EP1097255B1 - Verfahren zur vorbehandlung eines metallischen werkstücks für eine lackierung - Google Patents

Verfahren zur vorbehandlung eines metallischen werkstücks für eine lackierung Download PDF

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Publication number
EP1097255B1
EP1097255B1 EP99931072A EP99931072A EP1097255B1 EP 1097255 B1 EP1097255 B1 EP 1097255B1 EP 99931072 A EP99931072 A EP 99931072A EP 99931072 A EP99931072 A EP 99931072A EP 1097255 B1 EP1097255 B1 EP 1097255B1
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EP
European Patent Office
Prior art keywords
workpiece
solution
polyaspartic acid
acid
painted
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
EP99931072A
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German (de)
English (en)
French (fr)
Other versions
EP1097255A1 (de
Inventor
Johannes Lindemann
Karl Manderscheid
Rainer Kluth
Dirk Bohnes
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.)
Aware Chemicals LLC
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Aware Chemicals LLC
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Filing date
Publication date
Application filed by Aware Chemicals LLC filed Critical Aware Chemicals LLC
Publication of EP1097255A1 publication Critical patent/EP1097255A1/de
Application granted granted Critical
Publication of EP1097255B1 publication Critical patent/EP1097255B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
    • C23F11/173—Macromolecular compounds
    • 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
    • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/50—Treatment of iron or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/53—Treatment of zinc or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/56—Treatment of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions

Definitions

  • the invention relates to a method for pretreating a metallic Workpiece for painting, the surface to be painted using a Solution containing degreasing agent cleaned and with a corrosion-resistant layer is coated.
  • the surfaces of metallic workpieces to be painted are before painting to clean and degrease the necessary for permanent painting Requirements for good paint adhesion on the workpiece surface create.
  • the surfaces of the Workpiece with an appropriate degreasing solution treated which is either sprayed onto the surfaces to be painted or which serves as an immersion bath for the workpiece.
  • the workpieces after rinsing to improve corrosion resistance phosphated Following this degreasing the workpieces after rinsing to improve corrosion resistance phosphated.
  • the workpiece surface becomes oxidative due to the phosphating attacked, causing a slight removal of a surface covering layer comes The associated roughening of the surface improves the adhesion of the varnish applied later.
  • To the oxidative surface reaction too finish the workpiece surface in a further treatment step passivated, so that there is an overall laborious pretreatment of the workpiece results
  • the amino acid group can contain aspartic acid among others. If a comparatively low pH of at most 7, those with a such solution treated metallic surface cleaned of corrosion , but this does not result in any corrosion protection required for subsequent painting reached.
  • the invention is therefore based on the object of a method for pretreatment a metallic workpiece for painting the type described above to design that the procedural effort can be significantly reduced, without affecting paint adhesion or endangering corrosion protection.
  • the invention relates to a method for pretreating a metallic Workpiece for painting, the surface to be painted using a Solution containing degreasing agent cleaned and with a Corrosion-resistant layer is coated, characterized in that the varnishing surface of the workpiece to apply a corrosion-inhibiting Layer is treated with a solution of polyaspartic acid.
  • the solution containing a degreasing agent is preferably an aqueous solution of a so-called neutral cleaner or an alkaline Cleaner.
  • Neutral cleaners usually have a pH in the range between about 7 and about 9 and contain nonionic surfactants as degreasing agents.
  • Alkaline cleaners are made by adding alkalis or alkaline Builder substances adjusted to pH values above 8.5.
  • As a degreasing agent preferably contain anionic surfactants.
  • polyaspartic acid or one Aspartic acid-containing copolymer it is meant that the Solution containing free acid and / or acid anions. As is known, it is one Question of the pH of the solution, what ratio of free acid to Acid anions appear.
  • the aspartic acid units in polyaspartic acid can by so-called ⁇ or so-called ⁇ linkage with each other be connected. as a rule, both lie within one polymer strand Link types next to each other. For the present invention that is Ratio of ⁇ - to ⁇ -linkages insignificant.
  • An aspartic acid containing Copolymer is a copolymer in addition to aspartic acid units contains further monomeric assemblies. These can have other amino acids, however also represent polymerizable other carboxylic acids. Preferably you bet Copolymers containing at least 50 mol%, preferably at least 80 mol% consist of aspartic acid.
  • the metal surface coated with a layer of polyaspartic acid can be painted immediately. This means that between treatment with the Solution containing aspartic acid and the painting, if necessary rinsing steps, however, no other processes such as transporting the workpieces another processing facility, forming or joining processes.
  • the treatment described with the solution containing polyaspartic acid can also be used as a temporary corrosion protection measure. This means that they unite the metal surface even without immediate painting gives adequate corrosion protection to the metal workpieces in front of the Transporting, storing, reshaping or joining paint. Find such Processes takes place, is a post-treatment immediately before the final painting with a further solution to reinforce or extend the in step b) corrosion protection effect achieved.
  • This can be, for example are phosphating, treatment with a solution of chromium compounds, a solution of complex fluorides of boron, silicon, titanium and / or Zircon and / or a solution or dispersion of other organic polymers.
  • a solution of chromium compounds a solution of complex fluorides of boron, silicon, titanium and / or Zircon and / or a solution or dispersion of other organic polymers.
  • the surface of the workpiece to be painted for simultaneous degreasing and coating with a solution of polyaspartic acid or an aspartic acid-containing polymer and a degreasing agent is treated.
  • the solution preferably contains a degreasing agent on the basis of iminodisuccinic acid sodium salt.
  • the polyaspartic acid works for the detach the sodium iminosuccinic acid salt from the workpiece surface Fat particles as a dispersant, so that the detached fat particles through this Dispersant kept in dispersion and prevented from re-entering the To set down the workpiece surface.
  • polyaspartic acid does not bring only one Dispersion effect for the fat particles with it, but also requires one Particularly advantageous in terms of the imparting of adhesion, corrosion-inhibiting Surface layer, which are advantageous conditions for a creates permanent paint, especially since the iminodisuccinic acid sodium salt for one appropriate roughening of the workpiece surface ensures.
  • the weight ratio of polyaspartic acid to iminodisuccinic acid sodium salt should be between 10: 1 and 1:10, with a minimum concentration of polyaspartic acid of 2% in the solution to adjust the to achieve the desired effects.
  • the iminodisuccinic acid sodium salt Corresponding additives can of course be added, e.g. B. wetting agents or the like
  • the corrosion protection achieved when degreasing with iminodisuccinic acid sodium salt can be reinforced if necessary, that the surface to be painted of the workpiece after degreasing another treatment in a 10 to 40 percent solution of the polyaspartic acid is subjected to the coating with the organic polymer caused by the polyaspartic acid.
  • the solution obtained from this aftertreatment also be subjected to membrane filtration to the polyaspartic acid after removal of unwanted loads again for the workpiece treatment to be able to use.
  • the system has pretreatment a metallic workpiece, in particular made of sheet metal, a plunge pool 1 for the Workpiece treatment on with an aqueous solution of a degreasing agent based on iminodisuccinic acid sodium salt and a polyaspartic acid is filled.
  • the workpieces to be treated are immersed in this basin 1, to clean and degrease them on the one hand and with a corrosion-inhibiting, to coat organic polymer layer.
  • the through the use of Iminodisuccinic acid sodium salt dissolved fats and impurities are in the Bad kept in dispersion by the polyaspartic acid because the Polyaspartic acid acts as a dispersant.
  • Dip tank 1 connected to a membrane filter device 2, via the in particular the fat particles can be separated from the solution.
  • the Retentate is discharged from the membrane filter device 2 via a drain 3, while the permeate, the organic degreasing agent and Polyaspartic acid contains the via a return line 4 in the circuit again Plunge pool 1 is supplied.
  • the ongoing bath losses are over a Supply line 5 replaced, about the fresh solution of the degreasing agent and Polyaspartic acid can be refilled.
  • the invention is not is limited to the illustrated embodiment.
  • a conventional spray treatment the only decisive factor is that for corrosion protection and the improvement of Adhesion of the paint a polyaspartic acid is used, namely advantageous in combination with a degreasing agent based on Iminodisuccinic sodium salt.
  • the treatment the metal surface with polyaspartic acid or containing an aspartic acid Copolymer as a measure for temporary corrosion protection used.
  • Processing processes such as forming or joining (welding, Flanging). Forming processes through the polymer layer relieved on the metal surface After such processes the Metal surface usually dirty, so that it is before the final Corrosion protection treatment must be cleaned again.
  • the previous one Coating with polyaspartic acid or a containing polyaspartic acid Polymer has the advantage that in such a subsequent cleaning step the impurities can be removed more easily.
  • the surface to be painted is then coated with another one before painting Treated solution that creates a conversion layer on the surface.
  • this can be a layer-forming phosphating, such as in particular in the automotive industry and in the household appliance industry is common.
  • phosphating instead of phosphating, one can Chromating, treatment with a solution of complex fluorides, in particular the elements boron, silicon, titanium and / or zirconium, and / or one Other organic polymers are used.
  • Polymers can be, for example, polymers or copolymers of Acrylic acid or methacrylic acid or around polyvinylphenols.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
EP99931072A 1998-06-24 1999-06-15 Verfahren zur vorbehandlung eines metallischen werkstücks für eine lackierung Expired - Lifetime EP1097255B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT0109198A AT408103B (de) 1998-06-24 1998-06-24 Verfahren zur vorbehandlung eines metallischen werkstückes für eine lackierung
AT109198 1998-06-24
PCT/EP1999/004125 WO1999067442A1 (de) 1998-06-24 1999-06-15 Verfahren zur vorbehandlung eines metallischen werkstücks für eine lackierung

Publications (2)

Publication Number Publication Date
EP1097255A1 EP1097255A1 (de) 2001-05-09
EP1097255B1 true EP1097255B1 (de) 2002-09-04

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Application Number Title Priority Date Filing Date
EP99931072A Expired - Lifetime EP1097255B1 (de) 1998-06-24 1999-06-15 Verfahren zur vorbehandlung eines metallischen werkstücks für eine lackierung

Country Status (10)

Country Link
US (1) US6432220B1 (ja)
EP (1) EP1097255B1 (ja)
JP (1) JP2002518602A (ja)
AT (1) AT408103B (ja)
AU (1) AU4772499A (ja)
BR (1) BR9912205A (ja)
CA (1) CA2335987A1 (ja)
DE (1) DE59902585D1 (ja)
ES (1) ES2183578T3 (ja)
WO (1) WO1999067442A1 (ja)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT407227B (de) * 1998-06-26 2001-01-25 Aware Chemicals Llc Verfahren zum reinigen von lackführenden teilen einer lackieranlage, insbesondere von lackleitungen
EP1293589A3 (en) * 2001-09-17 2004-10-13 Nissan Motor Company, Limited Apparatus for pretreatment prior to painting
DE102004053015A1 (de) * 2004-11-03 2006-05-04 Lanxess Deutschland Gmbh Rußreiniger
JP5179482B2 (ja) 2007-05-09 2013-04-10 株式会社アルバック パージガスアセンブリ
WO2009130248A1 (de) * 2008-04-23 2009-10-29 Martin-Nikolaus Meyn Verfahren zum chemischen entgraten
AT508612B1 (de) * 2009-08-14 2011-05-15 Bohnes Alfred Verfahren zum aufbereiten von umlaufwasser einer lackieranlage
US9290850B2 (en) 2013-10-31 2016-03-22 U.S. Water Services Inc. Corrosion inhibiting methods
WO2016120669A1 (fr) 2015-01-30 2016-08-04 Arcelormittal Procédé de préparation d'une tôle revêtue comprenant l'application d'une solution aqueuse comprenant un aminoacide et utilisation associée pour améliorer la résistance à la corrosion
WO2016120671A1 (fr) * 2015-01-30 2016-08-04 Arcelormittal Procédé de préparation d'une tôle revêtue comprenant l'application d'une solution aqueuse comprenant un aminoacide et utilisation associée pour améliorer les propriétés tribologiques
WO2016120670A1 (fr) * 2015-01-30 2016-08-04 Arcelormittal Procédé de préparation d'une tôle revêtue comprenant l'application d'une solution aqueuse comprenant un aminoacide et utilisation associée pour améliorer la compatibilité avec un adhésif
ES2763038T3 (es) 2015-04-15 2020-05-26 Henkel Ag & Co Kgaa Revestimientos finos protectores contra corrosión que incorporan polímeros de poliamidoamina
CN104845522A (zh) * 2015-04-22 2015-08-19 重庆长安汽车股份有限公司 一种汽车刹车盘的防腐处理方法
CN109778211B (zh) * 2019-03-01 2021-04-20 统崴精密涂装(上海)有限公司 一种电泳前工件脱脂工艺以及脱脂装置
CN110253306B (zh) * 2019-07-09 2024-05-31 江苏金陵体育器材股份有限公司 一种篮球架生产线

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US3578508A (en) * 1967-04-12 1971-05-11 Martin B Pearlman Treatment of ferrous metal surfaces to prevent corrosion
US4299640A (en) * 1980-07-25 1981-11-10 The General Tire & Rubber Company Rubber-brass adhesion improved through treatment of the metal with amino carboxylic acid or salt thereof
US5443651A (en) * 1990-02-06 1995-08-22 Monsanto Company Process for metal cleaning
DE4239076A1 (de) * 1992-11-20 1994-05-26 Basf Ag Mischungen aus Polymerisaten von monoethylenisch ungesättigten Dicarbonsäuren und Polymerisaten ethylenisch ungesättigter Monocarbonsäuren und/oder Polyaminocarbonsäuren und ihre Verwendung
DE4244031A1 (de) * 1992-12-24 1994-06-30 Bayer Ag Verfahren zur Herstellung und Verwendung von Polyasparaginsäure und ihrer Salze
US5401428A (en) * 1993-10-08 1995-03-28 Monsanto Company Water soluble metal working fluids
US5531934A (en) * 1994-09-12 1996-07-02 Rohm & Haas Company Method of inhibiting corrosion in aqueous systems using poly(amino acids)
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US5607623A (en) * 1995-03-08 1997-03-04 Donlar Corporation Inhibition of carbon dioxide corrosion of metals
BR9610062A (pt) * 1995-07-20 1999-03-02 Monsanto Co Fluidos de processamento de metal solúveis em água melhorados
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DE19842053A1 (de) * 1998-09-15 2000-03-23 Bayer Ag Verwendung von Polyasparaginsäuren in Reinigerformulierungen mit abrasiver Wirkung

Also Published As

Publication number Publication date
DE59902585D1 (de) 2002-10-10
JP2002518602A (ja) 2002-06-25
EP1097255A1 (de) 2001-05-09
ES2183578T3 (es) 2003-03-16
US6432220B1 (en) 2002-08-13
BR9912205A (pt) 2001-04-10
AT408103B (de) 2001-09-25
AU4772499A (en) 2000-01-10
WO1999067442A1 (de) 1999-12-29
ATA109198A (de) 2001-01-15
CA2335987A1 (en) 1999-12-29

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