EP0045110B1 - Procédé pour la production de revêtements de phosphate sur les surfaces de fer et d'acier et son usage - Google Patents

Procédé pour la production de revêtements de phosphate sur les surfaces de fer et d'acier et son usage Download PDF

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Publication number
EP0045110B1
EP0045110B1 EP81200830A EP81200830A EP0045110B1 EP 0045110 B1 EP0045110 B1 EP 0045110B1 EP 81200830 A EP81200830 A EP 81200830A EP 81200830 A EP81200830 A EP 81200830A EP 0045110 B1 EP0045110 B1 EP 0045110B1
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Prior art keywords
weight
solution
iron
ratio
contact
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Expired
Application number
EP81200830A
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German (de)
English (en)
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EP0045110A1 (fr
Inventor
Kevin Brown
Jon Darby
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.)
Chemetall Ltd
Original Assignee
Metallgesellschaft AG
Continentale Parker Ste
Continentale Parker SA
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=10515046&utm_source=***_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0045110(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Metallgesellschaft AG, Continentale Parker Ste, Continentale Parker SA filed Critical Metallgesellschaft AG
Priority to AT81200830T priority Critical patent/ATE9823T1/de
Publication of EP0045110A1 publication Critical patent/EP0045110A1/fr
Application granted granted Critical
Publication of EP0045110B1 publication Critical patent/EP0045110B1/fr
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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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
    • C23C22/362—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing also zinc cations
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • C23C22/12—Orthophosphates containing zinc cations
    • C23C22/14—Orthophosphates containing zinc cations containing also chlorate anions
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • C23C22/22—Orthophosphates containing alkaline earth metal cations

Definitions

  • the invention relates to a process for the production of phosphate coatings on iron or steel surfaces by immersion or flooding with an aqueous acidic zinc phosphate solution and its application to the preparation of metal surfaces for cold forming.
  • phosphate coatings on metal surfaces in particular from iron and steel, by treatment with a zinc phosphate solution is generally common.
  • one or more oxidizing agents are added to the phosphating solution.
  • phosphating processes uses phosphating solutions which contain oxidizing agents which convert iron (II) to iron (III), so that insoluble iron phosphate is formed. With increasing throughput on the surface, considerable amounts of sludge then arise, which are physically removed. In some processes, however, the physical removal of sludge is difficult or difficult to carry out, so that it is more advantageous to conduct the phosphating process in such a way that practically no or only a little sludge is formed.
  • the phosphating solution is formulated from chemicals that do not convert the iron that is in solution into the trivalent state. This can be achieved, for example, by using nitrate or similarly weak oxidizing agents as accelerators.
  • urea is to be added to the phosphating bath, as a result of which the temperature during the phosphating can be increased without risking significantly increased sludge formation. Accelerated phosphate layer formation is also associated with this.
  • the other disadvantages mentioned above also remain here.
  • heating of the phosphating solution which is not per se energy-wasting, is required.
  • attempts have been made to solve the sludge problem by increasing its solids content and consequently reducing the amount of sludge (GB-PS 1 555 529).
  • the metal surfaces are treated with a solution which contains at least 6 g / 1 Zn, 5 g / IP 2 O 5 , 1 g / l C10 3 and 8 g / l NO 3 .
  • the ratio P 2 O 5 : Zn should be in the range of 1: (0.8--4).
  • the object of the invention is to provide a process for producing phosphate coatings on iron or steel surfaces which does not have the known, in particular the aforementioned disadvantages, and is simple to carry out without additional chemicals and without sacrificing layer quality.
  • the object is achieved by carrying out the method of the type mentioned at the outset in accordance with the invention in such a way that the surfaces are brought into contact with a solution which contains at least 0.3% by weight of Zn and at least 0.3% by weight of PO 4 and contains at least 0.75% by weight of NO 3 or a similarly acting iron (II) non-oxidizing accelerator, in which the weight ratio Zn: P0 4 is greater than 0.8, the ratio of total acid to free acid is at least 5 and in which an iron (II) content of 0.05 to 1% by weight is set by suitable dimensioning of ClO 3 or an accelerator which oxidizes iron (II) to iron (III).
  • a solution which contains at least 0.3% by weight of Zn and at least 0.3% by weight of PO 4 and contains at least 0.75% by weight of NO 3 or a similarly acting iron (II) non-oxidizing accelerator, in which the weight ratio Zn: P0 4 is greater than 0.8, the ratio of total acid to free acid is at least 5 and in which an iron (II
  • An advantageous embodiment of the invention consists in bringing the surface into contact with a solution which contains a maximum of 2.2% by weight of Zn, max. 2.2% by weight PO 4 and max. Contains 5.5% by weight of NO 3 or an accelerator with the same effect, in which the weight ratio Zn: PO 4 is less than 4 and the ratio of total acid to free acid is max. 30.
  • a treatment solution should preferably be used which contains 0.3 to 1% by weight of Zn, 0.3 to 1% by weight of PO 4 and 1 to 3% by weight of NO 3 or an accelerator with the same effect, in which the Weight ratio Zn: P0 4 0.8 to 2, in particular 0.8 to 1.4 and which is a ratio of total acid to free acid of max. 15, in particular 7 to 12, and in which one by suitable dimensioning of chlorate or an equivalent accelerator sets an iron (II) content of 0.08 to 0.5, in particular up to 0.2,% by weight.
  • nitroguanidine is also suitable, for example.
  • the expenditure of chlorate or an iron (II) which has the same effect as iron (III) oxidizing accelerator is such that its concentration in the treatment solution is generally less than 0.1% by weight (calc ClO 3 ). Higher doses cause the iron (II) content to be too low and considerable sludge formation occurs.
  • chlorate content or an equivalent accelerator is set to concentrations below 0.05% by weight, preferably below 0.035% by weight (calculated as CI0 3 ).
  • CI0 3 concentrations below 0.05% by weight
  • Optimal results are obtained at concentrations in the range of 0.001 to 0.035% by weight (calculated as ClO 3 ).
  • the phosphating bath e.g. does not contain any iron (II) ions in the starting phase. It is therefore not necessary to add the iron (II) oxidizing accelerator at this point. It is also not necessary to meter this accelerator continuously. It can also be introduced with the chemicals that are usually added to the bath supplement.
  • a further development of the method provides for the surfaces to be brought into contact with a solution which additionally contains calcium in quantities of 0.01 to 0.88% by weight, preferably 0.15 to 0.5% by weight.
  • the weight ratio Zn: Ca should be 1.5 to 4. Best results are achieved with a ratio of 2.5.
  • the phosphating solution can also contain other additives which are customary for zinc phosphating solutions, such as copper, cobalt, nickel, simple or complex fluoride. When dosing with fluoride, make sure that no calcium fluoride fails. Magnesium can partially or completely replace calcium.
  • urea can be added to the phosphating solution.
  • the surfaces to be brought into contact with the method according to the invention must be free of rust and scale and should therefore first be pickled with mineral acid, such as hydrochloric or sulfuric acid, and then rinsed with water. Depending on the level of contamination, degreasing or other treatment can also be carried out to clean the surfaces, for example with an organic solvent or an alkaline cleaner, followed by a water rinse.
  • mineral acid such as hydrochloric or sulfuric acid
  • the cleaned surfaces can be subjected to an activation treatment, e.g. B. by hot water rinsing or with a titanium orthophosphate dispersion.
  • an activation treatment e.g. B. by hot water rinsing or with a titanium orthophosphate dispersion.
  • the dipping or flooding of the surfaces which, in contrast to spraying, largely avoids sludge formation due to oxidation by atmospheric oxygen, is carried out according to a preferred embodiment of the process according to the invention at a temperature of 35 to 98 ° C., preferably 55 to 85 ° C.
  • the duration of the Contact between the surface and the phosphating solution is preferably in the range from 5 to 15 minutes.
  • the phosphate coating After the phosphate coating has been formed, it can be rinsed with cold water and treated with a passivating rinse solution. There can also be a lubricant coating on the Phosphate layer can be applied.
  • the method according to the invention has proven particularly useful as a preparation for non-cutting cold forming. However, it is also advantageous in the other fields of application of phosphating, e.g. for corrosion protection, to facilitate sliding friction and for electrical insulation.
  • a phosphating solution was prepared from a batch concentrate which contained and had a ratio of total acid to free acid of 7. The dilution was carried out in the ratio of one part of concentrate to 20 parts of water.
  • Wire was immersed in the phosphating bath kept at a temperature of 70 ° C. After a contact time of 10 minutes, the wire was removed, rinsed with water, provided with a lubricant coating and pulled in the usual way.
  • the phosphating bath could be kept practically constant at concentrations of being held.
  • the ratio of total acid to free acid was 8.7.
  • the process could be operated for a long time with only a small amount of sludge.

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Materials For Medical Uses (AREA)
  • Glass Compositions (AREA)
  • Treatment Of Sludge (AREA)
  • Paints Or Removers (AREA)

Claims (9)

1. Procédé de production de revêtements de phosphate sur des surfaces de fer ou d'acier par le procédé de d'immersion ou d'arrosage avec une solution aqueuse acide de phosphate de zinc, caractérisé en ce qu'on amène les surfaces en contact avec une solution qui contient au moins 0,3% en poids de Zn, au moins 0,3% en poids de P04, et au moins 0,75% en poids de N03 ou d'un accélérateur n'oxydant pas le fer (II) et agissant de la même façon, dans laquelle le rapport pondéral Zn : P04 est supérieur à 0,8, le rapport de l'acidité totale à l'acidité libre est d'aumoins 5 et dans laquelle, par un dosage approprié de ClO3 ou d'un accélérateur oxydant le fer (II) en fer (III) ayant la même action, on ajuste une teneur en fer (II) de 0,05 à 1% en poids.
2.Procédé suivant la revendication 1, caractérisé en ce qu'on amène les surfaces en contact avec une solution qui contient au maximum 2,2% en poids de Zn, au maximum 2,2% en poids de PO4 et au maximum 5,5% en poids de N03 ou d'un accélérateur agissant de la même façon, dans laquelle le rapport pondéral Zn : P04 est inférieur à 4 et le rapport de l'acidité totale à l'acidité libre est de 30 au maximum.
3. Procédé suivant la revendication 1 ou la revendication 2, caractérisé en ce qu'on amène les surfaces en contact avec une solution qui contient 0,3 à 1% en poids de Zn, 0,3 à 1% en poids de PO4 et 1 à 3% en poids de N03 ou d'un accélérateur agissant de la même façon, dans laquelle le rapport pondéral Zn : PO4 est de 0,8 à 2, en particulier de 0,8 à 1,4 et qui présente un rapport à l'acidité totale à l'acidité libre de 15 au maximum, en particulier de 7 à 12, et dans laquelle on ajuste, par un dosage approprié du chlorate ou d'un accélérateur agissant de la même façon, une teneur en Fe (II) de 0,08 à 0,5, en particulier jusqu'à 0,2% en poids.
4. Procédé suivant l'une quelconque des revendications 1, ou 3, caractérisé en ce qu'on amène les surfaces en contact avec une solution qui contient en outre du calcium à raison de 0,1 à 0,88% en poids, de préférence de 0,15 à 0,5% en poids.
5. Procédé suivant l'une quelconque des revendications 1, 2, 3 ou 4, caractérisé en ce qu'on amène les surfaces en contact avec une solution qui contient en outre du cuivre, du cobalt, du nickel, un fluorure simple ou complexe.
6. Procédé suivant l'une quelconque des revendications 1 à 5, caractérisé en ce qu'on amène les surfaces en contact avec la solution à une température de 35 à 98°C, de préférence de 55 à 85°C.
7. Procédé suivant l'une quelconque des revendications 1 à 6, caractérisé en ce qu'on amène les surfaces en contact avec la solution pendant une durée de 5 à 15 minutes.
8. Procédé suivant l'une quelconque des revendications 1 à 7, caractérisé en ce qu'on amène les surfaces en contact avec une solution qui est complétée avec un concentré qui contient:
Figure imgb0008
dans laquelle:
le rapport pondéral Zn : P04 est de 0,3 à 0,6, de préférence de 0,3 à 0,4,
le rapport pondéral Zn : Ca est de 2 à 8, de préférence de 3 à 6,

et le rapport de l'acidité totale à l'acidité libre est de 3 à 6, de préférence de 4 à 5.
9. Utilisation du procédé selon une ou plusieurs des revendications 1 à 8 pour la préparation de sur/faces métalliques au façonnage à froid.
EP81200830A 1980-07-25 1981-07-21 Procédé pour la production de revêtements de phosphate sur les surfaces de fer et d'acier et son usage Expired EP0045110B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81200830T ATE9823T1 (de) 1980-07-25 1981-07-21 Verfahren zur herstellung von phosphatueberzuegen auf eisen- und stahloberflaechen sowie dessen anwendung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB8024465 1980-07-25
GB8024465 1980-07-25

Publications (2)

Publication Number Publication Date
EP0045110A1 EP0045110A1 (fr) 1982-02-03
EP0045110B1 true EP0045110B1 (fr) 1984-10-10

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EP81200830A Expired EP0045110B1 (fr) 1980-07-25 1981-07-21 Procédé pour la production de revêtements de phosphate sur les surfaces de fer et d'acier et son usage

Country Status (8)

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EP (1) EP0045110B1 (fr)
JP (1) JPS5751266A (fr)
AT (1) ATE9823T1 (fr)
DE (1) DE3166602D1 (fr)
ES (1) ES8300874A1 (fr)
GB (1) GB2080835B (fr)
IT (1) IT1167480B (fr)
PT (1) PT73426B (fr)

Families Citing this family (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3244715A1 (de) * 1982-12-03 1984-06-07 Gerhard Collardin GmbH, 5000 Köln Verfahren zur phosphatierung von metalloberflaechen sowie hierfuer geeignete badloesungen
JPS6081850A (ja) * 1983-10-11 1985-05-09 Nec Kansai Ltd 半導体装置の製造方法
DE3407513A1 (de) * 1984-03-01 1985-09-05 Gerhard Collardin GmbH, 5000 Köln Verfahren zur zink-calcium-phosphatierung von metalloberflaechen bei niedriger behandlungstemperatur
DE3636390A1 (de) * 1986-10-25 1988-04-28 Metallgesellschaft Ag Verfahren zur erzeugung von phosphatueberzuegen auf metallen
JPS63270478A (ja) * 1986-12-09 1988-11-08 Nippon Denso Co Ltd リン酸塩化成処理方法
US5236565A (en) * 1987-04-11 1993-08-17 Metallgesellschaft Aktiengesellschaft Process of phosphating before electroimmersion painting
DE3712339A1 (de) * 1987-04-11 1988-10-20 Metallgesellschaft Ag Verfahren zur phosphatierung vor der elektrotauchlackierung
JPH01108754A (ja) * 1987-10-21 1989-04-26 Toshiba Corp 半導体装置用リードフレーム
DE3742634A1 (de) * 1987-12-16 1989-06-29 Collardin Gmbh Gerhard Verfahren zur entschlammung von phosphatierungsbaedern und vorrichtung fuer dieses verfahren
DE3800835A1 (de) * 1988-01-14 1989-07-27 Henkel Kgaa Verfahren zur phosphatierung von metalloberflaechen
EP0327153B1 (fr) * 1988-02-03 1993-08-04 Metallgesellschaft Ag Procédé pour former des couches de phosphates sur des métaux
JPH02101174A (ja) * 1988-10-06 1990-04-12 Nippon Paint Co Ltd 冷間加工用リン酸亜鉛処理方法
DE3840668A1 (de) * 1988-12-02 1990-06-07 Metallgesellschaft Ag Verfahren beim phosphatieren von metalloberflaechen
JPH0375379A (ja) * 1989-05-15 1991-03-29 Nippon Paint Co Ltd 塗装製品、その製造方法、濃厚リン酸塩処理剤および補充用濃厚処理剤
DE4306446A1 (de) * 1993-03-02 1994-09-08 Metallgesellschaft Ag Verfahren zur Erleichterung der Kaltumformung
DE19634685A1 (de) * 1996-08-28 1998-03-05 Metallgesellschaft Ag Wässrige Lösung und Verfahren zur Phosphatierung metallischer Oberflächen
US5954892A (en) * 1998-03-02 1999-09-21 Bulk Chemicals, Inc. Method and composition for producing zinc phosphate coatings on metal surfaces
JP4233565B2 (ja) 2002-07-10 2009-03-04 ヒェメタル ゲゼルシャフト ミット ベシュレンクテル ハフツング 金属表面を被覆する方法
DE10320313B4 (de) * 2003-05-06 2005-08-11 Chemetall Gmbh Verfahren zum Beschichten von metallischen Körpern mit einer Phosphatierungslösung, Phosphatierungslösung und die Verwendung des beschichteten Gegenstandes
CN101665936B (zh) * 2009-09-27 2012-11-28 大连三达奥克化学股份有限公司 钢板工件喷涂涂装前处理常温磷化剂及其制备方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5241735B2 (fr) * 1972-04-27 1977-10-20
DE2540685C2 (de) * 1975-09-12 1985-06-27 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur Herstellung von Phosphatüberzügen
DE2540684A1 (de) * 1975-09-12 1977-03-17 Metallgesellschaft Ag Verfahren zur herstellung von phosphatueberzuegen auf metalloberflaechen

Also Published As

Publication number Publication date
IT8123121A0 (it) 1981-07-24
JPS5751266A (en) 1982-03-26
GB2080835A (en) 1982-02-10
IT1167480B (it) 1987-05-13
ES504609A0 (es) 1982-11-16
ES8300874A1 (es) 1982-11-16
ATE9823T1 (de) 1984-10-15
DE3166602D1 (en) 1984-11-15
PT73426B (en) 1982-08-09
EP0045110A1 (fr) 1982-02-03
PT73426A (en) 1981-08-01
GB2080835B (en) 1984-08-30

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