EP0864666B1 - Method of manufacturing a tin plated strip - Google Patents
Method of manufacturing a tin plated strip Download PDFInfo
- Publication number
- EP0864666B1 EP0864666B1 EP98103664A EP98103664A EP0864666B1 EP 0864666 B1 EP0864666 B1 EP 0864666B1 EP 98103664 A EP98103664 A EP 98103664A EP 98103664 A EP98103664 A EP 98103664A EP 0864666 B1 EP0864666 B1 EP 0864666B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- tin
- base material
- effected
- layer
- manufacturing
- 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.)
- Expired - Lifetime
Links
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 238000000034 method Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 4
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 230000004907 flux Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical class [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 1
Images
Classifications
-
- 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 a method for Production of a band-shaped composite material with a base material Made of copper or a copper alloy and with a surface coating of pure tin or a tin 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 the type mentioned, in particular liability the tin layer on the base material made of copper or a copper alloy is improved while at the same time Formation of a tin layer of uniform thickness.
- 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
- US-A-5,077,094 does disclose a method of manufacture a band-shaped composite material with a Base material made of metal or a metal alloy, esp. Steel, and with a surface coating a tin alloy, in which the base material in a reducing gas atmosphere warms the base material tinned with a layer in the mm range and the composite material is cooled quickly.
- this is a one-sided coating a metal strip, esp. a steel strip, the also i.a. at a temperature of at least 400 ° C, especially for steel at at least 800 ° C must become.
- 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)
- Coating With Molten Metal (AREA)
- Electroplating Methods And Accessories (AREA)
- Laminated Bodies (AREA)
Description
Die Erfindung betrifft ein Verfahren zur Herstellung eines bandförmigen Verbundmaterials mit einem Grundmaterial aus Kupfer oder einer Kupferlegierung und mit einer oberflächenbeschichtung aus Reinzinn oder einer Zinnlegierung.The invention relates to a method for Production of a band-shaped composite material with a base material Made of copper or a copper alloy and with a surface coating of pure tin or a tin 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-A-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-A-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 to 900 ° C and at the and underside of the band by dipping in liquid tin Roll layers of tin of different thickness be generated.
Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren der genannten Art anzugeben, bei dem insbes. die Haftung der Zinnschicht auf dem Grundmaterial aus Kupfer oder einer Kupferlegierung verbessert wird, bei gleichzeitiger Ausbildung einer Zinnschicht gleichförmiger Dicke.The invention has for its object a method of the type mentioned, in particular liability the tin layer on the base material made of copper or a copper alloy is improved while at the same time Formation of a tin layer of uniform thickness.
Zur Lösung dieser Aufgabe werden erfindungsgemäß die in Anspruch 1 genannten Verfahrensschritte durch geführt.To achieve this object, those mentioned in claim 1 are inventively Process steps carried out.
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.
Die US-A-5.077.094 offenbart zwar ein Verfahren zur Herstellung eines bandförmigen Verbundmaterials mit einem Grundmaterial aus Metall oder einer Metallegierung, insbes. Stahl, und mit einer Oberflächenbeschichtung aus einer Zinnlegierung, bei dem das Grundmaterial in einer reduzierenden Gasatmosphäre erwärmt, das Grundmaterial mit einer Schicht im mm-Bereich verzinnt und das Verbundmaterial schnell abgekühlt wird.US-A-5,077,094 does disclose a method of manufacture a band-shaped composite material with a Base material made of metal or a metal alloy, esp. Steel, and with a surface coating a tin alloy, in which the base material in a reducing gas atmosphere warms the base material tinned with a layer in the mm range and the composite material is cooled quickly.
Dabei handelt es sich jedoch um die einseitige Beschichtung eines Metallbandes, insbes. eines Stahlbandes, die zudem i.a. bei einer Temperatur von mindestens 400 °C, insbes. bei Stahl bei mindestens 800 °C, durchgeführt werden muß.However, this is a one-sided coating a metal strip, esp. a steel strip, the also i.a. at a temperature of at least 400 ° C, especially for steel at at least 800 ° C must become.
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
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
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.
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)
- Method of manufacturing a strip-form composite material (10) having a base material (1) of copper or a copper alloy and having a surface coating of pure tin or a tin alloy, characterised in thata) the base material (1) is heated in a reducing gas atmosphere for from 3 to 30 s at a temperature T of from 80 to 300°C,b) the base material (1) is tin-plated with a layer in the µm range by being drawn through a tin or tin alloy bath (5), andc) the composite material (10) is rapidly cooled.
- Method according to claim 1, characterised in that the heating is effected inductively, conductively or convectively.
- Method according to claim 1 or 2, characterised in that the heating is effected at a temperature T of from 100 to 230°C.
- Method according to one or more of claims 1 to 3, characterised in that hydrogen or a hydrogen-nitrogen gas mixture is used as the reducing gas atmosphere.
- Method according to one or more of claims 1 to 4, characterised in that a layer of tin from 0.5 to 100 µm thick is applied.
- Method according to claim 5, characterised in that a layer of tin from 0.5 to 20 µm thick is applied.
- Method according to one or more of claims 1 to 6, characterised in that the cooling is effected at a rate of from 5 to 50°C/s.
- Method according to claim 7, characterised in that the cooling is effected by means of gas or water.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19710292 | 1997-03-13 | ||
| DE19710292A DE19710292C2 (en) | 1997-03-13 | 1997-03-13 | Process for the production of a tinned strip |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0864666A1 EP0864666A1 (en) | 1998-09-16 |
| EP0864666B1 true EP0864666B1 (en) | 2001-06-27 |
Family
ID=7823173
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP98103664A Expired - Lifetime EP0864666B1 (en) | 1997-03-13 | 1998-03-03 | Method of manufacturing a tin plated strip |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0864666B1 (en) |
| DE (2) | DE19710292C2 (en) |
| ES (1) | ES2159901T3 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104060210A (en) * | 2014-07-02 | 2014-09-24 | 天津百瑞杰焊接材料有限公司 | Dual-peak temperature tinning device with cold air blower |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (8)
| 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 |
| DE3663038D1 (en) * | 1985-03-04 | 1989-06-01 | Battelle Memorial Institute | Method for selectively forming at least a coating strip of a metal or alloy on a substrate of another 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 |
| 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 |
| JPH04107276A (en) * | 1990-08-28 | 1992-04-08 | Senju Metal Ind Co Ltd | Method and apparatus for producing laminated metal foil |
| US5429882A (en) * | 1993-04-05 | 1995-07-04 | The Louis Berkman Company | Building material coating |
| US5491036A (en) * | 1992-03-27 | 1996-02-13 | The Louis Berkman Company | Coated strip |
| DE4404699A1 (en) * | 1994-02-15 | 1995-08-17 | Kabelmetal Ag | Process for the production of tinned strips or sheets made of copper or a copper alloy |
-
1997
- 1997-03-13 DE DE19710292A patent/DE19710292C2/en not_active Expired - Fee Related
-
1998
- 1998-03-03 EP EP98103664A patent/EP0864666B1/en not_active Expired - Lifetime
- 1998-03-03 DE DE59800909T patent/DE59800909D1/en not_active Expired - Lifetime
- 1998-03-03 ES ES98103664T patent/ES2159901T3/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104060210A (en) * | 2014-07-02 | 2014-09-24 | 天津百瑞杰焊接材料有限公司 | Dual-peak temperature tinning device with cold air blower |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| DE19710292C2 (en) | 2001-05-03 |
| DE59800909D1 (en) | 2001-08-02 |
| EP0864666A1 (en) | 1998-09-16 |
| ES2159901T3 (en) | 2001-10-16 |
| DE19710292A1 (en) | 1998-09-17 |
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