EP2857560B2 - Procédé plasma-chimique destiné à fabriquer des couches en céramique oxydée noires et objet revêtu correspondant - Google Patents

Procédé plasma-chimique destiné à fabriquer des couches en céramique oxydée noires et objet revêtu correspondant Download PDF

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Publication number
EP2857560B2
EP2857560B2 EP14184217.9A EP14184217A EP2857560B2 EP 2857560 B2 EP2857560 B2 EP 2857560B2 EP 14184217 A EP14184217 A EP 14184217A EP 2857560 B2 EP2857560 B2 EP 2857560B2
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mol
electrolyte
oxide ceramic
iron
ammonium
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German (de)
English (en)
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EP2857560B1 (fr
EP2857560A1 (fr
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Dr. Kyriaki Dascoulidou-Gritner
Tamara SCHWARZ
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Aalberts Surface Technologies GmbH Landsberg am Lech
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Aalberts Surface Treatment GmbH
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/026Anodisation with spark discharge
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/14Producing integrally coloured layers
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/30Anodisation of magnesium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/16Pretreatment, e.g. desmutting

Definitions

  • Plasma chemical method for producing black oxide ceramic layers The invention relates to a plasma chemical method for producing black oxide ceramic layers on light metals, in particular aluminum, titanium, or their alloys after the process of anodic oxidation with spark discharge in aqueous electrolytes.
  • ANOF anodic oxidation under spark discharge
  • PCO plasma chemical oxidation
  • PEO plasma electrolytic oxidation
  • ASD anodic sparc deposition
  • MAO micro arc oxidation
  • this anodic oxidation in aqueous electrolytes is a gas-solid reaction under plasma conditions, in which the high energy input at the base of the discharge column generates liquid metal on the anode, which forms a briefly melted oxide with the activated oxygen.
  • the layer formation takes place via partial anodes.
  • There is a formation area in front of the spark discharge P. short; Dechema-Monographien Volume 121 - VCH Verlagsgesellschaft 1990, page 167-180 with further references).
  • the electrolytes were combined in such a way that their positive properties are combined and high-quality anodic oxide ceramic layers are created on aluminum.
  • the metal ion in the oxide ceramic layer comes from the metal, the oxygen from the anodic reaction in the aqueous electrolyte used.
  • the oxide ceramic is liquid at the determined plasma temperatures of around 7,000 Kelvin. There is enough time on the side of the metal so that the melt of the oxide ceramic can contract well and thus form a sintered, low-pore oxide ceramic layer. To the side of the electrolyte, the melt of the oxide ceramic is quickly cooled by the electrolyte and the gases that migrate, in particular oxygen and water vapor, leave an oxide ceramic layer with a wide-meshed capillary system.
  • Pore diameters from 0.1 ⁇ m to 30 ⁇ m were determined from scanning electron microscopic examinations ( CERAMIC COATINGS BY ANODIC SPARK DEPOSITION GP Wirtz et al, MATERIALS & MANUFACTURING PROCESSES 6 (1), 87-115 (1991 ), especially Figure 12).
  • Components provided with such resistant coatings are u. A. used in the automotive, aerospace and optical industries as well as medical technology.
  • the DD 299 595 and DD 299 596 describe the production of black conversion layers on light metals using electrolytes that contain chromate.
  • DD 221 762 A1 and DD 257 275 A1 For example, it is known to add metal salts, such as iron hexacyanoferrate, nickel, cobalt, or chromium salts, to the electrolyte to produce dark-colored oxide layers.
  • metal salts such as iron hexacyanoferrate, nickel, cobalt, or chromium salts
  • a method is also known with which black ceramic films can be produced by microarc oxidation (MAO) with an electrolyte which contains sodium fluoride (DATABASE WPI, Week 201163, Thomson Scientific, London, GB; AN 2011-L6540 & CN 102 154 673 A ).
  • MAO microarc oxidation
  • electrolytes containing molybdenum, cobalt, chromium or nickel or cyanide ions or other substances of concern should no longer be used in the future, as these can lead to problems related to occupational safety or the environment.
  • the object of the invention is therefore a method for producing black oxide ceramic layers on aluminum titanium or their alloys and to provide special materials containing these materials after the process of anodic oxidation under spark discharge (ANOF), in which electrolytes are used which are low in pollutants and easy to handle.
  • ANOF anodic oxidation under spark discharge
  • the electrolytes should not contain any molybdenum, cobalt, chromium and nickel ions as well as cyanide ions and borates.
  • an iron and vanadium-containing electrolyte, black oxide ceramic layers on aluminum, titanium or their alloys and special materials containing these materials can be produced by the process of anodic oxidation.
  • the electrolyte is therefore free of molybdenum, cobalt, chromium and nickel.
  • black and stable oxide ceramic layers can be produced, the layer thickness of which can be varied over a wide range.
  • deep black is understood to mean all layers which, according to the CIE L * a * b * system, have values of L * less than or equal to 30.
  • the aluminum and its alloys include pure aluminum and alloys with the main component aluminum, such as the wrought aluminum alloys of the EN-AW 1000, 2000, 3000, 4000, 5000, 6000, 7000 series, or the cast aluminum alloys of the EN-AC 21000, 21100 series , 42000, 43000, 43200, 43400, 44300, 46000, 46200, 47000, 47100, 48000, 51000, 51100 in question.
  • Pure titanium or titanium alloys such as TiAl6V4; Use TiAl5Fe2.5 and others.
  • Special materials with aluminum, titanium or their alloys are, for example, intermetallic compounds or phases such as titanium aluminides.
  • the electrolyte has a pH of 5.4 to 10.0 during the anodic oxidation.
  • the electrolyte can also contain inorganic or organic anions. It preferably contains 0.2 to 0.9 mol / L of a phosphate of an alkali metal, preferably a dihydrogen phosphate or pyrophosphate, in particular potassium dihydrogen phosphate or potassium pyrophosphate, and / or 0.15 to 0.5 mol / L of citric acid or its salts. Citrates are particularly preferred because they support a controlled sparking process. Phosphates allow better layer growth.
  • the electrolyte contains 0.8 to 2.9 mol / L, preferably 0.8 to 2.1 mol / L of a stabilizer, in particular hexamethylenetetramine.
  • iron and vanadium salts are added to the electrolyte in order to obtain the desired black color of the oxide ceramic layer.
  • the combination of iron and vanadium according to the invention gives deep black and thick layers (up to 100 ⁇ m).
  • the presence of both metal salts is absolutely necessary for their production.
  • no deep black layers in the sense of the invention are obtained with only one of the two metal salts.
  • ammonium iron (III) citrate and ammonium (mono) vanadate are used for this purpose, in a concentration of 0.04 to 0.09 mol / L and 0.035 to 0.090 mol / L.
  • An electrolyte temperature of 15 to 60, preferably up to 40 degrees Celsius has been found to be particularly suitable.
  • the current density used is preferably between 0.02 and 0.10 Acm -2 , preferably 0.04 to 0.08 Acm -2 , without having to compromise on the quality and layer thickness of the oxide ceramic layers.
  • the current density is advantageously kept constant until a final voltage below 1000 V, preferably 300 to 650 V, is reached.
  • the oxide ceramic layers obtainable by means of the invention can have a layer thickness of 5 ⁇ m to 100 ⁇ m and consist of oxides, in particular spinels, of aluminum, iron and vanadium.
  • the electrolyte combinations according to the invention With the electrolyte combinations according to the invention, deep black (of L * less than or equal to 30, see above) and also adherent layer thicknesses greater than 50 ⁇ m can be produced for the first time.
  • the electrolyte combination according to the invention allows the production of thin or thick jet black and also adhesive layers of up to 100 ⁇ m.
  • the electrolyte is low in pollutants and easy to handle, that is to say does not contain any molybdenum, cobalt, chromium and nickel ions, as well as cyanide ions and borate ions.
  • the electrolyte solutions were freshly prepared and placed in conventional devices for anodic oxidation. Before the oxidation, all sample plates were degreased with a commercially available cleaner and then immersed and contacted in the electrolyte baths. The voltage was applied with a rectifier from RGB (30A / 380V). After about 10 min. the voltages were in the range of 230 to 290 volts.
  • the characterization of the layer was carried out on the samples according to the CIE L * a * b * system according to DIN EN ISO 11664-4, layer thickness measurements and cross-cut tests according to DIN 2499.
  • the layer thickness measurements were carried out using the specified measuring device from Helmut Fischer GmbH & Co.KG (see above). 10 measurements of the layer thickness were carried out for each sample plate and the mean value was given.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Claims (10)

  1. Procédé plasma-chimique pour la production de couches de céramique oxydée noire sur de l'aluminium, du titane ou de leurs alliages ainsi que sur des matériaux spéciaux contenant ces matières, lesquels comportent des composés intermétalliques d'aluminium, de titane ou de leurs alliages, après le processus d'oxydation anodique dans un électrolyte aqueux qui présente une teneur en fer et en vanadium, caractérisé en ce que l'électrolyte contient de 0,04 à 0,09 mol/l de citrate de fer(III) et d'ammonium et de 0,035 à 0,090 mol/l de (mono)vanadate d'ammonium.
  2. Procédé selon la revendication 1, caractérisé en ce que l'électrolyte a une valeur de pH de 5,4 à 10,0.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'électrolyte contient de 0,15 à 0,5 mol/l d'acide citrique ou de ses sels.
  4. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'électrolyte contient de 0,8 à 2,9 mol/l d'un agent stabilisant, en particulier de l'hexaméthylènetétramine.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'électrolyte contient de 0,2 à 0,9 mol/l d'un phosphate d'un métal alcalin, de préférence un dihydrogénophosphate ou un pyrophosphate, en particulier du dihydrogénophosphate de potassium ou du pyrophosphate de potassium.
  6. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le bain d'électrolyte a une température de 15 à 60 degrés Celsius.
  7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la densité de courant appliquée est de 0,02 à 0,10 Acm-2, de préférence de 0,04 à 0,08 Acm-2.
  8. Procédé selon la revendication 7, caractérisé en ce qu'une tension finale inférieure à 1000 V, de préférence de 300 à 650 V, est atteinte.
  9. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les couches de céramique oxydée produites ont une épaisseur de couche dans la gamme de 5 µm à 100 µm.
  10. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les couches de céramique oxydée produites sont constituées d'oxydes, en particulier de spinelles, d'aluminium, de fer et de vanadium.
EP14184217.9A 2013-09-26 2014-09-10 Procédé plasma-chimique destiné à fabriquer des couches en céramique oxydée noires et objet revêtu correspondant Active EP2857560B2 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102013110660.9A DE102013110660A1 (de) 2013-09-26 2013-09-26 Plasmachemisches Verfahren zur Herstellung schwarzer Oxidkeramikschichten und entsprechend beschichteter Gegenstand

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EP2857560A1 EP2857560A1 (fr) 2015-04-08
EP2857560B1 EP2857560B1 (fr) 2017-03-22
EP2857560B2 true EP2857560B2 (fr) 2020-04-22

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Publication number Priority date Publication date Assignee Title
DE102013110660A1 (de) 2013-09-26 2015-03-26 AHC Oberflächentechnik GmbH Plasmachemisches Verfahren zur Herstellung schwarzer Oxidkeramikschichten und entsprechend beschichteter Gegenstand
WO2019098378A1 (fr) * 2017-11-17 2019-05-23 株式会社東亜電化 Élément métallique en magnésium ou en aluminium doté d'un revêtement d'oxyde noir, et son procédé de fabrication
DE102018110905A1 (de) 2018-05-07 2019-11-07 Lucas Automotive Gmbh Elektrode für ein Eloxal-Verfahren
US11032930B2 (en) * 2019-05-28 2021-06-08 Apple Inc. Titanium surfaces with improved color consistency and resistance to color change
CN114144545A (zh) * 2019-07-09 2022-03-04 Bsh家用电器有限公司 制造组件的方法、组件和燃气灶
CN111058077B (zh) * 2020-01-19 2022-03-22 常州大学 一种用于微弧氧化黑色陶瓷膜的电解液及其制备方法和微弧氧化方法
CN112663112B (zh) * 2020-12-02 2022-10-04 斯特凯新材料(上海)有限公司 一种电解液及镁合金复合氧化黑色陶瓷膜的制备方法
CN114016108B (zh) * 2021-12-20 2022-11-25 哈尔滨三泳金属表面技术有限公司 一种高硅高铜压铸铝合金的表面氧化膜及其制备工艺
DE102022206126A1 (de) 2022-06-20 2023-03-09 Carl Zeiss Smt Gmbh Bauteil zum Einsatz in einer Projektionsbelichtungsanlage

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EP2103718A1 (fr) 2006-09-28 2009-09-23 Nihon Parkerizing Co., Ltd. Procédé destiné à appliquer un film de céramique sur un métal, solution d'électrolyse destinée à être utilisée dans le procédé, film de céramique et matériau métallique

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WO2003021009A2 (fr) 2001-08-03 2003-03-13 Elisha Holding Llc Procede de traitement d'une surface conductrice et produits formes a partir de ladite surface
US20070221508A1 (en) 2006-03-25 2007-09-27 Hon Hai Precision Industry Co., Ltd. Method for anodizing magnesium products
US20070246691A1 (en) 2006-04-19 2007-10-25 Hon Hai Precision Industry Co., Ltd. Electrolyte for anodizing magnesium products
EP2103718A1 (fr) 2006-09-28 2009-09-23 Nihon Parkerizing Co., Ltd. Procédé destiné à appliquer un film de céramique sur un métal, solution d'électrolyse destinée à être utilisée dans le procédé, film de céramique et matériau métallique

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US20150083598A1 (en) 2015-03-26
DE102013110660A1 (de) 2015-03-26
EP2857560B1 (fr) 2017-03-22
EP2857560A1 (fr) 2015-04-08

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