EP0704558B1 - Zelle zur kontinuierlichen Elektrobeschichtung von Metalllegierungen - Google Patents

Zelle zur kontinuierlichen Elektrobeschichtung von Metalllegierungen Download PDF

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Publication number
EP0704558B1
EP0704558B1 EP95401908A EP95401908A EP0704558B1 EP 0704558 B1 EP0704558 B1 EP 0704558B1 EP 95401908 A EP95401908 A EP 95401908A EP 95401908 A EP95401908 A EP 95401908A EP 0704558 B1 EP0704558 B1 EP 0704558B1
Authority
EP
European Patent Office
Prior art keywords
strip
anode
edge
alloy
electroplating
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
Application number
EP95401908A
Other languages
English (en)
French (fr)
Other versions
EP0704558A1 (de
Inventor
Franco Delfrate
Claude Arnoux
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.)
Sollac SA
Original Assignee
Sollac SA
Lorraine de Laminage Continu SA SOLLAC
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sollac SA, Lorraine de Laminage Continu SA SOLLAC filed Critical Sollac SA
Publication of EP0704558A1 publication Critical patent/EP0704558A1/de
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Publication of EP0704558B1 publication Critical patent/EP0704558B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C25D7/0671—Selective plating
    • C25D7/0678—Selective plating using masks
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/22—Electroplating: Baths therefor from solutions of zinc
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/06—Wires; Strips; Foils
    • C25D7/0614—Strips or foils
    • C25D7/0642—Anodes

Definitions

  • the invention relates to an electroplating cell for the continuous coating of metal strips with a layer of metal alloy.
  • the strip is generally passed through an installation which comprises a succession of electroplating cells, each cell contributing to the formation of a portion of the layer, or "sublayer"; the stack of sub-layers forms the alloy layer.
  • such a sheet coated by electrodeposition with a layer of metal alloy and then painted, in particular by cataphoresis does not exhibit sufficient resistance to the gravel test, in particular for automotive applications;
  • the gravel test consists of projecting solid gravel onto the painted sheet and evaluating the resistance to gravel, for example by counting the number of impacts on the sheet where the paint has been torn off; after the graveling test of such a painted sheet metal, numerous flaking of paint is observed and it is found that the tearing off of the paint flakes actually occurs in the thickness of the coating or of the electrodeposited layer.
  • the object of the invention is to improve the quality, in particular the strength mechanical, coatings of metal alloys deposited continuously by electrodeposition on metal strips.
  • the invention therefore also aims to limit the aforementioned drawbacks concerning the shaping and painting of the metal strips or sheets coated with alloy.
  • the subject of the invention is an electroplating cell for the continuous coating of a metal strip, in particular with a layer of metallic alloy, comprising an electrolysis tank containing an electroplating bath, at least one anode immersed in said bath and having an active surface delimited by edges, means for passing the strip in the bath opposite said active surface from one edge of said surface to another opposite edge of the same surface, said means defining a path of strip running, and means for passing an electric current between said anode and said running strip serving as a cathode, characterized in that said active surface of each submerged anode is bordered on each of said two opposite edges by a mask having, along said corresponding edge and facing said travel path, an electrically insulating surface, closer to said travel path that said rim, said mask projecting towards the outside of said active anode surface with a width called overflow, measured along the direction of travel, at least equal to the distance which separates said edge from said travel path, and said mask covering the edge of said active anode surface over a width known as covering
  • the invention also relates to an electroplating installation for the continuous coating of a metal strip, in particular with a layer of metallic alloy, comprising a cascade succession of cells according to the invention.
  • the invention also relates to the use of electroplating cells according to the invention for the continuous coating of metal strips with a layer of metal alloy.
  • the subject of the invention is also a method of coating a metal strip by electrodeposition of a metal alloy, in particular based on zinc, using an installation comprising several cells according to the invention arranged in cascade in which said strip is passed successively through said cells of the installation, an electric current is circulated between the anodes of the cells and said moving strip, characterized in that the running speed of said strip in the installation is greater than 50 m / minute and / or the density of the electric current flowing between the anodes of the cells and said strip is greater than 50 A / dm2.
  • the plating installation comprises several identical plating cells arranged in cascade.
  • the first cell of the installation is represented in FIG. 1, designated as a whole by the reference 1, and comprises an electrolysis tank 2 containing an electroplating bath S, means ensuring the movement of a metal strip B in the bath S and defining a strip running path, and, positioned successively under the strip running path and facing it, two anodes 3; cell 1 also comprises means for circulating an electric current between said anodes 3 and strip B running as cathode, which are not shown here.
  • the electroplating cell can comprise a single anode or more than two successive anodes.
  • the running means comprise tape support cylinders with parallel axes, namely two tape entry cylinders 5, 6, two tape exit cylinders 7, 8 and an intermediate cylinder 9 for tape support in the tank.
  • tape support cylinders with parallel axes namely two tape entry cylinders 5, 6, two tape exit cylinders 7, 8 and an intermediate cylinder 9 for tape support in the tank.
  • the three cylinders 6, 9, 7 immersed in the electrolytic cell define the strip running path in the electrolytic cell, which here is approximately in a horizontal plane.
  • the two anodes 3 are each positioned between two submerged cylinders and each have a planar active surface 13 placed below the strip running path and oriented parallel to it and towards it.
  • the distance between the active surface 13 of the anodes 3 of the strip running path is generally between 0.5 and 10 cm in an industrial cell.
  • the active surfaces 13 of the anodes 3 extend transversely to the direction of travel over the entire width of the strip to be coated. Furthermore, the active surfaces 13 of the anodes 3 extend along the direction of travel of the strip between two opposite edges 3A, 3B.
  • the distance between the active surface 13 of the anodes 3 of the strip running path is commonly about 3 cm.
  • each anode 3 is bordered, along these two opposite edges 3A, 3B, by two masks 4A, 4B in the form of narrow flat panels.
  • Each panel-shaped mask 4A, 4B extends along a corresponding rim 3A, 3B of the active anode surface 3 and is arranged in a plane approximately parallel to the strip running path.
  • the masks are made of electrically insulating material, preferably of composite material or plastic.
  • the masks 4A, 4B which each run along an edge 3A, 3B of the active anode surface, are always closer to the strip running path than the anodes.
  • the distance which separates a mask 4A, 4B from the strip travel path is less than 0.5 times the inter-electrode distance, ie that which separates the corresponding flange 3A, 3B from the same travel path.
  • the masks can be in a form different from that of a narrow flat panel while offering, facing the running path and along an edge of the active anode surface, a surface electrically insulating masking and closer to the running path than said flange.
  • the thickness of the masks 4A, 4B is preferably much less than said inter-electrode distance, so that said masks can be partially inserted between the anode and the strip running path under the corresponding surface rim 3A, 3B active anode 13.
  • the thickness of the masks 4A, 4B is however sufficient to provide an electrical masking function between the active surface 13 of the anode and the running strip serving as the cathode.
  • the thickness of the masks is commonly of the order of 1 cm.
  • each mask 4A, 4B which runs along a rim 3A, 3B of active anode surface, has a continuous intersection with the abstract surface passing through said rim 3A, 3B and orthogonal to the strip running path.
  • the mask 4A, 4B in the form of a narrow flat panel, extends in width on each side of said intersection, that is to say, covering on one side the corresponding rim 3A, 3B of the active anode surface and largely protruding from the other side towards the outside of said active surface.
  • the so-called overlap width measured along the direction of travel, is less than the distance between said edge of said travel path.
  • the overlap width of the mask 4A, 4B relative to the rim 3A, 3B corresponding to the anode 3 is commonly less than 1 cm.
  • the overflow width of the mask 4A, 4B relative to the corresponding rim 3A, 3B of anode 3 is greater than or equal to the inter-electrode distance, at the level of said rim.
  • each anode 3 is thus bordered by two masks 4A, 4B along two opposite edges 3A, 3B; according to a variant of the invention, two masks, which immediately follow one another along the strip running path and which frame two successive anodes, can be contiguous and form only one flat panel. The same mask can thus be used to border two successive anodes.
  • the means for circulating an electric current between the anodes 3 and the running strip serving as the cathode comprise the two emerged cylinders 5, 8 which are conductive, are known in themselves and are not described here in detail.
  • FIG. 2 thus represents a cross-sectional diagram of a radial cell, designated as a whole by the reference 1 ′, comprising a tank 2 ′ containing an electroplating bath S ′, strip running means comprising two emerging conductive cylinders 5 ', 8' and a partially submerged cylinder 9 'whose surface defines the strip running path, two submerged anodes 3' in the shape of an arc of a circle facing the submerged part of said cylinder 9 ', and three masks 10, 11 and 12.
  • the first mask 10 is located at the level of the anode rim which sees the strip re-entering the bath and the third mask 12 is located at the level of the last anode rim which sees the strip exiting the bath.
  • the first and the third masks may have an emerged part.
  • the second mask 11 is an intermediate mask which extends between the two anodes 3 'and therefore borders both of the edges of each anode 3'.
  • the masks can be supported by said ramps.
  • said ejector can advantageously serve as a mask provided that it is electrically insulating and the masking surface which faces the path of tape scrolling is not necessarily flat.
  • Each cell of the installation contributes to the formation of a portion of the coating layer, or "sublayer" and the stacking of the sublayers forms the alloy layer.
  • the cells 1 of the installation have soluble zinc anodes.
  • the tanks 2 of the different cells 1 are filled with an electroplating bath S based on chloride anions and containing zinc cations and alloying elements in proportions and concentrations known in themselves to obtain said layer of alloy with the desired composition.
  • said alloying elements are chosen from nickel, iron or cobalt.
  • the tape B is scrolled successively in each of the cells of the installation.
  • an electric current is passed between the anodes of the different cells and the steel strip B serving as the cathode.
  • the tape running speed and the electric current density of the different cells are adjusted in a manner known per se, in particular as a function of the thickness of the desired plating layer.
  • the tape running speed is greater than 50 m / min.
  • the current density is greater than 50 A / dm2.
  • the steel strip B then emerges from the installation coated with a layer of alloy.
  • the Applicant has also surprisingly found that said painted strip, in particular by cataphoresis, withstood the gravel test much better than a sheet conventionally coated with the same layer of alloy and painted in the same way.
  • the cells of the electrodeposition installation are equipped with insoluble electrodes and the cells of the cells are filled with an electrolysis bath based on anions other than chloride ions, in particular of sulfate ions.
  • the electrodeposited layer is a metal alloy based on metals other than zinc, in particular based of tin and lead, or based on iron and nickel, or based on copper and nickel.
  • the composition of the electroplating bath is adapted in a manner known per se to the type of alloy of the coating to be deposited.
  • the above-described electrodeposition installation can be used to coat steel strip or other metal strips, in particular stainless steel strips.
  • the Applicant has found that by using an installation comprising a succession of cells according to the invention for continuously coating a metal strip, in particular of steel, with a layer of alloy, notably based on zinc, one obtains advantageously a coating having in its thickness a great homogeneity, in particular of composition, and excellent mechanical properties, in particular a resistance to delamination.
  • the applicant considers that the masks bordering the anodes of the electroplating cells of the installation cause a sudden variation in the current density at the input and at the output of the various anodes of the installation, which makes it possible to ensure deposition under more homogeneous current density conditions which guarantee a constant alloy composition over the thickness of the layer.
  • the purpose of this test is to prepare a coating of zinc alloy on a steel strip in electroplating cells according to the invention.
  • the electrodeposition installation comprises a succession of radial cells 1 ′ according to the invention, of the type previously described and shown in FIG. 2.
  • the partially submerged cylinder 9 ' which defines the strip running path in the cell has a width of 2 m and a diameter of 2 m.
  • the two 3 'anodes are made of zinc and soluble.
  • the average distance between the anodes and said cylinder 9 ' is 3 cm.
  • the three masks 10, 11 and 12 are arranged about 1 cm from said cylinder 9 'and barely penetrate, to a depth of less than 1 cm, in the interval which separates the anodes 3' from said cylinder 9 '.
  • the three masks 10, 11, 12 which border the two anodes are flat polypropylene panels 2 m long, about 20 cm wide and 1 cm thick.
  • the temperature of the bath is maintained at 57 ° C. and the pH of the bath is maintained at a value of approximately 4.5 by additions of hydrochloric acid.
  • the strip to be coated is made of steel, has a width of 1.5 m and a thickness of 1 mm.
  • the strip is scrolled through the installation at a speed of 100 m / min. and an electric current is passed between the anodes and the strip of 100 A / dm2.
  • a strip coated on one face with a layer of zinc alloy containing 12% by weight of nickel and with a thickness of approximately 4 micrometers is obtained.
  • the coating of the sheet blank A was prepared discontinuously in a manner known per se by immersing and maintaining the said sheet blank to be coated in an electroplating cell facing an anode, without scrolling, and by passing an electric current between said anode and the sheet blank serving as cathode.
  • the sheet blank B is cut from a strip of steel coated continuously according to the prior art, that is to say by scrolling of said strip in electroplating cells which are not provided with anode edge masks .
  • the sheet blank C is cut from a continuously coated steel strip according to test No. 1 above.
  • the sheet blanks A, B, C are stamped and, after the stamping operation, the weight loss of each sheet blank compared to the surface of the surface is measured. coating.
  • the result of the measurement is an indicator proportional to the crumbling or "dusting" of the coating.
  • the alloy coating continuously prepared on a steel sheet in electroplating cells according to the invention has excellent resistance to crumbling and "dusting".
  • each sheet blank A, B, C of test No. 2 is painted by cataphoresis and under the same conditions.
  • the thickness of the paint layer is approximately 100 micrometers.
  • Each sheet blank A, B, C is then subjected to the same gravel test, which consists in projecting gravel for a predetermined time on the sheet blanks to be tested.
  • the impact of gravel on the blanks of painted sheet A, B, C may or may not cause the paint and coating to tear off.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Secondary Cells (AREA)

Claims (10)

  1. Galvanisierungszelle (1) zur kontinuierlichen Beschichtung eines Metallbandes (B), insbesondere mit einem Überzug aus einer Metallegierung, die eine Elektrolysewanne (2), welche ein Galvanisierungsbad (S) enthält, mindestens eine Anode (3), die in das Bad eingetaucht ist und eine von Rändern begrenzte aktive Oberfläche (13) aufweist, Mittel, um das Band in dem Bad (S) vor der aktiven Oberfläche von einem Rand (3A) dieser aktiven Oberfläche zum gegenüberliegenden anderen Rand (3B) derselben Oberfläche vorbeizuführen, wobei diese Mittel einen Durchlaufweg für das Band definieren, und Mittel zum Fließenlassen eines elektrischen Stromes zwischen der Anode (3) und dem als Kathode dienenden vorbeilaufenden Band (B) umfaßt, dadurch gekennzeichnet, daß die aktive Oberfläche (13) jeder Tauchanode (3) an jedem der zwei gegenüberliegenden Ränder (3A, 3B) von einer Maske (4A, 4B) gesäumt wird, die entlang dem entsprechenden Rand (3A, 3B) und dem Durchlaufweg gegenüberliegend eine elektrisch isolierende Oberfläche aufweist, die sich näher an dem Durchlaufweg befindet als der Rand (3A, 3B), wobei diese Maske (4A, 4B) die aktive Anodenoberfläche (13) nach außen hin um eine Überstandsbreite überragt, die, in Durchlaufrichtung gemessen, mindestens dem Abstand entspricht, der den Rand (3A, 3B) von dem Durchlaufweg trennt, und diese Maske (4A, 4B) den Rand (3A, 3B) der aktiven Anodenoberfläche (13) auf einer sogenannten Abdeckbreite überdeckt, die, in Durchlaufrichtung gemessen, kleiner ist als der Abstand, der den Rand von dem Durchlaufweg trennt.
  2. Galvanisierungszelle nach Anspruch 1, dadurch gekennzeichnet, daß der Abstand, der jede Maske (4A, 4B), die einen Rand (3A, 3B) der aktiven Oberfläche (13) der Anode (3) säumt, von dem Durchlaufweg des Bandes trennt, kleiner ist als das 0,5fache des Abstands, der den Rand (3A, 3B) von dem Durchlaufweg des Bandes trennt.
  3. Galvanisierungszelle nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß die Maske (4A, 4B) die Form einer ebenen Platte besitzt und aus einem elektrisch isolierenden Material besteht.
  4. Galvanisierungszelle nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Zelle vom radialen Typ ist.
  5. Galvanisierungszelle nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Anoden (3) löslich sind und/oder daß das Galvanisierungsbad (S) auf Chloridanionen basiert.
  6. Galvanisierungsanlage zur kontinuierlichen Beschichtung eines Metallbandes (B), insbesondere mit einem Überzug aus einer Metallegierung, die eine kaskadenartige Folge von Zellen (1) nach einem der Ansprüche 1 bis 5 umfaßt.
  7. Verwendung einer Galvanisierungszelle nach einem der Ansprüche 1 bis 5 oder einer Galvanisierungsanlage nach Anspruch 6 zur kontinuierlichen Beschichtung von Metallbändern (B) mit einem Überzug aus einer Metallegierung.
  8. Verwendung nach Anspruch 7, dadurch gekennzeichnet, daß die Legierung auf Zink basiert.
  9. Verwendung nach Anspruch 8, dadurch gekennzeichnet, daß der Zinkgehalt der Legierung mehr als 10 Gew.-% beträgt.
  10. Verfahren zur Beschichtung eines Metallbandes (B) durch galvanische Abscheidung einer Metallegierung, insbesondere auf Zinkbasis, mittels einer Anlage, die mehrere kaskadenartig angeordnete Zellen (1) nach einem der Ansprüche 1 bis 5 umfaßt, bei dem man das Band (B) nacheinander durch die Zellen (1) der Anlage laufen läßt und man einen elektrischen Strom zwischen den Anoden (3) der Zellen und dem vorbeilaufenden Band (B) fließen läßt, dadurch gekennzeichnet, daß die Durchlaufgeschwindigkeit des Bandes (B) in der Anlage größer als 50 m/Minute ist und/oder die Dichte des zwischen den Anoden (3) der Zellen und dem Band (B) fließenden elektrischen Stromes größer als 50 A/dm2 ist.
EP95401908A 1994-09-29 1995-08-18 Zelle zur kontinuierlichen Elektrobeschichtung von Metalllegierungen Expired - Lifetime EP0704558B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9411610 1994-09-29
FR9411610A FR2725215B1 (fr) 1994-09-29 1994-09-29 Cellule d'electrodeposition en continu d'alliages metalliques

Publications (2)

Publication Number Publication Date
EP0704558A1 EP0704558A1 (de) 1996-04-03
EP0704558B1 true EP0704558B1 (de) 1997-11-19

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EP95401908A Expired - Lifetime EP0704558B1 (de) 1994-09-29 1995-08-18 Zelle zur kontinuierlichen Elektrobeschichtung von Metalllegierungen

Country Status (8)

Country Link
US (1) US5582708A (de)
EP (1) EP0704558B1 (de)
JP (1) JP3398776B2 (de)
KR (1) KR960010906A (de)
AT (1) ATE160389T1 (de)
DE (1) DE69501073T2 (de)
ES (1) ES2112025T3 (de)
FR (1) FR2725215B1 (de)

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Publication number Priority date Publication date Assignee Title
DE19717489B4 (de) * 1997-04-25 2008-04-10 Sms Demag Ag Anordnung zur elektrogalvanischen Metallbeschichtung eines Bandes
US6174425B1 (en) * 1997-05-14 2001-01-16 Motorola, Inc. Process for depositing a layer of material over a substrate
KR19990064747A (ko) * 1999-05-06 1999-08-05 이종구 Ｎｉ-Ｆｅ 합금 박판 제조방법 및 그 장치
US6231743B1 (en) 2000-01-03 2001-05-15 Motorola, Inc. Method for forming a semiconductor device
MXPA06007170A (es) * 2003-12-23 2006-09-04 Corus Staal Bv Electroplaqueado de cinta metalica mejorado.
ES2818224B2 (es) 2019-10-07 2021-11-16 Pueo Felix Prado Instalacion de electro-deposicion con barras inter-celda activas

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3692639A (en) * 1969-10-13 1972-09-19 Center Scient & Applied Res Multiplication of metal surface,by electroplating or anodic dissolution
US4128459A (en) * 1977-11-25 1978-12-05 Allied Chemical Corporation Continuous electroplating of alloy onto metallic strip
JPS5841358B2 (ja) * 1980-01-12 1983-09-12 株式会社小糸製作所 メツキ装置
JPS58181894A (ja) * 1982-04-14 1983-10-24 Nippon Kokan Kk <Nkk> 複層異種組成Ｆｅ−Ｚｎ合金電気鍍金鋼板の製造方法
JPS59160000A (ja) * 1983-02-28 1984-09-10 Kawasaki Steel Corp ストリツプ連続電気めつきのエツジオ−バ−コ−ト防止装置
JPS60121293A (ja) * 1983-12-03 1985-06-28 Kawasaki Steel Corp Ζｎ−Ｆｅ合金を主体とするΖｎ−Ｆｅ系合金電気めっき鋼板の製造方法
JPH07116636B2 (ja) * 1986-09-26 1995-12-13 川崎製鉄株式会社 ラジアル型めつきセル
GB8809750D0 (en) * 1988-04-25 1988-06-02 Beckswift Ltd Electrical apparatus
DE4139066A1 (de) * 1991-11-28 1993-06-03 Hans Josef May Vorrichtung zum elektrolytischen metallabscheiden auf metallbaendern

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Publication number Publication date
JP3398776B2 (ja) 2003-04-21
FR2725215B1 (fr) 1996-11-22
KR960010906A (ko) 1996-04-20
DE69501073D1 (de) 1998-01-02
ES2112025T3 (es) 1998-03-16
JPH08209394A (ja) 1996-08-13
US5582708A (en) 1996-12-10
FR2725215A1 (fr) 1996-04-05
DE69501073T2 (de) 1998-05-07
ATE160389T1 (de) 1997-12-15
EP0704558A1 (de) 1996-04-03

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