EP0575244B1 - Verfahren zur Behandlung eines Substrats auf Aluminiumbasis für die Eloxierung, das in diesem Verfahren verwendete Bad sowie ein Konzentrat zur Herstellung des Bades - Google Patents

Verfahren zur Behandlung eines Substrats auf Aluminiumbasis für die Eloxierung, das in diesem Verfahren verwendete Bad sowie ein Konzentrat zur Herstellung des Bades Download PDF

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Publication number
EP0575244B1
EP0575244B1 EP93401533A EP93401533A EP0575244B1 EP 0575244 B1 EP0575244 B1 EP 0575244B1 EP 93401533 A EP93401533 A EP 93401533A EP 93401533 A EP93401533 A EP 93401533A EP 0575244 B1 EP0575244 B1 EP 0575244B1
Authority
EP
European Patent Office
Prior art keywords
bath
acid
acids
concentration
group
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 - Lifetime
Application number
EP93401533A
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English (en)
French (fr)
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EP0575244A1 (de
Inventor
Joseph Schapira
Patrick Droniou
Patrice Pelletier
Stéphane Ganepain
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.)
Compagnie Francaise de Produits Industriels SA
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Compagnie Francaise de Produits Industriels SA
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Classifications

    • 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
    • C25D11/16—Pretreatment, e.g. desmutting

Definitions

  • the subject of the invention is a method of treatment aluminum-based substrates for anodizing.
  • It also relates to a bath used in this process as well as a concentrate for the preparation of the bath.
  • Substrates i.e. parts and profiles based on aluminum, in other words aluminum or one of its alloys, are used in industry and in particular in architectural application, in particular for the manufacture of frames.
  • above parts and profiles can be painted or be electrolytic anodizing treatment of aluminum in an acid medium.
  • the parts and profiles are protected by an artificially formed Al 2 O 3 oxide layer; according to the desired degree of protection which is a function of the use of the parts inside or outside, the alumina layer can be more or less thick; its thickness is generally between 2 and 30 micrometers.
  • the steps preceding the anodic oxidation include the so-called satin-finishing step producing a pickling which consists in removing the surface layer from the substrates; in practice, the treated parts or sections are pickled to a thickness of approximately 30 microns, which corresponds to a weight loss of approximately 90 g / m 2 .
  • complexing agents are added to the above-mentioned baths such as gluconate.
  • the invention therefore aims to provide a method and a bath of the kind in question which do not exhibit the disadvantages inherent in the prior art and thanks to which it is possible to impart excellent mattness treated substrates.
  • the Applicant Company has had the merit of find that, unexpectedly and surprisingly, it became possible to obtain substrates with a excellent mattness and appearance without risk of exploitation and while reducing the amount of alkaline releases (soda and aluminate) as well as the pickling thickness from then on that a bath is used for the satin-finishing step acid comprising at least one fluorinated derivative of titanium and / or zirconium and / or silicon as well as at least one acid from the group comprising nitric, sulfuric and phosphoric.
  • the subject of the invention is the use, for the satin-finishing step, in a treatment process for the anodizing of parts and profiles of aluminum or one of its alloys used in application architectural, in particular for the manufacture of frames, of an acid bath comprising at least one of the compounds of the group comprising the fluometallic acids H 2 TiF 6 , H 2 ZrF 6 and H 2 SiF 6 as well as their alkali salts or d ammonium at a concentration of at least 1 g / l and at least one of the acids of the group comprising nitric acid, sulfuric acid and phosphoric acid at a concentration of between 0.5 and 100 ml per liter of bath, expressed as concentrated commercial acid and advantageously non-ionic, anionic, cationic surfactants and third-party solvents.
  • the satin-finishing step using the acid bath is followed by a complementary light satin-finishing step using an alkaline bath, the conditions of this satin-finishing being such that it leads to pickling of '' not more than 40 g / m 2 of aluminum.
  • the bath according to the invention for the treatment is characterized by the fact that it comprises at least one of the compounds from the group comprising the fluometallic acids H 2 TiF 6 , H 2 ZrF 6 and H 2 SiF 6 as well as their alkali or ammonium salts at a concentration of at least 1 g / l and at least one of the acids from the group consisting of sulfuric and phosphoric acids at a concentration of between 0.5 and 100 ml per liter of bath, expressed as concentrated commercial acid and advantageously nonionic surfactants , anionic, cationic and third-party solvents.
  • the concentrate according to the invention which is capable of providing by dilution with water the bath according to the invention defined above, is characterized in that it contains at least one of the compounds of the group comprising fluometallic acids H 2 TiF 6 , H 2 ZrF 6 and H 2 SiF 6 as well as their alkali or ammonium salts at a concentration of commercial product of between 50 and 99.5% and at least one acid from the group consisting of sulfuric and phosphoric acids at a concentration of commercial product of 0.5 to 50%.
  • Sulfuric and phosphoric acids have the advantage of being present on the anodic oxidation lines in the acid degreasing (H 3 PO 4 ), bleaching (HNO 3 ) and anodic oxidation (H 2 SO 4 ) baths. ; they can also be regenerated from these baths by already known methods (ion exchange resins for example); they can also be used directly in the acid pickling bath if their pollution rate allows, which is the case in the context of the present invention.
  • the above concentrate can be diluted in water to a concentration between 1 per thousand and 10% for constitute the ready-to-use bath.
  • the above concentrations as well as the duration and the temperature of the satin-finishing step are adjusted so as to obtain a pickling rate of at least 5 g / m 2 of the substrate.
  • the surfactants in question may be chosen from the group comprising alkylphenols, polyalkoxylated alcohols and amines, alkyl-, alkylaryl- and arylsulfates, sulfonates, phosphates and quaternary ammoniums.
  • Third party solvents can for example be glycols.
  • the temperature of the satin-finishing bath is understood between 15 ° C and 80 ° C and, preferably, between 20 and 60 ° C.
  • the time during which the action of the bath is maintained is between 1 minute and 1 hour .
  • the processing time in industry will preferably not exceed about thirty minutes.
  • a complementary light alkaline pickling carried out according to a process in itself known and such that it leads to pickling of at most 40 g / m 2 aluminum;
  • Such an additive which is based on gluconate can be that marketed by the Applicant Company under the PROGAL G 313 TA brand.
  • the alkaline pickling bath thus formed is put for a period of 2 to 20 minutes on the parts coming out of the acid pickling bath.
  • Aluminum profiles are treated as follows: Step 1 Aqueous sodium degreasing in an aqueous solution at 100 g / l of IPRO 77 AP marketed by the Applicant Company, 2nd step Cold rinse with running water, Stage 3 Pickling (satin) acid (see the 8 comparative experiments whose characteristics result from Table I), Step 4 Cold rinse with running water, Step 5 Alkaline pickling (satin finishing) with a bath having the characteristics indicated below, Step 6 Cold rinse with running water, Step 7 Nitric bleaching in a 180 g / l bath of concentrated nitric acid in water, Step 8 Cold rinse with running water, Step 9 Anodic sulfuric oxidation in a bath with 180 g / l of concentrated sulfuric acid (temperature 18 ° C), Step 10 Cold rinse with running water, Step 11 Rinsing in demineralized water, Step 12 Clogging with hot demineralized water (98 ° C).
  • the temperature of the acid pickling bath is 30 ° C.
  • the treatment time is chosen to have a pickling of approximately 25 g / m 2 .
  • Step 5 uses a permanent satin-finishing bath, the characteristics of which are: free soda about 100 g / l aluminum about 140 g / l temperature 60 ° C.
  • the treatment time in this bath and when the acid pickling baths are those called b1 to b6, is that necessary to have a pickling rate of approximately 25 g / m 2 .
  • step 3 the baths b1 and b9 to b14 defined in Table III are used.
  • Baths b1 and b9 to b14 are used at 30 ° C and for the time necessary to cause the treated parts to lose weight in the order of 25 g / m 2 . These baths are used respectively to carry out experiments 1 and 9 to 14, the results of which are collated in Table IV. Exp. No.
  • Series 6063 aluminum profiles are treated by proceeding as in Example 1, but by varying in step 3 the concentration of potassium fluorotitanate K 2 TiF 6 as well as the temperature and by examining the influence of these variations on the pickling speed of aluminum parts.
  • the time required to obtain a pickling rate of approximately 24 g / m 2 was determined for each of the K 2 TiF 6 concentrations and for each of the temperatures chosen, the 98% sulfuric acid concentration being 3 ml / l .
  • the processing time is then understood between six minutes and about thirty minutes, time easily manageable on a production line.
  • the acid pickling bath (step 3) used is constituted by the bath bl described in Example 1. Sa working temperature is 30 ° C and soaking time is 15 minutes.
  • the dullness measured according to the same method at the end of step 12, is 5, that is to say clearly improved compared to the dullness measured in the same conditions according to experiment 8 of example 1 and which industrially located at 12-15.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • ing And Chemical Polishing (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Detergent Compositions (AREA)
  • Materials For Photolithography (AREA)
  • Printing Plates And Materials Therefor (AREA)

Claims (4)

  1. Verwendung eines Säurebads, umfassend mindestens eine der Verbindungen der Gruppe umfassend die Fluormetallsäuren H2TiF6, H2ZrF6 und H2SiF6 sowie deren Alkali- oder Ammoniumsalze in einer Konzentration von mindestens 1 g/l und mindestens eine Säure der Gruppe umfassend Salpetersäure, Schwefelsäure und Phosphorsäure in einer Konzentration zwischen 0,5 und 100 ml pro Liter Bad, ausgedrückt als handelsübliche konzentrierte Säure, und vorzugsweise nicht-ionische, anionische, kationische oberflächenaktive Substanzen und zusätzliche Lösungsmittel, für den Satinierschritt in einem Behandlungsverfahren zur anodischen Oxidation von für Bauzwecke verwendeten Werkstücken und Profilen aus Aluminium oder einer dessen Legierungen, insbesondere bei der Herstellung von Zargen.
  2. Satinierbad zur anodischen Oxidationsbehandlung von für Bauzwecke verwendeten Werkstücken und Profilen aus Aluminium oder einer dessen Legierungen, insbesondere bei der Herstellung von Zargen, dadurch gekennzeichnet, daß es mindestens eine der Verbindungen der Gruppe umfassend die Fluormetallsäuren H2TiF6, H2ZrF6 und H2SiF6 sowie deren Alkali- oder Ammoniumsalze in einer Konzentration von mindestens 1 g/l und mindestens eine Säure der aus Schwefelsäure und Phosphorsäure gebildeten Gruppe in einer Konzentration zwischen 0,5 und 100 ml pro Liter Bad, ausgedrückt als handelsübliche konzentrierte Säure, und vorzugsweise nichtionische, anionische, kationische oberflächenaktive Substanzen und zusätzliche Lösungsmittel enthält.
  3. Konzentrat, geeignet durch Verdünnung mit Wasser das Bad nach Anspruch 2 zu ergeben, dadurch gekennzeichnet, daß es mindestens eine der Verbindungen der Gruppe umfassend die Fluormetallsäuren H2TiF6, H2ZrF6 und H2SiF6 sowie deren Alkali- oder Ammoniumsalze in einer Konzentration zwischen 50 und 99,5 % im gewerblichen Produkt und mindestens eine Säure der aus Schwefelsäure und Phosphorsäure gebildeten Gruppe in einer Konzentration von 0,5 bis 50 % im gewerblichen Produkt enthält.
  4. Konzentrat, geeignet durch Verdünnung mit Wasser und Schwefelsäure oder Phosphorsäure das Bad nach Anspruch 2 zu ergeben, dadurch gekennzeichnet, daß es mindestens eine der Verbindungen der Gruppe umfassend die Fluormetallsäuren H2TiF6, H2ZrF6 und H2SiF6 sowie deren Alkali- oder Ammoniumsalze in einer Konzentration zwischen 50 und 99,5 % im gewerblichen Produkt enthält.
EP93401533A 1992-06-17 1993-06-15 Verfahren zur Behandlung eines Substrats auf Aluminiumbasis für die Eloxierung, das in diesem Verfahren verwendete Bad sowie ein Konzentrat zur Herstellung des Bades Expired - Lifetime EP0575244B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR929207352A FR2692599B1 (fr) 1992-06-17 1992-06-17 Procédé de traitement de substrats à base d'aluminium en vue de leur anodisation, bain mis en Óoeuvre dans ce procédé et concentré pour préparer le bain.
FR9207352 1992-06-17

Publications (2)

Publication Number Publication Date
EP0575244A1 EP0575244A1 (de) 1993-12-22
EP0575244B1 true EP0575244B1 (de) 1999-05-06

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EP93401533A Expired - Lifetime EP0575244B1 (de) 1992-06-17 1993-06-15 Verfahren zur Behandlung eines Substrats auf Aluminiumbasis für die Eloxierung, das in diesem Verfahren verwendete Bad sowie ein Konzentrat zur Herstellung des Bades

Country Status (8)

Country Link
US (1) US5460694A (de)
EP (1) EP0575244B1 (de)
JP (1) JPH06184791A (de)
AT (1) ATE179766T1 (de)
CA (2) CA2098689A1 (de)
DE (1) DE69324729T2 (de)
ES (1) ES2130236T3 (de)
FR (1) FR2692599B1 (de)

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US6043206A (en) 1996-10-19 2000-03-28 Samsung Electronics Co., Ltd. Solutions for cleaning integrated circuit substrates
US5932023A (en) * 1997-02-25 1999-08-03 Ward; Glen Douglas Method of washing a vehicle using a two-part washing composition
US7910218B2 (en) 2003-10-22 2011-03-22 Applied Materials, Inc. Cleaning and refurbishing chamber components having metal coatings
US7618769B2 (en) * 2004-06-07 2009-11-17 Applied Materials, Inc. Textured chamber surface
US7670436B2 (en) 2004-11-03 2010-03-02 Applied Materials, Inc. Support ring assembly
US8617672B2 (en) 2005-07-13 2013-12-31 Applied Materials, Inc. Localized surface annealing of components for substrate processing chambers
US7762114B2 (en) 2005-09-09 2010-07-27 Applied Materials, Inc. Flow-formed chamber component having a textured surface
US9127362B2 (en) 2005-10-31 2015-09-08 Applied Materials, Inc. Process kit and target for substrate processing chamber
US8647484B2 (en) 2005-11-25 2014-02-11 Applied Materials, Inc. Target for sputtering chamber
US7981262B2 (en) 2007-01-29 2011-07-19 Applied Materials, Inc. Process kit for substrate processing chamber
US7942969B2 (en) 2007-05-30 2011-05-17 Applied Materials, Inc. Substrate cleaning chamber and components
US8097093B2 (en) 2007-09-28 2012-01-17 Ppg Industries Ohio, Inc Methods for treating a ferrous metal substrate
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KR101475173B1 (ko) * 2011-06-24 2014-12-19 애플 인크. 양극산화처리된 부품의 미용적 결함 저감
TWI444508B (zh) * 2012-05-07 2014-07-11 Catcher Technology Co Ltd 具止滑皮革質感表面之金屬工件製造方法
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Also Published As

Publication number Publication date
FR2692599A1 (fr) 1993-12-24
CA2098690A1 (en) 1993-12-18
DE69324729T2 (de) 1999-12-02
DE69324729D1 (de) 1999-06-10
ATE179766T1 (de) 1999-05-15
ES2130236T3 (es) 1999-07-01
CA2098689A1 (en) 1993-12-18
EP0575244A1 (de) 1993-12-22
US5460694A (en) 1995-10-24
JPH06184791A (ja) 1994-07-05
FR2692599B1 (fr) 1994-09-16

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