EP1895023B1 - Mittel zur Behandlung der Oberfläche von Teilen aus Zink oder einer Zinklegierung - Google Patents

Mittel zur Behandlung der Oberfläche von Teilen aus Zink oder einer Zinklegierung Download PDF

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Publication number
EP1895023B1
EP1895023B1 EP20060254533 EP06254533A EP1895023B1 EP 1895023 B1 EP1895023 B1 EP 1895023B1 EP 20060254533 EP20060254533 EP 20060254533 EP 06254533 A EP06254533 A EP 06254533A EP 1895023 B1 EP1895023 B1 EP 1895023B1
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EP
European Patent Office
Prior art keywords
zinc
zinc alloy
surface treatment
agent
antimony
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Not-in-force
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EP20060254533
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English (en)
French (fr)
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EP1895023A1 (de
Inventor
Takashi Arai
Ro Bo Shin
Takahisa Yamamoto
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Publication of EP1895023A1 publication Critical patent/EP1895023A1/de
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Publication of EP1895023B1 publication Critical patent/EP1895023B1/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
    • C23C22/48—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
    • C23C22/46—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 oxalates
    • 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
    • C23C22/60—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 alkaline aqueous solutions with pH greater than 8
    • 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
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment

Definitions

  • the invention concerns agents for the surface treatment of zinc or zinc alloy products and a method for the surface treatment of zinc or zinc alloy products in which these agents are used.
  • JP-A-2001 279 462 , JP-A- 63161176 and GB-A-1 042 108 all disclose antimony-containing conversion coating solutions.
  • Zinc or zinc alloy products can be provided with excellent corrosion resistance at low cost by means of this invention.
  • An agent for the surface treatment of zinc or zinc alloy products as described includes at least one water-soluble compound which contains antimony, bismuth, tellurium or tin. Ideally it also includes nickel salts and/or manganese salts, and most desirably it also includes tannins and/or thioureas.
  • Die-cast zinc products and zinc plated products where zinc has been plated on steel or the like are included among the zinc or zinc alloy products, and at least the surface of the product should comprise zinc or zinc alloy.
  • the water-soluble compounds which contain antimony, bismuth, tellurium or tin are soluble in water under acidic or alkaline conditions, and they include, for example, antimony pentachloride, antimony pentoxide, antimony sulphate, antimony tribromide, antimony trichloride, antimony trioxide, antimony trisulphide, antimony benzoate, antimony tartrate, bismuth chloride, bismuth citrate, bismuth fluoride, bismuth hydroxide, bismuth tri-iodide, bismuth sulphate, bismuth oxychloride, bismuth acetate, bismuth benzoate, bismuth tartrate, bismuth carbonate, bismuth nitrate, bismuth salicylate, bismuth trisulphide, potassium tellurate, potassium tellutite, potassium stannate and tin sulphate.
  • the amounts compounded differ according to the type of water-soluble compound, but generally the amounts compound
  • the agents for the surface treatment of zinc or zinc alloy products as described include at least one of these water-soluble compounds which contain antimony, bismuth, tellurium or tin, but antimony or bismuth are especially desirable since they are reactive again on being wetted with water after a film has been formed on the surface of a zinc or zinc alloy product and a new film is formed so that the corrosion resistance life expectancy is prolonged. Furthermore, by using two, three or all four of antimony, bismuth, tellurium and tin conjointly the adhesion, hardness and smoothness of the film are improved and it is also possible to control the colour effectively. From these points of view the most ideal combinations in the case of conjoint use are those combinations of two or more including antimony and/or bismuth. In connection with the colour there is a tendency towards increased blackness, greyness, whiteness and whiteness as more antimony, bismuth, tellurium or tin, respectively, is compounded.
  • the inclusion in the agents for the surface treatment of zinc or zinc alloy products as described in addition to at least one of these water-soluble compounds which contains antimony, bismuth, tellurium or tin of a nickel salt and/or a manganese salt is ideal for reinforcing the corrosion resistance.
  • the amount compounded is generally of the order of from 1 to 20 g/L, and preferably of the order of from 5 to 10 g/L.
  • Salts selected from among the sulphates, chlorides, nitrates and phosphates are preferred for the nickel salts and manganese salts. These nickel salts and manganese salts can reinforce the corrosion resistance and, for example, manganese sulphate is most desirable for improving the corrosion resistance by improving adhesion, and in the case of the nickel salts, and especially nickel sulphate, the conjoint use of the hypophosphite is especially desirable for improving the hardness in addition to the corrosion resistance.
  • the amount of hypophosphite compounded is generally of the order of from 1 to 20 g/L and preferably of the order of from 5 to 10 g/L.
  • tannins such as tannic acid and the like and/or thioureas such as thiourea or salts thereof the dispersion properties are improved and the corrosion resistance is improved even more, and the gloss is increased and a beautiful colour can be obtained.
  • the amounts in which these materials are compounded are generally of the order of from 5 to 50 g/L and preferably of the order of from 10 to 30 g/L.
  • additives can be added to the agents for the surface treatment of zinc or zinc alloy products as described in accordance with the intended purpose.
  • examples include inorganic additives selected from among the inorganic acids, except for sulphuric acid and hydrochloric acid, and iodine compounds such as iodine and potassium iodide, and organic additives selected from among the amino acids, starch, cellulose, gelatin, rosin and poly(vinyl alcohol).
  • the amounts compounded are generally of the order of from 0.5 to 10 g/L, and preferably of the order of from 1 to 5 g/L.
  • the agents for the surface treatment of zinc or zinc alloy products of this invention may be used as acidic or alkaline baths.
  • the reaction rate is greater on the acidic side and tends to be low on the alkaline side and so they are preferably used at a pH of from 4 to 5 to obtain the optimum reactivity, but they are not limited to this pH range.
  • additives other than those indicated above such as dispersing agents, dispersion promoters and compounding ingredients for imparting an intended colour can be added appropriately to the agents for the surface treatment of zinc or zinc alloy products as described in accordance with the intended purpose.
  • the zinc or zinc alloy product When carrying out the surface treatment of a zinc or zinc alloy product using an agent for the surface treatment of zinc or zinc alloy products of this invention the zinc or zinc alloy product is immersed in an aqueous solution which contains this surface treatment agent and a corrosion resistant film is formed on the surface of the zinc or zinc alloy product.
  • the thickness of this film can be determined appropriately according to the intended purposes but it is generally from 0.5 to 2 ⁇ m.
  • the oxide which is attached to the surface has preferably been removed beforehand by the usual means such as de-greasing, acid washing, neutralization, etching and the like.
  • the immersion treatment of the zinc or zinc alloy product is generally carried out at a temperature of from 15 to 40°C, and preferably of from 20 to 30°C, and for a period of about 5 minutes. For example, if a temperature exceeding 40°C is used then the rate of formation of the film is increased and so more rigorous quality control is desirable.
  • the immersion treated zinc or zinc alloy product is then washed and dried in the usual way.
  • the colour of the film which is formed on the surface of the zinc or zinc alloy product in this way differs according to the components of the agent for surface treatment purposes.
  • the zinc or zinc alloy products which have been immersion treated in the way outlined above are preferably also immersed in an aqueous solution which contains a sealing treatment agent to seal the pinholes.
  • the sealing treatment agent is preferably selected in accordance with the colour of the zinc or zinc alloy product, and examples include (yellow) boric acid, ammonium oxalate; (yellow-brown) chromic acid, citric acid, tartaric acid, phthalic acid, malic acid; (whitish-yellow) succinic acid and (greyish-yellow) maleic acid.
  • the sealing treatment is preferably carried out by immersion in an aqueous solution which contains some 5 to 10 g/L of a sealing treatment agent as indicated above generally at a temperature of from 20 to 40°C for a period of the order of from 1 to 5 minutes. Then the product is preferably washed in pure water at a temperature of from 50 to 60°C and dried.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 35°C in an aqueous solution (pH 3 to 5) which contained 2 g/L of tin sulphate, 5 g/L of manganese sulphate, 2 g/L of iodine, 5 g/L of potassium iodide and 10 g/L of tannic acid and a green coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 35°C in an aqueous solution (pH 5 to 6) which contained 2 g/L of tin sulphate, 5 g/L of manganese sulphate, 1 g/L of selenous acid, 8 g/L of sulphuric acid and 10 g/L of tannic acid and a gold coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 20°C in an aqueous solution (pH about 5) which contained 2 g/L of tin sulphate, 25 g/L of nickel sulphate, 20 g/L of sodium hypophosphite, 30 g/L of ammonium sulphate, 15 g/L of boric acid and 15 g/L of glycerine and a bronze coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 20°C in an aqueous solution (pH 4 to 5) which contained 15 g/L of antimony tartrate, 25 g/L of manganese sulphate, 10 g/L of ammonium oxalate and 5 g/L of thiourea and a black coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 20°C in an aqueous solution (pH about 10) which contained 15 g/L of antimony tartrate, 25 g/L of manganese sulphate, 2 g/L of pyrophosphoric acid, 25 g/L of caustic soda, 5 g/L of thiourea and 5 g/L of potassium permanganate and a yellow coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 25°C in an aqueous solution (pH about 10) which contained 3 g/L of bismuth chloride, 25 g/L of manganese sulphate, 25 g/L of caustic soda, 5 g/L of thiourea and 2 g/L of potassium permanganate and a brown coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 3 minutes at 25°C in an aqueous solution (pH about 11) which contained 6 g/L of antimony dioxide, 25 g/L of manganese sulphate, 30 g/L of caustic soda, 5 g/L of thiourea and 5 g/L of potassium perchlorate and a coffee coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 40°C in an aqueous solution (pH about 11) which contained 5 g/L of bismuth nitrate, 25 g/L of manganese sulphate, 30 g/L of caustic soda, 40 g/L of zinc nitrate and 50 g/L of diethylene glycol and a grey coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 20°C in an aqueous solution (pH 4 to 5) which contained 15 g/L of potassium tellurate, 25 g/L of manganese sulphate, 10 g/L of ammonium oxalate and 5 g/L of thiourea and a black coloured film was obtained.
  • a zinc-plated steel bolt (length about 70 mm) was immersed and treated for 2 minutes at 20°C in an aqueous solution (pH 4 to 5) which contained 15 g/L of antimony tartrate, 5 g/L of bismuth chloride, 25 g/L of manganese sulphate, 10 g/L of ammonium oxalate and 5 g/L of thiourea and a black coloured film was obtained.
  • the immersion treated bolts obtained in Examples 1 to 10 described above were immersed generally at about 30°C for from 2 to 3 minutes in an aqueous solution which contained from 5 to 10 g/L of a sealing treatment agent as indicated below according to the colour, and then they were washed in pure water at from 50 to 60°C and dried and a further improvement in corrosion resistance was observed.

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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)

Claims (6)

  1. Mittel zur Oberflächenbehandlung von Zink- oder zinklegierungsprodukten, umfassend eine wässrige Lösung mindestens einer wasserlöslichen Verbindung, die Antimon enthält, dadurch gekennzeichnet, dass die Lösung
    (a) 15 g/L Antimontartrat, 25 g/L Mangansulfat, 10 g/L Ammoniumoxalat und 5 g/L Thioharnstoff enthält und einen pH-Wert von 4 bis 5 aufweist oder
    (b) 15 g/L Antimontartrat, 25 g/L Mangansulfat, 2 g/L Pyrophosphorsäure, 25 g/L Ätznatron, 5 g/L Kaliumpermanganat und 5 g/L Thioharnstoff enthält und einen pH-Wert von etwa 10 aufweist oder
    (c) 6 g/L Antimondioxid, 25 g/L Mangansulfat, 30 g/L Ätznatron, 5 g/L Thioharnstoff und 5 g/L Kaliumperchlorat enthält und einen pH-Wert von etwa 11 aufweist.
  2. Mittel nach Anspruch 1, dadurch gekennzeichnet, dass die Lösung, die 15 g/L Antimontartrat, 25 g/L Mangansulfat, 10 g/L Ammoniumoxalat und 5 g/L Thioharnstoff enthält, außerdem 5 g/L Bismutchlorid enthält.
  3. Verfahren zur Oberflächenbehandlung von Zink- oder Zinklegierungsprodukten durch Eintauchen des Zink- oder Zinklegierungsprodukts in ein Mittel zur Oberflächenbehandlung von Zink- oder Zinklegierungsprodukten, dadurch gekennzeichnet, dass es sich bei dem Mittel um ein Mittel nach einem der vorhergehenden Ansprüche handelt.
  4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass man das Zink- oder Zinklegierungsprodukt außerdem in eine wässrige Lösung, die ein Versiegelungsbehandlungsmittel enthält, eintaucht.
  5. Verfahren nach Anspruch 3 oder 4, wenn von Anspruch 1(c) oder 4 abhängig, dadurch gekennzeichnet, dass man das Zink- oder Zinklegierungsprodukt über einen Zeitraum von 3 Minuten bei einer Temperatur von 25°C in das Mittel zur Oberflächenbehandlung von Zink- oder Zinklegierungsprodukten eintaucht.
  6. Verfahren nach Anspruch 3 oder 4, dadurch gekennzeichnet, dass man das Zink- oder Zinklegierungsprodukt über einen Zeitraum von 2 Minuten bei einer Temperatur von 20°C in das Mittel zur Oberflächenbehandlung von Zink- oder Zinklegierungsprodukten eintaucht.
EP20060254533 2006-08-31 2006-08-31 Mittel zur Behandlung der Oberfläche von Teilen aus Zink oder einer Zinklegierung Not-in-force EP1895023B1 (de)

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Application Number Priority Date Filing Date Title
EP20060254533 EP1895023B1 (de) 2006-08-31 2006-08-31 Mittel zur Behandlung der Oberfläche von Teilen aus Zink oder einer Zinklegierung

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Application Number Priority Date Filing Date Title
EP20060254533 EP1895023B1 (de) 2006-08-31 2006-08-31 Mittel zur Behandlung der Oberfläche von Teilen aus Zink oder einer Zinklegierung

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EP1895023A1 EP1895023A1 (de) 2008-03-05
EP1895023B1 true EP1895023B1 (de) 2013-05-01

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3405600B1 (de) * 2016-01-19 2019-10-16 ThyssenKrupp Steel Europe AG Verfahren zum herstellen eines stahlprodukts mit einer zn-beschichtung und einer darauf aufgetragenen tribologisch aktiven schicht sowie entsprechend beschaffenes stahlprodukt
JP7347751B2 (ja) * 2019-06-21 2023-09-20 日本表面化学株式会社 金属表面処理方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE316668B (de) * 1963-09-23 1969-10-27 Parker Ste Continentale
DE2150143A1 (de) * 1971-05-24 1972-12-07 Cons Foods Corp Verfahren zur Erzeugung geschwaerzter UEberzuege auf Metallflaechen
JPS62174386A (ja) * 1986-01-27 1987-07-31 Nippon Parkerizing Co Ltd しゆう酸塩皮膜化成処理液および該処理液によるステンレス鋼材の化成処理方法
JPS63161176A (ja) * 1986-12-23 1988-07-04 Nkk Corp 亜鉛又は亜鉛合金の黒色化処理液及びその方法
JPH0293077A (ja) * 1988-09-27 1990-04-03 Kobe Steel Ltd 黒色めつき鋼板の製造方法
US5089349A (en) * 1989-06-05 1992-02-18 Calgon Corporation Compositions and method for applying coatings to metallic surfaces
KR100567176B1 (ko) * 1999-10-22 2006-04-03 제이에프이 스틸 가부시키가이샤 금속표면처리조성물 및 표면처리금속재료
JP2001279462A (ja) * 2000-03-30 2001-10-10 Boshin Ro 亜鉛又は亜鉛合金の表面処理剤及び表面処理方法

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