EP1357206A2 - Procédé d'anodisation d'une pièce en alliage d'aluminium - Google Patents
Procédé d'anodisation d'une pièce en alliage d'aluminium Download PDFInfo
- Publication number
- EP1357206A2 EP1357206A2 EP03290776A EP03290776A EP1357206A2 EP 1357206 A2 EP1357206 A2 EP 1357206A2 EP 03290776 A EP03290776 A EP 03290776A EP 03290776 A EP03290776 A EP 03290776A EP 1357206 A2 EP1357206 A2 EP 1357206A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- bath
- acid
- essentially
- constant
- concentration
- 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.)
- Withdrawn
Links
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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
-
- 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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
-
- 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
- C25D11/12—Anodising more than once, e.g. in different baths
Definitions
- the present invention relates to the treatment of aluminum alloy parts, in particular parts intended to constitute aeronautical components, and more specifically a process for anodizing a workpiece aluminum alloy.
- Such an anodizing process is relatively effective in applying an aluminum oxide coating on an aluminum alloy with a solution of sulfuric acid and boric acid.
- the anodized coating thus obtained is at least comparable and, as regards corrosion resistance, equivalent to the anodized and clogged coatings produced in baths containing an aqueous solution of sulfuric acid and chromic acid.
- the superiority of the process of document US-A-4,894,127 compared to other prior processes of sulfo-boric anodization lies in obtaining coatings of thin thickness, in particular from 1 ⁇ m to 3 ⁇ m, which is very particularly interesting in the field of aeronautics.
- compositions indicated for the implementation of such a process are very wide, which can lead to obtaining characteristics of great disparity for the layers obtained.
- a voltage which increases linearly from 5 V to 20 V is applied to the part which is immersed in the electrolytic bath, with a current density on said part which remains close to 100 A / m 2 .
- the presence sulfuric acid may, however, be undesirable in certain situations, if we are trying to get thin coating thicknesses, especially smaller at 3 ⁇ m.
- Anodization processes are commonly used in the aeronautical field with electrolytic baths comprising sulfuric acid with a concentration of between 180 g / l and 250 g / l.
- the existing techniques have systematically confined themselves to this high range of sulfuric acid concentrations for anodizing baths, due to a choice based on the curve giving the variations of the electrical conductivity as a function of the sulfuric acid concentration.
- this variation curve has substantially the shape of a parabola facing downward, and has a maximum in the zone corresponding to the concentrations between 180 g / l and 220 g / l for sulfuric acid.
- the specialists are therefore invariably based on the search for maximum electrical conductivity for the electrolytic bath. Indeed, it is known that this high electrical conductivity is favorable to rapid growth of the oxide thickness. This explains the systematic choice of high concentrations (at least equal to 200 g / l) for the sulfuric acid present in the electrolytic bath.
- anodizing in the middle acid is essentially porous, and that if we want to avoid high porosity on the treated parts, it is then necessary to refer to techniques anodization in a more neutral environment, making it possible to obtain barrier anodization with a non-porous layer.
- the object of the present invention is to provide a more efficient anodizing process, which is connected essentially to anodic sulfuric oxidation techniques, but allowing better control of coating thickness or weight, while avoiding to obtain a high porosity on the treated parts.
- the aqueous anodizing bath includes also an acid-alcohol having one to three functions acid, in order to limit the dissolution of the layer of coating obtained, this to have a perfect homogeneity porosity throughout the thickness of the layer, without losing electrical conductivity of the bath which promotes good growth of said layer.
- the first step in the anodizing process according to the invention consists in providing an anodization bath aqueous containing essentially sulfuric acid, with a concentration between 55 g / l and 85 g / l, at excluding any presence of phosphoric acid or boric acid.
- concentrations indicated in percentage by mass the species the aforementioned limits indicated in g / l correspond at concentration values ranging from 5.36% at 8.2% by weight.
- the concentration of sulfuric acid in the bath will be preferably essentially between 57 g / l and 67 g / l, a highly preferred value lying in the vicinity 62 g / l (slightly above 6% in weight).
- the second preparatory stage of the process anodizing according to the invention consists in maintaining the Aforementioned aqueous anodization bath at a constant temperature, which is essentially between 15 ° C and 27 ° C.
- the bath will be kept at a temperature constant close to 22 ° C.
- the voltage applied to the part immersed in the bath can be set to a constant value for the entire duration of the anodizing treatment, said value constant then being between 5 V and 30 V.
- a constant voltage value between 7 V and 20 V.
- first constant voltage value between 5 V and 11 V, this low value allowing to control the moderate growth of the layer of oxide
- second constant value of voltage included between 15 V and 30 V this to have the properties barrier layer.
- the use of two successive voltage steps, the duration of which will be essentially depending on the desired coating thickness, allows the barrier layer to be built more quickly retaining control over the growth of the coating.
- the Applicant has carried out numerous tests, and has particular observed in the light of the kinetic curves of growth plotted that we got excellent results with a first step at 10 V, for a period in the order of twenty-five minutes, followed by a second 20 V step for fifteen minutes.
- a relatively low current density is used on the part which is immersed in the electrolytic bath.
- the term "low” in this case means that this current density is significantly less than 100 A / m 2 .
- the part to be treated in the electrolytic bath As part of the anodization process such as previously described, finally maintaining the part to be treated in the electrolytic bath until the desired coating thickness, which is substantially between 1 ⁇ m and 3 ⁇ m.
- the acid-alcohol used in the bath will be tartaric acid (acid-alcohol having two acid functions, of formula C 4 H 6 O 6 ) or citric acid (acid-alcohol having three acid functions, of formula C 6 H 8 O 7 ).
- the concentration of tartaric acid or citric acid will then preferably be essentially between 12 g / l and 17 g / l, the optimal concentration noted during the tests carried out being in the vicinity of 17 g / l.
- tartaric acid and citric acid are also particularly interesting insofar as one wishes on the one hand to have a pH stabilized at a low value, and on the other hand have a strong oxidant, whose electrochemical activity is high without being aggressive, and therefore not generating of stings.
- anodic sulfo-tartaric or sulfo-citric oxidation appears much more attractive than anodic oxidation sulfo-boric of prior techniques, in particular that described in document US-A-4,894 127. Indeed, we obtain here an excellent stability of the dissolution of the alumina layer.
- Addition of tartaric or citric acid in the bath in the context of the invention allows to have dissolution of the weaker alumina layer than with sulfuric acid alone, and moreover the density of current in the bath does not drop as it would the case with other acids, like boric acid, in because of the action on surface tensions.
- the clogging of the coating must ensure a double function which is to develop both the promotion of adhesion and resistance to corrosion.
- This clogging is conventionally carried out by soaking in hot water at a temperature at least equal to 97 ° C., or in a dilute solution of potassium dichromate.
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
Description
- on fournit un bain d'anodisation aqueux comportant essentiellement de l'acide sulfurique, avec une concentration comprise entre 55 g/l et 85 g/l, à l'exclusion de toute présence d'acide phosphorique ou d'acide borique ;
- on maintient le bain précité à une température constante essentiellement comprise entre 15°C et 27°C ;
- on plonge ladite pièce dans ledit bain ;
- on applique à ladite pièce plongée dans ledit bain une tension essentiellement comprise entre 5 V et 30 V, avec une faible densité de courant sur ladite pièce ; et
- on maintient ladite pièce dans ledit bain jusqu'à obtention de l'épaisseur de revêtement désirée qui est sensiblement comprise entre 1 µm et 3 µm.
Claims (13)
- Procédé d'anodisation d'une pièce en alliage d'aluminium, comprenant les étapes successives suivantes :on fournit un bain d'anodisation aqueux comportant essentiellement de l'acide sulfurique, avec une concentration comprise entre 55 g/l et 85 g/l, à l'exclusion de toute présence d'acide phosphorique ou d'acide borique ;on maintient le bain précité à une température constante essentiellement comprise entre 15°C et 27°C ;on plonge ladite pièce dans ledit bain ;on applique à ladite pièce plongée dans ledit bain une tension essentiellement comprise entre 5 V et 30 V, avec une faible densité de courant sur ladite pièce ; eton maintient ladite pièce dans ledit bain jusqu'à obtention de l'épaisseur de revêtement désirée qui est sensiblement comprise entre 1 µm et 3 µm.
- Procédé selon la revendication 1, dans lequel la concentration du bain en acide sulfurique est essentiellement comprise entre 57 g/l et 67 g/l, en étant de préférence voisine de 62 g/l.
- Procédé selon la revendication 1 ou la revendication 2, dans lequel le bain est maintenu à une température constante voisine de 22°C.
- Procédé selon l'une des revendications 1 à 3, dans lequel la tension appliquée à la pièce plongée dans le bain est calée sur une valeur constante pendant toute la durée du traitement d'anodisation, ladite valeur constante étant comprise entre 5 V et 30 V.
- Procédé selon la revendication 4, dans lequel la valeur constante de tension est comprise entre 7 V et 20 V.
- Procédé selon l'une quelconque des revendications 1 à 3, dans lequel la tension appliquée à la pièce plongée dans le bain est d'abord calée sur une première valeur constante, puis, après une durée prédéterminée, sur une seconde valeur constante plus élevée que la première, lesdites première et seconde valeurs constantes étant toutes deux comprises entre 5 V et 30 V.
- Procédé selon la revendication 6, dans lequel la première valeur constante de tension est comprise entre 5 V et 11 V, et la seconde valeur constante de tension est comprise entre 15 V et 30 V.
- Procédé selon l'une quelconque des revendications 1 à 7, dans lequel la densité de courant sur la pièce plongée dans le bain reste notablement inférieure à 100 A/m2.
- Procédé selon la revendication 8, dans lequel la densité de courant est essentiellement inférieure à 80 A/m2, en étant de préférence comprise entre 30 A/m2 et 70 A/m2.
- Procédé selon l'une quelconque des revendications 1 à 9, dans lequel le bain d'anodisation aqueux comporte également un acide-alcool ayant une à trois fonctions acide, avec une concentration comprise entre 12 g/l et 22 g/l.
- Procédé selon la revendication 10, dans lequel l'acide-alcool utilisé dans le bain est l'acide tartrique ou l'acide citrique, et la concentration de cet acide-alcool est essentiellement comprise entre 12 g/l et 17 g/l.
- Procédé selon l'une quelconque des revendications 1 à 11, dans lequel la pièce à traiter subit un traitement préliminaire de dégraissage/décapage avant d'être plongée dans le bain.
- Procédé selon l'une quelconque des revendications 1 à 12, dans lequel la pièce traitée subit un traitement ultérieur de colmatage du revêtement.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0204984A FR2838754B1 (fr) | 2002-04-22 | 2002-04-22 | Procede d'anodisation d'une piece en alliage d'aluminium |
FR0204984 | 2002-04-22 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1357206A2 true EP1357206A2 (fr) | 2003-10-29 |
EP1357206A3 EP1357206A3 (fr) | 2004-05-12 |
Family
ID=28686230
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP03290776A Withdrawn EP1357206A3 (fr) | 2002-04-22 | 2003-03-27 | Procédé d'anodisation d'une pièce en alliage d'aluminium |
Country Status (4)
Country | Link |
---|---|
US (1) | US20030196907A1 (fr) |
EP (1) | EP1357206A3 (fr) |
CA (1) | CA2425296A1 (fr) |
FR (1) | FR2838754B1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109183114A (zh) * | 2018-09-30 | 2019-01-11 | 托伦斯半导体设备启东有限公司 | 一种硬质阳极氧化工艺 |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7527872B2 (en) * | 2005-10-25 | 2009-05-05 | Goodrich Corporation | Treated aluminum article and method for making same |
FR2986807B1 (fr) * | 2012-02-10 | 2015-05-15 | Mecaprotec Ind | Procede d'anodisation de pieces en alliage d'aluminium |
CN104087997A (zh) * | 2014-06-16 | 2014-10-08 | 北京工业大学 | 异酸异压二次氧化制备规则小孔径阳极氧化铝模板的方法 |
DE212014000273U1 (de) | 2014-08-29 | 2017-04-26 | Apple Inc. | Prozess zur Minderung der Spallation anodischer Oxidschichten von hochfesten Substratlegierungen |
WO2016111693A1 (fr) | 2015-01-09 | 2016-07-14 | Apple Inc. | Procédés de réduction de l'enrichissement interfacial d'éléments d'alliage sous des films d'oxyde anodique et aspect anodisé amélioré d'alliages pouvant être traités à chaud |
US9869623B2 (en) | 2015-04-03 | 2018-01-16 | Apple Inc. | Process for evaluation of delamination-resistance of hard coatings on metal substrates |
US20160289858A1 (en) * | 2015-04-03 | 2016-10-06 | Apple Inc. | Process to mitigate grain texture differential growth rates in mirror-finish anodized aluminum |
US10760176B2 (en) | 2015-07-09 | 2020-09-01 | Apple Inc. | Process for reducing nickel leach rates for nickel acetate sealed anodic oxide coatings |
US9970080B2 (en) | 2015-09-24 | 2018-05-15 | Apple Inc. | Micro-alloying to mitigate the slight discoloration resulting from entrained metal in anodized aluminum surface finishes |
US10711363B2 (en) | 2015-09-24 | 2020-07-14 | Apple Inc. | Anodic oxide based composite coatings of augmented thermal expansivity to eliminate thermally induced crazing |
US10174436B2 (en) | 2016-04-06 | 2019-01-08 | Apple Inc. | Process for enhanced corrosion protection of anodized aluminum |
CN109415836B (zh) * | 2016-04-18 | 2021-05-07 | 福克航空结构公司 | 铝或其合金制品的阳极氧化方法 |
US11352708B2 (en) | 2016-08-10 | 2022-06-07 | Apple Inc. | Colored multilayer oxide coatings |
US11242614B2 (en) | 2017-02-17 | 2022-02-08 | Apple Inc. | Oxide coatings for providing corrosion resistance on parts with edges and convex features |
US11549191B2 (en) | 2018-09-10 | 2023-01-10 | Apple Inc. | Corrosion resistance for anodized parts having convex surface features |
WO2020215041A1 (fr) * | 2019-04-18 | 2020-10-22 | Lopez Steven | Colorant d'anodisation fluorescent et procédés associés |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2855350A (en) * | 1954-09-20 | 1958-10-07 | Sanford Process Co Inc | Process for electrolytically producing oxide coating on aluminum and aluminum alloys |
US3563867A (en) * | 1965-12-09 | 1971-02-16 | Acorn Anodising Co Ltd | Anodising of aluminium and its alloys |
US4554216A (en) * | 1982-02-23 | 1985-11-19 | Hoechst Aktiengesellschaft | Process for manufacturing support materials for offset printing plates |
US4894127A (en) * | 1989-05-24 | 1990-01-16 | The Boeing Company | Method for anodizing aluminum |
JP2000026997A (ja) * | 1998-07-13 | 2000-01-25 | Yamaha Motor Co Ltd | アルミニウム合金の陽極酸化方法 |
EP1233084A2 (fr) * | 2001-02-20 | 2002-08-21 | Alenia Aeronautica S.P.A. | Procédé d'anodisation, ayant un effet faible pour l'environnement, pour une pièce en aluminium ou en alliage d'aluminium |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0050216B1 (fr) * | 1980-09-26 | 1985-01-09 | American Hoechst Corporation | Procédé pour l'oxydation anodique d'aluminium et son utilisation comme support pour planches d'imprimerie |
JPS6014838B2 (ja) * | 1980-09-30 | 1985-04-16 | ワイケイケイ株式会社 | アルミニウム表面に着色筋目模様を形成する方法 |
WO1986004618A1 (fr) * | 1985-02-06 | 1986-08-14 | Fujitsu Limited | Procede de formation d'une pellicule composite d'aluminium |
US4861440A (en) * | 1986-07-24 | 1989-08-29 | Covino Charles P | Electrolytic formation of an aluminum oxide surface |
US6149795A (en) * | 1998-10-27 | 2000-11-21 | The Boeing Company | Fungus resistant boric acid-sulfuric acid anodizing |
US7018521B2 (en) * | 2001-09-27 | 2006-03-28 | General Motors Corporation | Method of producing bright anodized finishes for high magnesium, aluminum alloys |
-
2002
- 2002-04-22 FR FR0204984A patent/FR2838754B1/fr not_active Expired - Lifetime
-
2003
- 2003-03-27 EP EP03290776A patent/EP1357206A3/fr not_active Withdrawn
- 2003-04-17 CA CA002425296A patent/CA2425296A1/fr not_active Abandoned
- 2003-04-21 US US10/419,152 patent/US20030196907A1/en not_active Abandoned
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2855350A (en) * | 1954-09-20 | 1958-10-07 | Sanford Process Co Inc | Process for electrolytically producing oxide coating on aluminum and aluminum alloys |
US3563867A (en) * | 1965-12-09 | 1971-02-16 | Acorn Anodising Co Ltd | Anodising of aluminium and its alloys |
US4554216A (en) * | 1982-02-23 | 1985-11-19 | Hoechst Aktiengesellschaft | Process for manufacturing support materials for offset printing plates |
US4894127A (en) * | 1989-05-24 | 1990-01-16 | The Boeing Company | Method for anodizing aluminum |
JP2000026997A (ja) * | 1998-07-13 | 2000-01-25 | Yamaha Motor Co Ltd | アルミニウム合金の陽極酸化方法 |
EP1233084A2 (fr) * | 2001-02-20 | 2002-08-21 | Alenia Aeronautica S.P.A. | Procédé d'anodisation, ayant un effet faible pour l'environnement, pour une pièce en aluminium ou en alliage d'aluminium |
Non-Patent Citations (2)
Title |
---|
"TECHNISCHE VERFAHREN DER ANODISCHEN OXIDATION" , PRAXIS DER ANODISCHEN OXIDATION DES ALUMINIUMS, XX, XX, PAGE(S) 137-173 XP008003644 * page 151-152 * * page 157 * * |
PATENT ABSTRACTS OF JAPAN vol. 2000, no. 04, 31 août 2000 (2000-08-31) -& JP 2000 026997 A (YAMAHA MOTOR CO LTD), 25 janvier 2000 (2000-01-25) * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109183114A (zh) * | 2018-09-30 | 2019-01-11 | 托伦斯半导体设备启东有限公司 | 一种硬质阳极氧化工艺 |
Also Published As
Publication number | Publication date |
---|---|
US20030196907A1 (en) | 2003-10-23 |
FR2838754A1 (fr) | 2003-10-24 |
CA2425296A1 (fr) | 2003-10-22 |
EP1357206A3 (fr) | 2004-05-12 |
FR2838754B1 (fr) | 2005-03-18 |
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