US20040256030A1 - Corrosion resistant, chromate-free conversion coating for magnesium alloys - Google Patents

Corrosion resistant, chromate-free conversion coating for magnesium alloys Download PDF

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Publication number
US20040256030A1
US20040256030A1 US10/601,247 US60124703A US2004256030A1 US 20040256030 A1 US20040256030 A1 US 20040256030A1 US 60124703 A US60124703 A US 60124703A US 2004256030 A1 US2004256030 A1 US 2004256030A1
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Prior art keywords
magnesium
solution
chromate
corrosion
phosphonic acids
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Abandoned
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US10/601,247
Inventor
Xia Tang
Mark Jaworowski
Kenneth Hammerschmidt
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Raytheon Technologies Corp
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United Technologies Corp
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Filing date
Publication date
Application filed by United Technologies Corp filed Critical United Technologies Corp
Priority to US10/601,247 priority Critical patent/US20040256030A1/en
Assigned to UNITED TECHNOLOGIES CORPORATION reassignment UNITED TECHNOLOGIES CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HAMMERSCHMIDT, KENNETH, JAWOROWSKI, MARK, TANG, XIA
Priority to SG200403770A priority patent/SG117497A1/en
Priority to KR1020040043886A priority patent/KR100611288B1/en
Priority to EP04253681A priority patent/EP1489199A1/en
Priority to JP2004180425A priority patent/JP2005008985A/en
Priority to CNB2004100714667A priority patent/CN100339507C/en
Priority to PL04368625A priority patent/PL368625A1/en
Publication of US20040256030A1 publication Critical patent/US20040256030A1/en
Abandoned legal-status Critical Current

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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
    • 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
    • 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
    • C23C22/40—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 molybdates, tungstates or vanadates
    • C23C22/44—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 molybdates, tungstates or vanadates containing also fluorides or complex fluorides
    • 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
    • C23C22/68—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 solutions with pH between 6 and 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
    • C23C22/73—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 characterised by the process
    • C23C22/77—Controlling or regulating of the coating process

Abstract

A chromate-free, phosphate-fluoride conversion coating, with or without vanadate, formed on a magnesium or a magnesium alloy substrate, includes an active corrosion inhibitor selected from the group consisting of organo-phosphonic acids. The phosphonic acid group reacts with the magnesium metal of the substrate to form an insoluble salt.

Description

    BACKGROUND OF THE INVENTION
  • The present invention relates to a corrosion resistant, chromate-free, phosphate-fluoride conversion coating, with or without vanadate, for a product formed from magnesium or a magnesium alloy and to a coating solution for use in a coating process. [0001]
  • Magnesium alloys are light and strong, but very vulnerable to corrosion due to the reactive nature of magnesium. Magnesium alloys are protected from corrosion in all practical applications. A commonly used, low cost, corrosion resistant treatment for magnesium alloys is a dichromate based conversion coating. While dichromate based conversion coatings provide good corrosion protection, they are based on a chemical compound (hexavalent chromium) that has many occupational exposure risks. A non-chromate, corrosion resistant magnesium conversion coating is required to meet industry demands. [0002]
  • Another treatment for protecting magnesium or magnesium alloy products is shown in U.S. Pat. No. 5,683,522 to Joesten, which is hereby incorporated by reference herein. In this treatment, a paint adherent and corrosion resistant coating of magnesium phosphate and magnesium fluoride is applied to a product formed from a magnesium alloy. The process for applying the coating involves immersing the magnesium alloy product in a solution having phosphate and fluoride ions. This treatment while providing a barrier film and very good paint adhesion, does not include electrochemically active ingredients to suppress corrosion. Co-pending application Ser. No. 10/073,688, filed Feb. 11, 2002, and incorporated herein by reference, discloses an improved phosphate-fluoride corrosion coating for magnesium and process for applying same. [0003]
  • It is an object of the present invention to provide an improved chromate-free corrosion resistant conversion coating for magnesium and magnesium alloy products. [0004]
  • It is a further object of the present invention to provide a coating solution for forming the chromate-free corrosion resistant coating. [0005]
    • SUMMARY OF THE INVENTION
  • The foregoing objects are attained by the present invention. [0006]
  • In accordance with the present invention, a chromate-free, phosphate-fluoride conversion coating, with or without vanadate, formed on a magnesium or a magnesium alloy substrate, includes an active corrosion inhibitor selected from the group consisting of organo-phosphonic acids. The phosphonic acid group reacts with the magnesium metal of the substrate to form an insoluble salt. The preferred organo-phosphonic acids used as corrosion inhibitors in accordance with the present invention are selected from the group consisting of straight chain or branched amino alkyl phosphonic acids, straight chain or branched alkyl phoshonic acids, and triphosphonic acids, particularly, nitrilotris (methylene) triphosphonic acid (NTMP). When the corrosion inhibitor includes amino alkyl phosphonic acids, the amine group can interact with vanadate ions in the coating solution to increase the vanadate incorporation into the conversion coating. [0007]
  • Other details of the magnesium-magnesium alloy conversion coating of the present invention, as well as objects and advantages attended thereto, are set forth in the following detailed description. [0008]
    • DETAILED DESCRIPTION
  • In accordance with the present invention, a solution for forming a chromate-free, corrosion resistant coating on a magnesium or magnesium alloy substrate comprises a solution having phosphate and fluoride ions and, an active corrosion inhibitor selected from the group consisting of organo-phosphonic acids. [0009]
  • The solution of the present invention may optionally include vanadate anions. The active corrosion inhibitor is selected from the group consisting of straight chained or branched amino-alkyl phosphonic acids, straight chained or branched alkyl phosphonic acids, triphosphonic acids, and mixtures thereof. A particular useful triphosphonic acid comprises nitrilotris (methylene) triphosphonic acid (NTMP). [0010]
  • As noted above, the chromate-free solution include phosphate and fluoride ions. Phosphate and fluoride ions are present in an amount of between about 1 g/L to 50 g/L and 1 g/L to 10 g/L, respectively, preferably between 10 g/L to 25 g/L and 3 g/L to 5 g/L, respectively. It is important in the present invention to control the pH of the solution and this is achieved by the amount of phosphate ions and fluoride ions in the solution. The pH of the solution is preferably in the range of 5 to 7. The particular phosphate and fluoride compounds employed in forming the solution having the appropriate pH is disclosed in detail in co-pending application Ser. No. 10/073,688, filed Feb. 11, 2002, and this co-pending application and the disclosure therein is incorporated herein by reference. [0011]
  • In accordance with the present invention, the corrosion inhibitor is present in the solution in an amount of between about 1 ppm to 1 wt %, preferably 10 ppm to 0.5 wt %. The corrosion inhibitor is in the form of an organo-phosphonic acid. Preferred organo-phosphonic acids include straight chained and branched amino-alkyl phosphonic acids, straight chained or branched alkyl phosphonic acids and triphosphonic acids. A particularly useful triphosphonic acid is nitrilotris (methylene) triphosphonic acid (NTMP). [0012]
  • In accordance with the present invention, the solution may optionally include vanadate anions. Sodium vanadate is a suitable source of vanadate ions for the solution of the present invention. In accordance with the present invention, the vanadate ions are present in an amount of between about 1.0 g/l to 5.0 g/l. It has been found that the vanadate anions interact with the amine group of the amino alkyl phosphonic acids increase incorporation of the vanadate into the conversion coating thereby improving the coating performance. In addition, the phosphonic acid groups of the corrosion inhibitor react with the magnesium metal substrate to form insoluble salts which improve corrosion performance. [0013]
  • The preferred chromate-free solution comprises phosphate ions in an amount of between 10 to 25 g/L, fluoride ions in an amount of between 3 g/L to 5 g/L, vanadate anions in an amount of between 1 g/L to 5 g/L, and the corrosion inhibitor in an amount of between 10 ppm to 0.5 wt %. [0014]
  • A magnesium or magnesium alloy substrate having a conversion coating in accordance with the present invention comprises mostly magnesium phosphate and magnesium fluoride. It is believed that the amino alkyl phosphonic acid will form insoluble magnesium salt as part of the conversion coating. This component will increase the interaction of vanadium with conversion coating, therefore increase vanadium content in the coating, should vanadium is used as corrosion inhibitor as well. [0015]
  • It is to be understood that the invention is not limited to the illustrations described and shown herein, which are deemed to be merely illustrative of the best modes of carrying out the invention, and which are susceptible of modification of form, size, arrangement of parts and details of operation. The invention rather is intended to encompass all such modifications which are within its spirit and scope as defined by the claims. [0016]

Claims (8)

1. A solution for forming a chromate-free, corrosion resistant coating on a product formed from magnesium or a magnesium alloy, comprising:
the solution having phosphate and fluoride ions; and
an active corrosion inhibitor selected from the group consisting of organo-phosphonic acids.
2. A solution according to claim 1, wherein the organo-phosphonic acid is selected from the group consisting of straight chained amino-alkyl phosphonic acids, branched amino-alkyl phosphonic acids, straight chained alkyl phosphonic acids, branched alkyl phosphonic acids, triphosphonic acids, and mixtures thereof.
3. A solution according to claim 2, wherein the triphosphonic acids comprise nitrilotris (methylene) triphosphonic acid (NTMP).
4. A solution according to claim 1, wherein the solution includes vanadate.
5. A solution according to claim 1, wherein the solution comprises 1 ppm to 1 wt % of the corrosion inhibitor, preferably 10 ppm to 0.5 wt %.
6. A solution according to claim 5, wherein phosphate ions are present in an amount of between 1 g/L to 50 g/L, preferably between 10 g/L to 25 g/L, and the fluoride ions are present in an amount of 1 g/L to 10 g/L, preferably 3 g/L to 5 g/L.
7. A process for preparing a corrosion-resistant, chromate free, coating on magnesium or a magnesium alloy substrate comprises treating the substrate with the solution of claims 1 through 6, wherein the phosphonic acid group reacts with magnesium metal forming an insoluble salt.
8. An article comprising the magnesium or the magnesium alloy substrate having a corrosion coating prepared in accordance with the process of claim 7.
US10/601,247 2003-06-20 2003-06-20 Corrosion resistant, chromate-free conversion coating for magnesium alloys Abandoned US20040256030A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
US10/601,247 US20040256030A1 (en) 2003-06-20 2003-06-20 Corrosion resistant, chromate-free conversion coating for magnesium alloys
SG200403770A SG117497A1 (en) 2003-06-20 2004-06-15 Corrosion resistant, chromate-free conversion coating for magnesium alloys
KR1020040043886A KR100611288B1 (en) 2003-06-20 2004-06-15 A Process for Preparing a Corrosion Resistant, Chromate-Free Conversion Coating for Magnesium Alloys
EP04253681A EP1489199A1 (en) 2003-06-20 2004-06-18 Corrosion resistant coating composition and process and coated magnesium
JP2004180425A JP2005008985A (en) 2003-06-20 2004-06-18 Solution for forming corrosion-resistant chromate-free converted coating for magnesium or magnesium alloy
CNB2004100714667A CN100339507C (en) 2003-06-20 2004-06-18 Corrosion resistant, chromate-free conversion coating for magnesium alloys
PL04368625A PL368625A1 (en) 2003-06-20 2004-06-18 Solution for producing coat, method for producing coat and coated product

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US10/601,247 US20040256030A1 (en) 2003-06-20 2003-06-20 Corrosion resistant, chromate-free conversion coating for magnesium alloys

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US20040256030A1 true US20040256030A1 (en) 2004-12-23

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US10/601,247 Abandoned US20040256030A1 (en) 2003-06-20 2003-06-20 Corrosion resistant, chromate-free conversion coating for magnesium alloys

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US (1) US20040256030A1 (en)
EP (1) EP1489199A1 (en)
JP (1) JP2005008985A (en)
KR (1) KR100611288B1 (en)
CN (1) CN100339507C (en)
PL (1) PL368625A1 (en)
SG (1) SG117497A1 (en)

Cited By (3)

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US20060237097A1 (en) * 2005-04-20 2006-10-26 Rohm And Haas Electronic Materials Llc Immersion method
US20090004486A1 (en) * 2007-06-27 2009-01-01 Sarah Arsenault Corrosion inhibiting additive
WO2009072905A2 (en) * 2007-12-04 2009-06-11 Katja Products Limited Surface coating

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JP2008174807A (en) * 2007-01-19 2008-07-31 Nippon Hyomen Kagaku Kk Chromium-free metal surface treatment liquid
TWI394863B (en) * 2007-12-27 2013-05-01 Kansai Paint Co Ltd Metal surface treatment composition, and surface-treated metal material with metal surface treatment layer obtained from the metal surface treatment composition
JP4908456B2 (en) 2008-06-02 2012-04-04 パンパシフィック・カッパー株式会社 Copper smelting method
US20130014670A1 (en) * 2010-04-01 2013-01-17 Commissariat a I'Energie Atomique et Aux Energies Altematives Use of anticorrosion agents for conditioning magnesium metal, conditioning material thus obtained and preparation process
JP5595874B2 (en) * 2010-11-04 2014-09-24 三井金属鉱業株式会社 Magnesium alloy surface treatment method
JP6089053B2 (en) * 2015-03-16 2017-03-01 有限会社エスク Biodegradable metal surface modified stent with anticorrosive ability
KR102142783B1 (en) * 2018-11-30 2020-08-07 주식회사 포스코 Surface-treating composition for magnesium or magnesium alloy and surface-treated magnesium or magnesium alloy using the same

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US4264378A (en) * 1979-02-14 1981-04-28 Oxy Metal Industries Corporation Chromium-free surface treatment
US4308079A (en) * 1980-06-16 1981-12-29 Martin Marietta Corporation Durability of adhesively bonded aluminum structures and method for inhibiting the conversion of aluminum oxide to aluminum hydroxide
US5143562A (en) * 1991-11-01 1992-09-01 Henkel Corporation Broadly applicable phosphate conversion coating composition and process
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US20060237097A1 (en) * 2005-04-20 2006-10-26 Rohm And Haas Electronic Materials Llc Immersion method
US20100101962A1 (en) * 2005-04-20 2010-04-29 Rohm And Haas Electronic Materials Llc Immersion method
US20090004486A1 (en) * 2007-06-27 2009-01-01 Sarah Arsenault Corrosion inhibiting additive
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WO2009072905A2 (en) * 2007-12-04 2009-06-11 Katja Products Limited Surface coating
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Also Published As

Publication number Publication date
PL368625A1 (en) 2004-12-27
JP2005008985A (en) 2005-01-13
KR20040110097A (en) 2004-12-29
EP1489199A1 (en) 2004-12-22
CN1572904A (en) 2005-02-02
CN100339507C (en) 2007-09-26
KR100611288B1 (en) 2006-08-10
SG117497A1 (en) 2005-12-29

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