EP2682502B1 - Behandlungsverfahren mit Anodisieren von Kupfer-enthaltenden Aluminiumlegierungen - Google Patents

Behandlungsverfahren mit Anodisieren von Kupfer-enthaltenden Aluminiumlegierungen Download PDF

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Publication number
EP2682502B1
EP2682502B1 EP13174807.1A EP13174807A EP2682502B1 EP 2682502 B1 EP2682502 B1 EP 2682502B1 EP 13174807 A EP13174807 A EP 13174807A EP 2682502 B1 EP2682502 B1 EP 2682502B1
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EP
European Patent Office
Prior art keywords
bath
rinsing
copper
anodizing
anode
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EP13174807.1A
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English (en)
French (fr)
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EP2682502A1 (de
Inventor
Emmanuel Rocca
Joffrey Tardelli
Myriam Augros
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.)
Universite de Lorraine
Safran Landing Systems SAS
Original Assignee
Messier Bugatti Dowty SA
Universite de Lorraine
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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
    • C25D11/16—Pretreatment, e.g. desmutting
    • 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

Definitions

  • the present invention relates to a process for treating an aluminum alloy part containing copper in a mass proportion of 0.1% to 10%.
  • Copper-containing aluminum alloys corrode primarily in the form of localized corrosion, in the form of pits or spots of corrosion. This phenomenon comes in line with the copper-rich particles that are present in these alloys.
  • anodizing (or chemical conversion) of these alloys is carried out which increases the thickness of the oxide layer (aluminum oxide in case of anodizing ) on their surface.
  • This pretreatment is usually carried out in an aqueous electrolyte chemically or electrochemically.
  • This electrolyte contains one or more acids such as sulfuric acid (H 2 SO 4 ) and phosphoric acid (H 3 PO 4 ).
  • the addition of one or more oxidants such as nitric acid, hydrogen persulfate, hydrogen perborate, and hydrogen peroxide (hydrogen peroxide H 2 O 2 ) in this electrolyte promotes the dissolution of the metal and emulsification of dirt or grease from the surface, and allows an acceptable rinsing of the aluminum alloy part.
  • the addition of an organic compound leads to the formation on the surface of the aluminum alloy of a viscous layer which contributes to the dissolution of the surface irregularities.
  • the copper-rich particles dissolve only partially, which causes the presence of numerous defects (holes, cracks, cavities) in the layers of copper. oxides subsequently formed by anodizing (or chemical conversion) on the surface of the alloy, these defects weakening these layers and resulting in premature corrosion of the alloy.
  • the present invention aims to remedy these disadvantages.
  • the aim of the invention is to propose a process for treating a copper-containing aluminum alloy with pretreatment and anodization which allows a complete dissolution of the copper particles, and which makes it possible to avoid a subsequent redeposition of copper on the surface of the copper. aluminum alloy, this method being further able to minimize the dimensional variations of the workpiece.
  • the surface of the workpiece is cleaned, the copper-rich particles are removed from the surface and the subsequent redeposition of the copper particles is prevented, thereby obtaining oxide deposition by anodizing. better quality.
  • the part is thus more resistant to corrosion.
  • the first potential difference ⁇ V1 is between 3 V and 12 V.
  • the pretreatment of the part is faster while resulting in a better quality of the pretreatment and subsequent anodization of the piece.
  • An aluminum alloy piece 50 containing copper is provided (step (a) of the method according to the invention).
  • the mass proportion of copper in this alloy is between 0.01% and 10%.
  • a first electrolytic bath 10 containing sulfuric acid and a first oxidizing compound are provided.
  • This first bath 10 is contained in a first tank 15.
  • the first bath 10 is dipped into a first cathode 11 and the piece 50, this piece 50 acting as a first anode.
  • the first cathode 11 is for example a titanium alloy or a lead alloy or a stainless steel.
  • the piece 50 is electrochemically treated in the first bath 10 by applying a first potential difference ⁇ V1 between the first cathode 11 and the part 50.
  • This treatment constitutes the electrochemical pretreatment (step (b)) of the process according to the invention. .
  • the concentration of the first oxidizing compound is chosen so that during this electrochemical pretreatment the corrosion potential of the aluminum alloy of the part 50 is greater than +100 mV with respect to the Normal Hydrogen Electrode.
  • the tests carried out by the inventors show that in this case there is a complete dissolution of the copper-rich particles while the amount of dissolved alloy is sufficiently low for the dimensional specifications of the part 50 remain satisfied. So, the amount of dissolved alloy is less than 0.1 mg / dm 2 / min (milligrams / decimetres 2 / minute).
  • the amount of dissolved alloy is between 0.4 mg / dm 2 / min and 4 mg / dm 2 / min.
  • concentrations of sulfuric acid and the first oxidizing compound necessary for the corrosion potential of the aluminum alloy of the part 50 to be greater than +100 mV depend on the aluminum alloy and the nature of the first oxidizing compound. .
  • the concentration of the first oxidizing compound must be greater than 0.1 mol / l.
  • the first oxidizing compound is NaBO 3
  • its concentration should be between 0.1 mol / L and 0.5 mol / L.
  • the first oxidizing compound is K 2 S 2 O 8
  • its concentration should be between 0.1 mol / L and 0.5 mol / L.
  • the first oxidizing compound is oxygenated water H 2 O 2 , its concentration must be between 0.1 mol / l and 1 mol / l.
  • the first oxidizing compound is hydrogen peroxide.
  • the tests carried out by the inventors show that the oxygenated water makes it possible to reach a corrosion potential of the aluminum alloy of the part 50 with respect to the Normal Hydrogen Electrode which is greater than the corrosion potential. obtained with another oxidizing compound.
  • the first potential difference ⁇ V1 is between 3 V and 12 V.
  • this first potential difference ⁇ V1 is greater than 12 V, an anodized layer is formed on the surface of the piece 50. quickly to allow the copper particles to dissolve and move away from the surface of the workpiece 50.
  • the first potential difference ⁇ V1 is between 5 V and 10 V.
  • the pretreatment time is between 2 and 30 minutes.
  • the piece 50 is anodized in a second electrolyte bath 20 containing sulfuric acid and a second oxidizing compound.
  • This second bath 20 is contained in a second tank 25.
  • This second bath 20 is dipped in a second cathode 21 and the piece 50, this piece 50 acting as a second anode.
  • the second cathode 21 is for example a lead alloy or a titanium alloy or a stainless steel.
  • the piece 50 is electrochemically treated in the second bath 20 by applying a second potential difference ⁇ V2 between the first cathode 11 and the piece 50. This treatment constitutes the anodization (step (c)) of the process according to the invention. .
  • the second oxidizing compound is for example selected from a group consisting of NaBO 3 , K 2 S 2 O 8 , and hydrogen peroxide H 2 O 2 .
  • the tests carried out by the inventors show that the anodizing layer that forms on the surface of the part 50 during anodization provides an even better protection (the impedance of the anodizing layer is higher) when the electrochemical pretreatment (step (b)) is carried out with a first potential difference ⁇ V1 of 10 V for 5 minutes or 5 V for 10 minutes.
  • the anodizing layer which forms on the surface of the part 50 during anodization offers better protection (its impedance is higher) when the concentration of hydrogen peroxide is between 5 g / L and 25 g / L for a 7050 aluminum alloy.
  • the anodization is carried out with a sulfuric acid concentration of between 100 g / l and 300 g / l depending on the thickness of the desired anodization layer.
  • this concentration is between 160 g / l and 240 g / l, which leads to a better efficiency of the process.
  • this concentration is approximately equal to 200 g / l.
  • the second oxidizing compound is hydrogen peroxide.
  • the anodization is carried out with a hydrogen peroxide concentration of between 15 g / l and 20 g / l.
  • the anodization is carried out with a bearing in the voltage, that is to say that a first voltage is applied between 12 and 17 V, then possibly a second voltage between 17 and 22 V so as not to damage electrical installations.
  • the part 50 is rinsed between step (b) (pretreatment) and step (c) (anodizing).
  • the anodization therefore takes place in a first bath 10 which is distinct from the second bath 20, the first tank 15 being distinct from the second tank 25.
  • the piece 50 is taken out of the first bath 10 and rinsed. This rinsing has the advantage of ridding the piece 50 of residues possibly present on its surface after the pretreatment.
  • the second bath 20 is distinct from the first bath 10, pollution of the second bath by elements dissolved during the pretreatment and which are present in the first bath 10 is avoided.
  • the piece 50 is immersed in the second bath 20 so that it undergoes the anodizing treatment.
  • the rinsing of the piece 50 is thus more efficient.
  • the anodizing step (c) is carried out in the same bath as the first bath 10 of the pretreatment step (b), without leaving the piece 50 of the first bath 10 between step (b) and step (c).
  • the second tank 25 is therefore the first tank 15, and the second tank 20 consists of the first tank 10 after the pretreatment.

Claims (6)

  1. Verfahren zur Behandlung eines Teils (50) aus Aluminiumlegierung, die Kupfer in einem Massenanteil von 0,1 % bis 10 % enthält, dadurch gekennzeichnet, dass es die folgenden Schritte umfasst:
    (a) das Teil (50) wird bereitgestellt,
    (b) es wird eine elektrochemische Vorbehandlung des Teils (50) in einem ersten Bad (10) aus Elektrolyt, der Schwefelsäure und eine erste oxidierende Verbindung enthält, durchgeführt, wobei eine erste Potentialdifferenz ΔV1 zwischen einer ersten Kathode (11) und einer ersten Anode, die in das erste Bad (10) eingetaucht sind, aufgebaut wird, wobei das Teil (50) die erste Anode ist, wobei die Konzentration der ersten oxidierenden Verbindung derart ist, dass das Korrosionspotential der Aluminiumlegierung größer als +100 mV gegenüber der Normalwasserstoffelektrode ist,
    (c) nach Schritt (b) wird ein Anodisieren des Teils (50) in einem zweiten Bad (20) aus Elektrolyt, der Schwefelsäure und eine zweite oxidierende Verbindung enthält, durchgeführt, wobei eine zweite Potentialdifferenz ΔV2 zwischen einer zweiten Kathode (21) und einer zweiten Anode, die in das zweite Bad eingetaucht sind, aufgebaut wird, wobei das Teil (50) die zweite Anode ist.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass bei Schritt (b) die erste Potentialdifferenz ΔV1 zwischen 3 V und 12 V beträgt.
  3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die erste oxidierende Verbindung Wasserstoffperoxid H2O2 ist.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass der Schritt (c) des Anodisierens in dem gleichen Bad wie das erste Bad (10) des Vorbehandlungsschrittes (b) erfolgt, ohne das Teil (50) zwischen Schritt (b) und Schritt (c) aus dem ersten Bad (10) herauszunehmen.
  5. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass zwischen Schritt (b) und Schritt (c) ein Spülen des Teils (50) durchgeführt wird.
  6. Verfahren nach Anspruch 5, dadurch gekennzeichnet, dass das Spülen von den folgenden Schritten gebildet ist:
    (b1) das Teil (50) wird in einem statischen Spülbad (91) gespült,
    (b2) anschließend wird das Teil (50) in einem fließenden Spülbad (92) mit durch Ionenaustauscher aufbereitetem Wasser gespült.
EP13174807.1A 2012-07-04 2013-07-02 Behandlungsverfahren mit Anodisieren von Kupfer-enthaltenden Aluminiumlegierungen Active EP2682502B1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR1256393A FR2992979B1 (fr) 2012-07-04 2012-07-04 Procede de traitement avec anodisation d'alliages d'aluminium contenant du cuivre

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EP2682502A1 EP2682502A1 (de) 2014-01-08
EP2682502B1 true EP2682502B1 (de) 2015-09-16

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US (1) US20140008236A1 (de)
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FR (1) FR2992979B1 (de)

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Publication number Priority date Publication date Assignee Title
CN111663163A (zh) * 2019-03-08 2020-09-15 核工业理化工程研究院 一种2a50铝合金的防腐处理方法及其应用

Citations (1)

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GB1215314A (en) * 1967-11-22 1970-12-09 Acorn Anodising Company Ltd Improvements in or relating to the anodising of aluminium and its alloys
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US20140008236A1 (en) 2014-01-09
EP2682502A1 (de) 2014-01-08
FR2992979A1 (fr) 2014-01-10
FR2992979B1 (fr) 2014-08-08

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