US3664887A - Process for increasing corrosion resistance of conversion coated metal - Google Patents

Process for increasing corrosion resistance of conversion coated metal Download PDF

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Publication number
US3664887A
US3664887A US816036A US3664887DA US3664887A US 3664887 A US3664887 A US 3664887A US 816036 A US816036 A US 816036A US 3664887D A US3664887D A US 3664887DA US 3664887 A US3664887 A US 3664887A
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corrosion resistance
metal
drying
rinse
coated metal
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US816036A
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Thomas Clifford Atkiss
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Pennwalt Corp
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Pennwalt Corp
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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
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment

Definitions

  • ABSTRACT The corrosion resistance of conversion coated metal is increased by a process which comprises the steps of applying a phosphate conversion coating, rinsing with water, applying a chromate rinse, drying the metal surface, rinsing with deionized water, and drying.
  • This invention concerns an improvement in the commercial processing of metal parts for painting, being adaptable for use in applying chemical coatings on the surface of any metal which is susceptible to corrosion in the atmosphere or under corrosive conditions, e.g., iron, steel, zinc and aluminum.
  • the first step in the conventional process of treating said metal surfaces is a conventional cleaning.
  • This is followed by the application of a phosphate conversion coating from an aqueous bath, especially the zinc, iron, and calcium-zinc phosphate types.
  • the phosphate conversion coating baths normally consist of an aqueous solution of metal phosphates dissolved in phosphoric acid solutions containing accelerators such as the chlorates, nitrates or nitrites, or other special additives well known to those in the art, such as fluorides.
  • the conversion coatings are applied to the metal surfaces from said aqueous baths at elevated temperatures, generally in the range of 120 to 180 F.
  • the conversion coating step is followed by a water rinse, normally at an ambient temperature of about 50 to 120 F.
  • the next essential step is a rinsing of the metal surface in a dilute chromic acid bath.
  • This standard and well known chromate rinse operation is carried out with an aqueous solution containing hexavalent chromium ion in a concentration ranging from about 0.001 percent to about 0.1 percent by weight.
  • the chromate rinse bath may contain other additives such as small amounts of trivalent chromium ion and calcium ions.
  • the chromate rinse is applied to the metal surface at a temperature within the range of about 60 to 170 F. It is followed by a deionized water rinse and the metal is then dried as the final step in the conventional process.
  • EXAMPLE 1 The tests were carried out using panels of 1010 cold rolled steel which were first cleaned with a conventional alkaline cleaner and rinsed with cold water.
  • a phosphate conversion coating bath as described in US. Pat. No. 3,203,835 was prepared comprised of [.22 percent of 75 percent phosphoric acid, 0.25 percent zinc oxide, 0.32 percent sodium chlorate, 0.27 percent nickel nitrate, 0.008 percent disodium arsenate and the balance water.
  • a chromate rinse concentrate was prepared by mixing 16.6 parts of chromic acid, l6.6 parts of chromium nitrate and 66.8 parts water.
  • the chromate rinse bath was prepared from the concentrate by diluting 10.5 volumes of the concentrate with 4,000 volumes of water.
  • the pH was adjusted to 3.5 with 10 percent sodium hydroxide solution.
  • the temperature of the chromate rinse was maintained at F.
  • Process A a method according to the present invention, consisted of the following steps:
  • Process B carried out according to the prior art methods, consisted of the following steps:
  • the panels were painted with a standard industrial alkyd paint and tested for corrosion resistance according to ASTM D l654-61 in a salt spray apparatus for 240 hours.
  • the panels prepared according to process A of the invention had only a trace of creep whereas the panels from process B had 1/1 6-inch creep, clearly indicating the superiority of process A. Creep" is defined as the distance the paint has peeled away from the score mark in the accelerated corrosion test.
  • EXAMPLE 2 The comparative tests of EXAMPLE 1 were repeated with these exceptions.
  • the chromate rinse concentrate was prepared by reacting 35 parts of chromic acid with 0.8 part methyl alcohol in 50 parts water.
  • the chromate rinse was prepared by diluting 4.5 volumes of this concentrate in 4,000 volumes of water.
  • the chromate rinse was adjusted to pH 3.5 and maintained at 160 F.
  • the panels were subjected to the two processes described in Example 1, then painted, and subjected at 240 hours in the salt spray cabinet. The process A panels showed no creep whereas those processed according to method B showed l/16-inch creep.
  • EXAMPLE 3 The tests of EXAMPLE 1 were repeated with these exceptions.
  • the chromate rinse concentrate was prepared by reacting 35 parts of chromic acid with 16.6 parts of calcium carbonate and 48.4 parts water.
  • the chromate rinse bath was prepared by diluting 3.5 volumes of the concentrate with 4000 volumes of water. No pH adjustment was made.
  • the treatment processes were carried out as described above. The process A panels had only l/32-inch creep while the process B panels showed 54-inch creep, 8 times as great.
  • a method of increasing the corrosion resistance of conversion coated metal which comprises the steps of treating the metal surface with a phosphate conversion coating bath, rinsing with water, applying a chromate rinse, drying, rinsing with deionized water, and drying the metal surface.
  • metal is selected from the group consisting of iron, steel, zinc and aluminum.

Abstract

The corrosion resistance of conversion coated metal is increased by a process which comprises the steps of applying a phosphate conversion coating, rinsing with water, applying a chromate rinse, drying the metal surface, rinsing with deionized water, and drying.

Description

United States Patent Atkiss [54] PROCESS FOR INCREASING CORROSION RESISTANCE OF CONVERSION COATED METAL [72] Inventor: Thomas Clifford Atkiss, Pottstown, Pa.
[73] Assignee:
[22] Filed:
[21] Appl. No.: 816,036
Pennwalt Corporation, Philadelphia, Pa.
Apr. 14, 1969 [52] US. Cl. ..l48/6.16,148/6.l5 R, 148/615 Z [5 l] Int. Cl. ..C23f 17/00 [58] Field ofSearch 148/615, 6.16, 6.2
[ 51 May 23, 1972 Primary ExaminerRalph S. Kendall Assistant Examiner-Caleb Weston Attorney-Stanley Litz and Carl A. Hechmer, Jr.
[57] ABSTRACT The corrosion resistance of conversion coated metal is increased by a process which comprises the steps of applying a phosphate conversion coating, rinsing with water, applying a chromate rinse, drying the metal surface, rinsing with deionized water, and drying.
2 Claims, No Drawings PROCESS FOR INCREASTNG CORROSION RESISTANCE OF CONVERSION COATED METAL This invention concerns improvements in metal coating and more particularly relates to a method of improving chemically formed coatings on metal surfaces as a base for the application of an organic finish such as paint, lacquer, varnish and the like, whereby the corrosion resistance of the metal surface is significantly increased.
This invention concerns an improvement in the commercial processing of metal parts for painting, being adaptable for use in applying chemical coatings on the surface of any metal which is susceptible to corrosion in the atmosphere or under corrosive conditions, e.g., iron, steel, zinc and aluminum. The first step in the conventional process of treating said metal surfaces is a conventional cleaning. This is followed by the application of a phosphate conversion coating from an aqueous bath, especially the zinc, iron, and calcium-zinc phosphate types. The phosphate conversion coating baths normally consist of an aqueous solution of metal phosphates dissolved in phosphoric acid solutions containing accelerators such as the chlorates, nitrates or nitrites, or other special additives well known to those in the art, such as fluorides. The conversion coatings are applied to the metal surfaces from said aqueous baths at elevated temperatures, generally in the range of 120 to 180 F.
In the conventional processes, the conversion coating step is followed by a water rinse, normally at an ambient temperature of about 50 to 120 F. The next essential step is a rinsing of the metal surface in a dilute chromic acid bath. This standard and well known chromate rinse operation is carried out with an aqueous solution containing hexavalent chromium ion in a concentration ranging from about 0.001 percent to about 0.1 percent by weight. The chromate rinse bath may contain other additives such as small amounts of trivalent chromium ion and calcium ions. The chromate rinse is applied to the metal surface at a temperature within the range of about 60 to 170 F. It is followed by a deionized water rinse and the metal is then dried as the final step in the conventional process.
It has now been discovered thatthe corrosion resistance of the treated metal is unexpectedly improved by a simple revision of the foregoing process. More particularly, in accordance with this invention it has been discovered that drying the chromate rinse on the metal prior to the deionized water rinse, followed by deionized water rinsing and final drying, significantly increases corrosion resistance compared to the traditional steps of chromate rinsing, deionized water rinsing and drying. Any conventional means of drying may be used in the drying steps, e. g., forced air drying hot air drying, infrared light banks and the like. Hot air drying in ovens is commonly used and is the preferred method.
The following examples are set forth to illustrate the results of the process of this invention but it is to be understood that they are not to be construed as limitative of the invention in any way. For instance, in the examples a representative zinc phosphate conversion coating was used, however, any suitable phosphate coating may be employed with similar results since this variation is not critical to the claimed method.
EXAMPLE 1 The tests were carried out using panels of 1010 cold rolled steel which were first cleaned with a conventional alkaline cleaner and rinsed with cold water. A phosphate conversion coating bath as described in US. Pat. No. 3,203,835 was prepared comprised of [.22 percent of 75 percent phosphoric acid, 0.25 percent zinc oxide, 0.32 percent sodium chlorate, 0.27 percent nickel nitrate, 0.008 percent disodium arsenate and the balance water. A chromate rinse concentrate was prepared by mixing 16.6 parts of chromic acid, l6.6 parts of chromium nitrate and 66.8 parts water. The chromate rinse bath was prepared from the concentrate by diluting 10.5 volumes of the concentrate with 4,000 volumes of water. The pH was adjusted to 3.5 with 10 percent sodium hydroxide solution. The temperature of the chromate rinse was maintained at F.
Two metal treating sequences were used in the test. Process A, a method according to the present invention, consisted of the following steps:
No. 1 Phosphate conversion coating treatment at 160 F.
. No. 2 Water rinse at ambient temperature No. 3 Chromate rinse at 160 F.
No. 4 Drying step at 212 F.
No. 5 Deionized water rinse at ambient temperature No. 6 Drying step at 212 F. Process B, carried out according to the prior art methods, consisted of the following steps:
No. 1 Phosphate conversion coating treatment at 160 F.
No. 2 Water rinse at ambient temperature No. 3 Chromate rinse at 160 F.
No. 4 Deionized water rinse at ambient temperature No. 5 Drying step at 212 F.
Subsequent to the foregoing process steps, the panels were painted with a standard industrial alkyd paint and tested for corrosion resistance according to ASTM D l654-61 in a salt spray apparatus for 240 hours. As a result of this accelerated corrosion test, the panels prepared according to process A of the invention had only a trace of creep whereas the panels from process B had 1/1 6-inch creep, clearly indicating the superiority of process A. Creep" is defined as the distance the paint has peeled away from the score mark in the accelerated corrosion test.
EXAMPLE 2 The comparative tests of EXAMPLE 1 were repeated with these exceptions. The chromate rinse concentrate was prepared by reacting 35 parts of chromic acid with 0.8 part methyl alcohol in 50 parts water. The chromate rinse was prepared by diluting 4.5 volumes of this concentrate in 4,000 volumes of water. The chromate rinse was adjusted to pH 3.5 and maintained at 160 F. The panels were subjected to the two processes described in Example 1, then painted, and subjected at 240 hours in the salt spray cabinet. The process A panels showed no creep whereas those processed according to method B showed l/16-inch creep.
EXAMPLE 3 The tests of EXAMPLE 1 were repeated with these exceptions. The chromate rinse concentrate was prepared by reacting 35 parts of chromic acid with 16.6 parts of calcium carbonate and 48.4 parts water. The chromate rinse bath was prepared by diluting 3.5 volumes of the concentrate with 4000 volumes of water. No pH adjustment was made. The treatment processes were carried out as described above. The process A panels had only l/32-inch creep while the process B panels showed 54-inch creep, 8 times as great.
I claim:
1. A method of increasing the corrosion resistance of conversion coated metal which comprises the steps of treating the metal surface with a phosphate conversion coating bath, rinsing with water, applying a chromate rinse, drying, rinsing with deionized water, and drying the metal surface.
2. The method of claim 1 wherein the metal is selected from the group consisting of iron, steel, zinc and aluminum.

Claims (1)

  1. 2. The method of claim 1 wherein the metal is selected from the group consisting of iron, steel, zinc and aluminum.
US816036A 1969-04-14 1969-04-14 Process for increasing corrosion resistance of conversion coated metal Expired - Lifetime US3664887A (en)

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BE (1) BE748690A (en)
CA (1) CA924616A (en)
CH (1) CH507381A (en)
DE (1) DE2017865A1 (en)
FR (1) FR2063845A5 (en)
GB (1) GB1247504A (en)
NL (1) NL7005136A (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3852123A (en) * 1972-11-20 1974-12-03 Pennwalt Corp Sealing rinses for phosphate coatings on metal
US3864175A (en) * 1973-04-25 1975-02-04 Pennwalt Corp Chromate rinse for phosphate coated metals and metal products
US4165242A (en) * 1977-11-21 1979-08-21 R. O. Hull & Company, Inc. Treatment of metal parts to provide rust-inhibiting coatings by phosphating and electrophoretically depositing a siccative organic coating
US4539051A (en) * 1983-03-02 1985-09-03 Parker Chemical Company Process for producing phosphate coatings
WO1999035307A1 (en) * 1998-01-07 1999-07-15 Henkel Corporation Composition and process for treating a metal surface
US20040119038A1 (en) * 2002-12-20 2004-06-24 Applied Materials, Inc. Micromachined integrated fluid delivery system with dynamic metal seat valve and other components
WO2004059474A2 (en) * 2002-12-20 2004-07-15 Applied Materials, Inc. Micromachined intergrated fluid delivery system
US20080296354A1 (en) * 2007-05-31 2008-12-04 Mark Crockett Stainless steel or stainless steel alloy for diffusion bonding
US20080296351A1 (en) * 2007-05-31 2008-12-04 Mark Crockett Diffusion bonded fluid flow apparatus useful in semiconductor manufacturing

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2245609A (en) * 1940-03-07 1941-06-17 American Chem Paint Co Metal finishing process
US2318656A (en) * 1941-04-25 1943-05-11 Parker Rust Proof Co Coated metal article and method of making same
US3338755A (en) * 1963-09-03 1967-08-29 Hooker Chemical Corp Production of phosphate coatings on metals

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2245609A (en) * 1940-03-07 1941-06-17 American Chem Paint Co Metal finishing process
US2318656A (en) * 1941-04-25 1943-05-11 Parker Rust Proof Co Coated metal article and method of making same
US3338755A (en) * 1963-09-03 1967-08-29 Hooker Chemical Corp Production of phosphate coatings on metals

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3852123A (en) * 1972-11-20 1974-12-03 Pennwalt Corp Sealing rinses for phosphate coatings on metal
US3864175A (en) * 1973-04-25 1975-02-04 Pennwalt Corp Chromate rinse for phosphate coated metals and metal products
US4165242A (en) * 1977-11-21 1979-08-21 R. O. Hull & Company, Inc. Treatment of metal parts to provide rust-inhibiting coatings by phosphating and electrophoretically depositing a siccative organic coating
US4539051A (en) * 1983-03-02 1985-09-03 Parker Chemical Company Process for producing phosphate coatings
WO1999035307A1 (en) * 1998-01-07 1999-07-15 Henkel Corporation Composition and process for treating a metal surface
US20070200082A1 (en) * 2002-12-20 2007-08-30 Applied Materials, Inc. Manufacture of an integrated fluid delivery system for semiconductor processing apparatus
US7459003B2 (en) 2002-12-20 2008-12-02 Applied Materials, Inc. In-line filter in a diffusion bonded layered substrate
WO2004059474A3 (en) * 2002-12-20 2004-11-25 Applied Materials Inc Micromachined intergrated fluid delivery system
US20070051080A1 (en) * 2002-12-20 2007-03-08 Applied Materials, Inc. In-line filter in a diffusion bonded layered substrate
US20070113663A1 (en) * 2002-12-20 2007-05-24 Applied Materials, Inc. Capacitance dual electrode pressure sensor in a diffusion bonded layered substrate
US20040119038A1 (en) * 2002-12-20 2004-06-24 Applied Materials, Inc. Micromachined integrated fluid delivery system with dynamic metal seat valve and other components
US7448276B2 (en) 2002-12-20 2008-11-11 Applied Materials, Inc. Capacitance dual electrode pressure sensor in a diffusion bonded layered substrate
WO2004059474A2 (en) * 2002-12-20 2004-07-15 Applied Materials, Inc. Micromachined intergrated fluid delivery system
US8017028B2 (en) 2002-12-20 2011-09-13 Applied Materials, Inc. Method of increasing etchability of metals having chemical etching resistant microstructure
US7984891B2 (en) 2002-12-20 2011-07-26 Applied Materials, Inc. Manufacture of an integrated fluid delivery system for semiconductor processing apparatus
US20090039057A1 (en) * 2002-12-20 2009-02-12 Applied Materials, Inc. Method of increasing etchability of metals having chemical etching resistant microstructure
US20090057375A1 (en) * 2007-05-31 2009-03-05 Applied Materials, Inc. Method of improving surface roughness of fluid flow conduits within a diffusion bonded fluid flow structure
US20090072009A1 (en) * 2007-05-31 2009-03-19 Applied Materials, Inc. Method of preventing bonding between a load distribution block and a plate set of stacked sheets during diffusion bonding of a fluid flow structure
US7798388B2 (en) 2007-05-31 2010-09-21 Applied Materials, Inc. Method of diffusion bonding a fluid flow apparatus
US20080296351A1 (en) * 2007-05-31 2008-12-04 Mark Crockett Diffusion bonded fluid flow apparatus useful in semiconductor manufacturing
US20080296354A1 (en) * 2007-05-31 2008-12-04 Mark Crockett Stainless steel or stainless steel alloy for diffusion bonding

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Publication number Publication date
FR2063845A5 (en) 1971-07-09
NL7005136A (en) 1970-10-16
BE748690A (en) 1970-10-09
GB1247504A (en) 1971-09-22
DE2017865A1 (en) 1970-10-15
CH507381A (en) 1971-05-15
CA924616A (en) 1973-04-17

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