US3101286A - Phosphate composition and method for coating metallic surfaces - Google Patents

Phosphate composition and method for coating metallic surfaces Download PDF

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US3101286A
US3101286A US69737A US6973760A US3101286A US 3101286 A US3101286 A US 3101286A US 69737 A US69737 A US 69737A US 6973760 A US6973760 A US 6973760A US 3101286 A US3101286 A US 3101286A
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ion
phosphate
coating
zinc
solutions
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Earl R Reinhold
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Henkel Corp
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Amchem Products Inc
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Priority to US69737A priority patent/US3101286A/en
Priority to FR879028A priority patent/FR1309514A/fr
Priority to DEA38817A priority patent/DE1211466B/de
Priority to GB41112/61A priority patent/GB938980A/en
Priority to BE610342A priority patent/BE610342A/fr
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
    • C23C22/362—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing also zinc cations

Definitions

  • This invention relates to improved solutions for, and to an improved method of, coating the surfaces of zinccoated steel and iron to provide thereon an adherent, corrosion-resistant coating suitable as a base for protective finishing materials such as paint, lacquer, varnish, enamel, etc.
  • the present invention relates to improved phosphate coating solutions and methods for their use in connection with certain types of hot-dipped galvanized iron and steel.
  • the art of applying phosphate coatings to iron and zinc is Well developed.
  • the products of certain types of high speed, continuous hot-dipped, zinc-coating processes such as those known commercially as Zincgrip or Ti-Co have proved unusually troublesome to the phosphate coating art.
  • An example of such a zinc-coating process is disclosed in U.S. Patent 2,197,622. Briefly, the process comprises the steps of oxidizing the ferrous surface to form a thin oxide film thereon having a color ranging from light yellow to purple and ranging as far as gray, then reducing the oxide film to a film of the pure metal.
  • the surface While the reduced film remains protected in a non-oxidizing atmosphere, the surface, in a flux-free condition, is immersed in a molten zinc bath containing a minor quantity of aluminum to thereby form a zinc coating when the surface is withdrawn from the bath and allowed to cool.
  • Galvanized surfaces of the kind produced by the above process are particularly hard to coat by the well-known methods of the phosphate coating art. Even those solutions which have been found to produce satisfactory coatings on most zinc and zinc alloy surfaces have been found to be unsatisfactory for use on hot-dipped, zinc-coated material under consideration here. Such solutions when used on hot-dipped galvanized iron and steel produce coatings which are extremely non-uniform. The surfaces so produced are covered with multitudinous small raised areas where the coating action was apparently far more intense than on other areas of the surface. This phenomenon has been called seediness and is peculiar to the situation where phosphate coatings are applied to hotdipped galvanized surfaces.
  • U.S. Patent 1,221,046 discloses the coating of zinc and its alloys by treatment with a solution of phosphoric acid containing a nitrate accelerator.
  • This patent and U.S. Patent 2,121,574 allege that more uniform phosphate coatings are obtained when nickel or cobalt ions are added to the phosphoric acid solution.
  • U.S. Patents 1,869,121 and 1,888,189 disclose that copper ion in certain concentrations is beneficial in speeding up the action of a phosphate solution on a zinc surface, The surfaces of certain zinc alloys containing aluminum, which are coated only with great difficulty in nickel-accelerated phosphate solutions, are said in U.S.
  • Patent 2,591,479 to be easily coated when fiuobor-ate ion is added to a phosphate solution in combination with nickel ions. All of these solutions are satisfactory in many applications, but it has been found that they all produce a seedy coating when used on hotdipped galvanized iron and steel.
  • U.S. Patent 2,835,617 discloses a method and solution for retarding seed formation in phosphate coatings by the introduction of soluble silicon containing ions, in particular, silicotluoride ions into the coating solution.
  • a further important object of my invention is the provision of methods and solutions for the production of seedfree phosphate coatings on hot-dipped, zinc-coated surfaces.
  • Still another object of my invention is the provision of solutions and methods for phosphate coating zinc and zinc-coated surfaces to provide coatings wherein the grain size is adjusted to provide optimum paint bonding properties for the particular paint or other siccative coating which is to be applied.
  • the coating solutions of this invention comprise generally aqueous solutions containing phosphate ion, an ion such as zinc or manganese in suflicient proportions to produce a dihydrogen phosphate with the phosphate ion, a small proportion of nickel ion, at least a small amount of soluble titanium preferably introduwd as a titanium fluoridecontaining ion such as may be derived from fiuotitanic acid, ammonium fluotitanate, etc. and an oxidant such as nitrite or nitrate ions.
  • the solution may contain a small amount of copper as an additional accelerator, if desired.
  • the phosphate ions should be present in an amount from about 0.5 to about 2.5% (weight/volume). Associated with the phosphate ions are zinc or manganese ions in an amount at least sufficient to form the dihydrogen phosphate with the phosphate ion. It has been found, however, that if the proportions of zinc or manganese in the solutions are too high, seed-free coatings cannot always be obtained. Therefore, it is preferred that the solutions contain less than about 0.4 to 0.5% zinc or manganese. It is also preferred that the ratio of phosphate ion to zinc or manganese ion not be allowed to exceed 5:1.
  • oxidizing ion such as nitrate or nitrite ion or a mixture of nitrate or nitrite ions is also present in the solutions of the invention.
  • the quantity of nitrate ion d which is desirable is about 0.2 to about 1.0%, with major benefits being obtained at about 0.3 to about 0.5% nitrate ion.
  • Substantially smaller amounts of nitrite ion are necessary to produce the desired results, hence the acceptable range for nitrite ion is from about 0.0002 to about 0.008%. I have found that if the concentration of the oxidant is too high, it is not always possible to obtain seed-free coatings (a situation similar to that noted with the zinc and manganese ions).
  • the zinc or manganese concentration be less than about 0.4 to 0.5% with a phosphate to zinc or manganese ratio of not more than :1 and that the oxidant concentration be less than about 0.5% nitrate ion or less than about 0.005% nitrite ion.
  • the inclusion of soluble titanium ions in the solutions of my invention improves the resultant coating in two respects, namely, the elimination of seeding and reduction in the size of the surface grains of the coating.
  • concentration of soluble titanium necessary for smooth, hard, and spot-free phosphate coatings is quite small. For example, as little as 0.009% titanium (supplied by ammonium fiuotitanate in the phosphating bath) is capable of producing spotfree coatings on hot-dipped galvanized surfaces. However, at this low concentration the reduction in grain size or grain refinement effected by the titanium is minimal. When the concentration is increased, until it approaches and exceeds about 2.5 grams per liter of soluble titanium expressed as ammonium fiuotitanate, visible grain refinement is brought about.
  • a further increase in the concentration of soluble titanium results in increased grain refinement, that is, greater reduction in the size of the grains.
  • the grain refinement is so pronounced that the grain structure loses most of its crystallinity and appears to become almost amorphous.
  • Example I Percent by wt. Zinc oxide 8.0 Phosphoric acid (75%) 39.5 Nickel carbonate Ni) 3.0 Nitric acid (38 B.) 8.0 Hydrofluoric acid 1.0 H TiF (56%) 1.0 Water 39.5
  • the total acidity given above is the milliliters of tenth normal sodium hydroxide (points) required to titrate a 10 ml. sample of the bath to a phenolphthalein endpoint, whereas, the free acidity is the mls. of tenth normal hydroxide (points) required to neutralize a 10 ml. sample of the bath to a brom cresol green endpoint.
  • soluble copper compounds may also be a component of a concentrate of the type illustrated in Example I, if it is desired to have copper present in the treating bath.
  • This diluted solution when heated '00 temperatures between about F., and preferably between F. and F., has been found to produce excellent, fine grain, seed-free, phosphate coatings on a variety of zinciferrous surfaces, especially hot-dipped galvanized steel panels.
  • Vwhcn similar hotdipped, zinc-coated, steel panels were coated in a bath similar to that of this example, except for the substitution of approximately equivalent amounts of hydrofluoric acid or hydroiluoooric acid for the soluble titanium, the phosphate coatings were objcctionably seedy. It is clear, therefore, that it was the soluble titanium and not the fluoride content that eliminated the scediness.
  • Example I may be diluted to a strength of about /2 to about 6% by volume with water; the preferred dilution being from about 1 to about by volume. Any conventional method of contacting the surface with the solution is satisfactory.
  • the treating time may vary from about 15 seconds to about 10 minutes, but I prefer treating times from about 45 seconds to about 2 minutes.
  • the surface should be rinsed with water or with one of the final rinses which are customary in the art.
  • Examples of such rinses are dilute solutions of chromic acid or phosphoric acid.
  • Example I when employed as a replenishing material for partially depleted solutions restores not only the desired level of the coating producing ingredients, but also the accelerators such as nickel and copper.
  • the nickel and copper ions can be provided by adding a salt which is soluble in the solution, for example, a carbonate, nitnate, chloride or sulfate.
  • a salt which is soluble in the solution for example, a carbonate, nitnate, chloride or sulfate.
  • the soluble titanium is added to the solution in the form of an acid or salt of an acid such as iluotitanic acid or a stable soluble salt such as the sodium and potassium and ammonium salts thereof or potassium titanium oxalate.
  • a concentrated solution consisting of:
  • FIGURE 1 is a photomicrognaph at the above magnification of the panel treated with the solution containing no soluble titanium.
  • FIGURES 2, 3, 4 and 5 are photomicrographs at the same magnification of panels sprayed in solutions containing 1, 2% 5 and 25 gnarns per liter respectively of ammonium fiuotitanate.
  • FIGURES l and 2 a comparison of FIGURES l and 2 reveals that, although the size of the crystals or gnains is approximately the same, the crystals in FIGURE 1 are more mu together and unevenly distributed across the surface than those of FIGURE 2. In other words, the coating of FIGURE 2 appears to be very even, Whereas that of FIGURE 1 is quite uneven.
  • FIGURE 5 which is a photomicrograph of the panel treated with the most concentrated titanium bearing solution, the grain refinement is so pronounced that it is difiicult to trace any pattern of crystallinity. The surface appears, even in the photomicrognaph, to be almost amorphous.
  • An aqueous solution for coating a continuous hotdipped, zinc-coated, ferrous surface the coating-producing ingredients of which consist essentially of about 0.5 to 2.5 phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least suflicicnt to form dihydrogen phosphate with said phosphate ion, 0.01 to 0.4% nickel ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.2 to 1% nitrate ion and 0.0002% to 0.008% nitrite ion, and a titanium containing ion in a proportion sufficient to produce at least 0.009% soluble titanium.
  • An aqueous solution for coating a continuous hotdipped, zinc-coated, ferrous surface the coating-producing ingredients of which consist essentially of about 0.5 to 2.5% phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sulficient to form dihydrogen phosphate with said phosphate ion, 0.01 to 0.4% nickel ion, from about 0.0003 to about 0.005% copper ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.2 to 1% nitrate ion and 0.0002% to 0.008% nitrite ion, and a titanium containing ion in a proportion suflicient to produce at least 0.009% soluble titanium.
  • An aqueous solution for coating a continuous hot dipped, zinc-coated, ferrous surface the coating-producing ingredients of which consist essentially of about 0.5 to 2.5 phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least suflicient to form dihydrogen phosphate with said phosphate ion, to not more than 0.5% metal ion, a ratio of phosphate ion to said metal ion of not more than 5:1, 0.01 to 0.3% nickel ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.3 to 0.5% nitrate ion and 0.0002 to 0.005% nitrite ion, and a titanium containing ion in a proportion sufficient to produce at least 0.009% soluble titanium.
  • An aqueous solution for coating a continuous hotdipped, zinc-coated, ferrous surface the coating-producing ingredients of which consist essentially of about 0.5% to 2.5% phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sufficient to form dihydrogen phosphate with said phosphate ion, 0.01 to 0.4% nickel ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.2 to 1% nitrate ion and 0.0002% to 0.008% nitrite ion, and from about 1 gram per liter to about 25 grams per liter of soluble titanium expressed as ammonium fiuotitanate.
  • An aqueous solution for coating a continuous hotdipped, zinc-coated, ferrous surface the coating-producing ingredients of which consist essentially of about 0.5% to 2.5% phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sufiicient to form dihydrogen phosphate with said phosphate ion, 0.01 to 0.4% nickel ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.2 to 1% nitrate ion and 0.0002% to 0.008% nitrite ion, and fluotitanic ion in a proportion sufiicient to produce at least 0.009% soluble titanium.
  • An aqueous solution for coating a continuous hotdipped, zinc-coated, ferrous surface the coating-producing ingredients of which consist essentially of about 0.5 to 2.5% phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sufficient to form dihydrogen phosphate with said phosphate ion, to not more than 0.5% metal ion, a ratio of phosphate ion to said metal ion of not more than 5 :1, 0.01 to 0.3% nickel ion, from about 0.0003 to about 0.001% copper ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.3 to 0.5 nitrate ion and 0.0002 to 0.005% nitrite ion, and fluotitanic ion in a proportion sufficient to produce at least 0.009% soluble titanium.
  • the coating-producing ingradients consist essentially of about 0.5% to 2.5 phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sufiicient to form dihydrogen phosphate with said phosphate ion, 0.01 to 0.4% nickel ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.2 to 1% nitrate ion and 0.0002% to 0.008% nitrite ion, the improvement which comprises including in said solutions a titanium containing ion in a proportion sufficient to produce at least 0.009% soluble titanium.
  • the method of providing seed-free phosphate coatings on continuous hot-dipped, zinc-coated, ferrous surfaces comprising contacting the said surfaces with an aqueous solution the coating-producing ingredients of which consist essentially of about 0.5 to 2.5% phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sufficient to form dihydrogen phosphate with said phosphate ion, 0.01 to 0.4% nickel ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in aconcentration of about 0.2 to 1% nitrate 7 ion and 0.0002% to 0.008% nitrite ion, and a titanium containing ion in a proportion sufficient to produce at least 0.009% soluble titanium.
  • the coating-producing ingredients consist essentially of about 0.5 to 2.5% phosphate ion, a metal ion selected from the group consist
  • the method of providing seed-free phosphate coatings on continuous hot-dipped, zinc-coated, ferrous surfaces comprising contacting the said surfaces which an aqueous solution the coating-producing ingredients of which consist essentially of about 0.5% to 2.5% phosphate ion, a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sufiicient to form dihydrogen phosphate with said phosphate ion, 0.01 to 0.4% nickel ion, from about 0.0003 to about 0.005% copper ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.2 to 1% nitrate ion and 0.0002% to 0.008% nitrite ion, and a titanium containing ion in a proportion sufficient to produce at least 0.009% soluble titanium.
  • An aqueous solution for coating :1 zinc-coated, ferrous surface the coating-producing ingredients of which consist essentially of about 0.5% to 2.5% phosphate ion,
  • a metal ion selected from the group consisting of the zinc ion and the manganese ion in a proportion at least sufficient to form dihydrogen phosphate with said phosphate ion, to not more than 0.5% metal ion, a ratio of phosphate ion to said metal ion of not more than 5:1, 0.01 to 0.3% nickel ion, at least one oxidizing ion selected from the group consisting of the nitrate ion and the nitrite ion in a concentration of about 0.3 to 0.5% nitrate ion and 0.0002 to 0.005% nitrite ion, and fluotitanic ion in a pro portion sufficient to produce at least 0.009% soluble tita mum.

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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)
US69737A 1960-11-16 1960-11-16 Phosphate composition and method for coating metallic surfaces Expired - Lifetime US3101286A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
NL271405D NL271405A (enrdf_load_stackoverflow) 1960-11-16
US69737A US3101286A (en) 1960-11-16 1960-11-16 Phosphate composition and method for coating metallic surfaces
FR879028A FR1309514A (fr) 1960-11-16 1961-11-15 Perfectionnements apportés aux solutions et procédés pour la production de revêtements de phosphates sur les surfaces de zinc ou d'acier et de fer galvanisés
DEA38817A DE1211466B (de) 1960-11-16 1961-11-16 Waessrige nickel-beschleunigte Phosphatierungs-loesungen und Verfahren zu ihrer Anwendung
GB41112/61A GB938980A (en) 1960-11-16 1961-11-16 Solutions and processes for producing phosphate coatings on the surfaces of zinc or zinc-coated steel and iron
BE610342A BE610342A (fr) 1960-11-16 1961-11-16 Solutions et procédés pour établir des revêtements de phosphate sur des surfaces de zinc ou des surfaces d'acier ou de fer recouvertes de zinc

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4110129A (en) * 1977-02-03 1978-08-29 Oxy Metal Industries Corporation Post treatment of conversion-coated zinc surfaces
US4220485A (en) * 1978-12-14 1980-09-02 Calgon Corporation Process for sealing phosphatized metal components
WO2004101850A1 (de) * 2003-05-19 2004-11-25 Henkel Kommanditgesellschaft Auf Aktien Vorbehandlung von metallloberflächen vor einer lackierung
CN103114282A (zh) * 2013-02-27 2013-05-22 湖南中骏科技有限公司 一种钢铁工件磷化后免水洗的常温磷化液及其制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2516008A (en) * 1948-06-19 1950-07-18 Westinghouse Electric Corp Composition and process for treating metal surfaces
GB757050A (en) * 1953-03-27 1956-09-12 Pyrene Co Ltd Improvements in the formation of phosphate coatings on metal surfaces
US2813812A (en) * 1952-06-24 1957-11-19 Parker Rust Proof Co Method for coating iron or zinc with phosphate composition and aqueous solution therefor

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2121574A (en) * 1936-11-30 1938-06-21 American Chem Paint Co Art of coating zinc
BE435584A (enrdf_load_stackoverflow) * 1938-07-25
US2322349A (en) * 1941-10-25 1943-06-22 Westinghouse Electric & Mfg Co Corrosion resistant coating for metal surfaces
DE1065246B (de) 1955-01-26 1959-09-10 Metallgesellschaft Aktiengesellschaft, Frankfurt/M Verfahren zur Herstellung von Phosphatüberzügen auf feuerverzinken eisernen Oberflächen
GB811645A (en) * 1956-04-13 1959-04-08 Pyrene Co Ltd Improvements relating to the formation of phosphate coatings

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2516008A (en) * 1948-06-19 1950-07-18 Westinghouse Electric Corp Composition and process for treating metal surfaces
US2813812A (en) * 1952-06-24 1957-11-19 Parker Rust Proof Co Method for coating iron or zinc with phosphate composition and aqueous solution therefor
GB757050A (en) * 1953-03-27 1956-09-12 Pyrene Co Ltd Improvements in the formation of phosphate coatings on metal surfaces

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4110129A (en) * 1977-02-03 1978-08-29 Oxy Metal Industries Corporation Post treatment of conversion-coated zinc surfaces
US4220485A (en) * 1978-12-14 1980-09-02 Calgon Corporation Process for sealing phosphatized metal components
WO2004101850A1 (de) * 2003-05-19 2004-11-25 Henkel Kommanditgesellschaft Auf Aktien Vorbehandlung von metallloberflächen vor einer lackierung
CN103114282A (zh) * 2013-02-27 2013-05-22 湖南中骏科技有限公司 一种钢铁工件磷化后免水洗的常温磷化液及其制备方法
CN103114282B (zh) * 2013-02-27 2015-04-29 湖南中骏科技有限公司 一种钢铁工件磷化后免水洗的常温磷化液及其制备方法

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DE1211466B (de) 1966-02-24
NL271405A (enrdf_load_stackoverflow)
GB938980A (en) 1963-10-09

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