EP0111897B1 - Procédé pour le traitement de surfaces métalliques, en particulier de celles en aluminium, en alliages d'aluminium et en acier, ainsi que solutions de bain aqueuses appropriées à cet effet - Google Patents

Procédé pour le traitement de surfaces métalliques, en particulier de celles en aluminium, en alliages d'aluminium et en acier, ainsi que solutions de bain aqueuses appropriées à cet effet Download PDF

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Publication number
EP0111897B1
EP0111897B1 EP83112610A EP83112610A EP0111897B1 EP 0111897 B1 EP0111897 B1 EP 0111897B1 EP 83112610 A EP83112610 A EP 83112610A EP 83112610 A EP83112610 A EP 83112610A EP 0111897 B1 EP0111897 B1 EP 0111897B1
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Prior art keywords
ions
chromium
iii
aqueous bath
metal surfaces
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Expired
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EP83112610A
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German (de)
English (en)
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EP0111897A1 (fr
Inventor
Raschad Mady
Christian Ries
Roland Dr. Morlock
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Gerhard Collardin GmbH
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Gerhard Collardin GmbH
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Priority to AT83112610T priority Critical patent/ATE23573T1/de
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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
    • 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
    • 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
    • C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/10—Use of solutions containing trivalent chromium but free of hexavalent chromium

Definitions

  • the invention relates to the preparation of cleaned metal surfaces, in particular of strips made of aluminum, aluminum alloys and cold-rolled steel - but also other metal surfaces - for a subsequent coating with organic coatings, in particular the manufacture of metal goods for the food packaging sector.
  • Such coatings can substantially improve the surface quality, in particular with regard to corrosion protection and adhesion of subsequently applied cover layers.
  • Treatment solutions containing hexavalent chromium were originally often proposed in the extensive relevant prior art. Because of the toxic nature of this compound, these processes and the rinsing water that they require require elaborate wastewater treatment.
  • treatment solutions which contain hexavalent chromium and trivalent chromium salts together with film formers are described, for example, in DE-AS 1 769 582 and in DE-OS 2 903 311.
  • alkali silicate is to be used as the inorganic film former.
  • the second reference uses polyacrylic acid as an organic film former. Due to the content of 6-valent chromium in the aqueous bath fluids, these materials are not suitable for use in the food sector.
  • DE-OS 2 711 431 describes a process for the surface treatment of metals, in particular iron, zinc and aluminum, in which the cleaned metal surface is to be wetted with an acidic aqueous solution, the chromium (III) ions; Contains phosphate ions and finely divided silica, it being possible for acetate ions, male ions, zinc ions and / or manganese ions to additionally be present in the treatment solution.
  • the toxic chromium (VI) ion can be dispensed with here, but acidic dispersions containing silica and phosphate ions have the disadvantage of a limited pot life
  • Japanese Patent Application 57-174,469 is referenced in “Patent Abstracts of Japan, unexamined applications •, Vol. 7, No. 19 (January 25, 1983), C Field, page 64 C 147. It was then known to use solutions containing Cr 2 O 3 , co-salts of inorganic acids, phosphoric acid, silica sol and suitable fluorides to form a chromate film on steel surfaces. After treating the surfaces with such solutions, the excess solution is removed and the steel surface is dried without rinsing.
  • DE-A-3 038 699 describes aqueous acidic chromate coating solutions for the treatment of zinc, zinc alloy or cadmium surfaces which contain trivalent chromium ions as practically the only chromium ions, fluoride ions and an acid and by mixing a green trivalent chromium ion solution with a blue trivalent one Chromium ion solution can be prepared.
  • the green solution containing trivalent chromium ions is obtained by reducing a solution containing hexavalent chromium.
  • phosphoric acid is mentioned as a suitable acid.
  • the present invention is based on the object of creating a “no-rinse” method of the type described at the outset or suitable treatment agents which do not have the disadvantages known hitherto for materials of this type and in particular for use in the food packaging sector are suitable.
  • the process according to the invention is intended to produce a glossy, visually appealing finish layer on the metal surface which, for example in the subsequent overlays with clear lacquers, meets the aesthetic requirements which are particularly desired in the field of food packaging.
  • the invention relates in a first embodiment to a method for treating metal surfaces, preferably aluminum, aluminum alloys and steel, in particular for a subsequent coating with coating compositions on an organic basis, the previously cleaned metal surfaces being wetted with an aqueous bath solution which contains chromium (III ) ions, fluoride ions and phosphate ions - but no chromium (VI) ions
  • the method according to the invention is suitable for the surface treatment of all metals relevant here, in particular therefore ferrous metals, aluminum or aluminum alloys, zinc and / or magnesium.
  • the invention is particularly suitable for the pretreatment of strips made of aluminum or aluminum alloys and cold-rolled steel for their subsequent use in the food packaging sector.
  • a conventionally cleaned and rinsed metal surface for example the surface of strips of the aforementioned metals, is squeezed in any way with the aqueous treatment solution after squeezing off the water film in such a way that expediently about 2 to 20 ml per square meter of the area , preferably about 3 to 7 ml of the aqueous treatment solution.
  • the content of the aforementioned active constituents of the aqueous treatment solution should continue to be within the following ranges per square meter of the metal surface: 5 to 100 mg of chromium (III) ions, 5.5 to 110 mg of fluoride ions and 6 to 125 mg of phosphate ions, and about 1 , 5 to 35 mg of the organic water-soluble or homogeneously water-dispersible film former.
  • the applied liquid film is allowed to act on the metal surface for a reaction time of about 1 to 10 seconds, whereupon the film is dried and thermally treated at an elevated temperature.
  • the process steps of acting on the metal surface and drying can also be summarized. After drying on the metal shell l Smile Friend a ver f ormungsstructer water-insoluble solid film with a basis weight of about 18 to 370 mg / m 2, preferably from about 50 to 250 mg / m 2 metal surface.
  • the drying and / or the thermal treatment of the applied liquid film or the chemicals applied with it can take place in particular in the temperature range from approximately 50 to 300 ° C.
  • Chromium (III) ions and fluoride ions are most easily introduced into the bath using chromium (III) fluoride, although the ratio of chromium (III) ions: fluoride ions is in the range from 1: 2.5 to 3.5 can fluctuate.
  • the phosphate content is adjusted by adding phosphates or phosphoric acid with subsequent partial neutralization. It applies that the phosphate content based on 1 mol of chromium (III) ions is preferably in a molar ratio of 0.3 to 3.0.
  • the organic film former is expediently a synthetic polymer with a sufficient content of free carboxyl groups, which is its water solubility. ensure homogeneous dispersibility in water.
  • Preferred organic film formers are clearly soluble polyacrylic acids, which retain their clear solubility in particular in the pH range of the aqueous treatment baths - which is usually between 2 and 3.
  • these are polyacrylic acids of a molecular weight which is not too high, for example those with molecular weights of up to about 150,000, preferably up to about 100,000.
  • aqueous treatment solutions according to the invention can be applied to the pre-cleaned metal strips in any type of application which is suitable for producing a uniform, defined liquid film in the specified quantity ranges on the metal surface.
  • the roller application process with two or three rollers has proven successful, but wetting of the strip by spraying or dipping with subsequent squeezing off of the excess liquid film by means of, for example, plastic-coated leveling rollers or adjustable air doctor blades can also be used.
  • Both acidic and alkaline cleaners are suitable for the pretreatment of the metal surfaces to be wetted according to the invention.
  • the layers obtained with the aqueous treatment solution according to the invention provide a uniform, glossy finish without discoloration of the base material.
  • suitable organic coatings applied below they meet the requirements for the food packaging sector.
  • Aluminum strip of the alloy AIMg 5 was first cleaned and degreased in a coil coating line. An acidic solution containing 1 g / IH 2 SO 4 , 0.2 g / l HF and 1 g / l surfactant combination was used for this. The cleaning was carried out at a temperature of 60 ° C., 8 seconds and at a spray pressure of 1.5 bar. The tape was then rinsed with warm demineralized water and the rinsing water squeezed out.
  • a liquid film of 5 ml / m 2 surface was then applied with the solution according to the invention by means of roller application processes, whereby the surface per m 2 is covered with a liquid film containing 25 mg Cr 3+ , 27.5 mg F-, 31.3 mg PO 4 - and 8.75 mg of polyacrylic acid ("Acrylsol® A 1 - from Röhm & Haas, Philadelphia. USA) contains.
  • the water contained in the liquid film was evaporated in a floating dryer with a circulating air temperature of 100 ° C. and a metal object temperature of approx. 50 ° C., and a water-insoluble film of 92.5 mg / m 2 was obtained on the metal surface.
  • the speeds of rotation of the chemcoater rollers were set such that a liquid film of 8 ml / m 2 of belt surface was applied to a cleaned and water-rinsed aluminum belt at a belt speed of 100 m / minute by means of the application rollers of the chemcoater.
  • the tape was wetted with a liquid film which contains 40 mg Cr 3+ , 44 mg F - , 50 mg PO 4 ---- and 14 mg polyacrylic acid 100% strength per m 2 of surface and, after drying, a mass per unit area of 148 mg / m 2 on the aluminum.
  • the water portion of the liquid film was removed by means of a warm air dryer and then the tape was heated to an object temperature of 200 ° C. After cooling, the film obtained on the tape was wetted with 8 to 10 mg of dioctyl sebacate to improve the sliding property.
  • the chemically pretreated aluminum surface thus obtained was coated with varnishes suitable for the food sector and tested for its resistance to filling goods and forming behavior. In all tests, technological values were found which, in comparison to conventional solutions and methods, achieved results which were at least equivalent, and in some cases even better, with the methods according to the invention.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Coating With Molten Metal (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)
  • Manufacturing Of Printed Wiring (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)

Claims (9)

1. Procédé de traitement de surfaces métalliques, de préférence d'aluminium, d'alliages d'aluminium et d'acier, en particulier pour une enduction consécutive avec des masses de revêtement de nature organique, dans lequel on mouille les surfaces métalliques préalablement nettoyées avec une solution aqueuse de bain qui contient des ions de chrome(III), des ions fluorure et des ions phosphate, mais pas d'ions de chrome(VI); on sèche ensuite la matière appliquée
- sans processus intermédiaire de rinçage - et on la convertit par chauffage en un film insoluble dans l'eau, caractérisé en ce que la solution aqueuse limpide de bain
a) contient les constituants suivants dans les gammes de quantités citées ci-après :
Figure imgb0008
b) le rapport molaire ions de chrome(III) : ions fluorure : ions phosphate se situe dans l'intervalle de 1 : 2,5 à 3,5 : 0,3 à 3,0.
2. Procédé selon la revendication 1, caractérisé en ce que l'agent formateur de film organique est un polymère avec groupes carboxyle libres et en particulier un homo- et/ou copolymère d'acide acrylique et/ou d'acide méthacrylique.
3. Procédé selon la revendication 2, caractérisé en ce que l'agent formateur de film organique est un polymère d'acide acrylique, soluble dans l'eau avec limpidité, dans l'intervalle de pH de 2 à 3.
4. Procédé selon les revendications 1 à 3, caractérisé en ce que la solution aqueuse de bain sur la surface métallique contient par m2 5 à 100 mg d'ions de chrome(III), 5,5 à 110 mg d'ions fluorure, 6 à 125 mg d'ions phosphate et 1,5 à 35 mg de l'agent formateur de film organique soluble dans l'eau.
5. Procédé selon les revendications 1 à 4, caractérisé en ce qu'on mouille la surface métallique avec 2 à 20 ml/m2, de préférence avec 3 à 7 ml/m2, de solution aqueuse de bain.
6. Procédé selon les revendications 1 à 5, caractérisé en ce que le film de liquide appliqué est tout d'abord séché à des températures de 50 à 300 °C puis traité thermiquement.
7. Procédé selon les revendications 1 à 6. caractérisé en ce que sur les surfaces métalliques sont formés des films insolubles dans l'eau ayant une masse, rapportée à la surface, de 18 à 370 mg/m2, de préférence ayant une masse de 50 à 250 mg/m2 de la surface métallique.
8. Solution aqueuse de bain pour le traitement de surfaces métalliques, en particulier d'aluminium, d'alliages d'aluminium et/ou d'acier, contenant des ions de chrome(III), des ions fluorure et des ions phosphate, mais non des ions de chrome(VI), caractérisée en ce que la solution, pour une valeur de pH de 2 à 3,
a) contient les constituants suivants en les gammes de quantités citées ci-après :
Figure imgb0009
b) le rapport molaire ions de chrome(III) : ions fluorure : ions phosphate se situe dans l'intervalle de 1 : 2,5 à 3,5 : 0,3 à 3,0.
9. Solution aqueuse de bain selon la revendication 8, caractérisée en ce que l'agent formateur de film organique est un polymère avec groupes carboxyle libres, en particulier un homo- et/ou copolymère d'acide acrylique et/ou méthacrylique.
EP83112610A 1982-12-23 1983-12-15 Procédé pour le traitement de surfaces métalliques, en particulier de celles en aluminium, en alliages d'aluminium et en acier, ainsi que solutions de bain aqueuses appropriées à cet effet Expired EP0111897B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT83112610T ATE23573T1 (de) 1982-12-23 1983-12-15 Verfahren zur behandlung von metalloberflaechen, insbesondere solchen von aluminium, aluminiumlegierungen und stahl, sowie hierfuer geeignete waessrige badloesungen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19823247729 DE3247729A1 (de) 1982-12-23 1982-12-23 Verfahren zur behandlung von metalloberflaechen, insbesondere solchen von aluminium, aluminiumlegierungen und stahl, sowie hierfuer geeignete waessrige badloesungen
DE3247729 1982-12-23

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EP0111897A1 EP0111897A1 (fr) 1984-06-27
EP0111897B1 true EP0111897B1 (fr) 1986-11-12

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US (1) US4761189A (fr)
EP (1) EP0111897B1 (fr)
JP (1) JPH076071B2 (fr)
AT (1) ATE23573T1 (fr)
AU (1) AU557724B2 (fr)
BR (1) BR8306981A (fr)
CA (1) CA1219790A (fr)
DE (2) DE3247729A1 (fr)
ES (1) ES528361A0 (fr)
GR (1) GR79449B (fr)
MX (1) MX7298E (fr)
NO (1) NO162623C (fr)
ZA (1) ZA839574B (fr)

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JP3239312B2 (ja) * 1994-03-31 2001-12-17 川崎製鉄株式会社 耐食性に優れた電気絶縁被膜を有する電磁鋼板
DE4412138A1 (de) * 1994-04-08 1995-10-12 Henkel Kgaa Chromfreies Verfahren zur No-Rinse Behandlung von Aluminium und seinen Legierungen sowie hierfür geeignete wäßrige Badlösungen
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JP2003147544A (ja) * 2001-11-07 2003-05-21 Nippon Parkerizing Co Ltd 亜鉛系メッキ膜の表面処理膜、亜鉛系メッキ膜の表面処理液、及び表面処理方法
PL1984536T3 (pl) * 2006-02-14 2012-09-28 Henkel Ag & Co Kgaa Kompozycje i sposoby odpornej na korozję powłoki trójwartościowego chromu do suszenia na miejscu do stosowania na powierzchniach metalicznych
JP5690485B2 (ja) * 2006-05-10 2015-03-25 ヘンケル・アクチェンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフト・アウフ・アクチェンＨｅｎｋｅｌ ＡＧ ＆ Ｃｏ．ＫＧａＡ 金属表面に耐食被膜として用いられる改良された三価クロム含有組成物
US10156016B2 (en) 2013-03-15 2018-12-18 Henkel Ag & Co. Kgaa Trivalent chromium-containing composition for aluminum and aluminum alloys
DE102014222024A1 (de) 2014-10-29 2016-06-16 MTU Aero Engines AG Schlicker und Verfahren zur Herstellung einer Oxidations- und Korrosionsbeständigen Diffusionschicht
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AU2272983A (en) 1984-06-28
DE3367629D1 (en) 1987-01-02
NO162623C (no) 1990-01-24
NO834243L (no) 1984-06-25
ES8406563A1 (es) 1984-08-01
ATE23573T1 (de) 1986-11-15
MX7298E (es) 1988-04-26
GR79449B (fr) 1984-10-30
AU557724B2 (en) 1987-01-08
JPH076071B2 (ja) 1995-01-25
ES528361A0 (es) 1984-08-01
JPS59133373A (ja) 1984-07-31
DE3247729A1 (de) 1984-07-05
CA1219790A (fr) 1987-03-31
US4761189A (en) 1988-08-02
ZA839574B (en) 1984-08-29
BR8306981A (pt) 1984-07-31
EP0111897A1 (fr) 1984-06-27
NO162623B (no) 1989-10-16

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