temperature close to 600 ° C., that is to say a temperature higher than the desorption temperature of the hydrides of the main phase of the material.
  • this thermal post-treatment makes it possible to obtain dehydriding of all the constituent phases of the base alloy. Indeed, as we know, whatever the method of obtaining the latter, we must go through a step of melting the base material in order to obtain an alloy in massive form. This fusion not being congruent, there exists between the preponderant entities, constitutive of the "magnetic" phase proper, one or more secondary phases with eutectic behavior, richer in rare earth elements. In fact, subsequent heat treatments aim to dehydrate this or these secondary phases. Finally, by a third heat treatment, the aim is to reshape the envelope with a concentration rich in rare earth elements.
  • primary vacuum is meant in the sense of the invention a vacuum preferably less than 10 ⁇ 2 to 10 ⁇ 4 millimeters of mercury (or about 1 to 10 ⁇ 2 Pa). This primary vacuum is intended to allow the evacuation of hydrogen gas as it is formed. The duration of the thermal dehydriding treatments is also linked to the restoration of the initial primary vacuum.
  • the duration of the dehydriding treatment depends on the base material used. It is followed by cooling at constant speed, speed also depending on the starting material.
  • this first post-treatment can be followed by a thermal plateau, then by subsequent thermal treatments, the aim of which is similar to the first.
  • Another approach consists of starting from an isotropic powder of fine and uniform particle size, obtained for example by decrepitation with hydrogen at very high temperature (500 to 1000 ° C), then to subject this powder to a treatment of the plastic deformation type hot (analogous to that carried out in the previous case at the level of the precursor) intended to induce in said powder a certain degree of anisotropy without however risking causing its sintering. It certainly results in powders of small particle size, but whose magnetic properties, in particular the possible anisotropy of the precursor, are considerably reduced or even canceled, due to the separation of the magnetic phases constituting the basic magnetic structure, this separation being inherent to treatment under hydrogen at high temperature.
  • a mode of treatment has been targeted associated with a composition of suitable precursor making it possible to induce a maximum level of magnetic anisotropy at the level of this precursor.
  • a size reduction technique was used, such as hydrogen decrepitation practiced under moderate temperature conditions, followed by an appropriate post-treatment of dehydrogenation, capable of fully preserving the very strong anisotropy of the precursor. implemented for this purpose.
  • the starting product therefore plays a fundamental role both in terms of its composition and its isotropic or anisotropic nature, the latter being preserved through successive stages of decrepitation and post-treatments.
  • this product is advantageously a rare earth / iron / boron alloy, the iron possibly being partially substituted by cobalt or by other transition elements (3d, 4d, 5d).
  • part of these iron or cobalt elements can be substituted by other elements such as copper or aluminum.
  • a highly anisotropic precursor is obtained (in terms of its magnetic characteristics) if materials from "powder metallurgy" are used, a technique described in more detail in document EP-A-0 101 552, or if the 'We start from massive magnet falls.
  • Solid or ribbon precursors having, on the contrary, isotropic magnetic properties are obtained within the framework of hot working process carried out by spinning, also described in document WO 87/07425, or in the hyper-quenching process on rollers, described in particular in document EP-A-0 108 474.
  • the invention also relates to the product obtained. It is a product with good magnetic properties, typically an internal energy (HB) max greater than or equal to 80 kJ / m3 for isotropic powders and 240 kJ / m3 for anisotropic powders, with a small homogeneous particle size, typically close to ten micrometers, or less, and in any event less than fifteen micrometers.
  • these products have a remanent magnetization, typically at least 40 Am2 / kg for isotropic powders and 80 Am2 / kg for oriented anisotropic powders, and a high coercivity of at least 700 kA / m.
  • the grains of the products obtained have a characteristic facies in the form of broken crystallites, typical of the morphology resulting from this manufacturing process.
  • the starting material is a material which in the solid state already has high magnetic properties.
  • the process according to the invention aims, following a decrepitation having reduced its magnetic properties, to restore them to result in magnetic properties, in particular in coercivity, and residual induction, close to those of the starting raw product.
  • the starting product is an isotropic or anisotropic polyphase alloy depending on the destination of the final product, of rare earth / iron / boron composition.
  • iron can be substituted by cobalt, in particular with a view to increasing the Curie point of the final product or by other 3d transition metals, such as copper, or 4d and 5d.
  • iron can also be partially substituted by other metallic elements such as aluminum, and this cumulatively with the transition elements.
  • This alloy is, as already said, in polyphase form, respectively a magnetic phase with high anisotropy, corresponding to the general formula R2-M14-B, and one or more other phases with a majority concentration of rare earth elements, consecutive to the mode of realization of the basic material.
  • this basic material is firstly hydrided by absorption of hydrogen under pressure (1 to 5 MPa) for example in an autoclave made of special steel, and generally at room temperature.
  • pressure 1 to 5 MPa
  • thermal activation is necessary.
  • one or a few thermal cycles during the hydrogenation phase ensure better chemical and particle size homogeneity of the material.
  • This hydriding leads to the fragmentation of the material, which thus becomes very easily dispersible.
  • the revelation of the pulverulent form of the material can be obtained by simple mechanical stirring, or by simple grinding.
  • the hydrogenated pulverulent material undergoes three treatment phases:
  • a partial dehydriding is carried out, which concerns the main hydrated phase R2-M14-BH x (where x is between 1 and 5), the latter transforming into R2-M14-B.
  • the hydrides formed being of the metastable type, the dehydriding must be carried out under primary vacuum at a temperature lower than their demixing temperature, otherwise, the formation of rare earth hydrides, iron and an ill-defined iron-boron phase, the magnetic properties of the material then being definitively and prohibitively altered.
  • the temperature of this partial dehydriding which can start under primary vacuum around 150 ° C, and which increases around 300 ° C, must not exceed 520 ° C, demixing temperature of hydrides R2-M14-BH x .
  • the complete dehydration of the decrepit material can be carried out, in particular at the level of the eutectic phase rich in rare earths , which constitutes the film envelope of the magnetic domains.
  • This second phase is also carried out under primary vacuum.
  • the dehydrated powder thus obtained can be subjected in a third phase, to an annealing treatment between 450 and 1000 ° C., aimed at completely restoring the magnetic properties, in particular the coercivity.
  • the treatment can advantageously be supplemented with an in-situ passivation by introducing argon under normal pressure, before bringing the product back to its normal temperature.
  • the purpose of the final heat treatments is to optimize the cohesion of the granular material at the level of the elementary particles, namely the phase of the R2-M14-B type and of its eutectic intergranular envelope.
  • the different parameters of these heat treatments are a function of the composition of the base material and their metallurgical synthesis process.
  • Figure 1 a block diagram of the different stages involved in the production of a bonded magnet.
  • the powders obtained after the various heat treatments are dispersed before being coated in a resin, then oriented in the field.
  • Example 1 Phase a
  • This material undergoes a decrepitation treatment by hydriding, and the desorption is carried out by a heat treatment beyond 180 ° C.
  • This treatment aimed at desorbing the hydrogen from the main phase, is carried out at a speed of 300 ° C / hour. It constitutes the so-called dehydriding phase, carried out under primary vacuum. It is followed by a thermal plateau for 1 hour at 520 ° C and finally by cooling at the speed of 150 ° C / hour.
  • This finely divided isotropic material gives a residual induction of 42 Am2 / kg, but a very reduced coercive field of 120 kA / m, which makes this material unusable for shaping in the state of a bonded magnet.
  • phase a The same treatment is repeated as phase a, from the same material and then subjected to the latter a second heating phase at 600 ° C, temperature obtained at the rate of 300 ° C / hour.
  • This treatment is followed by heating to 640 ° C, temperature obtained at the speed of 50 ° C / hour, the thermal plateau at 640 ° C being maintained for 30 minutes.
  • This phase is followed by rapid cooling down to 600 ° C, at the speed of 1000 ° C / hour, followed by a temperature drop of 150 ° C / hour.
  • Example 2 Phase a
  • This material is decrepit then heat treated, in the same manner as that described in Example 1 phase a.
  • the residual induction of the non-oriented 0.4 compaction sample is 43 Am2 / kg, the coercive field being only 320 kA / m.
  • Example 1 The same precursor material which has undergone the treatment of Example 1 (phase a), then undergoes heating at 600 ° C., temperature obtained at the speed of 300 ° C. / hour. It is then treated according to the same process as that indicated in example 1 phase b.
  • the residual induction measured on a non-oriented 0.4 compaction sample is 43 Am2 / kg, and the coercive field of 880 kA / m. As in the previous case, the isotropic magnetic characteristics of the solid material are therefore largely restored.
  • the material is decrepit by hydriding, then heated to 520 ° C under primary vacuum, temperature obtained at the speed of 300 ° C / hour. It undergoes a thermal plateau lasting one hour at this temperature and is then heated to 600 ° C., a temperature obtained at the speed of 300 ° C / hour. It is then heated to 680 ° C, obtained at the speed of 100 ° C / hour. It then undergoes a thermal plateau for 20 minutes at 680 ° C, then is rapidly cooled down to 600 ° C at the speed of 600 ° C / hour, followed by a temperature drop to 150 ° C / hour.
  • the sample in the form of a non-oriented anisotropic powder of compaction 0.4, exhibits a residual induction of 40 Am2 / kg for a coercive field of 1,200 kA / m.
  • the powders thus obtained taking into account their small homogeneous particle size on the one hand, and their high magnetic properties on the other hand, enabled the production of anisotropic bonded magnets, for which the measured remanent induction is increased by 30 at 40% compared to the anisotropic bonded magnets available today, and this for substantially the same charge of magnetic material.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Claims (9)

  1. Verfahren zum Optimieren der magnetischen Eigenschaften eines Multiphasenproduktes der Zusammensetzung Seltene Erden/Eisen/Bor, das bei Raumtemperatur permanentmagnetische Eigenschaften aufweist, das als Prekursor dient und das einer Dekreptierbehandlung durch Hydrieren unter schwachem Druck bei niederen Temperaturen unterzogen wurde, um ein intermediäres Hydrid in pulverisierter Form zu erhalten,
       bei dem das pulverisierte intermediäre Hydrid, nachfolgend auf die Hydrierung, einer ersten thermischen Teildehydrierungsbehandlung unter Vakuum unterworfen wird, und zwar bei einer Temperatur unterhalb dessen Entmischungstemperatur, und
       das so erhaltene, nicht entmischte Produkt, bei einer Temperatur von etwa 600 C°, einer zweiten thermischen Dehydrierungsnachbehandlung bei Drücken bis zum Primärvakuum unterworfen wird.
  2. Verfahren zum Optimieren der magnetischen Eigenschaften eines isotropen Multiphasenproduktes nach Anspruch 1, dadurch gekennzeichnet, daß der Prekursor ein isotropes Material ist, das durch ein Verfahren, ausgewählt aus der Gruppe bestehend aus Hyperabschrecken, wie Abschrecken auf Rädern und Heißschmieden mit einem Verschmiedungsgrad von zumindest gleich 10 erhalten wurde.
  3. Verfahren zum Optimieren der magnetischen Eigenschaften eines anisotropen Multiphasenproduktes nach Anspruch 1, dadurch gekennzeichnet, daß der Prekursor ein anisotropes Material ist, das durch Ausrichten in einem Magnetfeld und Pulversintern, oder durch Warmmassivumformung eines massiven Materials, oder aus einem Abfallmaterial aus der Produktion von Magneten erhalten wurde.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß das erhaltene dehydrierte Produkt einer dritten Wärmenachbehandlung unter atmosphärischem Druck oder unter Vakuum unterworfen wird, und zwar bei einer Temperatur zwischen 450 und 1.000 °C, wobei die beiden Nachbehandlungen durch eine Temperstufe getrennt sein können oder auch nicht.
  5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß der Prekursor im überwiegenden Anteil der quadratischen Phase R₂-M₁₄-B entspricht, deren Entmischungstemperatur bei etwa 520 °C liegt, in der:
    - B Bor bedeutet;
    - R ein Element der Familie der Seltenen Erden oder Yttrium bedeutet;
    - und M Eisen bedeutet, gegebenenfalls teilweise substituiert durch ein Übergangselement, wie beispielsweise Kobalt, und/oder durch andere metallische Elemente, wie insbesondere Aluminium und Kupfer.
  6. Magnetische Zusammensetzungen, erzielbar durch das Verfahren nach einem der Ansprüche 1 bis 5, mit homogener Morphologie der überwiegend quadratischen Phase R₂-M₁₄-B, in der:
    - B Bor bedeutet;
    - R ein Element der Familie der Seltenen Erden oder Yttrium bedeutet;
    - und M Eisen bedeutet, gegebenenfalls teilweise substituiert durch ein Übergangselement, wie Kobalt und/oder andere metallische Elemente;
    dadurch gekennzeichnet, daß diese in Form eines Pulvers homogener Korngröße mit der mittleren Größe kleiner oder gleich 15 »m vorliegen, und daß diese eine Koerzitivkraft von zumindest 700 kA/m und eine remanente Induktion von zumindest 0,4 Tesla (40 Am²/kg) aufweisen.
  7. Magnetische Zusammensetzungen nach Anspruch 6, dadurch gekennzeichnet, daß sie magnetisch isotrop sind.
  8. Magnetische Zusammensetzungen nach Anspruch 6, dadurch gekennzeichnet, daß sie magnetisch anisotrop sind, und daß sie in ausgerichteter Form Brausgerichtet eine remanente Induktion entfalten, bei der das Verhältnis: Br ausgerichtet - Br nicht ausgerichtet Br ausgerichtet
    Figure imgb0007
     größer oder gleich 80 % ist.
  9. Magnetische Zusammensetzungen nach einem der Ansprüche 6 bis 8, dadurch gekennzeichnet, daß die Partikel, die das Pulver bilden, im überwiegenden Anteil Kristallite der Phase R₂-M₁₄-B enthalten, und daß die magnetischen Eigenschaften dieser Partikel im wesentlichen identisch denen des massiven Prekursors sind.
EP91912597A 1990-07-02 1991-06-28 Behandlung von magnetpulvermaterialien und so erhaltene gegenstände Expired - Lifetime EP0538320B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9008582A FR2664086A1 (fr) 1990-07-02 1990-07-02 Procede perfectionne pour l'optimisation des proprietes magnetiques de materiaux magnetiques pulverulents et produits ainsi obtenus.
FR9008582 1990-07-02
PCT/FR1991/000517 WO1992000595A1 (fr) 1990-07-02 1991-06-28 Traitement de materiaux magnetiques pulverulents et produits ainsi obtenus

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EP (1) EP0538320B1 (de)
JP (1) JPH06501135A (de)
AT (1) ATE106600T1 (de)
DE (1) DE69102277T2 (de)
FR (1) FR2664086A1 (de)
WO (1) WO1992000595A1 (de)

Cited By (1)

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CN109604615A (zh) * 2018-12-17 2019-04-12 江苏晨朗电子集团有限公司 低成本制备烧结钕铁硼永磁体的方法

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US5834229A (en) 1991-05-24 1998-11-10 Genentech, Inc. Nucleic acids vectors and host cells encoding and expressing heregulin 2-α
IL101943A0 (en) * 1991-05-24 1992-12-30 Genentech Inc Structure,production and use of heregulin
FR2997095B1 (fr) * 2012-10-24 2014-11-28 Commissariat Energie Atomique Procede pour isoler les terres rares et/ou element(s) metallique(s) annexe(s) contenus dans la phase magnetique d'aimants permanents.
FR3030866B1 (fr) 2014-12-18 2021-03-12 Commissariat Energie Atomique Aimant permanent fritte
FR3044161B1 (fr) 2015-11-25 2019-05-03 Commissariat A L'energie Atomique Et Aux Energies Alternatives Aimant permanent fritte
SI4176094T1 (sl) * 2020-07-01 2025-06-30 Yeda Research And Development Co. Ltd Pridobivanje redkozemeljskih kovin iz feromagnetnih zlitin

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JPS60119701A (ja) * 1983-12-01 1985-06-27 Sumitomo Special Metals Co Ltd 希土類・ボロン・鉄系永久磁石用合金粉末の製造方法
FR2566758B1 (fr) * 1984-06-29 1990-01-12 Centre Nat Rech Scient Nouveaux hydrures de terre rare/fer/bore et terre rare/cobalt/bore magnetiques, leur procede de fabrication et de fabrication des produits deshydrures pulverulents correspondants, leurs applications
JPS6390104A (ja) * 1986-10-03 1988-04-21 Tdk Corp 希土類−鉄−ホウ素系永久磁石の製造方法
JPS6447841A (en) * 1987-08-12 1989-02-22 Tdk Corp Production of rare earth alloy magnet
JPS6445103A (en) * 1987-08-13 1989-02-17 Tdk Corp Manufacture of rare earth alloy magnet
JPS6448406A (en) * 1987-08-19 1989-02-22 Mitsubishi Metal Corp Magnet powder for sintering rare earth-iron-boron and manufacture thereof
EP0304054B1 (de) * 1987-08-19 1994-06-08 Mitsubishi Materials Corporation Magnetisches Seltenerd-Eisen-Bor-Puder und sein Herstellungsverfahren
US4760966A (en) * 1987-08-28 1988-08-02 The United States Of America As Represented By The Secretary Of The Army Method of comminuting rare earth magnet alloys into fine particles

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109604615A (zh) * 2018-12-17 2019-04-12 江苏晨朗电子集团有限公司 低成本制备烧结钕铁硼永磁体的方法

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EP0538320A1 (de) 1993-04-28
WO1992000595A1 (fr) 1992-01-09
DE69102277D1 (de) 1994-07-07
FR2664086A1 (fr) 1992-01-03
ATE106600T1 (de) 1994-06-15
FR2664086B1 (de) 1994-08-19
DE69102277T2 (de) 1994-09-15
JPH06501135A (ja) 1994-01-27

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