EP0367653A1 - Verfahren zur Beschichtung eines Metallsubstrats mit Pulvergrundierungsschicht und mittels Tauchen angebrachte Oberflächenbeschichtung, Grundierungszusammensetzung und so erhaltene Materialien - Google Patents

Verfahren zur Beschichtung eines Metallsubstrats mit Pulvergrundierungsschicht und mittels Tauchen angebrachte Oberflächenbeschichtung, Grundierungszusammensetzung und so erhaltene Materialien Download PDF

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Publication number
EP0367653A1
EP0367653A1 EP19890402897 EP89402897A EP0367653A1 EP 0367653 A1 EP0367653 A1 EP 0367653A1 EP 19890402897 EP19890402897 EP 19890402897 EP 89402897 A EP89402897 A EP 89402897A EP 0367653 A1 EP0367653 A1 EP 0367653A1
Authority
EP
European Patent Office
Prior art keywords
powder
primer
coating
substrate
epoxy resin
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
EP19890402897
Other languages
English (en)
French (fr)
Other versions
EP0367653B2 (de
EP0367653B1 (de
Inventor
Jean-Yves Dutheil
Eric Perraud
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.)
Arkema France SA
Original Assignee
Elf Atochem SA
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
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Application filed by Elf Atochem SA filed Critical Elf Atochem SA
Publication of EP0367653A1 publication Critical patent/EP0367653A1/de
Application granted granted Critical
Publication of EP0367653B1 publication Critical patent/EP0367653B1/de
Publication of EP0367653B2 publication Critical patent/EP0367653B2/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/52—Two layers
    • B05D7/54—No clear coat specified
    • B05D7/546—No clear coat specified each layer being cured, at least partially, separately
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
    • B05D1/22—Processes for applying liquids or other fluent materials performed by dipping using fluidised-bed technique
    • B05D1/24—Applying particulate materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/56—Three layers or more
    • B05D7/58—No clear coat specified
    • B05D7/587—No clear coat specified some layers being coated "wet-on-wet", the others not
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2202/00—Metallic substrate
    • B05D2202/10—Metallic substrate based on Fe
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2451/00—Type of carrier, type of coating (Multilayers)

Definitions

  • the present invention relates to a method for coating a metal substrate using a surface coating applied by dipping after coating said substrate with a powdered primer.
  • the soaking process in a fluidized bed requires a preliminary preheating of the metal part to be coated before its immersion in the tank with a porous bottom in which the powder of the coating in suspension is kept in suspension by air circulation: the powder then melts at contact with hot metal surfaces and forms a deposit, the thickness of which depends on the temperature of the substrate and its duration of immersion in the powder.
  • the part is preheated in an oven at a temperature determined according to the nature and thickness of the part to be coated.
  • an excessively high preheating temperature can be harmful, more particularly in the case where the metal part has previously been coated with an adhesion primer which can deteriorate during the passage of the part in the oven and / or no longer ensuring adhesion with the surface coating and the metal substrate.
  • the adhesion primers for surface coatings applied by dipping are exclusively in liquid form, that is to say the resins of the primer are either in suspension or in solution in one or more solvents.
  • the coating of metal substrates with these liquid primers is done for example using a pneumatic gun.
  • adhesion primers developed by the applicant are in the form of powder compositions, which can be applied as they are to metallic substrates.
  • the process for coating metallic substrates developed by the applicant implements: - a powder adhesion primer based on epoxy resin (s) and epoxy resin hardener (s), - And a surface coating applied by soaking in a fluidized bed.
  • the metal substrate which has previously been able to undergo one or more surface treatments such as alkaline degreasing, brushing, shot blasting, hot rinsing, etc., is coated with one or more layers of powder adhesion primer.
  • the metal substrate can be chosen from a wide range of products. These can be ordinary or galvanized steel parts, aluminum or aluminum alloy parts, the steel parts being more particularly targeted for the invention.
  • the thickness of the metal substrate is not critical in itself, it will most often be between 1 and 50 mm.
  • the application of the powder primer composition according to the invention can be carried out according to the powder application techniques usually used.
  • the powder application techniques there may be mentioned electrostatic spraying, a technique particularly preferred for the application of primer according to the invention, soaking in a fluidized bed.
  • the powder is introduced into a gun where it is conveyed by compressed air and passes through a nozzle brought to a high potential, generally between ten and one hundred kilovolts.
  • the applied voltage can be of positive or negative polarity, negative polarity being generally preferred.
  • the powder flow in the gun is generally between 10 and 200 g / min.
  • powders with an average particle size of between 5 and 100 ⁇ m, and preferably between 5 and 80 ⁇ m, can be used.
  • the average thickness of the primer can be between 5 and 60 ⁇ m, and preferably between 10 and 20 ⁇ m.
  • the powder compositions which constitute the adhesion primer according to the invention are based on solid thermosetting resins and preferably based on epoxy resins and epoxy resin hardener (s).
  • thermosetting resin is meant in the present description epoxy resins, phenolic resins, epoxyphenolic precondensates, alone or as a mixture.
  • epoxy resins By way of example of advantageously preferred epoxy resins, mention may be made of the products obtained by reaction of bisphenol-A and of epichlorohydrin and the degree of polymerization of which is greater than two, as well as the high molecular weight polycondensates of phenoxy type without free reactive group.
  • phenolic resins examples include the resins obtained by polycondensation of formaldehyde and of a phenol.
  • amine-type compound means aliphatic or aromatic amines and their derivatives, such as dicyandiamide, benzyldimethylamine, boron trifluoride monoethylamine.
  • acid anhydride By way of example of acid anhydride, mention may be made of aromatic anhydrides such as phthalic anhydride or cycloaliphtalic anhydrides such as hexahydrophthalic anhydride.
  • isocyanate type compound means a monomer, prepolymer or polymer compound containing at least two free or blocked isocyanate groups.
  • Polyisocyanate compounds with an aromatic or aliphatic structure whose isocyanate groups are blocked by condensation with phenol or caprolactam are particularly preferred.
  • the proportion of epoxy resin (s) and hardener (s) of the amine, acid anhydride or isocyanate type must be such that the number of epoxy functions is equal to the number of reactive functions of the amine of the acid anhydride or of the isocyanate compound.
  • the primers in accordance with the invention may also contain various additives and agents, alone or as a mixture, such as pigments, fillers, corrosion inhibiting agents, etc.
  • additives and agents such as pigments, fillers, corrosion inhibiting agents, etc.
  • strontium chromate such as strontium chromate.
  • zinc phosphate titanium dioxide
  • silica such as silica
  • the substrate is placed in an oven where it is heated to a determined temperature depending in particular on the nature of said substrate, its shape and the desired coating thickness.
  • the energy stored during the passage through the oven of the substrate coated with primer allows, in addition to the crosslinking of the primer, the melting and the adhesion of the surface coating applied by dipping on the substrate as soon as it leaves the oven.
  • the powder adhesion primers developed by the applicant resist particularly well at the high temperatures which may be necessary to ensure effective preheating of the substrate to be coated.
  • the powder primers according to the invention can not only be heated to 270-320 ° C, but they can, without damage to the quality of the final coating, undergo heating at higher temperatures, such as for example between 320 and 380 ° C, when necessary.
  • the average residence time of the substrate in the oven is generally between 1 and 30 min and preferably between 3 and 10 min.
  • the substrate is immersed in a soaking tank containing the surface coating as defined above.
  • the surface coatings in powder form, applied by dipping and in accordance with the invention are preferably based on polyamide and / or polyetheresteramide.
  • polyamide entering the powder surface coating is meant the aliphatic polyamides obtained from lactams or amino acids whose hydrocarbon chain has a number of carbon atoms between 4 and 20 such as, for example, caprolactam, enantholactam, dodecalactam, undecanolactam, 11-undecanoic amino acid, 12-dodecanoic amino acid, the condensation products of a dicarboxylic acid with a diamine such as, for example, polyamides 6.6 , 6.10, 6.12, 9.6, (products of the condensation of hexamethylene diamine with adipic acid, azelaic acid, sebacic acid, dodecanedioic acid-1,12 and nonamethylene diamine with acid adipic), the copolyamides resulting from the polymerization of the various monomers mentioned above or the mixtures of several polyamides mentioned above.
  • polyamide 11 obtained by polycondensation of amino-11 undecanoic acid
  • polyamide 12 obtained by polycondensation of 12-amino-dodecanoic acid or of dodecanolactam
  • copolyamides obtained by the polymerization of the monomers mentioned above.
  • the inherent viscosity (measured at 20 ° C for a solution of 0.5 g per 100 g of metacresol) of the polyamides can be between 0.20 and 2.0, and preferably between 0.60 and 1.30 dlg ⁇ 1.
  • polyamides also means semi-aromatic amorphous polyamides, and in particular as defined in French patents FR 1,588,130, 2,324,672 and 2,575,756, in European patent EP 53,876, in Japanese patents 59,015,447 and 60,217,237.
  • polyetheresteramides is intended to mean both the random polyetheresteramides (that is to say formed by the random sequence of the various monomer components) and the block polyetheresteramides, that is to say formed from blocks having a certain length of chain. their various constituents.
  • Polyetheresteramides are products of the copolycondensation of polyamide blocks with reactive ends with polyether sequences with reactive ends such as: - polyamide sequences for dicarboxylic chain ends with polyetherdiol sequences.
  • the number-average molecular mass of these polyamide blocks is generally between 500 and 10,000 and more particularly between 600 and 5,000.
  • the polyamide blocks of the polyetheresteramides are preferably formed from polyamide 6, 6.6, 6.12, 11 or 12 or from copolyamides resulting from the polycondensation of their monomers.
  • the number average molecular weight of the polyethers is generally between 200 and 6000 and more particularly between 600 and 3000.
  • the polyether blocks preferably consist of polytetramethylene glycol (PTMG), polypropylene glycol (PPG), or polyethylene glycol (PEG).
  • PTMG polytetramethylene glycol
  • PPG polypropylene glycol
  • PEG polyethylene glycol
  • the inherent viscosity of polyetheresteramides is advantageously between 0.8 and 2.05, and preferably between 0.80 and 1.20.
  • the inherent viscosity is measured in metacresol at 25 ° C with an initial concentration of 0.5 g per 100 g of metacresol. It is expressed in dlg ⁇ 1.
  • the polyetheresteramides according to the invention can be formed from 5 to 85% by weight of polyether and from 95 to 15% by weight of polyamide, and preferably from 30 to 80% by weight of polyether and from 70 to 20% by weight of polyamide.
  • the particle size of the surface coating powders can be between 20 and 300 ⁇ m, and preferably between 40 and 200 ⁇ m.
  • the soaking technique according to the invention is carried out in a non-electrostatic fluidized bed, the electrostatic fluidized beds being unsuitable and difficult to use for soaking in powders based on polyamide and / or polyetheresteramide which are particularly preferred by the applicant. .
  • the thickness of the surface coating can be between 150 and 600 ⁇ m, and preferably between 200 and 400 ⁇ m.
  • the substrate is cooled, for example with ambient air, by immersion in water or in any other suitable solvent, after having possibly undergone a post-melting.
  • the metal substrate consists of a steel plate 1 mm thick. This plate has previously been degreased and then shot blasted. 2 °)
  • the particle size of the primer composition is less than 80 ⁇ m. 3)
  • the surface coating consists of PA-11, in the form of a powder with a particle size between 40 and 200 ⁇ m. The inherent viscosity of PA-11, measured at 20 ° C for a solution of 0.5 g of polymer in 100 g of m-cresol, is equal to 1.
  • the powdered primer composition as described in A. 2 °) is deposited at room temperature on the steel plate by electrostatic spraying under a negative electrostatic charge of 40 kV, the metal surface being at potential O.
  • the substrate thus coated passes through an oven maintained at 380 ° C where it remains for 3 min.
  • the substrate thus coated is removed from the soaking tank and then cooled in air after post-melting.
  • the metal substrate is a sandblasted steel plate and the surface coating has the same characteristics as those of EXAMPLE 1.
  • the substrate is coated with the primer by electrostatic spraying under the same conditions as in 1.B.
  • the material obtained is a composite comprising successively: - a sandblasted steel plate (thickness 3 mm) - a primer layer of average thickness equal to 20 ⁇ m - a surface coating layer of thickness between 200 and 250 ⁇ m.
  • the materials undergo an adhesion test carried out according to standard NF T 58-112 and a salt spray aging test carried out according to standard NF X 41-002.
  • EXAMPLE 1 The test of EXAMPLE 1 is repeated using a powdered primer which comprises (in g).
  • A) - modified novolak epoxy resin (epoxy equivalent weight: 500-575; softening point between 90 and 98 ° C; d 1.19) 92 - micronized dicyandiamide 8
  • B) - poly p. vinylphenol Mw between 2000 and 30000, of epoxy equivalent weight 120 and having a softening weight between 140 and 210 ° C. 100
  • the metal substrate and the surface coating have the same characteristics as in EXAMPLE 2 and the conditions for placing work and evaluation of the materials obtained are identical to those described in EXAMPLE 2.
  • liquid primer which comprises the following resins: - epoxy resin obtained by reaction of epichlorohydrin and bisphenol A whose molecular mass is between 3000 and 3800 g and the weight of epoxide equivalent between 1600 and 4000. - resol phenophenol type resin - aminoplast melamine-formaldehyde resin dissolved in a mixture of ethylene glycol, solvent naphtha, butanol, isobutanol and methyl isobutyl ketone.
  • the metal substrate and the surface coating have the same characteristics as those of EXAMPLE 1.
  • the material obtained is such that the initial adhesion of the coating is zero (Class O) and the corrosion path is complete in a few hours.
  • a two-layer coating comprising - an epoxy undercoat (42% of the total thickness of the coating) - a polyamide layer, the total thickness of the coating being equal to 260 ⁇ m.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)
  • Laminated Bodies (AREA)
EP89402897A 1988-11-03 1989-10-20 Verfahren zur Beschichtung eines Metallsubstrats mit Pulvergrundierungsschicht und mittels Tauchen angebrachte Oberflächenbeschichtung und so erhaltene Materialien Expired - Lifetime EP0367653B2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8814332A FR2638466B1 (fr) 1988-11-03 1988-11-03 Procede pour revetir des substrats metalliques a l'aide d'un primaire en poudre et d'un revetement superficiel applique par trempage, compositions de primaire en poudre utilisees et materiaux composites obtenus
FR8814332 1988-11-03

Publications (3)

Publication Number Publication Date
EP0367653A1 true EP0367653A1 (de) 1990-05-09
EP0367653B1 EP0367653B1 (de) 1993-05-19
EP0367653B2 EP0367653B2 (de) 2001-11-21

Family

ID=9371527

Family Applications (1)

Application Number Title Priority Date Filing Date
EP89402897A Expired - Lifetime EP0367653B2 (de) 1988-11-03 1989-10-20 Verfahren zur Beschichtung eines Metallsubstrats mit Pulvergrundierungsschicht und mittels Tauchen angebrachte Oberflächenbeschichtung und so erhaltene Materialien

Country Status (14)

Country Link
US (1) US5891515A (de)
EP (1) EP0367653B2 (de)
JP (1) JPH0755306B2 (de)
AT (1) ATE89496T1 (de)
AU (1) AU628877B2 (de)
CA (1) CA2002109C (de)
DE (1) DE68906643T3 (de)
DK (1) DK174338B1 (de)
ES (1) ES2055133T5 (de)
FI (1) FI100661B (de)
FR (1) FR2638466B1 (de)
IE (1) IE63336B1 (de)
NO (1) NO306956B1 (de)
PT (1) PT92182B (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997037776A1 (en) * 1996-04-08 1997-10-16 E.I. Du Pont De Nemours And Company Process for coating a substrate
WO2000076677A1 (fr) * 1999-06-15 2000-12-21 Atofina Procede de recouvrement d'un objet par un film et appareillage pour la mise en oeuvre de ce procede
WO2006091440A1 (en) * 2005-02-23 2006-08-31 Ppg Industries Ohio, Inc. Methods of forming composite coatings
WO2011092444A1 (fr) 2010-02-01 2011-08-04 Arkema France Poudre a base de polyamide et procede de revetement d'objet par fusion de ladite poudre

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US6080310A (en) * 1999-03-17 2000-06-27 Alliedsignal Inc. Method of applying a slip-resistant coating to a spin-on filter using a fluidized bed coating apparatus, and spin-on filter which is a product thereof
US6692817B1 (en) 2000-04-04 2004-02-17 Northrop Grumman Corporation Apparatus and method for forming a composite structure
US6746719B2 (en) * 2000-10-13 2004-06-08 Atofina Chemicals, Inc. Process of priming a metal surface for attaching resin systems thereto utilizing aqueous emulsion of a polyfunctional epoxide compound as the primer
US20030068434A1 (en) * 2001-08-21 2003-04-10 Moore James B. Method for bonding thermoplastic films to metal surfaces of cylinders, vessels and component parts
US6537610B1 (en) * 2001-09-17 2003-03-25 Springco Metal Coating, Inc. Method for providing a dual-layer coating on an automotive suspension product
SE526172C2 (sv) * 2003-05-08 2005-07-19 Saab Ab Metod för behandling av en yta
DE10322678A1 (de) * 2003-05-20 2004-12-09 BSH Bosch und Siemens Hausgeräte GmbH Verfahren zur Sinterbeschichtung
JP4907054B2 (ja) * 2003-12-09 2012-03-28 中央発條株式会社 高耐久性ばねおよびその塗装方法
US7235278B2 (en) * 2004-03-31 2007-06-26 Mcneil-Ppc, Inc. Method and apparatus for applying particulate material to a substrate
EP3778809B1 (de) 2004-10-20 2023-04-26 Swimc Llc Beschichtungszusammensetzung für dosen und verfahren zur beschichtung
GB2428395B (en) * 2005-07-19 2007-09-05 Ian Webb A process of powder coating and a powder coating apparatus
WO2007048094A2 (en) * 2005-10-18 2007-04-26 Valspar Sourcing, Inc. Coating compositions for containers and methods of coating
CN102227515B (zh) 2008-11-27 2013-08-21 新日铁住金株式会社 电磁钢板及其制造方法
JP5721330B2 (ja) * 2010-01-27 2015-05-20 藤倉化成株式会社 ベースコート塗料組成物、および複合塗膜とその製造方法
JP5606807B2 (ja) * 2010-06-14 2014-10-15 中央発條株式会社 粉体塗装方法
CN103143488B (zh) * 2011-12-06 2014-10-22 苏州汉扬精密电子有限公司 塑胶与金属结合件的表面涂装方法
JP6132153B2 (ja) * 2013-07-18 2017-05-24 株式会社ジェイテクト 摺動軸およびステアリング装置
IT201900007422A1 (it) * 2019-05-28 2020-11-28 Sercolor Srl Un metodo e relativo macchinario per la realizzazione di un effetto di corrosione su pezzi metallici
EP3851211A1 (de) * 2020-01-14 2021-07-21 Triarca A/S Oberflächenbeschichtung von elektrischen gehäusen

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FR2340140A1 (fr) * 1976-02-05 1977-09-02 Canada Wire & Cable Co Ltd Revetements protecteurs en films minces appliques par depot electrostatique de poudre

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US3502492A (en) * 1965-12-13 1970-03-24 Ransburg Electro Coating Corp Metal substrate coated with epoxy powder primer and plasticized polyvinyl chloride topcoat and method of making same
FR2340140A1 (fr) * 1976-02-05 1977-09-02 Canada Wire & Cable Co Ltd Revetements protecteurs en films minces appliques par depot electrostatique de poudre

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997037776A1 (en) * 1996-04-08 1997-10-16 E.I. Du Pont De Nemours And Company Process for coating a substrate
WO2000076677A1 (fr) * 1999-06-15 2000-12-21 Atofina Procede de recouvrement d'un objet par un film et appareillage pour la mise en oeuvre de ce procede
FR2795004A1 (fr) * 1999-06-15 2000-12-22 Atofina Procede de recouvrement d'un objet par un film et appareillage pour la mise en oeuvre de ce procede
US6506455B1 (en) 1999-06-15 2003-01-14 Atofina Triboelectric fluidizded bed method and apparatus for coating an object
WO2006091440A1 (en) * 2005-02-23 2006-08-31 Ppg Industries Ohio, Inc. Methods of forming composite coatings
US7507440B2 (en) 2005-02-23 2009-03-24 Ppg Industries Ohio, Inc. Methods of forming composite coatings
WO2011092444A1 (fr) 2010-02-01 2011-08-04 Arkema France Poudre a base de polyamide et procede de revetement d'objet par fusion de ladite poudre

Also Published As

Publication number Publication date
IE63336B1 (en) 1995-04-19
DK546089A (da) 1990-05-04
JPH0755306B2 (ja) 1995-06-14
DE68906643T3 (de) 2002-05-29
CA2002109A1 (fr) 1990-05-03
DK546089D0 (da) 1989-11-02
EP0367653B2 (de) 2001-11-21
DE68906643D1 (de) 1993-06-24
ES2055133T3 (es) 1994-08-16
FI100661B (fi) 1998-01-30
NO894344D0 (no) 1989-11-01
US5891515A (en) 1999-04-06
FI895222A0 (fi) 1989-11-02
JPH02258084A (ja) 1990-10-18
IE893536L (en) 1990-05-03
DK174338B1 (da) 2002-12-16
CA2002109C (fr) 1999-02-16
AU628877B2 (en) 1992-09-24
PT92182B (pt) 2001-05-31
ES2055133T5 (es) 2002-05-01
NO894344L (no) 1990-05-04
FR2638466A1 (fr) 1990-05-04
DE68906643T2 (de) 1993-10-07
PT92182A (pt) 1990-05-31
ATE89496T1 (de) 1993-06-15
NO306956B1 (no) 2000-01-17
FR2638466B1 (fr) 1993-05-07
EP0367653B1 (de) 1993-05-19
AU4397989A (en) 1990-05-10

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