EP0039093B1 - Procédé de phosphatation des surfaces de métaux et application de ce procédé - Google Patents

Procédé de phosphatation des surfaces de métaux et application de ce procédé Download PDF

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Publication number
EP0039093B1
EP0039093B1 EP81200286A EP81200286A EP0039093B1 EP 0039093 B1 EP0039093 B1 EP 0039093B1 EP 81200286 A EP81200286 A EP 81200286A EP 81200286 A EP81200286 A EP 81200286A EP 0039093 B1 EP0039093 B1 EP 0039093B1
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EP
European Patent Office
Prior art keywords
solutions
metal surfaces
phosphating
ratio
brought
Prior art date
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Expired
Application number
EP81200286A
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German (de)
English (en)
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EP0039093A1 (fr
Inventor
Dieter Hauffe
Gerhard Müller
Werner Dr. Dipl.-Chem. Rausch
Gudrun Volling
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.)
GEA Group AG
Continentale Parker Ste
Continentale Parker SA
Original Assignee
Metallgesellschaft AG
Continentale Parker Ste
Continentale Parker SA
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Application filed by Metallgesellschaft AG, Continentale Parker Ste, Continentale Parker SA filed Critical Metallgesellschaft AG
Priority to AT81200286T priority Critical patent/ATE5332T1/de
Publication of EP0039093A1 publication Critical patent/EP0039093A1/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

Definitions

  • the invention relates to a process for phosphating metals, in particular iron and steel, with aqueous acidic oxidizing agent-containing zinc phosphate solutions, and to the use thereof for preparing the metal surfaces for electrocoating.
  • the reduced zinc content compared to the usual phosphating baths leads to improved thin and uniform phosphate coatings on metal surfaces, especially on iron and steel. These coatings are very adhesive and permanent and are particularly suitable as a basis for the subsequent electrocoating.
  • the object of the invention is to provide a method which avoids the known disadvantages, particularly those mentioned with reference to DE-OS 22 32 067, and leads to phosphate layers which, while maintaining the very good properties of the layers, eg. B. as the basis for a subsequent lacquer finish, the desired wet corrosion resistance of the phosphate layers.
  • the object is achieved by designing the method of the type mentioned at the outset in accordance with the invention in such a way that the metal surfaces are brought into contact with solutions which included, in which the weight ratio of Zn to Ni between 1: (0 to 1.5) and the weight ratio of Zn to P 2 O 5 between 1: (9 to 85) is set and in which the ratio required for phosphating of Free to total P 2 O 5 is essentially adjusted by alkali metal ions.
  • iron and steel are treated with the method according to the invention.
  • it is also suitable for the phosphating of zinc and aluminum materials as well as for steel with coatings made of zinc, zinc alloys, aluminum and aluminum alloys produced using a wide variety of processes.
  • the metal surfaces can be treated by spraying, flooding and also immersion. However, it is also with combined working methods, e.g. B. splash-dip-spray, flood-dive and the like applicable.
  • the contact times for the phosphating solution with the metal surface are in the usual range and can, for. B. for spraying 45 sec to 3 min, for diving 2 to 5 min and for spray-immersion spraying 20 sec spraying, 3 min diving, 20 sec spraying.
  • the bath temperatures are usually 40 to 70 ° C, preferably 50 to 60 ° C. If the contact times are extended, however, they can also be reduced to 30 ° C and below.
  • the phosphating bath essentially only contains alkali metal ions, in such an amount as is necessary to adjust the ratio of free to total P 2 0 5 required for the phosphating.
  • This acid ratio is generally between 0.04 and 0.09, and it increases with increasing bath temperature, increasing total concentration and increasing amount of zinc in relation to P 2 0 5 .
  • small quantities may also be present; these include in particular ammonium, calcium, manganese, copper and cobalt.
  • nickel to the bath has a favorable effect on the rate of phosphating, the formation of layers on steel surfaces that are more difficult to phosphate and on the phosphating of zinc surfaces.
  • the nickel concentration is not more than 1.5 times the zinc concentration.
  • the known advantage of the weight ratio of Zn to P 2 0 5 should lie in particular in the fact that, compared to phosphating processes based on zinc phosphate, in which the ratio of Zn to P 2 O 5 is higher, a zinc phosphate coating with a higher iron content is formed, which is more acid-resistant is. This will decrease the amount of phosphate coating detachment that occurs e.g. B. occurs when the pH value at the electrodeposition at the interface decreases. As a result, smaller amounts of layers get into the paint film, so. that the associated adverse influence on the film is significantly reduced. Since the solutions according to the invention lead to uniformly fine coatings with a low layer weight, the electrical resistance at the interface is lower, so that the paint film is deposited in a particularly adhesive manner.
  • the concentration is usually between 50 and 500 mg / l, the low to medium concentrations being preferably used at working temperatures of 50 to 60 ° C., while the higher contents are used at lower bath temperatures.
  • nitrobenzenesulfonate which e.g. B. is used in concentrations between 200 and 2,000 mg / I. The best results are generally found at levels of 300 to 700 mg / l.
  • the addition of simple and / or complex fluorides can improve the layer formation. So the baths SiF 6 - , z. B. in amounts up to 1.5 g / I, and / or F - , z. B. in amounts up to 0.8 g / l.
  • the use of other complex fluorides, e.g. B. BF 4 - is possible.
  • the phosphate layers produced by the method according to the invention are suitable in principle for all types of use of the phosphate layers known to date. In particular, however, they have proven themselves as a preparation for electrocoating, the best results being achieved in connection with cathodic electrocoating.
  • the method according to the invention finds practical application e.g. B. for the phosphating of car bodies.
  • Sheet steel test specimens degreased with mildly alkaline aqueous spray and dip cleaner at 60 ° C. and for 3 minutes were rinsed in water, then firstly sprayed for 20 seconds and then treated with dip at 55 ° C. for 180 seconds with the following phosphating bath:
  • This bath has the following titration data:
  • test specimens were then rinsed with water, rinsed with a chrome-containing rinse solution and dried.
  • the phosphate layers were uniformly gray opaque, extraordinarily fine crystalline and had a weight per unit area of 1.8 g / m 2 . This also applied to the surfaces of the test specimen that were created by the special treatment form was not hit by the spray jet, but was only treated in diving. The test specimens could be exposed to the nitrous gas-containing vapor space above the phosphating bath significantly more than 1 min after the phosphating, without rusting the surface. Test specimens which were phosphated in the claimed amounts without the addition of N0 3 and ClO 3 proved to be particularly sensitive to rust, particularly in the places accessible only by immersion treatment.
  • Example 1 The results mentioned in Example 1 were also achieved with this process.

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  • 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)
  • Catalysts (AREA)
  • Saccharide Compounds (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Glass Compositions (AREA)
  • Laminated Bodies (AREA)
  • Secondary Cells (AREA)
  • Materials For Medical Uses (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Claims (5)

1. Procédé de phosphatation de métaux, en particulier l'acier et le fer, avec des solutions aqueuses acides de phosphate de zinc contenant des oxydants, caractérisé en ce qu'on met en contact les surfaces métalliques avec des solutions qui contiennent :
Figure imgb0007
et dans lesquelles le rapport pondéral de Zn à Ni est ajusté entre 1 : (0 à 1,5) et le rapport pondéral Zn à P2O5 entre 1 : (9 à 85) et dans lesquelles le rapport du P2O5 libre au P2O5 total exigé par la phosphatation est essentiellement ajusté par des ions de métaux alcalins.
2. Procédé suivant la revendication 1, caractérisé en ce que les surfaces métalliques sont mises en contact avec des solutions qui contiennent en outre un nitrite de métal alcalin, de préférence en des quantités (calculées en NaN02) de 50 à 500 mg/1.
3. Procédé suivant la revendication 1, caractérisé en ce que les surfaces métalliques sont mises en contact avec des solutions qui contiennent en outre des composés nitrés organiques, en particulier un nitrobenzènesulfonate, dans des proportions de préférence de 200 à 2 000 mg/1.
4. Procédé suivant la revendication 1 ou 2, caractérisé en ce que les surfaces métalliques sont mises en contact avec des solutions qui contiennent en outre des fluorures simples et/ou complexes, par exemple jusqu'à 1,5 g/I de SiF6 et/ou jusqu'à 0,8 g/1 de F.
5. Utilisation du procédé suivant les revendications .1, 2, 3 ou 4, pour la préparation de surfaces métalliques en vue de la peinture par électro-immersion, en particulier en vue de la peinture par électro-immersion cathodique.
EP81200286A 1980-04-30 1981-03-13 Procédé de phosphatation des surfaces de métaux et application de ce procédé Expired EP0039093B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81200286T ATE5332T1 (de) 1980-04-30 1981-03-13 Verfahren zur phosphatierung von metalloberflaechen sowie dessen anwendung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19803016576 DE3016576A1 (de) 1980-04-30 1980-04-30 Verfahren zur phosphatierung von metalloberflaechen sowie dessen anwendung
DE3016576 1980-04-30

Publications (2)

Publication Number Publication Date
EP0039093A1 EP0039093A1 (fr) 1981-11-04
EP0039093B1 true EP0039093B1 (fr) 1983-11-16

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ID=6101283

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EP81200286A Expired EP0039093B1 (fr) 1980-04-30 1981-03-13 Procédé de phosphatation des surfaces de métaux et application de ce procédé

Country Status (8)

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EP (1) EP0039093B1 (fr)
AT (1) ATE5332T1 (fr)
BR (1) BR8102619A (fr)
DE (2) DE3016576A1 (fr)
ES (1) ES501701A0 (fr)
GB (1) GB2074611B (fr)
IT (1) IT1207959B (fr)
PT (1) PT72944B (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4498935A (en) * 1981-07-13 1985-02-12 Parker Chemical Company Zinc phosphate conversion coating composition
US4486241A (en) * 1981-09-17 1984-12-04 Amchem Products, Inc. Composition and process for treating steel
DE3311738A1 (de) * 1983-03-31 1984-10-04 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur phosphatierung von metalloberflaechen
DE3325974A1 (de) * 1983-07-19 1985-01-31 Gerhard Collardin GmbH, 5000 Köln Verfahren und universell anwendbare mittel zum beschleunigten aufbringen von phosphatueberzuegen auf metalloberflaechen
GB2148950B (en) * 1983-10-26 1987-02-04 Pyrene Chemical Services Ltd Phosphating composition and processes
GB8329250D0 (en) * 1983-11-02 1983-12-07 Pyrene Chemical Services Ltd Phosphating processes
DE3408577A1 (de) * 1984-03-09 1985-09-12 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur phosphatierung von metallen
JP2695963B2 (ja) * 1990-03-16 1998-01-14 マツダ株式会社 金属表面のリン酸塩処理方法
JPH07173643A (ja) * 1993-12-21 1995-07-11 Mazda Motor Corp 金属表面の燐酸塩処理方法及び処理液
DE4443882A1 (de) * 1994-12-09 1996-06-13 Metallgesellschaft Ag Verfahren zum Aufbringen von Phosphatüberzügen auf Metalloberflächen
EP1666745B1 (fr) 2003-09-16 2016-11-09 NTN Corporation Roulement a aiguilles du type coque, structure de support pour arbre principal de compresseur, et structure de support pour section d'entrainement d'une pompe a piston

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT211625B (de) * 1956-01-25 1960-10-25 Metallgesellschaft Ag Verfahren zur Vobenhandlung von Bandstahl für das Kaltwalzen durch Aufbringen eines Zinkphosphatüberzuges
DE2540685C2 (de) * 1975-09-12 1985-06-27 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur Herstellung von Phosphatüberzügen

Also Published As

Publication number Publication date
GB2074611A (en) 1981-11-04
IT8121425A0 (it) 1981-04-29
ATE5332T1 (de) 1983-12-15
DE3161398D1 (en) 1983-12-22
ES8207233A1 (es) 1982-09-16
PT72944A (fr) 1981-05-01
DE3016576A1 (de) 1981-11-05
ES501701A0 (es) 1982-09-16
PT72944B (fr) 1982-03-26
GB2074611B (en) 1984-10-03
IT1207959B (it) 1989-06-01
BR8102619A (pt) 1982-01-19
EP0039093A1 (fr) 1981-11-04

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