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GB1590597A - Treating a1 or a1 alloy surfaces - Google Patents

Treating a1 or a1 alloy surfaces Download PDF

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Publication number
GB1590597A
GB1590597A GB42769/77A GB4276977A GB1590597A GB 1590597 A GB1590597 A GB 1590597A GB 42769/77 A GB42769/77 A GB 42769/77A GB 4276977 A GB4276977 A GB 4276977A GB 1590597 A GB1590597 A GB 1590597A
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GB
United Kingdom
Prior art keywords
coating
solution
aluminium
nitrite
silicate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB42769/77A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pyrene Chemical Services Ltd
Original Assignee
Pyrene Chemical Services Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pyrene Chemical Services Ltd filed Critical Pyrene Chemical Services Ltd
Publication of GB1590597A publication Critical patent/GB1590597A/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/60Chemical 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 alkaline aqueous solutions with pH greater than 8
    • C23C22/66Treatment of aluminium or alloys based thereon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24SSOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
    • F24S70/00Details of absorbing elements
    • F24S70/20Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
    • F24S70/25Coatings made of metallic material
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/40Solar thermal energy, e.g. solar towers

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Sustainable Energy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Sustainable Development (AREA)
  • Combustion & Propulsion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Description

(54) TREATING Al OR Al SURFACES (71) We, PYRENE CHEMICAL SERVICES LIMITED, a British company of Ridgeway, Iver, Buckinghamshire, SLO 9JJ, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: The present invention relates to a method for forming black coloured coatings on aluminium or aluminium alloy surfaces to improve their corrosion resistance and their stability as a base for paints. The invention also relates to a composition for use in such a method.
Conventionally, black coloured coatings have been formed by electrolytically developed colouration using anodic oxidation, electrolytic colouration, or dyeing painting or blackening by electroplating. However, it is not easy to obtain uniformly coloured coatings by electrolytic reactions, and these methods are complex, expensive and difficult to control.
Another known method for forming a black coating involves a chemical conversion using an aqueous solution containing a sulphide, a cyanide and molybdate and chromate ions. The waste from that treatment is difficult to treat and leads to undesirable pollution. It is also difficult to form uniform black coatings having sufficiently good appearance on a continuous basis.
A composition according to the invention comprises an aqueous solution which has a pH of from 9 to 12 and which contains nitrite, silicate, zinc and calcium and/or magnesium ions. A process for forming a black coloured coating on an aluminium or aluminium alloy surface, according to the invention, comprises contacting such a surface with a composition of the invention.
The structure and composition of the black coloured coating obtained by the process of the invention, and the conversion mechanism which is involved have not been elucidated, but it has been confirmed by fluorescent X-ray analysis that the coating comprises predominantly silicic acid, calcium and zinc. Such metal silicates are known to act as inhibitors on aluminium. It has been found that the addition of nitrite ion effectively promotes the chemical conversion reaction involved in forming the coating, and gives a uniform coating.
The aqueous treatment solution of the invention may be prepared either by dissolving each component separately in water and mixing the solutions or by preparing a dry mixture of the essential components and dissolving the mixture in water.
Suitable sources of nitrite ion include sodium nitrite and potassium nitrite. The concentration of this ion in the treatment solution must be from 0.1 to 15 g/l, calculated as NO2. At a concentration less than 0.1 g/l, no promotion effect in the black coloured coating is observed. A concentration higher than 15 g/l is uneconomic.
Zinc ion may be supplied in the form of, for example, the sulphate, phosphate or halide. Its concentration must be from 1 to 100 mg/l. At a concentration less than 1 mg/l, no black coloured coating is formed.
At a concentration higher than 100 mg/l, the coating is not satisfactory.
Calcium and/or magnesium ions may be included in the form of their halides, sulphates or phosphates, at a concentration of from I to 100 mg/l. At a concentration below this range, insufficient coating is obtained. At a concentration higher than 100 mg/l, the formation of the coating may be suppressed.
Silicate ion may be included in the treatment solution as, for example, a form of sodium silicate. Suitable forms are sodium metasilicate, sodium orthosilicate, sodium monosilicate and sodium bisilicate. The silicate concentration must be from I to 30 mg/l, calculated as SiO2. At a concentration less than I mg/l, etching will occur but no coating will be formed. At a concentration higher than 30 mg/l, the silicate inhibition effect is too great and the formation of a coating is inhibited.
The pH of the solution may be adjusted to a value of from 9 to 12 by using an alkali metal or ammonium hydroxide or carbonate.
If the pH of the composition is less than 9, the colouration of the black coating may be uneven and, at a pH higher than 12, the aluminium surface may be etched to an undesirable extent. thereby decreasing the colouration rate.
In use, the temperature of the solution is preferably from 80"C to its boiling point. At lower temperatures the colouration rate is relatively slow. The contact time, during which the coating is formed, is suitably from 10 to 40 minutes (by immersion in the treatment solution).
Prior to the coating step, the aluminium or aluminium alloy workpiece will usually be cleaned in a conventional manner. When the coating has been formed, the workpiece is usually rinsed with water and then dried in hot air.
Aluminium or aluminium alloys which can be treated in accordance with the process of the invention include rolled materials such as Al loop, 5052 S, 5082 S and 6063 S, as well as die-cast articles.
After the black coloured coating has been formed, conventional post-treatment steps can be carried out, if desired, to improve the corrosion resistance, workability for painting and fastness of the treated workpieces. These steps include the immersion into, or spraying with, a commercially available aqueous solution of a chromate or silicate, followed by drying. The corrosion resistance of the coating can be further improved by applying a clear paint, thereby ensuring also that the black coating is not easily stripped off on impact.
The following Examples illustrate the invention.
Example I Specimens of Al 100 PH 24 aluminium alloy and 6063 S aluminium alloy were degreased with trifluoroethylene and then with an alkali.
A treatment solution was made up to contain 0.1 g/l of Na2O.SiO2.9H2O, 0.02 g/l of ZnSO4.7H2O, 0 08 g/l of CaCl2.2H2O and 2 g/l of sodium nitrite in water, and the pH of the solution was adjusted to 10-5 with sodium hydroxide. The temperature of a bath containing the solution was controlled within the range 80 to 100"C. and the degreased specimens were immersed in the solution for 30 minutes. Uniform deep black coloured coatings were obtained on both Al 100 P and 6063 S.
Immediately after the subsequent rinsing and drying, the resulting sample was immersed in a treating bath containing 8 4 g/l of Parcolene (registered Trade Mark) at 60"C. for 15 seconds and then dried. The resulting sample was then coated with a commercially available clear acrylic paint and baked at 130"C. for 20 minutes. The thickness of the coating ranged from 20 to 25 microns and the appearance of the sample was brown in colour.
Example 2 A sample of Al 100 PH 24 aluminium alloy was degreased with trifluoroethylene and then with an alkali.
An aqueous solution was made up to contain 002 g/l of Na2O.SiO2.9H2O, 002 g/l of ZnSO4.7H2O, 0 15 g/l of CaCI2.2H2O and 10 g/l of sodium nitrite, and the pH was adjusted to a value of I 110 with sodium hydroxide. The degreased aluminium sample was immersed in the resulting solution at a temperature of from 80 to 100"C. for 20 minutes to obtain a uniform coating.
Immediately after the subsequent rinsing and drying, the resulting sample was immersed in a treating bath and then coated with an acrylic paint and baked, all as described in Example 1.
The test pieces obtained in Examples I and 2 were then subjected to the salt spray test according to JIS Z-237 1. In both cases, the time in which white stains were developed was 48 hours when only the conversion coating had been applied but 120 hours after the chromate sealing step. For the product of Example 2, the time in which white stains developed was 500 hours after the acrylic paint had been applied. These results show that the durability of the chromate-sealed coating is about 2 5 times as high as that of the unsealed coating, and that the painted surface is more than 10 times as durable as the conversion coated surface.
It will be appreciated that the working solution of this invention may be prepared from a more concentrated composition. Accordingly, this invention provides dry compositions and aqueous concentrates which are suitable for dilution and, if necessary, basification to form such a working solution.
WHAT WE CLAIM IS: 1. An aqueous solution which has a pH of from 9 to 12 and which contains, per litre thereof, from 0.1 to 15 g nitrite ions calculated as NO2, from 1 to 30 mg silicate ions calculated as SiO2, from 1 to 100 mg zinc ions, and from 1 to 100 mg calcium and/or magnesium ions.
2. A solution according to claim 1 substantially as described in either of the Examples.
3. A dry composition which is suitable for dilution and, if necessary, basification to form a working solution according to claim 1 or claim 2 and which comprises nitrite, silicate, zinc and calcium and/or magnesium.
4. An aqueous concentrate suitable for dilution and, if necessary, basification to form a working solution according to claim 1 or claim 2 and which contains nitrite, silicate, zinc and calcium and/or magnesium ions.
**WARNING** end of DESC field may overlap start of CLMS **.

Claims (7)

  1. **WARNING** start of CLMS field may overlap end of DESC **.
    uneven and, at a pH higher than 12, the aluminium surface may be etched to an undesirable extent. thereby decreasing the colouration rate.
    In use, the temperature of the solution is preferably from 80"C to its boiling point. At lower temperatures the colouration rate is relatively slow. The contact time, during which the coating is formed, is suitably from 10 to 40 minutes (by immersion in the treatment solution).
    Prior to the coating step, the aluminium or aluminium alloy workpiece will usually be cleaned in a conventional manner. When the coating has been formed, the workpiece is usually rinsed with water and then dried in hot air.
    Aluminium or aluminium alloys which can be treated in accordance with the process of the invention include rolled materials such as Al loop, 5052 S, 5082 S and 6063 S, as well as die-cast articles.
    After the black coloured coating has been formed, conventional post-treatment steps can be carried out, if desired, to improve the corrosion resistance, workability for painting and fastness of the treated workpieces. These steps include the immersion into, or spraying with, a commercially available aqueous solution of a chromate or silicate, followed by drying. The corrosion resistance of the coating can be further improved by applying a clear paint, thereby ensuring also that the black coating is not easily stripped off on impact.
    The following Examples illustrate the invention.
    Example I Specimens of Al 100 PH 24 aluminium alloy and 6063 S aluminium alloy were degreased with trifluoroethylene and then with an alkali.
    A treatment solution was made up to contain 0.1 g/l of Na2O.SiO2.9H2O, 0.02 g/l of ZnSO4.7H2O, 0 08 g/l of CaCl2.2H2O and 2 g/l of sodium nitrite in water, and the pH of the solution was adjusted to 10-5 with sodium hydroxide. The temperature of a bath containing the solution was controlled within the range 80 to 100"C. and the degreased specimens were immersed in the solution for 30 minutes. Uniform deep black coloured coatings were obtained on both Al
    100 P and 6063 S.
    Immediately after the subsequent rinsing and drying, the resulting sample was immersed in a treating bath containing 8 4 g/l of Parcolene (registered Trade Mark) at 60"C. for 15 seconds and then dried. The resulting sample was then coated with a commercially available clear acrylic paint and baked at 130"C. for 20 minutes. The thickness of the coating ranged from 20 to 25 microns and the appearance of the sample was brown in colour.
    Example 2 A sample of Al 100 PH 24 aluminium alloy was degreased with trifluoroethylene and then with an alkali.
    An aqueous solution was made up to contain 002 g/l of Na2O.SiO2.9H2O, 002 g/l of ZnSO4.7H2O, 0 15 g/l of CaCI2.2H2O and 10 g/l of sodium nitrite, and the pH was adjusted to a value of I 110 with sodium hydroxide. The degreased aluminium sample was immersed in the resulting solution at a temperature of from 80 to 100"C. for 20 minutes to obtain a uniform coating.
    Immediately after the subsequent rinsing and drying, the resulting sample was immersed in a treating bath and then coated with an acrylic paint and baked, all as described in Example 1.
    The test pieces obtained in Examples I and 2 were then subjected to the salt spray test according to JIS Z-237 1. In both cases, the time in which white stains were developed was 48 hours when only the conversion coating had been applied but 120 hours after the chromate sealing step. For the product of Example 2, the time in which white stains developed was 500 hours after the acrylic paint had been applied. These results show that the durability of the chromate-sealed coating is about 2 5 times as high as that of the unsealed coating, and that the painted surface is more than 10 times as durable as the conversion coated surface.
    It will be appreciated that the working solution of this invention may be prepared from a more concentrated composition. Accordingly, this invention provides dry compositions and aqueous concentrates which are suitable for dilution and, if necessary, basification to form such a working solution.
    WHAT WE CLAIM IS: 1. An aqueous solution which has a pH of from 9 to 12 and which contains, per litre thereof, from 0.1 to 15 g nitrite ions calculated as NO2, from 1 to 30 mg silicate ions calculated as SiO2, from 1 to 100 mg zinc ions, and from 1 to 100 mg calcium and/or magnesium ions.
  2. 2. A solution according to claim 1 substantially as described in either of the Examples.
  3. 3. A dry composition which is suitable for dilution and, if necessary, basification to form a working solution according to claim 1 or claim 2 and which comprises nitrite, silicate, zinc and calcium and/or magnesium.
  4. 4. An aqueous concentrate suitable for dilution and, if necessary, basification to form a working solution according to claim 1 or claim 2 and which contains nitrite, silicate, zinc and calcium and/or magnesium ions.
  5. 5. A process of forming a coating on an
    aluminium or aluminium alloy surface comprising contacting the surface with a solution according to claim 1 or claim 2.
  6. 6. A process according to claim 5 in which the solution is at a temperature of from 80"C to the boiling point of the solution.
  7. 7. A process according to claim 5 substantially as described in either of the Examples.
GB42769/77A 1976-11-05 1977-10-14 Treating a1 or a1 alloy surfaces Expired GB1590597A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13232176A JPS5357142A (en) 1976-11-05 1976-11-05 Process for forming black coating on aluminum or aluminum alloy

Publications (1)

Publication Number Publication Date
GB1590597A true GB1590597A (en) 1981-06-03

Family

ID=15078571

Family Applications (1)

Application Number Title Priority Date Filing Date
GB42769/77A Expired GB1590597A (en) 1976-11-05 1977-10-14 Treating a1 or a1 alloy surfaces

Country Status (7)

Country Link
JP (1) JPS5357142A (en)
CH (1) CH615462A5 (en)
DE (1) DE2739576A1 (en)
FR (1) FR2370107A1 (en)
GB (1) GB1590597A (en)
IT (1) IT1089033B (en)
SE (1) SE425008B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2223239A (en) * 1988-08-24 1990-04-04 Ardrox Pyrene Ltd Phosphating process
CN114990538A (en) * 2022-08-04 2022-09-02 山东一立动力科技股份有限公司 Aluminum alloy surface blackening treatment method

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NO146439C (en) * 1979-11-09 1982-09-29 Inst Energiteknik PROCEDURE FOR THE PREPARATION OF A DARK COLOR, WAVE LENGTH SELECTIVE ALUMINUM OIL
IT1152657B (en) * 1982-09-28 1987-01-07 Italia Alluminio PROCEDURE FOR THE FORMATION OF A BLACK SELECTIVE LAYER ON SURFACES OF ALUMINUM BODIES AND ITS ALLOYS AND PRODUCTS SO OBTAINED
US4586977A (en) * 1984-04-03 1986-05-06 Imperial Clevite Inc. Method of bonding a high temperature resistant polymeric material to an aluminum base substrate
US4555294A (en) * 1984-04-03 1985-11-26 Imperial Clevite Inc. Inorganic composition adapted for use in bonding a high temperature resistant polymeric material to an aluminum base substrate
JP2756169B2 (en) * 1990-02-26 1998-05-25 古河電気工業株式会社 Manufacturing method of colored aluminum transmission line and its accessories
US5441773A (en) * 1992-01-21 1995-08-15 Betz Laboratories, Inc. Composition and method of forming a black no-rinse conversion coating on metal surfaces
JP5634000B2 (en) * 2006-04-06 2014-12-03 新日鐵住金株式会社 Surface treated metal parts
FR3041695B1 (en) 2015-09-25 2019-03-29 Illinois Tool Works Inc. DEGASSING TANK AND MOTOR VEHICLE COMPRISING SUCH A TANK

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1846844A (en) * 1929-07-16 1932-02-23 Gen Electric Process of treating aluminum
FR1007070A (en) * 1948-02-19 1952-04-30 Vernal S A Process for improving the appearance of the surface of objects made of aluminum or aluminum alloys
DE1914759A1 (en) * 1969-03-22 1970-10-01 Dettner Dr Heinz W Hot alkaline baths
US3971674A (en) * 1975-03-03 1976-07-27 Aluminum Company Of America Selective black coating for aluminum
US4145462A (en) * 1976-06-09 1979-03-20 Toyo Aluminium Kabushiki Kaisha Process for producing solar collectors

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2223239A (en) * 1988-08-24 1990-04-04 Ardrox Pyrene Ltd Phosphating process
GB2223239B (en) * 1988-08-24 1992-09-23 Ardrox Pyrene Ltd Phosphating process
CN114990538A (en) * 2022-08-04 2022-09-02 山东一立动力科技股份有限公司 Aluminum alloy surface blackening treatment method
CN114990538B (en) * 2022-08-04 2022-11-25 山东一立动力科技股份有限公司 Aluminum alloy surface blackening treatment method

Also Published As

Publication number Publication date
CH615462A5 (en) 1980-01-31
FR2370107B1 (en) 1980-06-20
SE425008B (en) 1982-08-23
JPS5551030B2 (en) 1980-12-22
IT1089033B (en) 1985-06-10
JPS5357142A (en) 1978-05-24
FR2370107A1 (en) 1978-06-02
DE2739576A1 (en) 1978-05-18
SE7712511L (en) 1978-05-06

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Legal Events

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PS Patent sealed [section 19, patents act 1949]
PCNP Patent ceased through non-payment of renewal fee