EP0931322B1 - Soft magnetic, deformable composite material and process for producing the same - Google Patents

Soft magnetic, deformable composite material and process for producing the same Download PDF

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Publication number
EP0931322B1
EP0931322B1 EP98948761A EP98948761A EP0931322B1 EP 0931322 B1 EP0931322 B1 EP 0931322B1 EP 98948761 A EP98948761 A EP 98948761A EP 98948761 A EP98948761 A EP 98948761A EP 0931322 B1 EP0931322 B1 EP 0931322B1
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Prior art keywords
powder
composite material
process according
solvent
coated
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EP98948761A
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German (de)
French (fr)
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EP0931322A1 (en
Inventor
Wilfried Aichele
Hans-Peter Koch
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Robert Bosch GmbH
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Robert Bosch GmbH
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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
    • H01F1/12—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 soft-magnetic materials
    • H01F1/14—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 soft-magnetic materials metals or alloys
    • H01F1/20—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H01F1/26—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
    • 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
    • H01F1/12—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 soft-magnetic materials
    • H01F1/14—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 soft-magnetic materials metals or alloys
    • H01F1/20—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—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 soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus 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
    • H01F41/02—Apparatus 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
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder

Definitions

  • the invention relates to a soft magnetic, mouldable Composite material with soft magnetic properties containing powder containing a non-magnetic Have coating, and a method for its Production.
  • Soft magnetic materials are required for the production of temperature, corrosion and solvent resistant magnetic components in the electronics sector and especially in electromechanics. These soft magnetic components require certain properties: they should have a high permeability ( ⁇ max ), a high magnetic saturation (B s ), a low coercive force (H c ) and a high specific electrical resistance ( ⁇ spec ). The combination of these magnetic properties with a high specific electrical resistance results in high switching dynamics, that is to say that the magnetic saturation and demagnetization of such a component take place within a short time.
  • thermosetting resins for example, epoxies or phenolic resins
  • the previously used thermoplastic and thermosetting binder at elevated temperature in organic solvents for example fuels for Internal combustion engines are soluble or strong swell.
  • the corresponding composite components change under these conditions lose their dimensions Strength and fail completely. So far it has not been possible, corresponding composite materials with high Temperature and media resistance, for example in organic solvents, especially fuels for To manufacture internal combustion engines.
  • Another Problem so far provided the operating conditions for this Components include both thermoplastics and Thermosets are no longer a suitable binder because otherwise they would decompose completely.
  • this is Polyphtalamide as a thermoplastic compound from a solution applied to the powder grains.
  • the powder grains are introduced into the polymer solution and the solvent under continuous movement of the powder at elevated temperature or in a vacuum. Thereby receive the powder grains in a simple manner a thin polymer coating ("coating"), so that complicated process processes are eliminated.
  • Thermoplastics with high heat resistance show in Compared to low-melting thermoplastics much less cold flow.
  • Thermoplastic powders are therefore only produced with ductile ones Thermoplastic powders around a sufficient insulation layer the magnetic particles.
  • high-melting Thermoplastics not as a powder with the necessary low Grain size of ⁇ 5 microns commercially available. Both Difficulties are caused by the invention handled that the magnetic powder before the axial pressing is coated with a polymer solution. if the Solubility of the polymer only given at higher temperatures is the dissolving of the polymer and coating the Magnetic powder to avoid thermo-oxidative Damage to the thermoplastic material under protective gas occur.
  • the cold pressing of the coated magnetic powder is followed by a heat treatment of the compact under protective gas above the melting point of the polymer (PPA, 320 ° C).
  • the samples obtained have a strength of approx. 80 N / mm 2 and a specific electrical resistance of at least 400 ⁇ Ohm * m.
  • a better demoldability of the pressed components from the molding press is achieved by surface treatment of the coated powder with a lubricant.
  • the lubricant is added in a much smaller proportion than the thermoplastic coating in order to reduce the density of the pressed parts as little as possible and it should be so volatile that it volatilizes before the polymer melts during the subsequent heat treatment and does not react chemically with the polymer .
  • suitable lubricants are, for example, punch oils, such as those used for punching sheet metal, or rapeseed oil methyl ester and stearic acid amide in additions of about 0.2%, based on the weight of the magnetic powder.

Description

Stand der TechnikState of the art

Die Erfindung betrifft einen weichmagnetischen, formbaren Verbundwerkstoff, der weichmagnetische Eigenschaften aufweisende Pulver enthält, die eine nichtmagnetische Beschichtung aufweisen, sowie ein Verfahren zu dessen Herstellung.The invention relates to a soft magnetic, mouldable Composite material with soft magnetic properties containing powder containing a non-magnetic Have coating, and a method for its Production.

Weichmagnetischen Werkstoffe werden zur Herstellung von temperatur-, korrosions- und lösungsmittelbeständigen magnetischen Bauteilen im Elektroniksektor und insbesondere in der Elektromechanik benötigt. Dabei bedürfen diese weichmagnetischen Bauteile gewisser Eigenschaften: sie sollen eine hohe Permeabilität (µmax), eine hohe magnetische Sättigung (Bs), eine geringe Koerzitivfeldstärke (Hc) und einen hohen spezifischen elektrischen Widerstand (ρspez) aufweisen. Die Kombination dieser magnetischen Eigenschaften mit einem hohen spezifischen elektrischen Widerstand ergibt eine hohe Schaltdynamik, das heißt, die magnetische Sättigung und die Entmagnetisierung eines derartigen Bauteiles erfolgen innerhalb kurzer Zeit.Soft magnetic materials are required for the production of temperature, corrosion and solvent resistant magnetic components in the electronics sector and especially in electromechanics. These soft magnetic components require certain properties: they should have a high permeability (µ max ), a high magnetic saturation (B s ), a low coercive force (H c ) and a high specific electrical resistance (ρ spec ). The combination of these magnetic properties with a high specific electrical resistance results in high switching dynamics, that is to say that the magnetic saturation and demagnetization of such a component take place within a short time.

Bislang werden beispielweise Weicheisenbleche zu Lamellenpaketen verklebt, um als Anker von Elektromotoren zu dienen. Die Lagenisolation wirkt jedoch nur in einer Richtung. Aus dem EP 0 540 504 B1 ist bekannt, weichmagnetische Pulvern mit einem Kunststoffbinder aufzubereiten und damit durch ein Spritzgußverfahren entsprechende Bauteile herzustellen. Um die für das Spritzgießen notwendige Fließfähigkeit zu gewährleisten, sind die Pulveranteile in spritzgießfähigen Verbundwerkstoffen auf maximal 65 Vol.-% begrenzt. Demgegenüber erfolgt beispielsweise bei axialem Verpressen die Verdichtung von rieselfähigen Pulvern nahezu ohne Materialfluß. Die Füllgrade dieser Verbundwerkstoffe liegen typischerweise bei 90-98 Vol.-%. Die durch axiales Verpressen von Pulvern geformten Bauteile zeichnen sich im Vergleich zu spritzgegossenen deshalb durch wesentlich höhere Permeabilitäten und höhere magnetische Feldstärken im Sättigungsbereich aus. Axiales Verpressen von Pulvern aus Reineisen oder Eisen-Nickel mit Duroplastharzen, beispielweise Epoxiden oder Phenolharzen hat jedoch den Nachteil, daß die bislang verwendeten thermoplastischen und duroplastischen Bindemittel bei erhöhter Temperatur in organischen Lösungsmitteln, beispielsweise Kraftstoffen für Verbrennungsmotoren, löslich sind, beziehungsweise stark aufquellen. Die entsprechenden Verbundbauteile ändern unter diesen Bedingungen ihre Abmessungen, verlieren ihre Festigkeit und versagen gänzlich. Es war bislang nicht möglich, entsprechende Verbundwerkstoffe mit hoher Temperatur- und Medienbeständigkeit, beispielsweise in organischen Lösungsmitteln, insbesondere Kraftstoffen für Verbrennungsmotoren, herzustellen. Ein weiteres Problem stellten bislang diejenigen Einsatzbedingungen dieser Bauteile dar, unter denen sowohl Thermoplaste als auch Duroplaste kein geeignetes Bindemittel mehr darstellen, da sie sich sonst vollständig zersetzen würden.For example, soft iron sheets have become too Lamella packs glued to anchor electric motors serve. The layer insulation only works in one Direction. From EP 0 540 504 B1 it is known soft magnetic powders with a plastic binder prepare and thus by an injection molding process to manufacture corresponding components. To the for that Injection molding to ensure necessary flowability are the powder parts in injection moldable Composite materials limited to a maximum of 65% by volume. In contrast, for example, in the case of axial pressing the compression of free-flowing powders almost without Material flow. The fill levels of these composite materials are typically 90-98% by volume. The through axial Pressing powder-shaped components are characterized in the Compared to injection molded, therefore, by essential higher permeabilities and higher magnetic field strengths in the Saturation range. Axial pressing of powders Pure iron or iron-nickel with thermosetting resins, for example, epoxies or phenolic resins, however Disadvantage that the previously used thermoplastic and thermosetting binder at elevated temperature in organic solvents, for example fuels for Internal combustion engines are soluble or strong swell. The corresponding composite components change under these conditions lose their dimensions Strength and fail completely. So far it has not been possible, corresponding composite materials with high Temperature and media resistance, for example in organic solvents, especially fuels for To manufacture internal combustion engines. Another Problem so far provided the operating conditions for this Components include both thermoplastics and Thermosets are no longer a suitable binder because otherwise they would decompose completely.

In dem Artikel von H. P. Baldus und M. Jansen in:
"Angewandte Chemie 1997, 109, Seite 338-394", werden moderne Hochleistungskeramiken beschrieben, die aus molekularen Vorläufern durch Pyrolyse gebildet werden und teilweise ebenfalls magnetische Eigenschaften aufweisen. Diese Keramiken sind äußerst temperatur- und lösungsmittelstabil. In the article by HP Baldus and M. Jansen in:
"Angewandte Chemie 1997, 109, pages 338-394" describes modern high-performance ceramics which are formed from molecular precursors by pyrolysis and in some cases also have magnetic properties. These ceramics are extremely temperature and solvent stable.

Aus WO 92/04127 ist ein Werkstoff mit einem Eisenpulver bekannt, wobei die Eisenpulverteilchen mit einem thermoplastischen Material beschichtet sind. Weiter ist diesem Werkstoff auch ein Bornitridpulver zugesetzt. Der beschriebene Werkstoff weist weichmagnetische Eigenschaften auf und ist formbar. From WO 92/04127 a material with an iron powder is known, the iron powder particles are coated with a thermoplastic material. This material is also a further Boron nitride powder added. The material described has soft magnetic properties and is malleable.

Vorteile der ErfindungAdvantages of the invention

Durch die Beschichtung von oberflächenphosphatisiertem Reineisenpulver mit Polyphtalamid ist es möglich, in vorteilhafter Weise den Anteil des Weichmagnetpulvers im Verbundwerkstoff zu erhöhen, eine gute Temperatur- und Lösemittelbeständigkeit des daraus hergestellten Formteiles zu erzielen.It is through the coating of surface phosphated pure iron powder with polyphthalamide possible to advantageously increase the proportion of soft magnetic powder in the composite material, to achieve good temperature and solvent resistance of the molded part produced therefrom.

In dem Verfahren zur Herstellung des weichmagnetischen Verbundwerkstoffes, wird das Polyphtalamid als thermoplastische Verbindung aus einer Lösung auf die Pulverkörner aufgebracht. Dabei werden die Pulverkörner in die Polymerlösung eingebracht und das Lösungsmittel unter ständiger Bewegung des Pulvers bei erhöhter Temperatur oder im Vakuum abgezogen. Dadurch erhalten die Pulverkörner auf einfache Weise einen dünnen Polymerüberzug ("coating"), so dass komplizierte Verfahrensprozesse entfallen.In the process for producing the soft magnetic composite material, this is Polyphtalamide as a thermoplastic compound from a solution applied to the powder grains. The powder grains are introduced into the polymer solution and the solvent under continuous movement of the powder at elevated temperature or in a vacuum. Thereby receive the powder grains in a simple manner a thin polymer coating ("coating"), so that complicated process processes are eliminated.

Vorteilhafte Ausgestaltungen und Weiterbildungen der Erfindung sind in den Unteransprüchen aufgeführt.Advantageous refinements and developments of the invention are in the subclaims listed.

Ausführungsbeispieleembodiments

Im folgenden werden nachstehende Abkürzungen verwendet:

  • PPA: Polyphthalamid
  • NMP: N-Methylpyrrolidon
    • The following abbreviations are used:
  • PPA: polyphthalamide
  • NMP: N-methylpyrrolidone

    • Kraftstoffbeständige Thermoplaste mit hoher Wärmeformbeständigkeit:Fuel-resistant thermoplastics with high heat resistance:

    Thermoplaste mit hoher Wärmeformbeständigkeit weisen im Vergleich zu niedrigschmelzenden Thermoplasten einen wesentlich geringeren kalten Fluß auf. Bei Verpressen eines Gemisches aus Magnetpulver mit geringen Anteilen an Thermoplastpulvern entsteht somit nur bei duktilen Thermoplastpulvern eine ausreichende Isolationsschicht um die Magnetteilchen. Darüberhinaus sind hochschmelzende Thermoplaste nicht als Pulver mit der notwendigen geringen Korngröße von < 5 Mikrometer im Handel erhältlich. Beide Schwierigkeiten werden durch die Erfindung dadurch umgegangen, daß das Magnetpulver vor dem axialen Verpressen mit einer Polymerlösung ummantelt wird. Falls die Löslichkeit des Polymers nur bei höherer Temperatur gegeben ist, muß das Lösen des Polymers und das Beschichten des Magnetpulvers zur Vermeidung einer thermooxidativen Schädigung des Thermoplastmaterials unter Schutzgas stattfinden.Thermoplastics with high heat resistance show in Compared to low-melting thermoplastics much less cold flow. When pressing one Mixture of magnetic powder with small proportions Thermoplastic powders are therefore only produced with ductile ones Thermoplastic powders around a sufficient insulation layer the magnetic particles. In addition, are high-melting Thermoplastics not as a powder with the necessary low Grain size of <5 microns commercially available. Both Difficulties are caused by the invention handled that the magnetic powder before the axial pressing is coated with a polymer solution. if the Solubility of the polymer only given at higher temperatures is the dissolving of the polymer and coating the Magnetic powder to avoid thermo-oxidative Damage to the thermoplastic material under protective gas occur.

    Ausführungsbeispielembodiment

    17,5 g eines handelsüblichen Granulates aus unverstärktem PPA (Amodel 1000 GR der Firma Amoco) wird grob aufgemahlen und in einem Sigma-Kneter mit 2500g ABM 100.32 (oberflächenphosphatiertes Reineisenpulver der Firma Höganäs) trockengemischt. Nach Zusatz von NMP wird so lange Stickstoff durch die Knetkammer geleitet, bis der Sauerstoff verdrängt ist. Anschließend wird der Stickstoffstrom abgestellt und die Kammer auf 200°C (Siedepunkt NMP: 204 °C) aufgeheizt. Nach einer Knetdauer von ca. 1 h, welche abhängig von der Größe des Thermoplastmaterials ist, hat sich das PPA in NMP vollständig gelöst. Daraufhin wird das Lösungsmittel durch erneutes Durchleiten von Schutzgas durch die Knetkammer abgezogen und in einem Kühler wieder kondensiert, der Kneter abgekühlt und das mit PPA beschichtete Magnetpulver entnommen. Letzte Lösungsmittelreste lassen sich durch Vakuumtrocknen entfernen.17.5 g of a commercial granulate made of unreinforced PPA (Amodel 1000 GR from Amoco) is roughly ground and in a Sigma kneader with 2500g ABM 100.32 (surface-phosphated pure iron powder from the company Höganäs) dry mixed. After adding NMP it will be so long Nitrogen passed through the kneading chamber until the oxygen is ousted. Then the nitrogen flow turned off and the chamber to 200 ° C (boiling point NMP: 204 ° C) heated. After a kneading time of approx. 1 h, which depends on the size of the thermoplastic material the PPA completely resolved in NMP. Then it will Solvent by passing protective gas through again the kneading chamber is withdrawn and placed in a cooler again condensed, the kneader cooled and with PPA coated magnetic powder removed. Latest Residual solvents can be dried by vacuum drying remove.

    An das kalte Verpressen des gecoateten Magnetpulvers schließt sich eine Wärmebehandlung des Preßlings unter Schutzgas über den Schmelzpunkt des Polymers hinaus (PPA, 320 °C) an. Die erhaltenen Proben weisen eine Festigkeit von ca. 80 N/mm2 und einen spezifischen elektrischen Widerstand von mindestens 400 µOhm*m auf. Eine bessere Entformbarkeit der verpreßten Bauteile aus der Formpresse erreicht man durch eine Oberflächenbehandlung des beschichteten Pulvers mit einem Gleitmittel. Das Gleitmittel wird in einen wesentlich geringeren Anteil als die Thermoplastbeschichtung zugegeben, um die Dichte der verpreßten Teile möglichst wenig zu verringern und es sollte derart flüchtig sein, daß es sich vor dem Aufschmelzen des Polymers bei der anschließenden Wärmebehandlung verflüchtigt und mit dem Polymer nicht chemisch reagiert. Beispiele für geeignete Gleitmittel sind beispielsweise Stanzöle, wie sie beim Stanzen von Blechen eingesetzt werden, oder Rapsölmethylester und Stearinsäureamid in Zusätzen von etwa 0.2% bezogen auf das Gewicht des Magnetpulvers.The cold pressing of the coated magnetic powder is followed by a heat treatment of the compact under protective gas above the melting point of the polymer (PPA, 320 ° C). The samples obtained have a strength of approx. 80 N / mm 2 and a specific electrical resistance of at least 400 µOhm * m. A better demoldability of the pressed components from the molding press is achieved by surface treatment of the coated powder with a lubricant. The lubricant is added in a much smaller proportion than the thermoplastic coating in order to reduce the density of the pressed parts as little as possible and it should be so volatile that it volatilizes before the polymer melts during the subsequent heat treatment and does not react chemically with the polymer , Examples of suitable lubricants are, for example, punch oils, such as those used for punching sheet metal, or rapeseed oil methyl ester and stearic acid amide in additions of about 0.2%, based on the weight of the magnetic powder.

    Claims (11)

    1. Soft-magnetic, formable composite material, including a powder which has soft-magnetic properties and a nonmagnetic thermoplastic compound, the grains of the powder being coated with the thermoplastic compound, characterized in that the thermoplastic compound is polyphthalamide, and the powder which has soft-magnetic properties is surface-phosphated pure iron powder.
    2. Composite material according to Claim 1, characterized in that the thermoplastic compound content is from 0.2 to 1% by weight, preferably 0.3 to 0.8% by weight, based on the total charge weight.
    3. Composite material according to Claim 1 or 2, characterized in that a lubricant is added to the composite material.
    4. Process for producing a composite material according to Claim 1, 2 or 3, characterized in that the surface-phosphated pure iron powder is coated with the polyphthalamide with the addition of a solvent, and in that the solvent is then extracted.
    5. Process according to Claim 4, characterized in that the solvent is N-methylpyrrolidone.
    6. Process according to Claim 4 or 5, characterized in that the solvent is added and extracted under inert gas or nitrogen.
    7. Process according to Claim 5, characterized in that the coating of the powder takes place by kneading at a temperature of 200°C.
    8. Process according to one of Claims 4 to 7, characterized in that the coated powder is cold-pressed.
    9. Process according to Claim 8, characterized in that the shaped and pressed body is heat-treated.
    10. Process according to one of Claims 4 to 9, characterized in that the pressing operation is followed by a heat treatment of the pressed body at above the melting point of the polyphthalamide.
    11. Process according to one of Claims 4 to 10, characterized in that a lubricant is added to the polyphthalamide-coated powder before the pressing operation.
    EP98948761A 1997-08-14 1998-08-11 Soft magnetic, deformable composite material and process for producing the same Expired - Lifetime EP0931322B1 (en)

    Priority Applications (1)

    Application Number Priority Date Filing Date Title
    EP00119956A EP1061534A3 (en) 1997-08-14 1998-08-11 Soft magnetic, deformable composite material and process for producing the same

    Applications Claiming Priority (3)

    Application Number Priority Date Filing Date Title
    DE19735271 1997-08-14
    DE19735271A DE19735271C2 (en) 1997-08-14 1997-08-14 Soft magnetic, mouldable composite material and process for its production
    PCT/DE1998/002297 WO1999009565A1 (en) 1997-08-14 1998-08-11 Soft magnetic, deformable composite material and process for producing the same

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    EP0931322A1 EP0931322A1 (en) 1999-07-28
    EP0931322B1 true EP0931322B1 (en) 2003-05-21

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    US (1) US6537389B1 (en)
    EP (2) EP0931322B1 (en)
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    DE (2) DE19735271C2 (en)
    WO (1) WO1999009565A1 (en)

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    JP2001504283A (en) 2001-03-27
    EP0931322A1 (en) 1999-07-28
    WO1999009565A1 (en) 1999-02-25
    EP1061534A2 (en) 2000-12-20
    DE19735271C2 (en) 2000-05-04
    DE19735271A1 (en) 1999-02-25
    EP1061534A3 (en) 2000-12-27
    US6537389B1 (en) 2003-03-25
    DE59808444D1 (en) 2003-06-26

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