EP1281461A1 - Process for preparing near net shape workpieces from light metal alloys that are difficult to work, and workpieces obtained thereby - Google Patents

Process for preparing near net shape workpieces from light metal alloys that are difficult to work, and workpieces obtained thereby Download PDF

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Publication number
EP1281461A1
EP1281461A1 EP01127413A EP01127413A EP1281461A1 EP 1281461 A1 EP1281461 A1 EP 1281461A1 EP 01127413 A EP01127413 A EP 01127413A EP 01127413 A EP01127413 A EP 01127413A EP 1281461 A1 EP1281461 A1 EP 1281461A1
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EP
European Patent Office
Prior art keywords
light metal
semi
workpieces
components
extrusion
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
EP01127413A
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German (de)
French (fr)
Other versions
EP1281461B1 (en
Inventor
Arlt Manfred
Bölster Alfred
Eiberger Anton
Franz Thomas
Heinritz Dr.Manfred
Laag Dr.Rainhard
Pohl Dr.Angelika
Schmid Jochem
Stock Otto
Subeck Gerard
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.)
Schwaebische Huettenwerke Automotive GmbH
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Schwaebische Huettenwerke Automotive GmbH
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=7692559&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP1281461(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Schwaebische Huettenwerke Automotive GmbH filed Critical Schwaebische Huettenwerke Automotive GmbH
Priority to HU0401206A priority Critical patent/HUP0401206A2/en
Priority to KR10-2004-7000580A priority patent/KR20040030054A/en
Priority to CA002438397A priority patent/CA2438397A1/en
Priority to DE10293319T priority patent/DE10293319D2/en
Priority to AT02754408T priority patent/ATE280647T1/en
Priority to EP20020754408 priority patent/EP1412113B1/en
Priority to ES02754408T priority patent/ES2231721T3/en
Priority to BR0211267-1A priority patent/BR0211267A/en
Priority to JP2003516724A priority patent/JP2004536232A/en
Priority to PCT/DE2002/002692 priority patent/WO2003011501A2/en
Priority to DE50201420T priority patent/DE50201420D1/en
Publication of EP1281461A1 publication Critical patent/EP1281461A1/en
Publication of EP1281461B1 publication Critical patent/EP1281461B1/en
Application granted granted Critical
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

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Classifications

    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B22F2003/206—Hydrostatic or hydraulic extrusion
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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 a method for the near-net-shape production of components or semi-finished products made of hard-to-cut light metal alloys and one made by the process Component or semi-finished product.
  • powder-metallurgical manufacturing is highly wear-resistant Components of the material delivered as powder, processed in the classic powder press process, sintered, heat treated and calibrated.
  • the peculiarity of such a highly wear-resistant the material is very distorted during sintering due to the necessary liquid phase sintering is caused.
  • the required dimensional and dimensional accuracy in the subsequent Calibration is restricted here.
  • the invention can also be referred to are used as a method for producing a sintered part from sintered light metal with variable Proportions of wear protection particles as an alloy component.
  • this is a method for producing Sintered molded parts made of light metals, preferably aluminum with 10 - 30% silicon content, Mg 0-3%, Cu 0-5%, Zn and Fe 0-7%.
  • Other light metals with changed Si components can be produced in this way.
  • hard material particle additives can also be used such as oxides, carbides and silicates with proportions of 0-30%.
  • the process advantageously combines the processes of cold or hot isostatic presses, Extrusion, sawing and calibration with preferably integrated faceting, if necessary Heat treatment and forging into a new whole.
  • the starting point of the invention is the powder metallurgical material Aluminum with Si fractions of approx. 14% which, among other things, is used in an application Sprocket against a steel chain, as a rotor and stator in a camshaft phasing system or an oil pump has excellent, previously unknown, good wear properties.
  • the precision that is customary in sintered parts is generated.
  • the big delays like in the classic sintering process described above no longer occur here.
  • the highly wear-resistant Material can be manufactured within narrow dimensional tolerances.

Abstract

Production of components and semi-finished products comprises: preparing a powder material made from light metal and alloying components, especially wear-resistant carriers; isostatically pressing into a molded body; and extruding close to the sintering temperature of the light metal. Preferred Features: The light metal is aluminum. The alloying components comprise 10-30 wt.% silicon, 0-3 wt.% magnesium, 0-5 wt.% copper, 0-7 wt.% zinc, and 0-7 wt.% iron. The wear-resistant carriers are selected from silicon and/or hard material particle additives, especially oxides, carbides and silicates in an amount of 0-30 wt.%.

Description

Die Erfindung betrifft ein Verfahren zur endkonturnahen Fertigung von Bauteilen bzw. Halbzeugen aus schwer zerspanbaren Leichtmetalllegierungen und ein durch das Verfahren hergestelltes Bauteil bzw. Halbzeug.The invention relates to a method for the near-net-shape production of components or semi-finished products made of hard-to-cut light metal alloys and one made by the process Component or semi-finished product.

Herkömmlicherweise wird bei der pulvermetallurgischen Herstellung von hochverschleißfesten Bauteilen der Werkstoff als Pulver angeliefert, im klassischen Pulverpressverfahren verarbeitet, gesintert, wärmebehandelt und kalibriert. Die Eigenart eines solchen hochverschleißfesten Werkstoffes ist jedoch ein starker Verzug beim Sintern, der durch die notwendige Flüssigphasensinterung hervorgerufen wird. Die geforderte Form- und Maßgenauigkeit beim anschließenden Kalibrieren ist hier eingeschränkt.Traditionally, powder-metallurgical manufacturing is highly wear-resistant Components of the material delivered as powder, processed in the classic powder press process, sintered, heat treated and calibrated. The peculiarity of such a highly wear-resistant However, the material is very distorted during sintering due to the necessary liquid phase sintering is caused. The required dimensional and dimensional accuracy in the subsequent Calibration is restricted here.

Um diesen Nachteil der oben genannten Werkstoffe im Punkt Genauigkeit zu beheben, wird erfindungsgemäß ein Verfahren gemäß dem Anspruch 1 und ein Bauteil bzw. Halbzeug gemäß dem Anspruch 11 zur Verfügung gestellt. Die Unteransprüche richten sich auf bevorzugte Ausführungsformen der Erfindung.To eliminate this disadvantage of the above materials in terms of accuracy, according to the invention a method according to claim 1 and a component or semi-finished product according to the claim 11 provided. The subclaims are directed towards preferred Embodiments of the invention.

Mit anderen Worten und in einer Ausführungsvariante kann die Erfindung auch bezeichnet werden als Verfahren zur Herstellung eines Sinterteiles aus Sinterleichtmetall mit veränderlichen Anteilen an Verschleißschutzpartikeln als Legierungsanteil.In other words and in an embodiment variant, the invention can also be referred to are used as a method for producing a sintered part from sintered light metal with variable Proportions of wear protection particles as an alloy component.

Gemäß einer Ausführungsform der Erfindung ist diese ein Verfahren zur Herstellung von Sinterformteilen aus Leichtmetallen, vorzugsweise Aluminium mit 10 - 30 % Siliziumanteilen, Mg 0 - 3 %, Cu 0 - 5 %, Zn und Fe 0 - 7 %. Auch andere Leichtmetalle mit veränderten Si-Anteilen sind so herstellbar. Alternativ zu Si als Verschleißträger können auch Hartstoffpartikelzusätze wie Oxide, Carbide und Silikate mit Anteilen von 0 - 30 % eingesetzt werden. According to one embodiment of the invention, this is a method for producing Sintered molded parts made of light metals, preferably aluminum with 10 - 30% silicon content, Mg 0-3%, Cu 0-5%, Zn and Fe 0-7%. Other light metals with changed Si components can be produced in this way. As an alternative to Si as a wear carrier, hard material particle additives can also be used such as oxides, carbides and silicates with proportions of 0-30%.

Das Verfahren vereinigt vorteilhafterweise die Verfahren Kalt- oder Heißisostatpressen, Strangpressen, Sägen und Kalibrieren mit vorzugsweise integriertem Facettieren, gegebenenfalls Warmbehandeln und Schmieden zu einer neuartigen Gesamtheit.The process advantageously combines the processes of cold or hot isostatic presses, Extrusion, sawing and calibration with preferably integrated faceting, if necessary Heat treatment and forging into a new whole.

Ausgangspunkt der Erfindung ist bei einer Ausführungsform der pulvermetallurgische Werkstoff Aluminium mit Si-Anteilen von ca. 14 % der unter anderem in einer Anwendung als Kettenrad gegen eine Stahlkette, als Rotor und Stator in einem Nockenwellenverstellersystem oder einer Ölpumpe hervorragende, bisher nicht gekannte, gute Verschleißeigenschaften besitzt.In one embodiment, the starting point of the invention is the powder metallurgical material Aluminum with Si fractions of approx. 14% which, among other things, is used in an application Sprocket against a steel chain, as a rotor and stator in a camshaft phasing system or an oil pump has excellent, previously unknown, good wear properties.

In bevorzugter Ausführung wird die Erfindung mit folgenden Verfahrensschritten umgesetzt:

  • Verpressen des Rohpulvers in einer Kalt- oder Heißisostatpresse zu einem Bolzen oder einer Form, die zum späteren Strangpressen geeignet ist. Vorteilhaft ist hier der Einsatz eines gepressten Bolzens aus Leichtmetallpulver, um im Gegensatz zu schmelzmetallurgisch hergestellten Bolzen ein gleichmäßigeres Gefüge ohne Lunker und Seigerungen etc. (mit gleichmäßig guter Si-Verteilung und damit guten Verschleißeigenschaften) zu erhalten;
  • Strangpressen des Bolzens nahe der Sintertemperatur des Leichtmetalls. Dabei Rekristallisation des Gefüges und Temperaturerhöhung bis zur optimalen Temperatur. Der Strangpressbolzen hat nun schon eine sehr gute Maßtoleranz, die für manche Bauteile schon genügen kann;
  • wenn die Maßtoleranz noch nicht ausreichend ist, um hochpräzise, einbaufertige Konturen zu erhalten, wird der stranggepresste Bolzen noch weiter nachkalibriert;
  • der Strangpressbolzen wird in das für das Bauteil später notwendige Maß in geeigneter Weise getrennt. Gegebenenfalls wird er dann noch warmbehandelt, einem Nachkalibrierarbeitsgang unterzogen und an definierten Kanten facettiert. Denkbar ist auch, den Strang als Ganzes in einer Art Ziehprozess auf genaue Maße zu bringen und danach zu trennen.
In a preferred embodiment, the invention is implemented with the following process steps:
  • Pressing the raw powder in a cold or hot isostatic press into a bolt or a mold that is suitable for later extrusion. It is advantageous to use a pressed bolt made of light metal powder in order to obtain a more uniform structure without blowholes and segregations etc. (with uniformly good Si distribution and thus good wear properties), in contrast to bolts produced using melt metallurgy;
  • Extrusion of the bolt near the sintering temperature of the light metal. Thereby recrystallization of the structure and temperature increase up to the optimal temperature. The extrusion bolt now has a very good dimensional tolerance, which may be sufficient for some components;
  • if the dimensional tolerance is not yet sufficient to obtain high-precision, ready-to-install contours, the extruded bolt is recalibrated;
  • the extrusion billet is separated in a suitable manner to the extent later required for the component. If necessary, it is then heat treated, subjected to a recalibration process and faceted on defined edges. It is also conceivable to bring the strand as a whole to exact dimensions in a kind of drawing process and then to separate it.

Erfindungsgemäß wird die bei Sinterteilen übliche Präzision erzeugt. Die großen Verzüge wie im oben beschriebenen klassischen Sinterverfahren treten hier nicht mehr auf. Der hochverschleißfeste Werkstoff ist in engen Maßtoleranzen herstellbar.According to the invention, the precision that is customary in sintered parts is generated. The big delays like in the classic sintering process described above no longer occur here. The highly wear-resistant Material can be manufactured within narrow dimensional tolerances.

Claims (11)

Verfahren zur endkonturnahen Fertigung von Bauteilen bzw. Halbzeugen aus schwer zerspanbaren Leichtmetalllegierungen mit den folgenden Schritten: ein Pulvermaterial, welches Leichtmetall und Legierungsbestandteile, insbesondere Verschleißträger aufweist, wird bereitgestellt; das Pulvermaterial wird isostatisch zu einem Formkörper gepresst; und der Formkörper wird einem Strangpressvorgang nahe der Sintertemperatur des Leichtmetalls unterzogen. Process for the near-net-shape production of components or semi-finished products made of hard-to-machine light metal alloys with the following steps: a powder material which has light metal and alloy components, in particular wear carriers, is provided; the powder material is pressed isostatically into a shaped body; and the molded body is subjected to an extrusion process near the sintering temperature of the light metal. Verfahren nach Anspruch 1, bei dem als Leichtmetall Aluminium verwendet wird.Method according to Claim 1, in which aluminum is used as the light metal. Verfahren nach Anspruch 1 oder 2, bei dem die Legierungsbestandteile Silizium, vorzugsweise 10 - 30 % Si, Magnesium, vorzugsweise 0 - 3 % Mg, Kupfer, vorzugsweise 0 - 5 % Cu, Zink, vorzugsweise 0 - 7 % Zn, Eisen, vorzugsweise 0 - 7 % Fe umfassen.The method of claim 1 or 2, wherein the alloy components are silicon, preferably 10-30% Si, magnesium, preferably 0-3% Mg, copper, preferably 0 - 5% Cu, zinc, preferably 0-7% Zn, iron, preferably 0-7% Fe. Verfahren nach einem der Ansprüche 1 bis 3, bei dem als Verschleißträger Silizium und/oder Hartstoffpartikelzusätze, insbesondere Oxide, Carbide und Silikate, bevorzugt mit Anteilen von 0-30% eingesetzt werden.Method according to one of claims 1 to 3, in which silicon as the wear carrier and / or hard particle additives, in particular oxides, carbides and silicates, are preferred with proportions of 0-30%. Verfahren nach einem der Ansprüche 1 bis 4, bei dem das Pulvermaterial heiß- bzw. kaltisostatisch zu dem Formkörper gepresst wird.Method according to one of claims 1 to 4, in which the powder material is hot or is cold isostatically pressed to the shaped body. Verfahren nach einem der Ansprüche 1 bis 5, bei dem das Strangpressen so durchgeführt wird, dass eine Rekristallisation des Gefüges und Temperaturerhöhung bis zur optimalen Temperatur eintritt.Method according to one of claims 1 to 5, in which the extrusion is carried out in this way is that a recrystallization of the structure and temperature increase to the optimum Temperature occurs. Verfahren nach einem der Ansprüche 1 bis 6, bei dem der gepresste Strang nach dem Strangpressen vereinzelt wird, insbesondere durch einen Schneidvorgang zu einhöhigen Bauteilen bzw. Halbzeugen vereinzelt wird. Method according to one of claims 1 to 6, wherein the pressed strand after the Extrusion is isolated, in particular by a cutting process Components or semi-finished products is isolated. Verfahren nach einem der Ansprüche 1 bis 7, bei dem nach der Vereinzelung eine Weiterverarbeitung bzw. Kalibrierung des Bauteils bzw. Halbzeuges durchgeführt wird, wenn vorgegebene Eigenschaften bzw. Maßtoleranzen noch nicht erreicht sind, insbesondere durch eine Nachkalibrierung und/oder eine Facettierung.Method according to one of claims 1 to 7, in which after the separation a Further processing or calibration of the component or semi-finished product is carried out, if specified properties or dimensional tolerances have not yet been achieved, in particular through recalibration and / or faceting. Verfahren nach einem der Ansprüche 1 bis 7, bei dem das Strangpressprodukt durch einen Ziehvorgang weiterverarbeitet wird, wenn vorgegebene Eigenschaften bzw. Maßtoleranzen noch nicht erreicht sind, worauf dann eine Vereinzelung erfolgt.Method according to one of claims 1 to 7, wherein the extruded product by a drawing process is further processed if specified properties or Dimensional tolerances have not yet been reached, whereupon a separation takes place. Verfahren nach einem der Ansprüche 1 bis 9, bei dem das Strangpressprodukt wärmebehandelt wird.A method according to any one of claims 1 to 9, in which the extruded product is heat treated becomes. Bauteil bzw. Halbzeug, dadurch gekennzeichnet, dass es durch ein Verfahren nach einem der Ansprüche 1 bis 10 hergestellt ist.Component or semi-finished product, characterized in that it is produced by a method according to one of claims 1 to 10.
EP01127413A 2001-07-20 2001-11-23 Process for preparing near net shaped workpieces from light metal alloys that are difficult to work Revoked EP1281461B1 (en)

Priority Applications (11)

Application Number Priority Date Filing Date Title
ES02754408T ES2231721T3 (en) 2001-07-20 2002-07-22 SINTERED METAL PARTS WITH HOMOGENOUS DISTRIBUTION OF COMPONENTS THAT ARE NOT FOUND HOMOGENOUSLY, AS WELL AS PROCEDURES FOR MANUFACTURING.
BR0211267-1A BR0211267A (en) 2001-07-20 2002-07-22 Sintered metal parts with homogeneously distributed molten components as well as processes for their manufacture
CA002438397A CA2438397A1 (en) 2001-07-20 2002-07-22 Sintered metal parts with homogeneous distribution of non-homogeneously melting components and method for the production thereof
DE10293319T DE10293319D2 (en) 2001-07-20 2002-07-22 Sintered metal parts with homogeneous distribution of non-homogeneously melting components, and process for their production
AT02754408T ATE280647T1 (en) 2001-07-20 2002-07-22 SINTERED METAL PARTS WITH HOMOGENEOUS DISTRIBUTION OF NON-HOMOGENEOUSLY MELTING COMPONENTS, AND METHOD FOR THEIR PRODUCTION
EP20020754408 EP1412113B1 (en) 2001-07-20 2002-07-22 Sinter metal parts with homogeneous distribution of non-homogeneously melting components and method for the production thereof
HU0401206A HUP0401206A2 (en) 2001-07-20 2002-07-22 Sinter metal parts with homogeneous distribution of non-homogeneously melting components and method for the production thereof
KR10-2004-7000580A KR20040030054A (en) 2001-07-20 2002-07-22 Sinter metal parts with homogeneous distribution of non-homogeneously melting components and method for production thereof
JP2003516724A JP2004536232A (en) 2001-07-20 2002-07-22 Sintered metal parts having a homogeneous distribution of components that melt inhomogeneously and a method of making the same
PCT/DE2002/002692 WO2003011501A2 (en) 2001-07-20 2002-07-22 Sinter metal parts with homogeneous distribution of non-homogeneously melting components and method for the production thereof
DE50201420T DE50201420D1 (en) 2001-07-20 2002-07-22 SINTER METAL PARTS WITH HOMOGENIC DISTRIBUTION OF NON-HOMOGENIC MELTING COMPONENTS, AND METHOD FOR THEIR PRODUCTION

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10135485 2001-07-20
DE10135485A DE10135485A1 (en) 2001-07-20 2001-07-20 Process for the near-net-shape production of components or semi-finished products made of light-metal alloys that are difficult to machine, and component or semi-finished product produced by the method

Publications (2)

Publication Number Publication Date
EP1281461A1 true EP1281461A1 (en) 2003-02-05
EP1281461B1 EP1281461B1 (en) 2004-09-01

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Application Number Title Priority Date Filing Date
EP01127413A Revoked EP1281461B1 (en) 2001-07-20 2001-11-23 Process for preparing near net shaped workpieces from light metal alloys that are difficult to work
EP20020754408 Revoked EP1412113B1 (en) 2001-07-20 2002-07-22 Sinter metal parts with homogeneous distribution of non-homogeneously melting components and method for the production thereof

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP20020754408 Revoked EP1412113B1 (en) 2001-07-20 2002-07-22 Sinter metal parts with homogeneous distribution of non-homogeneously melting components and method for the production thereof

Country Status (11)

Country Link
US (1) US20040208772A1 (en)
EP (2) EP1281461B1 (en)
JP (1) JP2004536232A (en)
KR (1) KR20040030054A (en)
AT (2) ATE275015T1 (en)
BR (1) BR0211267A (en)
CA (1) CA2438397A1 (en)
DE (4) DE10135485A1 (en)
ES (2) ES2227044T3 (en)
HU (1) HUP0401206A2 (en)
WO (1) WO2003011501A2 (en)

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DE50103474D1 (en) 2004-10-07
ES2231721T3 (en) 2005-05-16
ES2227044T3 (en) 2005-04-01
WO2003011501A2 (en) 2003-02-13
ATE280647T1 (en) 2004-11-15
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KR20040030054A (en) 2004-04-08
WO2003011501A3 (en) 2003-05-01
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HUP0401206A2 (en) 2004-10-28
DE50201420D1 (en) 2004-12-02
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EP1281461B1 (en) 2004-09-01
US20040208772A1 (en) 2004-10-21

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