EP0015020B1 - Procédé de traitement de surfaces de métaux et son utilisation pour le traitement de surfaces en aluminium - Google Patents

Procédé de traitement de surfaces de métaux et son utilisation pour le traitement de surfaces en aluminium Download PDF

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Publication number
EP0015020B1
EP0015020B1 EP80200096A EP80200096A EP0015020B1 EP 0015020 B1 EP0015020 B1 EP 0015020B1 EP 80200096 A EP80200096 A EP 80200096A EP 80200096 A EP80200096 A EP 80200096A EP 0015020 B1 EP0015020 B1 EP 0015020B1
Authority
EP
European Patent Office
Prior art keywords
process according
wetted
metal
liquid
metal surface
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
Application number
EP80200096A
Other languages
German (de)
English (en)
Other versions
EP0015020A1 (fr
EP0015020B2 (fr
Inventor
Dieter Dr. Oppen
Karl Lampatzer
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
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 Metallgesellschaft AG, Continentale Parker Ste, Continentale Parker SA filed Critical Metallgesellschaft AG
Publication of EP0015020A1 publication Critical patent/EP0015020A1/fr
Publication of EP0015020B1 publication Critical patent/EP0015020B1/fr
Application granted granted Critical
Publication of EP0015020B2 publication Critical patent/EP0015020B2/fr
Expired 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
    • 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
    • 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
    • C23C22/40—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 molybdates, tungstates or vanadates
    • C23C22/42—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 molybdates, tungstates or vanadates containing also phosphates
    • 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
    • C23C22/40—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 molybdates, tungstates or vanadates
    • C23C22/44—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 molybdates, tungstates or vanadates containing also fluorides or complex fluorides

Definitions

  • the invention relates to a process for the preparation of metal surfaces for subsequent coating with organic coatings by applying a phosphate coating by wetting with a phosphating liquid containing at least 2 cations and then drying the liquid film and applying it to the treatment of aluminum surfaces.
  • the so-called three-step process is becoming increasingly important.
  • the metal surface is cleaned to remove oil, dirt and corrosion products.
  • the second stage is a rinse with water, chemical residues from the first stage being removed from the metal surface.
  • the metal surface is wetted with an aqueous chemical reaction solution and the liquid film is dried.
  • DE-B-1 769 582 describes a process in which an aqueous solution which contains hexavalent chromium, trivalent chromium, alkali ions and silicon dioxide in certain proportions is dried on the metal.
  • the coatings formed are e.g. well suited as electrical insulation, as corrosion protection and as a primer for paints and the like
  • the object of the invention is to provide a method which avoids the known, in particular the aforementioned disadvantages, and yet can be carried out simply and without additional effort.
  • 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 surface is wetted with a phosphating liquid which has a pH of 1.5 to 3.0, is chromium-free and, in addition to metal phosphate, soluble molybdate - Contains, tungstate, vanadate, niobate and / or tantalate ions.
  • the wetting of the metal surface can e.g. by dipping and then draining, pouring over and spinning off, brushing, spraying with compressed air, air-less and also electrostatically, spraying, rolling on with structured and smooth rollers in the same direction and in the opposite direction.
  • the phosphating liquid to be used according to the method according to the invention can be modified by additionally adding simple or complex-bound fluoride ions, such as fluotitanate, fluozirconate, fluostannate, fluoborate and / or fluosilicate. This results in an increased improvement in the anchoring as a result of a corresponding pickling attack on the metal surface.
  • simple or complex-bound fluoride ions such as fluotitanate, fluozirconate, fluostannate, fluoborate and / or fluosilicate.
  • Metal phosphates are preferably used in which the cationic component of the metal phosphate consists of calcium, magnesium, barium, aluminum, zinc, cadmium, iron, nickel. Cobalt and / or manganese is formed. they form easily adhering tertiary phosphates.
  • a reduction equivalent here means the amount of reducing agent that is able to increase the valency of the introduced molybdate, tungstate, vanadate, niobate and / or tantalate ions by one valence level, that is, for. B. from Mo VI to Mo V to reduce. It must be taken into account here that individual reducing agents within a molecule can have several groups capable of reduction.
  • phosphating liquids which additionally contain finely divided silica and / or dispersible, film-forming organic polymers, such as polyacrylate.
  • organic polymers such as polyacrylate.
  • pyrogenic silica obtained from silicon tetrachloride or silicic acid precipitated in an aqueous medium from alkali silicates have proven to be the source of the finely divided silica. What is important here is the small grain size of the silica, since it ensures a uniform, stable suspension in the aqueous, acidic reaction liquid.
  • the organic polymers which can be used are those which are customary in paint production.
  • the addition of the abovementioned substances serves in particular to thicken the phosphating liquid and thus represents one of the possibilities for regulating the thickness of the liquid film to be applied.
  • the addition of organic polymers has an advantageous effect on the adhesion in individual applications dependent on the subsequent treatment.
  • Further preferred configurations of the method according to the invention consist in wetting the metal surface with a phosphating liquid in which the molar ratio of metal phosphate (calculated as Me n + (H 2 PO 4 ) n ) to molybdate, tungstate, niobate, tantalate and / or vanadate ion (calculated as MoO 3 , WO a , N 2 O 5 , Ta 2 O 5 , V 2 O 5 ) in the range from 1: (0.4 to 0.01) and / or in which the molar ratio of Metal phosphate (calculated as Me n + (H 2 PO 5 ) n ) to silica (calculated as SiO 2 ) to fluoride (calculated as (Me n + F n + 2 ) 2- ) in the range of 1: (0.2 to 5, 0) :( 0.04 to 2.0) and / or in which the weight ratio of metal phosphate (calculated as Me n + (H
  • the liquids used according to the invention preferably contain the components in an amount such that they have an evaporation residue of 5 to 150 g / l.
  • a liquid film quantity of between 2.5 and 25 ml / m 2 workpiece surface is preferably used.
  • Particularly good application results are achieved if the film of the phosphating liquid is dimensioned such that a layer weight of 0.03 to 0.6 g / m 2 is obtained after drying.
  • the drying after the wetting of the metal surface can already take place at room temperature. However, better results are achieved at higher temperatures, preferably temperatures between 50 and 100 ° C.
  • the metallic workpieces can be in various forms, e.g. as a shaped body, tube, rod, wire, but preferably as a sheet or strip, are used.
  • the method according to the invention is suitable for a large number of metals and metal alloys.
  • a special application is in the treatment of metal surfaces made of iron, zinc or alloys thereof.
  • the method according to the invention is of outstanding importance for the coating of surfaces made of aluminum or aluminum alloys.
  • the main advantages of the process according to the invention are that the layers obtained are non-toxic, have high corrosion protection and good adhesion and adhesion-promoting properties and that the treatment liquid is stable, i.e. does not experience a change in composition due to reaction or precipitation of components. In addition, the process has no wastewater problems.
  • the subsequent treatment following the method according to the invention consists in particular in the application of lacquers, adhesives or plastics, which can be carried out in the manner customary for this.
  • aluminum strip was wetted with the phosphating liquids described in more detail below using a roll coating machine.
  • the drying temperature was 80 ° C in each case.
  • the aluminum strip was in a solution containing which had a pH of 1.3, was cleaned.
  • the contents of the individual treatment liquids of active substances as well as those per square meter The amount of liquid applied in ml, the evaporation residue of the treatment liquid in g / l and the layer weight obtained in mg / m 2 surface are tabulated.

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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)
  • Application Of Or Painting With Fluid Materials (AREA)

Claims (13)

1. Procédé de préparation de surfaces métalliques pour l'application ultérieure d'une couche de revêtements organiques par dépôt d'un recouvrement de phosphate réalisé en mouillant avec un liquide de phosphatation contenant des cations au moins divalents et en séchant ensuite le film liquide, caractérisé en ce qu'on mouille la surface métallique avec un liquide de phosphatation qui présente un pH de 1,5 à 3,0, qui est exempt de chrome et qui contient en plus du phosphate métallique des ions molybdate, tungstate, vanadate, niobiate et/ou tantalate solubles.
2. Procédé suivant la revendication 1, caractérisé en ce que la surface métallique est mouillée avec un liquide de phosphatation qui contient aussi des ions fluorure simples ou complexes, tels que fluoroborate ou fluorosilicate.
3. Procédé suivant les revendications 1 ou 2, caractérisé en ce que la surface métallique est mouillée avec un liquide dé phosphatation dans lequel le composant cationique du phosphate métallique est formé par le calcium, le magnésium, le baryum, l'aluminium, le zinc, le cadmium, le fer, le nickel, le cobalt et/ou le manganèse.
4. Procédé suivant l'une des revendications 1, 2 ou 3, caractérisé en ce que la surface métallique est mouillée avec un liquide de phosphatation qui contient aussi une substance réductrice, particulièrement une substance appartenant au groupe comprenant les aldéhydes, les acides hydroxy- carboxyliques, les hydrazines, les hydroxylamines et/ou les hypophosphites, avantageusement en quantités d'au moins un équivalent de réduction.
5. Procédé suivant l'une ou plusieurs des revendications. 1 à 4, caractérisé en ce que la surface métallique est mouillée avec un liquide de phosphatation qui contient en plus de l'acide silicique finement divisé.
6. Procédé suivant l'une ou plusieurs des revendications 1 à 5, caractérisé en ce que la surface métallique est mouillée avec un liquide de phosphatation qui contient en plus un polymère organique dispersable, filmogène tel qu'un polyacrylate.
7. Procédé suivant l'une ou plusieurs des revendications 1 à 6, caractérisé en ce que la surface métallique est mouillée avec un liquide de phosphatation dans lequel le rapport molaire du phosphate métallique (calculé à l'état de Me"+ (H2PO4)n) aux ions molybdate, tungstate, vanadate, niobiate et/ou tantalate (calculés à l'état de MoO3, WO,, V2O5, Nb2O5, Ta2O5) est situé dans l'intervalle de 1:(0,4 à 0,01).
8. Procédé suivant l'une ou plusieurs des revendications 1 à 7, caractérisé en ce que la surface métallique est mouillée avec un liquide de phosphatation dans lequel le rapport molaire du phosphate métallique (calculé à l'état de Men+ (H2PO4)n) à l'acide silicique (calculé à l'état de SiO2) et du fluorure (calculé à l'état de Men+Fn+2)2-) est situé dans l'intervalle de 1 :(0,2 à 5,0):(0,04 à 2,0).
9. Procédé suivant l'une ou plusieurs des revendications 1 à 8, caractérisé en ce que la surface métallique est mouillée avec un liquide de phosphatation dans lequel le rapport pondéral du phosphate métallique (calculé à l'état de Men+ (H2PO4)n) au polymère est situé dans l'intervalle de 1:(0,1 à 2,0).
10. Procédé suivant l'une ou plusieurs des revendications 1 à 9, caractérisé en ce que le film de liquide de phosphatation est tel qu'on obtienne après séchage un poids de revêtement de 0,03 à 0,6 g/m2.
11. Procédé suivant l'une ou plusieurs des revendications 1 à 10, caractérisé en ce qu'on effectue le séchage du film de liquide à des températures comprises entre 50 et 100°C.
12. Application du procédé suivant l'une ou plusieurs des revendications 1 à 11 pour le traitement préalable de l'aluminium.
13. Application suivant la revendication 12, caractérisée en ce que la surface d'aluminium est préalablement nettoyée avec une solution aqueuse acide.
EP80200096A 1979-02-14 1980-02-05 Procédé de traitement de surfaces de métaux et son utilisation pour le traitement de surfaces en aluminium Expired EP0015020B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2905535 1979-02-14
DE19792905535 DE2905535A1 (de) 1979-02-14 1979-02-14 Verfahren zur oberflaechenbehandlung von metallen

Publications (3)

Publication Number Publication Date
EP0015020A1 EP0015020A1 (fr) 1980-09-03
EP0015020B1 true EP0015020B1 (fr) 1983-02-23
EP0015020B2 EP0015020B2 (fr) 1986-02-05

Family

ID=6062856

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80200096A Expired EP0015020B2 (fr) 1979-02-14 1980-02-05 Procédé de traitement de surfaces de métaux et son utilisation pour le traitement de surfaces en aluminium

Country Status (7)

Country Link
US (1) US4264378A (fr)
EP (1) EP0015020B2 (fr)
JP (1) JPS5931593B2 (fr)
CA (1) CA1133362A (fr)
DE (2) DE2905535A1 (fr)
GB (1) GB2041987B (fr)
IT (1) IT1149291B (fr)

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Publication number Publication date
IT8019877A0 (it) 1980-02-13
DE2905535A1 (de) 1980-09-04
EP0015020A1 (fr) 1980-09-03
US4264378A (en) 1981-04-28
GB2041987A (en) 1980-09-17
GB2041987B (en) 1983-07-27
DE3062096D1 (en) 1983-03-31
JPS5931593B2 (ja) 1984-08-02
IT1149291B (it) 1986-12-03
CA1133362A (fr) 1982-10-12
EP0015020B2 (fr) 1986-02-05
JPS55131176A (en) 1980-10-11

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