US2478954A - Method of treating phosphate coated surfaces - Google Patents

Method of treating phosphate coated surfaces Download PDF

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Publication number
US2478954A
US2478954A US533062A US53306244A US2478954A US 2478954 A US2478954 A US 2478954A US 533062 A US533062 A US 533062A US 53306244 A US53306244 A US 53306244A US 2478954 A US2478954 A US 2478954A
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United States
Prior art keywords
phosphate
coating
solution
metal
phosphate coating
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Expired - Lifetime
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US533062A
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English (en)
Inventor
Bertha S Tuttle
Navoy Thaddeus
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J N TUTTLE Inc
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J N TUTTLE Inc
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Priority to BE462686D priority Critical patent/BE462686A/xx
Application filed by J N TUTTLE Inc filed Critical J N TUTTLE Inc
Priority to US533062A priority patent/US2478954A/en
Priority to GB10139/45A priority patent/GB590852A/en
Priority to FR912794D priority patent/FR912794A/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
    • C23C22/82—After-treatment
    • C23C22/84—Dyeing
    • 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

  • This invention relates to a method of treating phosphate-coated surfaces, such as are commonly applied to ferrous and ferrous alloy articles, to increase their corrosion resistance and if desired to impart a color thereto.
  • phosphate treatments Since the essential ingredient embodied in such treatments is the phosphate radical, the processes are generally referred to as phosphate treatments, being commercially known as Parkerizing, Bonderizing, Granodizing, etc. It has also been found that the efficacy of the phosphate treatment may be enhanced and the character of the resultant phosphate coating varied by the use of salts of metals below iron in the electromotive series, and to this end minor amounts of salts of such elements as copper, silver, lead, tin, antimony,
  • arsenic, etc. along with the principal ingredient, e. g.,' M(H2PO4)2, have been suggested.
  • the essential or primary ingredient is the metal phosphate which provides at least the major-portion of the corrosion resistant coating, the other ingredients being of secondary importance in that they either concomitantly form an additional phosphate complex along with the principal phosphate coating, or function apparently as an accelerator, catalyst or the like.
  • the principal objects of the present invention are to provide a composition for and method of treating phosphate-coated surfaces so as greatly to increase their corrosion resistance; to provide a composition for and method of simultaneously increasing the corrosion resistance of phosphate coated articles and imparting thereto a desired coloration which can not 'be rubbed or washed off, which does not produce appreciable dimensional changes and which is relativel fast to light; and to provide a protective phosphate coating which is denser, more adherent, refined and smoother than the phosphate coatings heretofore produced, and which is resistant to heat and generally more attractive.
  • the material to be treated for example an article composed of iron, steel, a ferrous alloy, etc.
  • any treatment capable ofproducing a phosphate coating is first subjected to any treatment capable ofproducing a phosphate coating, and to this end the article may be treated in accordance with any of the well known commercial procedures such, for example, as are disclosed in U. S. Patents Nos. 1,007,069, 1,651,694 and.1,911,726.
  • the phosphate coating thus produced consists essentially of a relatively insoluble porous crystalline film-like structure formed on or: integral with the surface of the treated article, and, without supplemenprocedures may be s tary treatment suchas oiling, waxing.'etc.. has,
  • a corrosion resistance oi the order of two to six temperature which may vary from room temperature'to the boiling point of the solution and for a period which may vary from a few seconds to severalminutes, depending upon the particular stanncus salt used, the character of the basic phosphate coating, and the desired degree of core rosion resistance.
  • the resultant coating is the reaction product of the stanncus salt and the original phosphate coating and consists essentially of a tin-metal-phosphate complex which is not only smoother, more dense, flue-grained and scratch resistant than the phosphate coating base, but also many'times more corrosion resistant.
  • a dye soluble in and compatible with the stanncus salt solution may be incorporated in the treating bath or solution, and in either case.
  • a suitable stabilizer or inhibitor may also be added to the treating solution.
  • the resultant coating consists essentially of a tin-metal-phosphate-dye complex which not only possesses increased corrosion resistance, as compared to the tin-metal-phosphate coating, but also an attractive coloration which is relatively fast to light and heat, and unafl'ected by water and solvents, and furthermore does not undergo an objectionable darkening when treated with oil and wax.
  • the article may then be rinsed off, dried, and, if desired, oiled or waxed in accordance with conventional practices.
  • the stanncus salts suitable for use in our process are limited to those that are water soluble and relatviely stable, and whose acidity may, if necessary, be adjusted so that the phosphate coating base is not stripped.
  • Such salts comprise the stanncus halides, stanncus sulphate, stannous fiuoborate, and certain organic stanncus salts. such as the acetate, oxalate and tartrate.
  • the amount or concentration of the dye will depend on'the particular dye and the depth of saturation point of the salt, although preferred working limits are between 2 and
  • the dye or coloring agents suitable for use in our process include the synthetic organic dyestuffs and certain animal and vegetable dyes which are compatible with an aqueous stanncus salt solution having an acid pH. Recognized classifications of dyes, such as are found in the Colour Index (edited by F. M. Rowe and published under the auspices of the Society of Dyers and Colourists), off little or no assistance in determining the particular types of dyes which are operative or suitable in our process.
  • stabilizer or inhibitor may be desired, particularly where maximum corrosion resistance is of the utmost importance, and to this end the treating bath or solution may include such stabilizers or inhibitors as mannitol, gum arable, dextrose, sugar and the like carbohydrates, or gelatine and other types of hydrophilic colloids.
  • the use of a stabilizer or inhibitor although sometimes advisable, is generally unnecessary,
  • amount to be used may, as a. practical matter, vary between 10% and 40%, based on the weight of the stannous salt, depending upon the length of the period during which the treating solution or bath is to be used.
  • Example 1 A stanncus salt solution is first cipitate or becomes discolored it is incompatible.
  • 76 prepared by dissolving parts (by weight) of commercial stannous chloride in 1000 parts of water, after which the solution is brought to boiling.
  • Metallic tin may, if desired, be added to stabilize the bath, although satisfactory results may be secured without such addition.
  • Steel, iron or other ferrous metal pieces, previously phosphate coated in conventional manner employing the Parkerizing Process are then dipped in the stannous chloride for approximately one minute while at boiling temperature, after which the pieces are removed, rinsed and dried. A smooth, fine-grained, dense coating having a gray coloration is produced.
  • Example 2 The procedure set forth in Example 1 was followed, except'that parts of Fast- Acid Green B dye were incorporated in the stannous chloride solution with the result that a dark green coloration, fast to light and washing, was imparted to the coating.
  • Example 3 The procedure set forth in Ex ample 1 was followed, except that 10 parts of mannitol were added to the stannous chloride 2 and 4 to 6) indicated that the coloration a g I Further tests on the dyed coatings (Examples was fast to strong light, water and solvents.
  • Example 4 The-procedure set forth in Ex-- ample 2 was followed using 10 parts of Wool Green S and 2 parts of sodium carbonate in place of the East Acid Green B. The resultant coating was similar to that produced by Example 1, except the coloration was a dark green-blue.
  • Example 5 The same procedure as set forth, in Example 2 was followed using 0 parts of Quinolene Yellow and the resultant coating had a light green-yellow coloration.
  • Example 6 The same procedure set forth in Example 2 was followed using approximately 10 parts of a dye mixture which produced a coatin having an olive drab coloration. 1
  • Ezample 15 A stannous salt solution was first prepared by dissolving 50 parts (by weight) of stannous sulfate in 1000 parts of water, after which 13 parts of sodium carbonate were added. A piece of ferrous metal having a phosphate coating was then dipped into the treating solution for aperiod of ten minutes during which the solution was maintained at boiling temperature. A smooth, fine-grained, dense coating, comparable to that of Example 1, was produced. Salt spray tests showed an initial corrosion resistance of 15 hours as compared to 2-3 hours for the untreated phosphate coating, a corrosionresistance rating after 33 hours of 7, as compared to a rating of 3 for the untreated coating, and a 7 70 hours.
  • Example 16 A stannous sulfate solution was prepared as in Example 15, and 10 parts of Fast Acid Green 13 were added thereto. A piece of ferrous metal having a phosphate coating was then subjected to treatment as in Example 15,
  • the coating showed an initial corrosion resistance of 33 hours and substantial rusting after more than 70 hours.
  • Example 17 A stannous sulfate treating solution was prepared as in Example 16, except that 12.5 parts of sodium carbonate and 10 parts of Wool Green S were used. The phosphate coated metal was treated for ten minutes at boiling temperature with the result that a coating having a blue green coloration was produced. This coating showed an initial corrosion resistance of approximately 35 and substantial rusting after l hours.
  • Example 18 A stannous salt solution was prepared by dissolving 50 parts of stannous fiuoborate in 1000 parts of water, after which parts of sodium carbonate was added. A phosphate coated piece of ferrous metal was then dipped into the solution maintained at boiling temperature for one minute. A coating comparable to that of Example 1 .was produced, which had an initial corrosion resistance or 6 to 15 hours and substantial rusting after 50 hours.
  • Example 19 -A stannous fiuoborate solution was prepared as in Example 18, and 10 parts of Fast Acid Green B were added to the solution. The test pieces were dipped for one minute in the solution while maintained at boiling temperature. A colored coating similar to that of Example 16 was produced, which coating had an initial corrosion resistance of approximately hours with substantial rusting after more than Example 20.-A stannous fiuoborate solution was prepared as in Example 19, except that 10 parts of Wool Green S were added instead of the Fast Acid Green B. The test pieces were dipbed in the treating .solution for five minutes while maintained at boiling temperature. The
  • Example 17 having a corrosion resistance, better than that of Example 8, but less than that of Example 19.
  • a stannous salt solution alone is capable of greatly increasing the corrosion resistance of phosphatecoated ferrous metals and alloys, and that when used in conjunction with a compatible dye, it not only produces a further increase in corrosion radical with the metal surface.
  • the method of treating metallic articles which comprises first forming a phosphate coating thereon by treatment with an aqueous solution containing a salt having the general formula M(H2PO4)2, wherein M is a metal in the electromotive series from manganese to iron, both inclusive and subsequently subjecting said phosphate coating to the. action of an aqueous solution of a stannous salt which is water soluble and water stable, the solution having an acidity insufilcient to strip said phosphate coating, and thereby to form an insoluble tin-metal-phosphate complex having a corrosion resistance greatly exceeding the original phosphate coating.
  • the method of treating metallic articles which comprises first forming a phosphate coating thereon by treatment with an aqueous solution containing a salt having the general formula M(H:PO4) wherein M is a metal in the electromotive series from manganese to iron, both inclusive and subsequently subjecting said phosphate coating to the action of an aqueous stannous chloride solution, the solution having an acidity insufllcient to strip said phosphate coating, thereby to form an insoluble tin-metal-phosphate complex having a corrosion resistance greatly exceeding the original phosphate coating.
  • the method of treating a metal article having an insoluble metal phosphate coatin thereon produced by chemical reaction of the phosphate radical with the metal surface which comprises subjecting said phosphate coating to the action of an aqueous treating solution containing from 2% to of a stannous salt which is water soluble and water stable, the solution having an acidity insufllcient to strip said phosphate coating, thereby to form an insoluble tin-metal-phosphate complex having a corrosion resistance greatly exceeding the original phosphate coating.
  • the method of treating metallic articles which comprises first forming a phosphate coating thereon by treatment with an aqueous solution containing a salt having the general formula M(H2PO4)2, wherein M is a metal in the electromotive series from manganese to iron, both in-' clusive and subsequently subjecting said phosphate coating to the action of an aqueous treating solution containing from 2% to 25% of a stannous salt which is water soluble and water stable, the solution having an acidity insuficient to strip said phosphate coating, thereby to form an insoluble tin-metal-phosphate complex having a corrosion resistance greatly exceeding the original phosphate coating.
  • M is a metal in the electromotive series from manganese to iron
  • the method of treating metallic articles which comprises first forming a phosphate coating thereon by treatment with an aqueous solution containing a salt having the general formula M(H2PO4)2, wherein M is a metal in the electromotive series from manganese to iron, both inclusive and subsequently subjecting said phosphate coating to the action of a. treating solution containing 2% to 25% stannous chloride, the solution having an acidity insufflcient to strip said phosphate coating, thereby to form an insoluble tin-metal-phosphate complex having a corrosion resistance greatly exceeding the original phosphate coating.
  • the method of treating a metal article having an insoluble metal phosphate coating thereon 10 producedby chemical reaction of the phosphate radical with the metal surface which comprises subjecting said phosphate coating to the action of an aqueous treating solution containing from 2% to 25% of a stannous salt which is water soluble and water stable, the solution having an acidity insufllcient to strip said phosphate coating, and from 0.1% to 10% (based on the weight of the treating solution) of a dye compatible with said stannous salt solution, thereby to form an insoluble tin-metal-phosphate-dye' complex having a corrosion resistance greatly exceeding the original phosphate coating.
  • the method of treating a metal article having an insoluble metal phosphate coating thereon produced by chemical reaction of the phosphate radical with the metal surface which comprises subjecting said phosphate coating to the action of an aqueous treating solution containing from 2% to 25% ofstannous chloride and from 0.1% to 10% (based on the weight of the treating solution) of a dye compatible with said stannous chloride solution, the said stannous chloride solution having an acidity insufllcient to strip said phosphate coating thereby to form an insoluble tin-metal-phosphate-dye complex having a corrosion resistance greatly exceeding the original phosphate coating.

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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)
US533062A 1944-04-27 1944-04-27 Method of treating phosphate coated surfaces Expired - Lifetime US2478954A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
BE462686D BE462686A (enrdf_load_stackoverflow) 1944-04-27
US533062A US2478954A (en) 1944-04-27 1944-04-27 Method of treating phosphate coated surfaces
GB10139/45A GB590852A (en) 1944-04-27 1945-04-23 Improvements in and relating to the treatment of phosphate-coated metal surfaces
FR912794D FR912794A (fr) 1944-04-27 1945-07-26 Procédé et composition pour le traitement des surfaces phosphatées

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US533062A US2478954A (en) 1944-04-27 1944-04-27 Method of treating phosphate coated surfaces

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BE (1) BE462686A (enrdf_load_stackoverflow)
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GB (1) GB590852A (enrdf_load_stackoverflow)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2608496A (en) * 1950-04-01 1952-08-26 J N Tuttle Inc Composition for producing protective coatings
US2854367A (en) * 1954-08-19 1958-09-30 Second Bank State Street Trust Composition and method for producing protective coatings
US2871769A (en) * 1955-03-18 1959-02-03 Bolton John W & Sons Inc Jordan plug body
US3118792A (en) * 1960-11-04 1964-01-21 J N Tuttle Inc Method for providing protective surfaces
DE1175524B (de) * 1957-03-26 1964-08-06 Pechiney Cie Des Prod Chim Et Loesungen und Verfahren zum UEberziehen von Metallflaechen
DE1192904B (de) * 1958-01-29 1965-05-13 J N Tuttle Inc Mittel zum Nachbehandeln von Phosphatueberzuegen
US3193416A (en) * 1962-09-10 1965-07-06 Olin Mathieson Process of dyeing anodized aluminum
DE1199417B (de) * 1960-04-18 1965-08-26 Rudolf Peck Spruehfunkensichere Schweisszwinge
US3262197A (en) * 1963-07-16 1966-07-26 Peck Rudolph Spatter proof welding clamp and welding method
EP0245597A1 (en) * 1986-05-12 1987-11-19 Lea Manufacturing Company Corrosion resistant coating
US4897129A (en) * 1986-05-12 1990-01-30 The Lea Manufacturing Company Corrosion resistant coating

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1102522B (de) * 1952-05-03 1961-03-16 Felix Ritter Von Rueling Heissspritzverfahren zur chemischen Behandlung von Oberflaechen
NL84245C (enrdf_load_stackoverflow) * 1952-06-12
US2873196A (en) * 1956-04-16 1959-02-10 Du Pont Rust preventative and anti-rust stabilizing compositions

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1303627A (en) * 1919-05-13 Treatment of iron or steel or other articles
US1329573A (en) * 1919-09-25 1920-02-03 William H Allen Rust preventing and arresting solution
US1426675A (en) * 1920-07-13 1922-08-22 Richardson Lawrence Feeding device for locomotive tenders
US1466126A (en) * 1922-02-01 1923-08-28 Guggenheim Brothers Electrolytic refining or depositing of tin
US1514494A (en) * 1922-05-29 1924-11-04 Randall Williams Company Rust remover and preventative
US1694820A (en) * 1925-12-21 1928-12-11 Harris Neal Rust-resisting can
FR731994A (fr) * 1930-12-17 1932-09-10 Perfectionnements au traitement de la surface de l'aluminium et des alliages d'aluminium
US2200615A (en) * 1937-12-01 1940-05-14 Clete L Boyle Method of and composition for cleaning and rendering metal surfaces immune from rust
US2236549A (en) * 1937-06-11 1941-04-01 Parker Rust Proof Co Method of coloring metals and product
US2295063A (en) * 1940-03-26 1942-09-08 James N Tuttle Protective coating
US2304299A (en) * 1940-05-13 1942-12-08 Boyle Composition for treating metal surfaces preparatory to painting
US2314565A (en) * 1940-05-29 1943-03-23 Parker Rust Proof Co Coated ferrous article and method of making the same

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1303627A (en) * 1919-05-13 Treatment of iron or steel or other articles
US1329573A (en) * 1919-09-25 1920-02-03 William H Allen Rust preventing and arresting solution
US1426675A (en) * 1920-07-13 1922-08-22 Richardson Lawrence Feeding device for locomotive tenders
US1466126A (en) * 1922-02-01 1923-08-28 Guggenheim Brothers Electrolytic refining or depositing of tin
US1514494A (en) * 1922-05-29 1924-11-04 Randall Williams Company Rust remover and preventative
US1694820A (en) * 1925-12-21 1928-12-11 Harris Neal Rust-resisting can
FR731994A (fr) * 1930-12-17 1932-09-10 Perfectionnements au traitement de la surface de l'aluminium et des alliages d'aluminium
US2236549A (en) * 1937-06-11 1941-04-01 Parker Rust Proof Co Method of coloring metals and product
US2200615A (en) * 1937-12-01 1940-05-14 Clete L Boyle Method of and composition for cleaning and rendering metal surfaces immune from rust
US2295063A (en) * 1940-03-26 1942-09-08 James N Tuttle Protective coating
US2304299A (en) * 1940-05-13 1942-12-08 Boyle Composition for treating metal surfaces preparatory to painting
US2314565A (en) * 1940-05-29 1943-03-23 Parker Rust Proof Co Coated ferrous article and method of making the same

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2608496A (en) * 1950-04-01 1952-08-26 J N Tuttle Inc Composition for producing protective coatings
US2854367A (en) * 1954-08-19 1958-09-30 Second Bank State Street Trust Composition and method for producing protective coatings
US2871769A (en) * 1955-03-18 1959-02-03 Bolton John W & Sons Inc Jordan plug body
DE1175524B (de) * 1957-03-26 1964-08-06 Pechiney Cie Des Prod Chim Et Loesungen und Verfahren zum UEberziehen von Metallflaechen
DE1192904B (de) * 1958-01-29 1965-05-13 J N Tuttle Inc Mittel zum Nachbehandeln von Phosphatueberzuegen
DE1199417B (de) * 1960-04-18 1965-08-26 Rudolf Peck Spruehfunkensichere Schweisszwinge
US3118792A (en) * 1960-11-04 1964-01-21 J N Tuttle Inc Method for providing protective surfaces
US3193416A (en) * 1962-09-10 1965-07-06 Olin Mathieson Process of dyeing anodized aluminum
US3262197A (en) * 1963-07-16 1966-07-26 Peck Rudolph Spatter proof welding clamp and welding method
EP0245597A1 (en) * 1986-05-12 1987-11-19 Lea Manufacturing Company Corrosion resistant coating
US4749417A (en) * 1986-05-12 1988-06-07 The Lea Manufacturing Company Corrosion resistant coating
US4897129A (en) * 1986-05-12 1990-01-30 The Lea Manufacturing Company Corrosion resistant coating

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BE462686A (enrdf_load_stackoverflow)
GB590852A (en) 1947-07-30
FR912794A (fr) 1946-08-20

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