EP3430185B1 - Stark reflektierende anodisierte al-oberflächen mit massgeschneidertem diffusem und spiegelndem gehalt - Google Patents

Stark reflektierende anodisierte al-oberflächen mit massgeschneidertem diffusem und spiegelndem gehalt Download PDF

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Publication number
EP3430185B1
EP3430185B1 EP16727968.6A EP16727968A EP3430185B1 EP 3430185 B1 EP3430185 B1 EP 3430185B1 EP 16727968 A EP16727968 A EP 16727968A EP 3430185 B1 EP3430185 B1 EP 3430185B1
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Prior art keywords
aluminium
acid
anodising
titanium
embedded
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English (en)
French (fr)
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EP3430185A1 (de
Inventor
Ib Kongstad
Flemming Jensen
Rajan Ambat
Kirill BORDO
Visweswara Chakravarthy GUDLA
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Bang and Olufsen AS
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Bang and Olufsen AS
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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
    • C25D11/06—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
    • C25D11/024—Anodisation under pulsed or modulated current or potential
    • 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
    • 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
    • C25D11/14—Producing integrally coloured layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires

Definitions

  • the present invention relates to a method to obtain a reflective anodised aluminium surface on an object.
  • the present invention relates in particular to a method to obtain a reflective, anodised aluminium surface having a white appearance.
  • White surfaces are ubiquitous in a huge number of applications (window frames, panels, doors, lamps, etc.), and while a white surface can be achieved using paint or even white plastics, a white wear-resistant aluminium surface would often be the number one choice if such a surface would be available.
  • White aluminium surfaces can be produced by embedding titanium dioxide (TiO 2 ) or other white pigments into an anodic film.
  • the white pigments opacify the films primarily by diffusely reflecting light. This reflection occurs because the white pigment scatters or bends light strongly. If there is enough white pigment in an anodic film almost all visible light striking it will be reflected, and the anodic film will appear opaque, white, and bright.
  • anodised surface is significantly higher than that of a traditional painted surface.
  • anodised surfaces are usually preferred to painted surfaces when it comes to both practical applications and long-lasting decorative purposes. Therefore white anodized surfaces are preferred and have high value compared to the white painted aluminium.
  • Embedding white pigments into an anodic film is not a straight-forward operation, considering that the pigments are typically magnitudes larger than the nanoscaled pores that are created in an anodizing process. It is known from EP 2 649 224 B1 to obtain a radiation scattering surface finish on an object by providing the object with a top layer, comprising aluminium or an aluminium alloy, the top layer comprising added discrete inclusions of a second material being different from aluminium and the first alloy, and subsequently anodising said top layer to form an anodic oxide layer and to generate from the inclusions discrete radiation scattering elements.
  • said radiation scattering elements are selected from particles of titanium, tin, zirconium, iron, titanium oxide, tin oxide, zirconium oxide, and iron oxide.
  • An anodising method using high-frequency switching anodising is disclosed in " Anodizing method for aluminum alloy by using high-frequency switching electrolysis" H.Tanaka, M.Fujita, T.Yamamoto, H.Muramatsu Suzuki Motor Corporation; H.Asoh, S.Ono, Kogakuin University .
  • Multi-pass friction stir processing to impregnate TiOz particles into the surface of an aluminium alloy and subsequent anodising in a sulphuric acid electrolyte is disclosed by V.C. Gudla, F. Jensen, A. Simar, R. Shabadi, R. Ambat,: Friction stir processed Al-TiO2 surface composites: Anodising behaviour and optical appearance, Appl. Surf. Sci. 324 (2015) 554-562 .
  • High frequency anodising of friction stir processed Al-TiO2 surface composites using a high frequency pulse and pulse reverse pulse technique at a fixed frequency in a sulfuric acid bath is disclosed by V. C. Gudla, F. Jensen, K. Bordo, A. Simar, R. Ambat, Effect of High Frequency Pulsing on the Interfacial Structure of Anodized Aluminium-TiO2, Journal of The Electrochemical Society, 162 (7) C303-C310 (2015 ).
  • Anodizing of aluminium-TiO2 may also be seen in "High frequency anodising of aluminium-TiO2 composites: Anodising behaviour and optical appearance" by Gudla et al, Surface and coatings tech. Vol. 277, pp 67-73, September 2015 .
  • Multi-pass friction stir processing to impregnate metal oxide (TiOz, Y 2 O 3 and CeOz) particles into the surface of an aluminium alloy and subsequent anodising in a sulphuric acid electrolyte is disclosed by V. C. Gudla, F. Jensen, S. Canulescu, A. Simar, R. Ambat, Friction stir processed Al - metal oxide surface composites: anodization and optical appearance, 28th international conference on surface modification technologies, June 16th - 18th, 2014, Tampere University of Technology, Tampere, Finl and.
  • FSP Multi-pass friction stir processing
  • US 2009/0236228 A1 relates to an anodizing method and apparatus.
  • US 2006/0037866 relates to an anodic oxide film and anodizing method.
  • US 2008/0087551 relates to a method for anodizing aluminum alloy and power supply for anodizing aluminum alloy.
  • JP2004-035930 relates to an aluminum alloy material and anodization treatment method therefor.
  • JP2008-0085574 relates to a method for anodizing an aluminum member.
  • JP2007-154301 relates to an aluminum alloy anodic oxidation method and power source for aluminum alloy anodic oxidation.
  • the present invention relates to a method according to claim 1.
  • the embedded discrete particles are titanium oxide particles.
  • Titanium dioxide exhibits a light refractive index much different than sealed anodic alumina, making it an ideal pigment for obtaining good light scattering.
  • pigments with other chemical compositions can be used, if they possess properties similar to those of titanium dioxide.
  • the particle size of the embedded discrete particles is in the range 100-500 nm, preferably in the range 150-400 nm, such as 200-300 nm.
  • the size of TiOz particles should preferably be 200-300 nm to secure light scattering of all visible wavelengths, making the surface perceived as white.
  • the aluminium or aluminium alloy comprises at least 95% by weight of aluminium, preferably at least 96% by weight of aluminium, such as at least 97% by weight of aluminium, such as at least 98% by weight of aluminium, more preferably at least 99% by weight of aluminium.
  • a pure aluminium alloy is required for the anodic film to become as optically transparent as possible. Alloying elements such as Fe, Mn and Cu must be kept to an absolute minimum, knowing that these elements will give rise to a certain degree of light absorption, which will compromise the anodic film whiteness. Using an alloy with a composition equivalent to a 6060 (or even purer), has proven to give good results.
  • the discrete particles of a metal or metal oxide are embedded by a solid state process.
  • Non-limiting examples of solid state processes include a solid state process selected from the group consisting of friction stir processing (FSP), additive friction stir processing (AFSP), and powder metallurgy.
  • FSP friction stir processing
  • AFSP additive friction stir processing
  • powder metallurgy powder metallurgy
  • Friction stir processing is a solid state process known for its ability to modify microstructures and provide improved properties over conventional processing technologies.
  • the development of friction stir processing (FSP) is based on the friction stir welding (FSW) technology.
  • FSW works by plunging a spinning tool into the joint of two materials and then traversing the rotating tool along the interface. The friction caused by the tool heats up the materials around the pin to a temperature below the melting point. The rotation of the tool "stirs" the material together and results in a mixture of the two materials.
  • FSW friction stir welding
  • FSW and FSP share the same mechanism, however, have completely different purposes in practical applications.
  • the goal of FSW is to join two plates together, whereas FSP aims at modifying the microstructure of a single or multiple workpieces.
  • FSP has emerged as an advanced tool to produce surface composites by embedding second phase particles into the matrix. It is exactly this feature that is utilized in this patent application as to embed white pigments into the aluminium bulk, considering that the FSP process has the required advantages of:
  • Friction Stir Processing is a very time-consuming batch process
  • AFSP Additive Friction Stir Processing
  • AFSP is the preferred technique for embedding white pigments into an aluminium matrix
  • Other techniques are also available.
  • An further example of solid state processing (route 2) is powder metallurgy, where pigments are mechanically alloyed into the aluminium powder.
  • the composite powder is subsequently compressed and shaped in a normal powder metal route such as forging, cold isostatic pressing (CIP), hot isostatic pressing (HIP), direct profile extrusion, direct rolling of sheets, cold spraying, thermal spraying etc.
  • the discrete particles of a metal or metal oxide are embedded by a liquid state process, such as e.g. Stir Casting or Investment Casting.
  • the discrete particles of a metal or metal oxide are embedded by a vapour state process such as e.g. Physical Vapour Deposition (PVD) or Chemical Vapour Deposition (CVD).
  • PVD Physical Vapour Deposition
  • CVD Chemical Vapour Deposition
  • any of the above major processing routes can be used, as long as they fulfil the considerations mentioned above.
  • Anodizing secures the conversion of aluminium into aluminium oxide.
  • the pigments which were embedded into the top aluminium layer will become embedded into the aluminium oxide after anodizing.
  • the difference in refractive index between the anodic oxide and the white pigments secures scattering of all visible wavelengths that finally makes the anodized surface appear white.
  • Anodic films are traditionally formed by passing a direct current (DC) through an electrolyte, with the aluminium part working as the anode and a suitable material serving as the cathode.
  • DC anodizing has proven problematic in anodizing the aforementioned composite alloy, due to the regions that are underneath each individual pigment. Anodic pores formed through a DC process are almost completely parallel and do not reach the regions underneath the pigments. This leaves an anodic film with embedded pigments that have a small area of non-anodized aluminium underneath them. In turn this is a very unfortunate situation, considering the light absorption properties of metallic aluminium, which finally makes the entire anodic film be perceived as dark rather than white.
  • the white anodizing must be carried out at low temperature and in low-aggressive electrolyte to decrease the degree of pore wall attack.
  • the electrolyte used in an anodising process is traditionally water based and has an active content of acid. Almost all weak and strong organic acids can function as an electrolyte in the anodizing step of the process according to the invention.
  • the anodising of step b. takes place in an aqueous solution of an organic acid selected from the group consisting of oxalic acid, succinic acid, tartaric acid, malic acid, maleic acid, formic acid, citric acid and acetic acid.
  • the anodising of step b. takes place in an aqueous solution of an organic acid selected from the group consisting of oxalic acid, formic acid and citric acid, preferably oxalic acid.
  • the high frequency signal which is a time varying signal, may comprise a square wave signal having pulses with amplitudes between -5 V and +5 V in the low period and between +15 V and 100 V in the high period. Moreover, the voltage ramp up/down times of the pulses may be in the range between 0 and 15% of the ideal square wave pulse duration.
  • the frequency of the square wave signal may typically be around 1 kHz.
  • the thickness of the anodized film determines how white the surface appears. To secure a total white light scattering effect in the visible spectrum - normally about 100 ⁇ m oxide is necessary. Thus in an embodiment of the invention the thickness of the anodized film is in the range 50-300 ⁇ m, such as about 75-200 ⁇ m, preferably in the range 100-150 ⁇ m, such as in the range 80-130 ⁇ m.
  • the pigment concentration determines how white the surface appears.
  • the pigment concentration is in the range 2-25 wt%, such as about 5-20 wt%, preferably in the range 10-15 wt%.
  • optical properties can be characterized by a standard spectrophotometer, where the degree of reflected light is measured.
  • Hardness can be measured with a standard microhardness testing unit, where a diamond indenter is pressed into the surface. The diagonal (in case of Vickers hardness testing) of the resulting indentation gives a figure for the surface hardness.
  • Tribological properties can be found by a standardised wear tester such as a ball-on-disc setup.
  • the thick anodic film obtained above may be slightly dissolved in the upper part because of the prolonged exposure to the acid electrolyte, a phenomenon known as "pore wall attack".
  • the porous oxide can be stabilized by impregnating it with an agent that fills the anodic pores.
  • the method comprises a further step of impregnating the anodised aluminium oxide layer.
  • said impregnation is performed by means of an impregnating substance selected from the group consisting of a silicate, a lacquer, and a sol-gel substance.
  • an impregnating substance selected from the group consisting of a silicate, a lacquer, and a sol-gel substance.
  • lacquers and sol-gel substances include acrylics, silanes and silane based sol-gels.
  • Aluminium plates with dimensions 200 mm ⁇ 60 mm ⁇ 6 mm were used for the FSP trials.
  • Commercial TiOz powder in rutile phase was used.
  • the median diameter of the powder particles was 210 nm.
  • Processing the FSP process was performed using a hermle milling machine equipped with a steel tool having 20 mm shoulder diameter, 1.5 mm pin length with a m6 thread.
  • the backwards tilt angle of the tool was maintained at 1°.
  • a groove 0.5 mm deep, 10 mm wide, and 180 mm long in the Al plates which was compactly filled with TiOz powder.
  • the filled plates were then covered by the same Al sheet rolled down to a thickness of 0.25mm to prevent loss of TiOz powder during the initial FSP pass.
  • Rotational speed of the tool was 1000 rpm and the advancing speed was 200 mm/min for the first pass to insure correct closure of the groove and 1000 mm/min for the next six passes.
  • a surface of 175 mm long ⁇ 20 mm wide was processed for each pass with a total processing time of roughly 2 min. All seven passes were performed one over the other without any shift.
  • the samples were then mechanically polished, buffed to a mirror finish and then degreased in a mild alkaline solution at 60°C.
  • the samples were subsequently desmutted by immersing in diluted HNOs followed by demineralized water rinsing. Anodising was carried out in a saturated oxalic acid bath maintained at 10°C.
  • a square wave high frequency signal of 1 kHz from 0 to 40V was applied, with a controlled ramp up/down duration which corresponds to 10% of the pulse duration.
  • the process continues until the film thickness has grown to approximately 100 ⁇ m. After anodising the surface appears white, with both specular and diffuse reflections.
  • the sample is rinsed and transferred to a hot water sealing tank for closing the open-pored anodic structure. The process is illustrated in Fig. 2 .

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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)
  • Optical Elements Other Than Lenses (AREA)

Claims (13)

  1. Verfahren zum Erzielen einer reflektierenden anodisierten Aluminiumoberfläche auf einem Objekt, umfassend folgende Schritte:
    a) Versehen des Objekts mit einer Deckschicht, die Aluminium oder eine Aluminiumlegierung umfasst, wobei die Deckschicht eingebettete diskrete Partikel von Titan oder Titanoxid umfasst,
    b) anschließendes Anodisieren der Deckschicht, um eine anodische Oxidschicht zu bilden, wobei das Anodisieren in Schritt b) durch Anlegen eines zeitvariablen Signals erfolgt, das ein Hochfrequenzsignal in der Form eines Rechtecksignals umfasst, das eine Frequenz zwischen 500 Hz und 5 kHz, wie etwa ungefähr 1 kHz, aufweist;
    dadurch gekennzeichnet, dass das Anodisieren in Schritt b) in einer wässrigen Lösung einer organischen Säure erfolgt.
  2. Verfahren nach einem der vorhergehenden Ansprüche, wobei die Partikelgröße der eingebetteten diskreten Partikel in dem Bereich von 100 bis 500 nm, bevorzugt in dem Bereich von 150 bis 400 nm, wie etwa zwischen 200 und 300 nm, liegt.
  3. Verfahren nach einem der vorhergehenden Ansprüche, wobei das Aluminium oder die Aluminiumlegierung mindestens 95 Gewichtsprozent Aluminium, bevorzugt mindestens 96 Gewichtsprozent Aluminium, wie etwa mindestens 97 Gewichtsprozent Aluminium, wie etwa mindestens 98 Gewichtsprozent Aluminium, weiter bevorzugt mindestens 99 Gewichtsprozent Aluminium umfasst.
  4. Verfahren nach einem der vorhergehenden Ansprüche, wobei die diskreten Partikel von Titan oder Titanoxid durch einen Festphasenprozess eingebettet werden.
  5. Verfahren nach Anspruch 4, wobei der Festphasenprozess ein Prozess ist, der aus der Gruppe ausgewählt wird, die aus Reibschweißverarbeitung (FSP), additiver Reibschweißverarbeitung (AFSP) und Pulvermetallurgie besteht.
  6. Verfahren nach einem der Ansprüche 1 bis 4, wobei die diskreten Partikel von Titan oder Titanoxid durch einen Flüssigphasenprozess eingebettet werden.
  7. Verfahren nach einem der Ansprüche 1 bis 4, wobei die diskreten Partikel von Titan oder Titanoxid durch einen Dampfphasenprozess eingebettet werden.
  8. Verfahren nach einem der vorhergehenden Ansprüche, wobei das Anodisieren in Schritt b) in einer wässrigen Lösung einer organischen Säure erfolgt, die aus der Gruppe ausgewählt wird, die aus Oxalsäure, Bernsteinsäure, Weinsäure, Apfelsäure, Maleinsäure, Ameisensäure, Zitronensäure und Essigsäure besteht.
  9. Verfahren nach Anspruch 8, wobei die organische Säure aus der Gruppe ausgewählt wird, die Oxalsäure, Bernsteinsäure, Weinsäure, Apfelsäure, Maleinsäure und Zitronensäure umfasst.
  10. Verfahren nach Anspruch 1, wobei das Rechtecksignal eine Amplitude zwischen -5 V und 100 V, wie etwa zwischen 0 V und 40 V, aufweist.
  11. Verfahren nach Anspruch 1 oder 10, wobei das Rechtecksignal Hochlauf- und/oder Rücklaufzeiten zwischen 0 und 15 % einer Impulsdauer umfasst.
  12. Verfahren nach einem der vorhergehenden Ansprüche, ferner umfassend einen weiteren Schritt des Imprägnierens der anodisierten Aluminiumoxidschicht.
  13. Verfahren nach Anspruch 12, wobei das Imprägnieren anhand einer Imprägniersubstanz erfolgt, die aus der Gruppe ausgewählt wird, die aus einem Silikat, einem Lack und einer Sol-Gel-Substanz besteht.
EP16727968.6A 2016-04-27 2016-05-20 Stark reflektierende anodisierte al-oberflächen mit massgeschneidertem diffusem und spiegelndem gehalt Active EP3430185B1 (de)

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PCT/EP2016/061383 WO2017186315A1 (en) 2016-04-27 2016-05-20 Highly reflecting anodised al surfaces with tailored diffuse and specular content

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JP2004035930A (ja) 2002-07-02 2004-02-05 Suzuki Motor Corp アルミニウム合金材及びその陽極酸化処理方法
US7838120B2 (en) 2004-08-20 2010-11-23 Suzuki Motor Corporation Anodic oxide film
CN100383292C (zh) * 2004-12-29 2008-04-23 湖南大学 一种铝及其合金材料表面生成陶瓷膜的阳极化处理方法
JP2007154301A (ja) 2005-11-30 2007-06-21 Idx Corp アルミニウム合金陽極酸化方法およびアルミニウム合金陽極酸化用電源
TW200804629A (en) 2006-07-05 2008-01-16 Idx Corp Power supply for anodizing
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EP2649224B1 (de) 2010-12-06 2016-03-23 Bang & Olufsen A/S Verfahren zur herstellung einer strahlungsstreuungsendoberfläche auf einem gegenstand
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WO2013192579A1 (en) * 2012-06-22 2013-12-27 Apple Inc. White appearing anodized films and methods for forming the same
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US9512536B2 (en) * 2013-09-27 2016-12-06 Apple Inc. Methods for forming white anodized films by metal complex infusion
EP3063314B1 (de) * 2013-10-30 2023-06-14 Apple Inc. Verfahren zur erzeugung weisser metalloxidfilme durch positionierung reflektierender teilchen vor oder während eines anodisierungsverfahrens
US9181629B2 (en) * 2013-10-30 2015-11-10 Apple Inc. Methods for producing white appearing metal oxide films by positioning reflective particles prior to or during anodizing processes

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CN109072473B (zh) 2021-03-30
WO2017186315A1 (en) 2017-11-02
HK1259273A1 (zh) 2019-11-29
US20190136399A1 (en) 2019-05-09
CN109072473A (zh) 2018-12-21
DK3430185T3 (da) 2023-04-24

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