EP0864666A1 - Method of manufacturing a tin plated strip - Google Patents

Method of manufacturing a tin plated strip Download PDF

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Publication number
EP0864666A1
EP0864666A1 EP98103664A EP98103664A EP0864666A1 EP 0864666 A1 EP0864666 A1 EP 0864666A1 EP 98103664 A EP98103664 A EP 98103664A EP 98103664 A EP98103664 A EP 98103664A EP 0864666 A1 EP0864666 A1 EP 0864666A1
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EP
European Patent Office
Prior art keywords
tin
base material
application
alloy
copper
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
EP98103664A
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German (de)
French (fr)
Other versions
EP0864666B1 (en
Inventor
Gert Dipl.-Ing. Dr.rer.nat. Müller
Leszek Dr.-Ing. Poletek
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.)
Wieland Werke AG
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Wieland Werke AG
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Publication of EP0864666A1 publication Critical patent/EP0864666A1/en
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Publication of EP0864666B1 publication Critical patent/EP0864666B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/08—Tin or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/003—Apparatus
    • C23C2/0038—Apparatus characterised by the pre-treatment chambers located immediately upstream of the bath or occurring locally before the dipping process
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C23C2/022—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating
    • C23C2/0222—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating in a reactive atmosphere, e.g. oxidising or reducing atmosphere

Definitions

  • the invention relates to the use of a method for Production of a tinned tape on a base material made of copper or a copper alloy.
  • tin-plating Bands made of copper materials and. a.
  • Connectors, cable lugs, contact parts, solder thread and Battery clips used.
  • the processors set high quality standards both the basic material and the Covers. The quality of tinned strips depends crucially from the initial state of the basic material, from the careful Surface preparation before tinning and from the proper one Execution of the tinning process.
  • This process also creates a slag as Product of the chemical reaction between the flux and the oxides that negatively affect the production process can. Delayed foot remnants, e.g. B. chlorides in certain cases on the tinned surface Form stains.
  • the invention has for its object a method of for the purpose of improving the liability of Vary the tin layer on the base material so that it is in simply on a base material made of copper or a Copper alloy more uniform when forming a tin layer Thickness can be applied.
  • the method according to the invention surprisingly adequate deoxidation and activation achieved the strip surface, so that a full-surface tin layer defined thickness can be applied.
  • This Layer is also dense, i. H. there are no continuous Pores on. Forms between the strip surface and the tin layer an intermetallic phase (IMP), which is good Adhesion resistance of the tin layer on the strip surface worries.
  • IMP intermetallic phase
  • the invention is explained in more detail using the following exemplary embodiment.
  • the figure shows schematically the process sequence according to the invention in the tinning of a strip-shaped base material 1 made of copper or a copper alloy.
  • the basic material 1 running from a decoiler 2 is heated to a temperature T of about 200 ° C. after passing through a deflection roller 3 in a prechamber 4 while maintaining a hydrogen-nitrogen atmosphere and immediately thereafter through a tin bath 5 (temperature: 240 ° C.) guided with pulley 6. Excess tin is retained by the stripping 7.
  • the composite material 10 arrives at a reel 11.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Coating With Molten Metal (AREA)
  • Laminated Bodies (AREA)

Abstract

The method for producing a compound strip (10) with a base strip (1) consisting of a metal or an alloy, and a coating consisting of tin or a tin alloy consists of the following steps; a) the base material is heated in a reducing atmosphere; b) it is then coated with a layer within a mu m range; c) the resulting compound material is rapidly cooled. When the base strip consists of copper or a copper alloy, the step a) involves heating to 80-300 degrees C for 3-30 s. The step b) is carried out by pulling the base strip through a bath (5) with a tin alloy.

Description

Die Erfindung betrifft die Anwendung eines Verfahrens zur Herstellung eines verzinnten Bandes auf ein Grundmaterial aus Kupfer oder einer Kupferlegierung.The invention relates to the use of a method for Production of a tinned tape on a base material made of copper or a copper alloy.

In der elektrotechnischen Industrie werden feuerverzinnte Bänder aus Kupferwerkstoffen u. a. für die Herstellung von Steckverbindern, Kabelschuhen, Kontaktteilen, Lötfaden und Batterieklemmen verwendet. Die Verarbeiter stellen hohe Qualitätsansprüche sowohl an das Grundmaterial als auch an die Überzüge. Die Qualität verzinnter Bänder hängt entscheidend vom Ausgangszustand des Grundmaterials, von der sorgfältigen Oberflächenvorbereitung vor dem Verzinnen und von der sachgemäßen Ausführung des Verzinnungsvorganges ab.In the electrotechnical industry, tin-plating is used Bands made of copper materials and. a. For the production of Connectors, cable lugs, contact parts, solder thread and Battery clips used. The processors set high quality standards both the basic material and the Covers. The quality of tinned strips depends crucially from the initial state of the basic material, from the careful Surface preparation before tinning and from the proper one Execution of the tinning process.

Es hat sich gezeigt, daß die Verzinnung von Kupferbändern mit herkömmlichen Mitteln und Methoden, wie z. B. Einsatz von Flußmitteln, bei höchsten Qualitätsansprüchen nicht immer zufriedenstellend und darüber hinaus noch umweltbelastend sein kann, weil z. B. Ammoniumchloride, Zinkchloride oder bromidhaltige Lösungen zum Einsatz gelangen.It has been shown that the tinning of copper strips with conventional means and methods, such as. B. Use of flux, not always with the highest quality standards satisfactory and also polluting can be because z. B. ammonium chlorides, zinc chlorides or solutions containing bromide are used.

Außerdem entsteht bei diesem Verfahren eine Schlacke als Produkt der chemischen Reaktion zwischen dem Flußmittel und den Oxiden, die den Produktionsprozeß negativ beeinflussen kann. Verschleppte Fußmittelrückstände, z. B. Chloride, können in bestimmten Fällen auf der verzinnten Oberfläche Flecken bilden. This process also creates a slag as Product of the chemical reaction between the flux and the oxides that negatively affect the production process can. Delayed foot remnants, e.g. B. chlorides in certain cases on the tinned surface Form stains.

Weiterhin ist aus der US-PS 2.937.108 ein Verfahren zur Verzinnung von Stahlband als Grundmaterial bekannt, bei dem das Stahlband in einer reduzierenden Gasatmosphäre auf eine Temperatur von 900 °C erwärmt werden muß und bei dem auf Ober- und Unterseite des Bandes durch in flüssiges Zinn eintauchende Walzen jeweils Zinnschichten unterschiedlicher Dicke erzeugt werden.Furthermore, a process for tinning is known from US Pat. No. 2,937,108 of steel strip known as the base material, in which the Steel strip in a reducing gas atmosphere to one temperature must be heated from 900 ° C and at the top and Underside of the band by immersing it in liquid tin Roll layers of tin of different thickness be generated.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren der genannten Art zum Zweck der Verbesserung der Haftung der Zinnschicht auf dem Grundmaterial so zu variieren, daß es in einfacher Weise auf ein Grundmaterial aus Kupfer oder einer Kupferlegierung bei Ausbildung einer Zinnschicht gleichförmiger Dicke angewandt werden kann.The invention has for its object a method of for the purpose of improving the liability of Vary the tin layer on the base material so that it is in simply on a base material made of copper or a Copper alloy more uniform when forming a tin layer Thickness can be applied.

Zur Lösung dieser Aufgabe werden die in Anspruch 1 genannten Verfahrensschritte angewendet.To solve this problem, those mentioned in claim 1 Process steps applied.

Durch das erfindungsgemäße Verfahren werden überraschenderweise eine hinreichende Desoxidation und eine Aktivierung der Bandoberfläche erzielt, so daß eine vollflächige Zinnschicht definierter Dicke aufgebracht werden kann. Diese Schicht ist auch dicht, d. h. es treten keine durchgehenden Poren auf. Zwischen Bandoberfläche und der Zinnschicht bildet sich eine intermetallische Phase (IMP) aus, die für gute Haftungsbeständigkeit der Zinnschicht auf der Bandoberfläche sorgt.The method according to the invention surprisingly adequate deoxidation and activation achieved the strip surface, so that a full-surface tin layer defined thickness can be applied. This Layer is also dense, i. H. there are no continuous Pores on. Forms between the strip surface and the tin layer an intermetallic phase (IMP), which is good Adhesion resistance of the tin layer on the strip surface worries.

Weitere bevorzugte Ausführungsformen des Verfahrens ergeben sich aus den Verfahrensschritten nach den Ansprüchen 2 bis 8.Further preferred embodiments of the method result itself from the process steps according to claims 2 to 8th.

Die Erfindung wird anhand des folgenden Ausführungsbeispiels näher erläutert.
Die Figur zeigt schematisch den erfindungsgemäßen Verfahrensablauf bei der Verzinnung eines bandförmigen Grundmaterials 1 aus Kupfer oder einer Kupferlegierung. Das von einem Abhaspel 2 ablaufende Grundmaterial 1 wird nach Passieren einer Umlenkrolle 3 in einer Vorkammer 4 unter Einhaltung einer Wasserstoff-Stickstoff-Atmosphäre auf eine Temperatur T von etwa 200 °C erwärmt und unmittelbar anschließend durch ein Zinnbad 5 (Temperatur: 240 °C) mit Umlenkrolle 6 geführt. Überflüssiges Zinn wird von der Abstreifung 7 zurückgehalten. Nach Passieren einer Kühlstrecke 8 und einer Umlenkrolle 9 gelangt das Verbundmaterial 10 (verzinntes Band) auf einen Aufhaspel 11.The invention is explained in more detail using the following exemplary embodiment.
The figure shows schematically the process sequence according to the invention in the tinning of a strip-shaped base material 1 made of copper or a copper alloy. The basic material 1 running from a decoiler 2 is heated to a temperature T of about 200 ° C. after passing through a deflection roller 3 in a prechamber 4 while maintaining a hydrogen-nitrogen atmosphere and immediately thereafter through a tin bath 5 (temperature: 240 ° C.) guided with pulley 6. Excess tin is retained by the stripping 7. After passing through a cooling section 8 and a deflection roller 9, the composite material 10 (tinned strip) arrives at a reel 11.

Zahlenbeispiel: Numerical example :

Es wurden vier Bänder aus Kupferwerkstoffen unterschiedlicher Abmessung gemäß folgender Tabelle in einer Vorkammer 4 konvektiv auf eine Temperatur von etwa 200 °C erwärmt (Atmosphäre: 90/10 Stickstoff-Wasserstoff-Gasgemisch / 10 % H2 in N2) und durch ein Zinnbad 5 aus Reinzinn geführt. In der Tabelle sind gleichzeitig die eingehaltenen Bandgeschwindigkeiten v angegeben. Legierung Abmessung (mm) v (m/min) Sn (Dicke D) (µm) CuSn6 (C 51900) 0,35 x 200 40 4 - 6 CuFe2P (C 19400) 0,25 x 180 45 ca 6 CuNi2Si (C 70250) 0,15 x 180 80 3 - 4 CuFe2P (C 19400) 0,25 x 120 55 4 - 6 Four strips of copper materials of different dimensions were convectively heated in a prechamber 4 to a temperature of about 200 ° C (atmosphere: 90/10 nitrogen-hydrogen gas mixture / 10% H 2 in N 2 ) and through a tin bath 5 made of pure tin. The table also shows the belt speeds v observed. alloy Dimension (mm) v (m / min) Sn (thickness D) (µm) CuSn6 (C 51900) 0.35 x 200 40 4 - 6 CuFe2P (C 19400) 0.25 x 180 45 about 6 CuNi2Si (C 70250) 0.15 x 180 80 3-4 CuFe2P (C 19400) 0.25 x 120 55 4 - 6

Es zeigte sich eine einwandfreie Benetzung der Bänder. Es wurden Zinnschichtdicken D gemäß der Tabelle erzielt.A perfect wetting of the tapes was shown. It tin layer thicknesses D according to the table were achieved.

Claims (8)

Anwendung eines Verfahrens zur Herstellung eines bandförmigen Verbundmaterials (10) mit einem Grundmaterial (1) aus Metall oder einer Metallegierung und mit einer Oberflächenbeschichtung aus Reinzinn oder einer Zinnlegierung,
bei dem a) das Grundmaterial (1) in einer reduzierenden Gasatmosphäre erwärmt, b) das Grundmaterial (1) mit einer Schicht im µm-Bereich verzinnt und c) das Verbundmaterial (10) schnell abgekühlt wird, auf ein Grundmaterial (1) aus Kupfer oder einer Kupferlegierung zum Zweck der Verbesserung der Haftung der Zinn- oder Zinnlegierungsschicht auf dem Grundmaterial (1), mit der Maßgabe, daß im Verfahrensschritt a) das Grundmaterial (1) für 3 bis 30 s auf eine Temperatur T von 80 bis 300 °C erwärmt wird und daß im Verfahrensschritt b) das Grundmaterial (1) durch ein Zinn- oder Zinnlegierungsbad (5) gezogen wird. Application of a method for producing a band-shaped composite material (10) with a base material (1) made of metal or a metal alloy and with a surface coating made of pure tin or a tin alloy,
in which a) the base material (1) is heated in a reducing gas atmosphere, b) the base material (1) tinned with a layer in the µm range and c) the composite material (10) is rapidly cooled, to a base material (1) made of copper or a copper alloy for the purpose of improving the adhesion of the tin or tin alloy layer to the base material (1), with the proviso that that in process step a) the base material (1) is heated to a temperature T of 80 to 300 ° C. for 3 to 30 s and that in process step b) the base material (1) is drawn through a tin or tin alloy bath (5). Anwendung des Verfahrens nach Anspruch 1 für den Zweck nach Anspruch 1, dadurch gekennzeichnet, daß die Erwärmung induktiv, konduktiv oder konvektiv erfolgt. Application of the method according to claim 1 for the purpose according to claim 1, characterized in that the heating is inductive, conductive or convective. Anwendung des Verfahrens nach Anspruch 1 oder 2 für den Zweck nach Anspruch 1, dadurch gekennzeichnet, daß die Erwärmung auf eine Temperatur T von 100 bis 230 °C erfolgt. Application of the method according to claim 1 or 2 for the purpose according to claim 1, characterized in that the heating to a temperature T of 100 to 230 ° C takes place. Anwendung des Verfahrens nach einem oder mehreren der Ansprüche 1 bis 3 für den Zweck nach Anspruch 1, dadurch gekennzeichnet, daß als reduzierende Gasatmosphäre Wasserstoff oder ein Wasserstoff-Stickstoff-Gasgemisch verwendet wird. Application of the method according to one or more of claims 1 to 3 for the purpose according to claim 1, characterized in that that hydrogen or a hydrogen-nitrogen gas mixture is used as the reducing gas atmosphere. Anwendung des Verfahrens nach einem oder mehreren der Ansprüche 1 bis 4 für den Zweck nach Anspruch 1, dadurch gekennzeichnet, daß eine 0,5 bis 100 µm dicke Zinnschicht aufgebracht wird. Application of the method according to one or more of claims 1 to 4 for the purpose according to claim 1, characterized in that that a 0.5 to 100 µm thick tin layer is applied. Anwendung des Verfahrens nach Anspruch 5 für den Zweck nach Anspruch 1, dadurch gekennzeichnet, daß eine 0,5 bis 20 µm dicke Zinnschicht aufgebracht wird. Application of the method according to claim 5 for the purpose according to claim 1, characterized in that that a 0.5 to 20 µm thick tin layer is applied. Anwendung des Verfahrens nach einem oder mehreren der Ansprüche 1 bis 6 für den Zweck nach Anspruch 1, dadurch gekennzeichnet, daß die Abkühlung mit einer Geschwindigkeit von 5 bis 50 °C/s erfolgt. Application of the method according to one or more of claims 1 to 6 for the purpose of claim 1, characterized in that that the cooling takes place at a speed of 5 to 50 ° C / s. Anwendung des Verfahrens nach Anspruch 7 für den Zweck nach Anspruch 1, dadurch gekennzeichnet, daß die Abkühlung mittels Gas oder Wasser erfolgt. Application of the method according to claim 7 for the purpose according to claim 1, characterized in that the cooling takes place by means of gas or water.
EP98103664A 1997-03-13 1998-03-03 Method of manufacturing a tin plated strip Expired - Lifetime EP0864666B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19710292A DE19710292C2 (en) 1997-03-13 1997-03-13 Process for the production of a tinned strip
DE19710292 1997-03-13

Publications (2)

Publication Number Publication Date
EP0864666A1 true EP0864666A1 (en) 1998-09-16
EP0864666B1 EP0864666B1 (en) 2001-06-27

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EP (1) EP0864666B1 (en)
DE (2) DE19710292C2 (en)
ES (1) ES2159901T3 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115449737A (en) * 2022-09-26 2022-12-09 先之科半导体科技(东莞)有限公司 Material belt straightening assembly for assisting diode to invade tin charging clamp

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104060210B (en) * 2014-07-02 2016-05-11 天津百瑞杰焊接材料有限公司 With the bimodal temperature tin equipment of air-cooler

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4719962A (en) * 1985-03-04 1988-01-19 Battelle Memorial Institute Method for selectively forming at least one coating strip consisting of a metal or alloy on a substrate consisting of another metal
US5077094A (en) * 1989-12-11 1991-12-31 Battelle Development Corp. Process for applying a metal coating to a metal strip by preheating the strip in a non-oxidizing atmosphere, passing the strip through a melt pool of the metal coating material, and rapidly cooling the back surface of the strip
EP0667403A1 (en) * 1994-02-15 1995-08-16 KM Europa Metal Aktiengesellschaft Method of manufacturing tin plated strips or plates of copper or copper alloy
DE19501747A1 (en) * 1994-06-15 1995-12-21 Berkman Louis Co Coated metal material, in particular building material
US5491036A (en) * 1992-03-27 1996-02-13 The Louis Berkman Company Coated strip

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1446228B2 (en) * 1960-09-03 1970-05-27 Robinson, Myron Lee, Monterey Park, Calif. (V.St.A.) Method and apparatus for coating the inner surface of windable metal tubes with a metal
JP2727184B2 (en) * 1987-07-11 1998-03-11 臼井国際産業株式会社 Method for producing metal tube having inner surface coated with tin or tin-based alloy
JPH04107276A (en) * 1990-08-28 1992-04-08 Senju Metal Ind Co Ltd Method and apparatus for producing laminated metal foil

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4719962A (en) * 1985-03-04 1988-01-19 Battelle Memorial Institute Method for selectively forming at least one coating strip consisting of a metal or alloy on a substrate consisting of another metal
US5077094A (en) * 1989-12-11 1991-12-31 Battelle Development Corp. Process for applying a metal coating to a metal strip by preheating the strip in a non-oxidizing atmosphere, passing the strip through a melt pool of the metal coating material, and rapidly cooling the back surface of the strip
US5491036A (en) * 1992-03-27 1996-02-13 The Louis Berkman Company Coated strip
EP0667403A1 (en) * 1994-02-15 1995-08-16 KM Europa Metal Aktiengesellschaft Method of manufacturing tin plated strips or plates of copper or copper alloy
DE19501747A1 (en) * 1994-06-15 1995-12-21 Berkman Louis Co Coated metal material, in particular building material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115449737A (en) * 2022-09-26 2022-12-09 先之科半导体科技(东莞)有限公司 Material belt straightening assembly for assisting diode to invade tin charging clamp
CN115449737B (en) * 2022-09-26 2023-07-28 先之科半导体科技(东莞)有限公司 Material belt straightening assembly for auxiliary diode tin-immersing charging fixture

Also Published As

Publication number Publication date
DE19710292A1 (en) 1998-09-17
ES2159901T3 (en) 2001-10-16
DE59800909D1 (en) 2001-08-02
EP0864666B1 (en) 2001-06-27
DE19710292C2 (en) 2001-05-03

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