EP0132424A1 - Corrosion-resistant steel wire - Google Patents

Corrosion-resistant steel wire Download PDF

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Publication number
EP0132424A1
EP0132424A1 EP84401266A EP84401266A EP0132424A1 EP 0132424 A1 EP0132424 A1 EP 0132424A1 EP 84401266 A EP84401266 A EP 84401266A EP 84401266 A EP84401266 A EP 84401266A EP 0132424 A1 EP0132424 A1 EP 0132424A1
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EP
European Patent Office
Prior art keywords
steel wire
mischmetal
zinc
addition
layer
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
EP84401266A
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German (de)
French (fr)
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EP0132424B1 (en
Inventor
Bruno Thomas
Guy Viart
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Trefilunion SA
Original Assignee
Fils et Cables D'acier de Lens (Fical)
Trefilunion SA
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Application filed by Fils et Cables D'acier de Lens (Fical), Trefilunion SA filed Critical Fils et Cables D'acier de Lens (Fical)
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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
    • C23C2/06—Zinc or cadmium or alloys based thereon
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12785—Group IIB metal-base component
    • Y10T428/12792—Zn-base component
    • Y10T428/12799—Next to Fe-base component [e.g., galvanized]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
    • Y10T428/2958—Metal or metal compound in coating

Definitions

  • the present invention relates to a hard steel wire with high carbon content, perfectly ductile, used for the manufacture of cables and springs, having a protective coating consisting of several layers of different alloys based on zinc, aluminum and of iron.
  • the wire is characterized in that it is coated with a first internal layer of alloy A1 (Al-Fe-Zn) containing at least 15% of aluminum and with a second external layer A2 ( Zn-Al-Fe) containing at least 3% aluminum and 90% zinc.
  • A1 Al-Fe-Zn
  • Zn-Al-Fe Zn-Al-Fe
  • the first stage of the process according to the invention consists of galvanizing with pure zinc by hot immersion in a bath of pure zinc followed by controlled cooling and / or heating (R1).
  • the process targeted by the invention therefore consists of two consecutive immersions with controlled cooling and / or heating to obtain a controlled diffusion of Al and Fe.
  • the wire obtained as defined has a significantly improved corrosion resistance compared to the usual galvanized wires, while retaining excellent ductility and deformability characteristics (bending, winding, wire drawing, etc.).
  • the resistance to accelerated corrosion in salt spray according to standard NFX41-002 (August 1975) of the wire according to the invention is at least twice greater than that of a traditional galvanized wire as shown in the tests carried out.
  • rust will appear after approximately 150 hours on a traditional galvanized wire, and after 400 hours on a wire provided with a coating according to the invention. For coatings 40 microns thick, these times are 300 hours and 800 hours respectively.
  • cathodic protection in a chlorinated medium of the coating according to the invention is at least equal to that of traditional galvanized wire.
  • the samples were wound on a 10 mm diameter mandrel before the test.
  • Wires with a low zinc coating (10 ⁇ m) show red rust after 3 days of exposure.
  • Coated thickness galvanized wires 21 ⁇ m are corroded (with attack by steel) after one week and those with a thickness of 35 ⁇ m reveal rust after two weeks of exposure.
  • the corrosion resistance of the wire obtained according to the invention is higher than that of similar Zn-Al coatings, but deposited in a single operation, without controlled diffusion.
  • the controlled cooling R1 of the wire at the outlet of the first bath was 20 ° C per second, the heating before the second bath of 100 ° C per second, the cooling R2 after the second bath (zinc alloy + Al + additions) of 100 ° C per second.

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)
  • Non-Insulated Conductors (AREA)
  • Conductive Materials (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)

Abstract

Fil d'acier dur à revêtements superposés, résistant à la corrosion, parfaitement ductile, caractérisé en ce qu'il est revêtu d'une première couche interne d'alliage A1 (Al-Fe-Zn) et d'une deuxième couche externe A2 (Zn-Al-Fe) et en ce que la première couche de revêtement interne est composée comme suit:

  • Al compris entre 15% et 45%
  • Fe compris entre 5% et 25%
  • A1 Zn faisant la balance avec des éléments d'addition en faible quantité comme Mg, Sn, Ni, Cu, Cr, Mischmetal, etc., dont le total n'excède pas 0,5%.
Corrosion resistant, perfectly ductile, hard steel wire with overlapping coatings, characterized in that it is coated with a first internal layer of alloy A1 (Al-Fe-Zn) and a second external layer A2 (Zn-Al-Fe) and in that the first internal coating layer is composed as follows:
  • Al between 15% and 45%
  • Fe between 5% and 25%
  • A1 Zn balancing with elements of addition in small quantity like Mg, Sn, Ni, Cu, Cr, Mischmetal, etc., the total of which does not exceed 0.5%.

Ce fil présente une résistance à la corrosion très supérieure à celle des fils galvanisés classiques et à celle des revêtements Zn-AI analogues mais déposés en un seul stade.This wire has a corrosion resistance much higher than that of conventional galvanized wires and that of similar Zn-AI coatings but deposited in a single stage.

Description

La présente invention concerne un fil d'acier dur à haute teneur en carbone, parfaitement ductile, utilisé pour la fabrication de câbles et de ressorts, présentant un revêtement protecteur constitué de plusieurs couches d'alliages différents à base de zinc, d'aluminium et de fer.The present invention relates to a hard steel wire with high carbon content, perfectly ductile, used for the manufacture of cables and springs, having a protective coating consisting of several layers of different alloys based on zinc, aluminum and of iron.

Suivant l'invention, le fil est caractérisé en ce qu'il est revêtu d'une première couche interne d'alliage A1 (Al-Fe-Zn) contenant au moins 15% d'aluminium et d'une deuxième couche externe A2 (Zn-Al-Fe) contenant au moins 3% d'aluminium et 90% de zinc.According to the invention, the wire is characterized in that it is coated with a first internal layer of alloy A1 (Al-Fe-Zn) containing at least 15% of aluminum and with a second external layer A2 ( Zn-Al-Fe) containing at least 3% aluminum and 90% zinc.

Selon un mode de réalisation de l'invention, la composition de ces couches de revêtement est la suivante :

  • - la première couche (interne) d'alliage A1 contient du fer, de l'aluminium et du zinc, la teneur globale de cette couche étant la suivante :
    • ( . Al compris entre 15% et 45%
    • ( . Fe compris entre 5% et 25%
    • A1 ( . Zn faisant la balance avec des éléments
    • ( d'addition en faible qùantité comme Mg, ( Sn, Ni, Cu, Cr, Mischmetal, etc....
  • - la deuxième couche (externe) d'alliage A2, située sur la première couche contient du zinc, de l'aluminium et du fer, et sa teneur globale est la suivante :
    • ( . Al compris entre 3% et 20%
    • ( . Fe compris entre 0,5% et 5%
    • A2 (.Zn faisant la balance avec des éléments ( d'addition en faible quanttié comme Mg, ( Sn, Ni, Cu, Cr, Mischmetal, etc...
    • Ces revêtements sont obtenus par un procédé de fabrication à deux stades.
According to one embodiment of the invention, the composition of these coating layers is as follows:
  • the first (internal) layer of alloy A1 contains iron, aluminum and zinc, the overall content of this layer being as follows:
    • (Al between 15% and 45%
    • (. Fe between 5% and 25%
    • A1 (. Zn weighing with elements
    • (low quantity addition such as Mg, (Sn, Ni, Cu, Cr, Mischmetal, etc ...
  • - the second (external) layer of alloy A2, located on the first layer contains zinc, aluminum and iron, and its overall content is as follows:
    • (Al between 3% and 20%
    • (. Fe between 0.5% and 5%
    • A2 (.Zn making the balance with elements (of addition in small quantity like Mg, (Sn, Ni, Cu, Cr, Mischmetal, etc ...
    • These coatings are obtained by a process two-stage manufacturing.

Depuis longtemps, la préparation de revêtements protecteurs en deux stades est connue, mais les procédés antérieurs ne prévoient pas de traitements thermiques volontaires avant et après les deux immersions.For a long time, the preparation of protective coatings in two stages has been known, but the prior processes do not provide for voluntary heat treatments before and after the two immersions.

Le premier stade du procédé selon l'invention consiste en une galvanisation au zinc pur par immersion à chaud dans un bain de zinc pur suivi d'un refroidissement et/ou d'un chauffage contrôlés (R1).The first stage of the process according to the invention consists of galvanizing with pure zinc by hot immersion in a bath of pure zinc followed by controlled cooling and / or heating (R1).

Le deuxième stade de ce procédé est une immersion du premier revêtement de galvanisation dans un bain d'alliage zinc-aluminium fondu, de composition suivante :

  • - Al compris entre 3% et 10X;
  • - Zn faisant la balance avec des éléments d'addition en faible quantité : Mg, Sn, Cr, Ni, Cu, Mischmetal, etc.... dont le total n'excède pas 0,5y.
The second stage of this process is an immersion of the first galvanizing coating in a bath of molten zinc-aluminum alloy, of the following composition:
  • - Al between 3% and 10X;
  • - Zn making the balance with elements of addition in small quantity: Mg, Sn, Cr, Ni, Cu, Mischmetal, etc .... whose total does not exceed 0.5y.

L'immersion dans cette deuxième cuve, suivie d'un refroidissement et/ou d'un chauffage contrôlés (R2), provoque une modification thermochimique considérable des couches d'alliage obtenues par la première galvanisation pour faire place à l'alliage A1 (Al-Zn-Fe).Immersion in this second tank, followed by controlled cooling and / or heating (R2), causes a considerable thermochemical modification of the alloy layers obtained by the first galvanization to make room for the alloy A1 (Al -Zn-Fe).

De plus, la couche de zinc pur de la première galvanisation disparait complètement pour donner la couche d'alliage A2 (Al-Zn-Fe).In addition, the layer of pure zinc from the first galvanization disappears completely to give the layer of alloy A2 (Al-Zn-Fe).

Ces refroidissements et/ou chauffages successifs réalisent ainsi un traitement thermochimique de diffusion contrôlée.These successive coolings and / or heatings thus carry out a thermochemical treatment of controlled diffusion.

Ces deux couches ont pour analyse globale respective : A1,et A2.These two layers have their respective global analysis: A1, and A2.

On constate donc un très fort enrichissement en aluminium de la couche intérieure, alors que le premier bain ne contient que du zinc pur.There is therefore a very strong enrichment aluminum of the inner layer, while the first bath contains only pure zinc.

Le procédé visé par l'invention, consiste donc en deux immersions consécutives avec refroidissement et/ou chauffage contrôlés pour obtenir une diffusion contrôlée de Al et Fe.The process targeted by the invention therefore consists of two consecutive immersions with controlled cooling and / or heating to obtain a controlled diffusion of Al and Fe.

Le fil obtenu comme défini, présente une tenue à la corrosion très nettement améliorée par rapport aux fils galvanisés habituels, tout en conservant d'excellentes caractéristiques de ductilité et de déformabilité (pliage, enroulement, tréfilage...).The wire obtained as defined has a significantly improved corrosion resistance compared to the usual galvanized wires, while retaining excellent ductility and deformability characteristics (bending, winding, wire drawing, etc.).

On a établi que la résistance à la corrosion accélérée en brouillard salin suivant la norme ASTM B-117 du fil, objet de la présente invention est au moins le double de celle du fil galvanisé traditionnel.It has been established that the resistance to accelerated corrosion in salt spray according to the ASTM B-117 standard of the wire which is the subject of the present invention is at least twice that of traditional galvanized wire.

D'autre part, la résistance à la corrosion accélérée en brouillard salin suivant la norme NFX41-002 (Août 1975) du fil selon l'invention est au minimum deux fois supérieure à celle d'un fil galvanisé traditionnel comme l'on montré les essais réalisés. A titre d'exemples numériques indicatifs, pour des revêtements anti-corrosion d'une épaisseur de 20 microns exposés au brouillard salin, la rouille appa- rait au bout d'environ 150 heures sur un fil galvanisé traditionnel, et après 400 heures sur un fil pourvu d'un revêtement selon l'invention. Pour des revêtements de 40 microns d'épaisseur, ces temps sont respectivement de 300 heures et 800 heures.On the other hand, the resistance to accelerated corrosion in salt spray according to standard NFX41-002 (August 1975) of the wire according to the invention is at least twice greater than that of a traditional galvanized wire as shown in the tests carried out. As indicative numerical examples, for anti-corrosion coatings with a thickness of 20 microns exposed to salt spray, rust will appear after approximately 150 hours on a traditional galvanized wire, and after 400 hours on a wire provided with a coating according to the invention. For coatings 40 microns thick, these times are 300 hours and 800 hours respectively.

On a également vérifié que la protection cathodique en milieu chloruré du revêtement selon l'invention est au moins égale à celle du fil galvanisé traditionnel.It has also been verified that the cathodic protection in a chlorinated medium of the coating according to the invention is at least equal to that of traditional galvanized wire.

On a également exécuté des tests de corrosion en atmosphère S02, à 10 ppm SO2, dont le tableau ci-dessous présente les résultats exprimés en perte de poids due à la corrosion pour différents échantillons exposés en atmosphère à 10 ppm S02 et examinés après 3 jours, 1, 2, 3 et 4 semaines.

Figure imgb0001
We also performed corro tests sion in an atmosphere of S0 2 , at 10 ppm SO 2 , the table of which presents the results expressed in weight loss due to corrosion for various samples exposed in an atmosphere of 10 ppm S0 2 and examined after 3 days, 1, 2 , 3 and 4 weeks.
Figure imgb0001

Les échantillons on été enroulés sur un mandrin de 10 mm de diamètre avant le test.The samples were wound on a 10 mm diameter mandrel before the test.

Les fils à faible revêtement de zinc (10 µm) présentent de la rouille rouge après 3 jours d'exposition.Wires with a low zinc coating (10 µm) show red rust after 3 days of exposure.

Les fils galvanisés d'épaisseur de revêtement de 21 µm sont corrodés (avec attaque de l'acier) après une semaine et ceux d'épaisseur de 35 µm laissent apparaître la rouille après deux semaines d'exposition.Coated thickness galvanized wires 21 µm are corroded (with attack by steel) after one week and those with a thickness of 35 µm reveal rust after two weeks of exposure.

Aucune trace de rouille rouge n' a été observée sur les échantillons de fil selon l'invention même sur ceux de faible épaisseur de revêtement (10 µm) après quatre semaines d'exposition.No trace of red rust was observed on the wire samples according to the invention even on those of thin coating thickness (10 μm) after four weeks of exposure.

Enfin, la résistance à la corrosion du fil obtenu selon l'invention est supérieure à celle des revêtements Zn-Al analogues, mais déposés en une seule opération, sans diffusion contrôlée.Finally, the corrosion resistance of the wire obtained according to the invention is higher than that of similar Zn-Al coatings, but deposited in a single operation, without controlled diffusion.

A titre d'exemple, le refroidissement contrôlé R1 du fil à la sortie du premier bain (zinc pur) a été de 20°C par seconde, le chauffage avant le deuxième bain de 100°C par seconde, le refroidissement R2 après le deuxième bain (alliage zinc + Al + additions) de 100°C par seconde.For example, the controlled cooling R1 of the wire at the outlet of the first bath (pure zinc) was 20 ° C per second, the heating before the second bath of 100 ° C per second, the cooling R2 after the second bath (zinc alloy + Al + additions) of 100 ° C per second.

Claims (4)

1 - Fil d'acier dur à revêtements superposés, résistant à la corrosion, parfaitement ductile, caractérisé en ce qu'il est revêtu d'une première couche interne d'alliage A1 (A1-Fe-Zn) contenant au moins 15% d'aluminium et d'une deuxième couche externe A2 (Zn-Al-Fe) contenant au moins 3 % d'aluminium et 90% de zinc.1 - Hard steel wire with superimposed coatings, corrosion resistant, perfectly ductile, characterized in that it is coated with a first internal layer of alloy A1 (A1-Fe-Zn) containing at least 15% d aluminum and a second outer layer A2 (Zn-Al-Fe) containing at least 3% aluminum and 90% zinc. 2 - Fil d'acier dur selon la revendication 1, caractérisé en ce que la première couche de revêtement interne est composée comme suit : ( Al compris entre 15% et 45% ( Fe compris entre 5% et 25% A1 ( Zn faisant la balance avec des éléments ( d'addition en faible quantité comme Mg, ( Sn, Ni, Cu, Cr, Mischmetal, etc... dont ( le total n'excède pas 0,5%. 3 - Fil d'acier dur selon les revendications 1 et 2, caractérisé en ce que la deuxième couche externe de revêtement est composée comme suit : ( Al compris entre 3% et 20% ( Fe compris entre 0,5% et 5% A2 ( Zn faisant la balance avec des éléments ( d'addition en faible quantité comme Mg, ( Sn, Ni, Cu, Cr, Mischmetal, etc... dont ( le total n'excède pas 0,5%. 2 - Hard steel wire according to claim 1, characterized in that the first internal coating layer is composed as follows: (Al between 15% and 45% (Fe between 5% and 25% A1 (Zn weighing with elements (addition in small quantities such as Mg, (Sn, Ni, Cu, Cr, Mischmetal, etc ... of which (the total does not exceed 0.5%. 3 - Hard steel wire according to claims 1 and 2, characterized in that the second external coating layer is composed as follows: (Al between 3% and 20% (Fe between 0.5% and 5% A2 (Zn balancing with elements (addition in small quantities such as Mg, (Sn, Ni, Cu, Cr, Mischmetal, etc ... of which (the total does not exceed 0.5%. 4 - Procédé de fabrication d'un fil d'acier selon l'une des revendications 1 à 3, caractérisé en ce qu'on obtient les deux couches de revêtement par deux immersions successives avec un refroidissement et/ou un chauffage contrôlés pour réaliser un traitement thermochimique de diffusion contrôlée.4 - A method of manufacturing a steel wire according to one of claims 1 to 3, characterized in that the two coating layers are obtained by two successive immersions with controlled cooling and / or heating to achieve a thermochemical treatment of controlled diffusion. 5 - Procédé de fabrication de fil d'acier dur selon les revendications 1, 2, 3 et 4, caractérisé en ce que la première immersion est faite dans un bain de zinc pur, la deuxième immersion dans un alliage zinc-aluminium de composition : 3%<Al<10%, Zn faisant la balance avec des additions en faible quantité comme Mg, Sn, Ni, Cu, Cr, Mischmetal, et que ces deux immersions sont suivies d'un refroidissement et/ou d'un chauffage contrôlés (R1 et R2) pour assurer un traitement thermochimique de diffusion contrôlée.5 - A method of manufacturing hard steel wire according to claims 1, 2, 3 and 4, characterized in that the first immersion is made in a bath of pure zinc, the second immersion in a zinc-aluminum alloy with a composition: 3% <Al <10%, Zn balancing with additions in small quantities such as Mg, Sn, Ni, Cu, Cr, Mischmetal, and that these two immersions are followed by controlled cooling and / or heating (R1 and R2) to ensure thermochemical treatment of controlled diffusion.
EP84401266A 1983-06-28 1984-06-19 Corrosion-resistant steel wire Expired EP0132424B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8310660 1983-06-28
FR8310660A FR2548216B1 (en) 1983-06-28 1983-06-28 STEEL WIRE WITH CORROSION RESISTANT COATINGS

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Publication Number Publication Date
EP0132424A1 true EP0132424A1 (en) 1985-01-30
EP0132424B1 EP0132424B1 (en) 1989-04-12

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US (1) US4605598A (en)
EP (1) EP0132424B1 (en)
JP (1) JPS6052568A (en)
AU (1) AU567948B2 (en)
DE (1) DE3477676D1 (en)
ES (1) ES533776A0 (en)
FR (1) FR2548216B1 (en)

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JP2019096492A (en) * 2017-11-23 2019-06-20 株式会社オートネットワーク技術研究所 Aluminum-based single wire, twisted wire conductor, braided wire and wire harness

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DE3477676D1 (en) 1989-05-18
FR2548216B1 (en) 1988-10-21
AU567948B2 (en) 1987-12-10
JPH0573824B2 (en) 1993-10-15
ES8601327A1 (en) 1985-10-16
ES533776A0 (en) 1985-10-16
EP0132424B1 (en) 1989-04-12
FR2548216A1 (en) 1985-01-04
JPS6052568A (en) 1985-03-25
US4605598A (en) 1986-08-12
AU2989484A (en) 1985-01-03

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