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WO1995000680A1 - Composition et procede de traitement d'une surface zincifere - Google Patents

Composition et procede de traitement d'une surface zincifere Download PDF

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Publication number
WO1995000680A1
WO1995000680A1 PCT/US1994/007003 US9407003W WO9500680A1 WO 1995000680 A1 WO1995000680 A1 WO 1995000680A1 US 9407003 W US9407003 W US 9407003W WO 9500680 A1 WO9500680 A1 WO 9500680A1
Authority
WO
WIPO (PCT)
Prior art keywords
concentration
composition according
acid
resin
composition
Prior art date
Application number
PCT/US1994/007003
Other languages
English (en)
Inventor
Shinobu Komiyama
Kyosuke Hori
Kenji Aizawa
Original Assignee
Henkel Corporation
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
Application filed by Henkel Corporation filed Critical Henkel Corporation
Priority to US08/569,177 priority Critical patent/US6071435A/en
Publication of WO1995000680A1 publication Critical patent/WO1995000680A1/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
    • C23C22/24—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 hexavalent chromium compounds
    • C23C22/30—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 hexavalent chromium compounds containing also trivalent chromium
    • 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
    • C23C22/24—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 hexavalent chromium compounds
    • C23C22/33—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 hexavalent chromium compounds containing also phosphates

Definitions

  • the invention relates to a composition and process for treating the surface of zinciferous metal, particularly of steel sheet coated with zinciferous metal.
  • the invention will be generally illustrated below by use of metal-plated steel sheet, but other zinciferous surfaces are equally suited to treatment according to the in ⁇ vention.
  • the invention relates to a composition and process, for treating the surface of zinciferous metal-plated steel sheet, that are capable of inhibiting both the development of white rust and the development of blackening on the surface of zinciferous metal-plated steel sheet.
  • zinciferous metal-plated steel sheet is a general desig ⁇ nation for steel sheet that is plated with zinc or zinc alloy.
  • Said zinc alloy encom ⁇ passes, for example, zinc/aluminum alloys, which may additionally contain one or more of iron, magnesium, manganese, silicon, titanium, nickel, cobalt, molyb- denum, lead, tin, chromium, and rare earths such as La, Ce, Y, and Nb.
  • Zinciferous metal-plated steel sheet has an excellent corrosion resistance and for this reason is widely used in applications such as, for example, building materials, household electrical appliances, and automobiles. Zinciferous metal- plated steel sheet is frequently not painted when used as a structural member or as an interior component of household electrical appliances.
  • Zinciferous metal-plated steel sheet is ordinarily subjected to a chromate treatment in the case of such unpainted service in order to inhibit white rust.
  • a surface-treatment process has also recently appeared that uses a resin contain- ing chromate treatment bath. This process increases the added value by in ⁇ creasing the corrosion resistance, pressability, fingerprint resistance, and chrom ⁇ ium fixation ratio of zinciferous metal-plated steel sheet.
  • Japanese Patent Publication Number Hei 1 -53353 [53,353/1989] teaches a process for treating the surface of Zn/AI alloy-plated steel sheet in ord ⁇ er to prevent blackening.
  • This process uses a treatment bath that contains chromic acid and/or chromate salt in combination with water soluble resin or emulsified resin.
  • the results afforded by this process are still not com- pletely satisfactory.
  • Japanese Patent Publication Number Hei 3-49982 [49,982/1991] also dis ⁇ closes a process for preventing blackening.
  • hot-dip zinciferous metal-plated steel sheet is first treated with a bath that contains Co ion and/or Ni ion in order to deposit these metals on the surface.
  • the surface of the sheet is then subjected to a chromate treatment.
  • This process consists of a two-step method (Ni and/or Co plating treatment and chromate treatment) or a three-step method (the preceding plus a water wash after the Ni and/or Co plat ⁇ ing treatment) and is therefore difficult to implement in existing surface treatment facilities. Disclosure of the Invention
  • the present invention seeks to introduce a surface-treatment compo- sition and a surface-treatment process that can impart an excellent corrosion re ⁇ sistance, excellent pressability, excellent fingerprint resistance, and high chrom- ium fixation ratio to zinciferous metal-plated steel sheet and that, by a simple pro ⁇ cedure, can form thereon a surface coating layer that strongly inhibits blackening.
  • the inventors have found that the problems described above can be elim- inated by the addition of trivalent chromium ion and nickel ion to a (Cr 6* + resin) containing aqueous surface-treatment composition for application to zinciferous metal-plated steel sheet and by controlling the nickel content therein to specific proportions.
  • the present invention was achieved based on this discovery.
  • a composition according to the invention for treating the surface of zinciferous metal-plated steel sheet is a liquid aqueous composition that has a pH not exceeding 2.5 and that comprises, preferably consists essen ⁇ tially of, or more preferably consists of, hexavalent chromium ion, trivalent chrom ⁇ ium ion, nickel ion, inorganic acid, and resin material composed of at least 1 type of water-based emulsified resin, with the characteristic feature that the nickel content therein is adjusted so as to give a weight ratio between the nickel content and the total chromium content of 0.05 to 1.
  • step (II) subsequently drying the liquid film of the aqueous surface treatment agent applied in step (I) in order thereby to form on the treated metal a blacken- ing-resistant dry coating layer, which preferably contains 0.1 to 10 g/m 2 of the aforesaid resin material and 2 to 150 mg/m 2 of total chromium.
  • the inorganic acid used in the present invention preferably consists of one or more selections from phosphoric acid, nitric acid, fluosilicic acid, fluozirconic acid, boric acid, and fluoboric acid.
  • the nickel ion is preferably supplied by ad ⁇ dition to the subject aqueous composition of one or more nickel compounds se- lected from nickel carbonate, nickel oxide, and nickel hydroxide.
  • the aforemen ⁇ tioned resin material preferably includes at least 1 selection from water-based emulsified polyacrylic resins and water-based emulsified polyurethane resins.
  • the inorganic acid is preferably phosphoric acid, and the phosphoric acid con- tent, which is to be understood for this purpose as the stoichiometric equivalent as phosphoric acid of not only any undissociated phosphoric acid present in the solution but also of any phosphorus containing anions produced by any degree of ionization of phosphoric acid, is preferably from 5 to 30 times (on a weight bas ⁇ is) of the nickel content.
  • the hexavalent chromium ion present in the surface-treatment composi ⁇ tion of the present invention can be supplied by addition to the aqueous composi ⁇ tion of one or more selections from among the hexavalent chromium compounds heretofore used for chromate treatment baths, for example, chromic acid, chrom ⁇ ic anhydride, chromate salts (e.g., ammonium chromate), and dichromate salts (e.g., ammonium dichromate).
  • the hexavalent chromium ion acts to improve the corrosion resistance conferred on zinciferous metal-plated steel sheet by the su ⁇ rface coating layer afforded by the present invention.
  • the trivalent chromium ion present in the surface-treatment composition of the present invention can be supplied by reduction of hexavalent chromium ion and/or by addition to the aqueous composition of at least 1 trivalent chromium compound, for example, chromium phosphate, chromium nitrate, or chromium hydroxide.
  • the trivalent chromium ion is the component effective for increasing the chromium fixation ratio in the surface coating layer afforded by the present invention on zinciferous metal-plated steel sheet.
  • the nickel ion used in the present invention may be supplied by the addi ⁇ tion of nickel chromate or nickel dichromate to the aqueous composition, but is preferably supplied by the addition of at least 1 nickel compound selected from nickel carbonate, nickel oxide, and nickel hydroxide.
  • a particularly important fea ⁇ ture of the present invention is that the nickel ion does not impair the excellent properties of zinciferous metal-plated steel sheet, while at the same time it is par ⁇ ticularly effective for inhibiting the blackening associated with resin containing chromate treatment systems.
  • Other metal ions for example, even cobalt ions, do not exhibit this anti-blackening activity.
  • the inorganic acid used in the present invention is selected from inorganic acids that are capable of adjusting the pH of the aqueous surface treatment com- position to 2.5 or below and preferably consists of at least 1 selection from phos ⁇ phoric acid, nitric acid, fluosilicic acid, fluozirconic acid, boric acid, and fluoboric acid.
  • the use of phosphoric acid is preferred. Sat ⁇ isfactorily achieving the desired anti-blackening activity becomes highly proble ⁇ matic when the pH of the surface-treatment composition exceeds 2.5.
  • the resin material used by the present invention comprises at least 1 type of water-based emulsified resin and. has the capacity to form a film.
  • This resin material should be selected from those that are stable (i.e., exhibit no gelation or precipitation) even at pH ⁇ 2.5 and that resist oxidation by the chromic acid, dichromic acid, or salts thereof present in the surface-treatment composition.
  • the subject resin material should be selected as is appropriate, as a function of the stability desired for the surface-treatment composition, but in general prefer ⁇ ably includes at least 1 selection from water-based emulsified polyurethane res ⁇ ins and water-based emulsified polyacrylic resins, e.g., polymers or copolymers of at least 1 selection from acrylic acid, methacrylic acid, acrylonitrile, acrylates (e.g., n-butyl acrylate, 2-ethylhexyl acrylate, etc.), methacrylates (e.g., methyl methacrylate, methoxyethylene methacrylate, etc.), styrene, and the like.
  • the resin material may contain water-soluble resin.
  • the hexavalent chromium ion concentration and trivalent chromium ion concentration in the surface-treatment composition of the present invention are each preferably 2 to 5 g/L.
  • the nickel ion concentration is preferably 1 to 3 g/L.
  • the inorganic acid is preferably present in the quantity necessary to adjust the pH of the aqueous composition to ⁇ 2.5, for example, 3 to 10 g/L.
  • the resin material is preferably present in the surface-treatment composi ⁇ tion of the present invention at a concentration of 100 to 300 g/L as weight of so- lids.
  • the nickel content in the surface-treatment composition of the present in ⁇ vention is adjusted so as to give a weight ratio between the nickel content and the total chromium content of 0.05 to 1.
  • the anti-blackening activity is inade- quate when this parameter is less than 0.05, while the corrosion resistance be ⁇ comes unsatisfactory when this parameter exceeds 1.
  • the inorganic acid content in the surface-treatment composition of the present invention is preferably from 5 to 30 times (on a weight basis) that of the nickel. Adjusting the inorganic acid/nickel weight ratio in this manner affords the maximum level of anti-blackening activity.
  • the aqueous surface-treatment agent as described above is coated on the surface of zinciferous metal-plated steel sheet and is then solidified by drying.
  • No particular limitations apply to the application technique, and typical application techniques, for example, roll coat- ing, roll squeegee coating, and so forth, can be used here.
  • the technique for drying/solidification is also not specifically restricted, and hot-air drying, infrared drying, etc., can be used. Hot-air temperatures of 100° C to 400° C are pre ⁇ ferred, or the steel sheet can be heated to 60° C to 250° C.
  • the surface-treatment composition preferably should be applied in the in- vention process so as to yield a resin material content of 0.1 to 10 g/m 2 , more preferably 0.5 to 3 g/m 2 , and a total chromium content of 2 to 150 mg/m 2 and preferably 10 to 70 mg/m 2 in the blackening-resistant coating layer formed by drying and solidification.
  • the final product has a reduced weldability and the economics become undesirable when the resin material con ⁇ tent exceeds 10 g/m 2 .
  • the anti-corrosion activity of the final coating layer is in ⁇ adequate when the total chromium content falls below 2 mg/m 2 , while a total chromium content in excess of 150 mg/m 2 results in an unsatisfactory blackening inhibition by the final coating layer and also results in a reduced chromium fixa ⁇ tion ratio.
  • the surface-treatment composition in accordance with the present invention may contain, for example, cobalt ion, manganese ion, zinc ion, SiO 2 , nitrate ion, and/or ammonium ion.
  • test specimen was held for 24 hours in a humidity tester at 80° C and 98 % relative humidity, and the change in the lightness ( ⁇ L) before and after testing was measured with a color difference meter and scored on the fol ⁇ lowing scale:
  • test sample was subjected to salt-spray testing for 240 hours in accordance with JIS Z 2371. It was then visually inspected and the area of white rust development was scored on the following scale: Symbol Area of White Rust Development
  • the Cr add-on was measured before and after subjecting the test spec ⁇ imen to alkaline degreasing.
  • Alkaline degreasing consisted of a 2 minute spray at 60° C with 2 % aqueous FINECLEANERTM 4326T from Nihon Parkerizing Company, Limited.
  • the proportion of Cr remaining on the test specimen was cal ⁇ culated and scored on the following scale: Symbol Residual Cr Ratio
  • the surface-treatment compositions were prepared using the components described below.
  • Tables 1 and 2 report the phosphoric acid/nickel weight ratio, pH, and type of resin for the surface-treatment compositions in the respective examples and comparative examples. The following resins were used:
  • Resin A styrene/n-butyl acrylate copolymer resin in water-based emulsion form
  • Resin B polyurethane resin in water-based emulsion form.
  • the surface-treatment compo- sition was applied to the plated steel sheet specimen by roll coating.
  • a solid dry coating layer was then produced by drying and solidification of the liquid coating layer by raising the temperature of the plated steel sheet specimen to 100° C us ⁇ ing hot air.
  • the resin add-on and Cr add-on were measured on the resulting product, which was also subjected to the tests described above. These results are reported in Tables 1 and 2.
  • composition and process of the present invention for treating the sur ⁇ face of zinciferous metal-plated steel sheet can prevent the blackening of this type of plated steel sheet while providing an excellent corrosion resistance, fin- gerprint resistance, and chromium fixation ratio.
  • Example 12 ⁇ ame composition as Example 12 except for the addition of cobalt carbonate in a quantity equimolar to the nickel content.
  • Example 12 Same composition as Example 12 except for the addition of manganese carbonate in a quantity equimolar to the nickel content.
  • Example 12 A composition like Example 12 except without the addition of nickel.
  • Note 7 A composition like Example 12 except without the nickel compound, phosphoric acid, and trivalent chromium compou
  • Note 8 A composition like Example 12 except without the nickel compound, phosphoric acid, and trivalent chromium compou
  • Note 9 A composition like Example 12 except that the nickel compound has been replaced by an equimolar quantity of the cor sponding cobalt compound.

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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)
  • Coating With Molten Metal (AREA)

Abstract

Afin d'inhiber le noircissement de la tôle d'acier zincifère à placage métallique tout en générant une bonne résistance à la corrosion, une bonne résistance à l'empreinte des doigts et un taux de fixage du chrome pour la tôle d'acier ou recouvre cette dernière d'une composition liquide aqueuse dont le pH ne dépasse pas 2,5 et contenant un ion de chrome hexavalent, un ion de chrome trivalent, un ion de nickel, de l'acide inorganique (de préférence de l'acide phosphorique), une résine filmogène, avec un rapport massique entre la teneur en nickel et la teneur totale en chrome de 0,05 à 1. On laisse ensuite sécher le revêtement liquide sur la surface métallique traitée de manière à former un revêtement résistant au noircissement contenant 0,1 à 10 g/m2 de résine et 2 à 150 mg/m2 au total de chrome.
PCT/US1994/007003 1993-06-25 1994-06-23 Composition et procede de traitement d'une surface zincifere WO1995000680A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US08/569,177 US6071435A (en) 1993-06-25 1994-06-23 Composition and process for treating a zinciferous surface

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP5/155184 1993-06-25
JP15518493A JP3290509B2 (ja) 1993-06-25 1993-06-25 亜鉛含有金属めっき鋼板の表面処理組成物および表面処理方法

Publications (1)

Publication Number Publication Date
WO1995000680A1 true WO1995000680A1 (fr) 1995-01-05

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PCT/US1994/007003 WO1995000680A1 (fr) 1993-06-25 1994-06-23 Composition et procede de traitement d'une surface zincifere

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JP (1) JP3290509B2 (fr)
CN (1) CN1105713A (fr)
WO (1) WO1995000680A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0810297A1 (fr) * 1996-05-31 1997-12-03 Tsubakimoto Chain Co. Pièces résistant à la chaleur pour chaîne
WO1999031294A1 (fr) * 1997-12-12 1999-06-24 Henkel Kommanditgesellschaft Auf Aktien Agent anticorrosion conducteur chrome et procede anticorrosion
US6294262B1 (en) * 1998-04-03 2001-09-25 Nippon Paint Co., Ltd. Composition and process for anticorrosive treatment of non-ferrous metal

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998000579A1 (fr) * 1996-07-02 1998-01-08 Nkk Corporation Procede de production de feuilles d'acier chromees et galvanisees a chaud, contenant du plomb et ayant une excellente resistance au noircissement et a la formation de rouille blanche
US8273190B2 (en) * 2009-05-29 2012-09-25 Bulk Chemicals, Inc. Method for making and using chromium III salts
CN104928677A (zh) * 2015-07-16 2015-09-23 胡家辉 碳素钢或合金铝水镀铬与真空镀钛结合的方法
ES2942284T3 (es) * 2016-09-15 2023-05-31 Chemetall Gmbh Pretratamiento protector mejorado contra la corrosión de una superficie metálica, que contiene acero, acero galvanizado, aluminio, una aleación de aluminio, magnesio y/o una aleación de zinc-magnesio
CN106756928A (zh) * 2016-12-27 2017-05-31 昆明理工大学 一种镀锌用高效钝化处理剂及其配备方法
JP7266459B2 (ja) * 2019-05-16 2023-04-28 Ｊｆｅ鋼板株式会社 表面処理鋼板の製造方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3718509A (en) * 1971-02-03 1973-02-27 Diamond Shamrock Corp Coated metal and method
US3755018A (en) * 1971-04-26 1973-08-28 Eltzroth & Ass J M Composition and process for inhibiting corrosion of non-ferrous metal surfaced articles and providing receptive surface for synthetic resin coating compositions
US3966502A (en) * 1972-08-17 1976-06-29 Amchem Products, Inc. Zirconium rinse for phosphate coated metal surfaces

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3718509A (en) * 1971-02-03 1973-02-27 Diamond Shamrock Corp Coated metal and method
US3755018A (en) * 1971-04-26 1973-08-28 Eltzroth & Ass J M Composition and process for inhibiting corrosion of non-ferrous metal surfaced articles and providing receptive surface for synthetic resin coating compositions
US3966502A (en) * 1972-08-17 1976-06-29 Amchem Products, Inc. Zirconium rinse for phosphate coated metal surfaces

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0810297A1 (fr) * 1996-05-31 1997-12-03 Tsubakimoto Chain Co. Pièces résistant à la chaleur pour chaîne
WO1999031294A1 (fr) * 1997-12-12 1999-06-24 Henkel Kommanditgesellschaft Auf Aktien Agent anticorrosion conducteur chrome et procede anticorrosion
US6294262B1 (en) * 1998-04-03 2001-09-25 Nippon Paint Co., Ltd. Composition and process for anticorrosive treatment of non-ferrous metal

Also Published As

Publication number Publication date
CN1105713A (zh) 1995-07-26
JP3290509B2 (ja) 2002-06-10
JPH0711453A (ja) 1995-01-13

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