US3672966A - Process for the treatment of anodic oxidized aluminum surfaces - Google Patents

Process for the treatment of anodic oxidized aluminum surfaces Download PDF

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Publication number
US3672966A
US3672966A US53318A US3672966DA US3672966A US 3672966 A US3672966 A US 3672966A US 53318 A US53318 A US 53318A US 3672966D A US3672966D A US 3672966DA US 3672966 A US3672966 A US 3672966A
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United States
Prior art keywords
sealing
acid
treatment
solution
aluminum
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Expired - Lifetime
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US53318A
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English (en)
Inventor
Roland Geisler
Hans Gunther Germscheid
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C25D11/246—Chemical after-treatment for sealing layers

Definitions

  • Anodic oxide coatings are frequently applied to aluminum surfaces for the purpose of corrosion protection. These oxide coatings protect the aluminum surface against the effects of the atmosphere and other corrosive media. Furthermore, anodic oxide coatings are also applied so as to obtain a harder surface and thus improve wear resistance of the aluminum. By virtue of the color of the oxide coatings or their readily partial colorability, particularly decorative effects can be achieved.
  • a number of processes are known for the production of anodic oxide coatings on aluminum.
  • the production of the oxide coatings takes place, for example, by direct current in solutions of sulfuric acid (direct current-sulfuric acid process).
  • solutions of organic acids such as, in particular, sulfophthalic acid or sulfanilic acid or mixtures of these acids with sulfuric acid are used.
  • the last mentioned processes are known, in particular, as hard anodizing processes.
  • oxide coatings do not fulfill all requirements in respect of corrosion protection, however, since they provide a porous structure. For this reason it is necessary subsequently to seal the oxide coatings. This after-sealing is usually carried out with hot or boiling water or steam and is known by the name of sealing. In this way the pores are closed and thus the corrosion protection is substantially enhanced.
  • An object of the present invention is the development in the process for treating aluminum surfaces which comprises subjecting aluminum and aluminum alloy surfaces to an anodic oxidation and subsequent sealing with hot water or steam, the improvement selected from the group consisting essentially of (A) applying a solution from 0.01 to 10 gm. per liter of an acid selected from the group consisting of (1) acrylic acid at a pH of from 5 to 6 and (2) a polymer of acrylic acid, a polymer of methacrylic acid, a polymer of maleic acid, copolymers of maleic acid with ethylene or vinyl alcohol, and mixtures thereof, said polymers having a specific viscosity of up to 0 :0.75 cp. in a 0.7% solution in 2 N NaOH at 20 C., to the anodic oxidized surfaces at temperatures of from 15 C. to C. prior to said sealing and (B) applying said solution to the anodic oxidized surfaces simultaneously with said sealing with hot water.
  • A applying a solution from 0.01 to 10 gm. per liter of an acid selected
  • the present invention provides a process for the treatment of aluminum or aluminum alloy surfaces by anodic oxidation with a subsequent sealing by water or steam in which prior to the completion of the sealing, the said surfaces are treated at a temperature of from 15 C. to 95 C. with a solution containing acrylic acid and/or a polymer of acrylic acid, methacrylic acid or maleic acid having a specific viscosity of up to 1 :0.75 cp. in a 0.7% solution in 2 N NaOH at 20 C.
  • the said intermediate treating solution contains from 0.01 to 10 gm./liter of acrylic acid and/or a polymer of acrylic acid, methacrylic acid or maleic acid.
  • acrylic acid and polymers of acrylic, methacrylic and maleic acid can be used.
  • the polymers of maleic acid may be pure polymers or copolymers, for example, with ethylene or vinyl alcohol. It has been found appropriate to use polymers Whose specific viscosity does not exceed a value of 0.75 cp. The specific viscosity measured is always that of a 0.7% solution in 2 N NaOH at 20 C. in a Brookfield rotary viscometer.
  • the intermediate treatment is carried out with solutions containing polyacrylic acid and/or polymethacrylic acid with viscosities of from 1 :0.05 to 0.2.5 cp.
  • the solution for the intermediate treatment preferably contains 0.1 to 10 gm./liter of the said compounds which may be used singly or in a mixture, though it is also possible to use larger quantities,,but this brings no further advantages.
  • the above described solutions for the intermediate treatment preferably have a pH value situated between 5 and 6.
  • This pH value has proved appropriate, particularly with the polymers in that an additional pH adjustment is not required.
  • Such a pH value should be adjusted to this value however, if for the preparation of as potassium, sodium or ammonium salts of the acids are used."' In"general, sucha'procedure is not recommended since as a result neutral salts enter into the solutions. It is more advantageous, in fact, to prepare the solutions with the free acids by using fully demineralized or distilled or condensed water.
  • the intermediate treatment is carried out at temperatures between 15 C. and 95 C., preferably at temperatures of over 50 C., the anodized articles of aluminum or aluminum alloys being either dipped into solutions or are sprayed with the same.
  • the duration of treatment is from 0.5 to 60 minutes but generally under minutes. Longer treatment times; however, have no detrimental eifect.
  • rinsing with water may be eifected to avoid an entrainment of substances which are removable by rinsing in the subsequent sealing stage. This rinsing is not essential, however, and no disadvantages result if the aluminum parts are transferred, immediately after the intermediate treatment, to the aftersealing.
  • the aftersealing with water and the intermediate treatment are carried out in one operating stage.
  • the water provided for the after-sealing is mixed with the said compounds in the specified quantities and the sealing is carried out in the customary manner.
  • The'after-sealing solutions may also contain additives known for such purposes, such as nickel acetate, in small quantities. It is possible by the new process to prevent the formation of sealing films without impairing the anodic oxide coating or diminishing the quality of the after-sealing. The appearance of the surface is not affected by the process in accordance with the invention. The effects, as achieved by pretreatment and anodizing, remain unchanged.
  • the quality of theoxide coatings is determined by the so-called Testal value according to DIN 50 949. Values which according to this test are above are technically not satisfactory.
  • the designation of the aluminum alloys in the examples is in accordance with DIN 1725. DIN is the abbreviation for "Deutsche Industrie-Norm representing a series of standard German published test procedures.
  • EXAMPLE 4 Aluminum shaped specimens (AlMgSi0.5), alkaline degreased and pickled in :the' customary mannerand anodically oxidized by the direct current sulfuric acid process (thickness, of coating 20 to.30;i), were sealed. in a solutionwhich'contained 5 gm./liter of the chemicals listed in the following table 'and which had 'been"adjusted to a pH value of 5 to 6 for 60 minutes at 100 C., or they were pretreatedin the solution for 10 minutes at C. and after an intermediate rinsing sealed in hot water at C. for'60 minutes. . The thickness of the coating remained unchanged on the different specimens.
  • the improvement consisting essentially of applying a solution containing from 0.01 to 1.0 gm; per liter of an acid selected from the group consisting of (1) acrylic. acidat a pH of'from 5 to 6" and 2) a polymer of acrylic acid, a polymer of methacrylic acid, a polymer of maleic acid, copolymers of maleic acid with ethylene or vinyfalcohol, and mixtures ,thereof,.jsaid polymers having a specific viscosity of up to 1 :0.75, cp. in a 0.7% solution in 2N NaOH at 20 C., to the anodic oxidized surfaces attemperatures of from 15 C. to 100 C. prior to completion of said sealing.
  • an acid selected from the group consisting of (1) acrylic. acidat a pH of'from 5 to 6" and 2) a polymer of acrylic acid, a polymer of methacrylic acid, a polymer of maleic acid, copolymers of maleic acid with ethylene or vinyfalcohol,

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Joining Of Glass To Other Materials (AREA)
  • Electrochemical Coating By Surface Reaction (AREA)
US53318A 1969-07-26 1970-07-08 Process for the treatment of anodic oxidized aluminum surfaces Expired - Lifetime US3672966A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1938039A DE1938039C3 (de) 1969-07-26 1969-07-26 Verfahren zur Behandlung von anodisch oxydierten Aluminiumoberflächen

Publications (1)

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US3672966A true US3672966A (en) 1972-06-27

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ID=5740973

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US53318A Expired - Lifetime US3672966A (en) 1969-07-26 1970-07-08 Process for the treatment of anodic oxidized aluminum surfaces

Country Status (15)

Country Link
US (1) US3672966A (enrdf_load_stackoverflow)
JP (1) JPS4947618B1 (enrdf_load_stackoverflow)
AT (1) AT295952B (enrdf_load_stackoverflow)
BE (1) BE753900A (enrdf_load_stackoverflow)
CA (1) CA922262A (enrdf_load_stackoverflow)
CH (1) CH558427A (enrdf_load_stackoverflow)
DE (1) DE1938039C3 (enrdf_load_stackoverflow)
ES (1) ES382171A1 (enrdf_load_stackoverflow)
FR (1) FR2053182B1 (enrdf_load_stackoverflow)
GB (1) GB1265424A (enrdf_load_stackoverflow)
NL (1) NL168015C (enrdf_load_stackoverflow)
NO (1) NO125686B (enrdf_load_stackoverflow)
SE (1) SE367439B (enrdf_load_stackoverflow)
YU (1) YU34914B (enrdf_load_stackoverflow)
ZA (1) ZA705096B (enrdf_load_stackoverflow)

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3961111A (en) * 1975-03-18 1976-06-01 Pennwalt Corporation Method of increasing corrosion resistance of anodized aluminum
US4024039A (en) * 1972-08-31 1977-05-17 Honny Chemicals Company, Ltd. Coloring methods for aluminum and aluminum alloys
US4130466A (en) * 1978-05-31 1978-12-19 The United States Of America As Represented By The Secretary Of The Navy Antifouling coating for aluminum structures
US4310390A (en) * 1977-08-10 1982-01-12 Lockheed Corporation Protective coating process for aluminum and aluminum alloys
EP0072384A1 (de) * 1981-08-14 1983-02-23 Cowa chemische Fabrikation GmbH Konservierungsmittel für Metalloberflächen sowie Verfahren zu deren Beschichtung
US4427765A (en) 1981-07-06 1984-01-24 Hoechst Aktiengesellschaft Hydrophilic coating of salt-type phosphorus or sulfur polymer on aluminum support materials for offset printing plates and process for manufacture and use with light sensitive layer thereon
US4427766A (en) 1981-07-06 1984-01-24 Hoechst Aktiengesellschaft Hydrophilic coating of salt type nitrogen polymer on aluminum support materials for offset printing plates and process for manufacture and use with light sensitive layer thereon
US5178961A (en) * 1990-07-21 1993-01-12 Hoechst Aktiengesellschaft Thermally crosslinkable hydrophilic copolymers and their use in reprography
US5178963A (en) * 1990-07-21 1993-01-12 Hoechst Aktiengesellschaft Hydrophilic copolymers and their use in reprography
US5219664A (en) * 1990-07-21 1993-06-15 Hoechst Aktiengesellschaft Hydrophilic copolymers and their use in reprography
US5262244A (en) * 1990-07-21 1993-11-16 Hoechst Aktiengesellschaft Hydrophilic copolymers and their use in reprography
US5302460A (en) * 1990-07-21 1994-04-12 Hoechst Aktiengesellschaft Support material for offset-printing plates in the form of a sheet, a foil or a web process for its production and offset-printing plate comprising said material
US6410197B1 (en) 1998-09-18 2002-06-25 Lexmark International, Inc. Methods for treating aluminum substrates and products thereof
CN109518252A (zh) * 2017-09-18 2019-03-26 中铝材料应用研究院有限公司 一种基于铝合金的高胶接和耐腐蚀的阳极氧化方法
CN109518253A (zh) * 2017-09-18 2019-03-26 中铝材料应用研究院有限公司 一种基于铝合金表面的高胶接和耐腐蚀的阳极氧化方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3434668A1 (de) * 1984-09-21 1986-04-03 Henkel KGaA, 4000 Düsseldorf Konservierungsmittel fuer aluminium-oberflaechen
JP3803353B2 (ja) * 2003-06-17 2006-08-02 中国電化工業株式会社 表面処理アルミニウム材とその製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1246106A (fr) * 1957-04-12 1960-11-18 Pechiney Prod Chimiques Sa Protection des surfaces métalliques
FR1255294A (fr) * 1960-04-25 1961-03-03 Perfectionnement apporté au traitement de surface des alliages légers à base d'aluminium

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4024039A (en) * 1972-08-31 1977-05-17 Honny Chemicals Company, Ltd. Coloring methods for aluminum and aluminum alloys
US3961111A (en) * 1975-03-18 1976-06-01 Pennwalt Corporation Method of increasing corrosion resistance of anodized aluminum
US4310390A (en) * 1977-08-10 1982-01-12 Lockheed Corporation Protective coating process for aluminum and aluminum alloys
US4130466A (en) * 1978-05-31 1978-12-19 The United States Of America As Represented By The Secretary Of The Navy Antifouling coating for aluminum structures
US4427765A (en) 1981-07-06 1984-01-24 Hoechst Aktiengesellschaft Hydrophilic coating of salt-type phosphorus or sulfur polymer on aluminum support materials for offset printing plates and process for manufacture and use with light sensitive layer thereon
US4427766A (en) 1981-07-06 1984-01-24 Hoechst Aktiengesellschaft Hydrophilic coating of salt type nitrogen polymer on aluminum support materials for offset printing plates and process for manufacture and use with light sensitive layer thereon
EP0072384A1 (de) * 1981-08-14 1983-02-23 Cowa chemische Fabrikation GmbH Konservierungsmittel für Metalloberflächen sowie Verfahren zu deren Beschichtung
US5178963A (en) * 1990-07-21 1993-01-12 Hoechst Aktiengesellschaft Hydrophilic copolymers and their use in reprography
US5178961A (en) * 1990-07-21 1993-01-12 Hoechst Aktiengesellschaft Thermally crosslinkable hydrophilic copolymers and their use in reprography
US5219664A (en) * 1990-07-21 1993-06-15 Hoechst Aktiengesellschaft Hydrophilic copolymers and their use in reprography
US5262244A (en) * 1990-07-21 1993-11-16 Hoechst Aktiengesellschaft Hydrophilic copolymers and their use in reprography
US5302460A (en) * 1990-07-21 1994-04-12 Hoechst Aktiengesellschaft Support material for offset-printing plates in the form of a sheet, a foil or a web process for its production and offset-printing plate comprising said material
US6410197B1 (en) 1998-09-18 2002-06-25 Lexmark International, Inc. Methods for treating aluminum substrates and products thereof
CN109518252A (zh) * 2017-09-18 2019-03-26 中铝材料应用研究院有限公司 一种基于铝合金的高胶接和耐腐蚀的阳极氧化方法
CN109518253A (zh) * 2017-09-18 2019-03-26 中铝材料应用研究院有限公司 一种基于铝合金表面的高胶接和耐腐蚀的阳极氧化方法
CN109518252B (zh) * 2017-09-18 2021-05-21 中铝材料应用研究院有限公司 一种基于铝合金的高胶接和耐腐蚀的阳极氧化方法
CN109518253B (zh) * 2017-09-18 2021-05-21 中铝材料应用研究院有限公司 一种基于铝合金表面的高胶接和耐腐蚀的阳极氧化方法

Also Published As

Publication number Publication date
CA922262A (en) 1973-03-06
ES382171A1 (es) 1972-11-01
DE1938039A1 (de) 1971-02-11
YU34914B (en) 1980-04-30
DE1938039C3 (de) 1978-04-06
NL7009365A (enrdf_load_stackoverflow) 1971-01-28
YU181770A (en) 1979-10-31
JPS4947618B1 (enrdf_load_stackoverflow) 1974-12-17
CH558427A (de) 1975-01-31
DE1938039B2 (de) 1971-10-21
BE753900A (fr) 1971-01-25
ZA705096B (en) 1971-04-28
AT295952B (de) 1972-01-25
FR2053182B1 (enrdf_load_stackoverflow) 1973-05-25
NL168015C (nl) 1982-02-16
NL168015B (nl) 1981-09-16
SE367439B (enrdf_load_stackoverflow) 1974-05-27
GB1265424A (enrdf_load_stackoverflow) 1972-03-01
FR2053182A1 (enrdf_load_stackoverflow) 1971-04-16
NO125686B (enrdf_load_stackoverflow) 1972-10-16

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