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WO2012119306A1 - Procédé de production d'oxyde d'aluminium anodisé blanc - Google Patents

Procédé de production d'oxyde d'aluminium anodisé blanc Download PDF

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Publication number
WO2012119306A1
WO2012119306A1 PCT/CN2011/071616 CN2011071616W WO2012119306A1 WO 2012119306 A1 WO2012119306 A1 WO 2012119306A1 CN 2011071616 W CN2011071616 W CN 2011071616W WO 2012119306 A1 WO2012119306 A1 WO 2012119306A1
Authority
WO
WIPO (PCT)
Prior art keywords
aluminum
aluminum oxide
oxide layer
substantially white
barium
Prior art date
Application number
PCT/CN2011/071616
Other languages
English (en)
Inventor
Jianying Miao
Un Teng LAM
Richard Hon Wai AU
Ying Liang
Man Ho YIM
Original Assignee
Nano And Advanced Materials Institute Limited
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nano And Advanced Materials Institute Limited filed Critical Nano And Advanced Materials Institute Limited
Priority to CN201180012356.1A priority Critical patent/CN102834551B/zh
Priority to PCT/CN2011/071616 priority patent/WO2012119306A1/fr
Priority to US13/577,911 priority patent/US20140209467A1/en
Publication of WO2012119306A1 publication Critical patent/WO2012119306A1/fr

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
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C25D11/243—Chemical after-treatment using organic dyestuffs
    • 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

Definitions

  • the present invention relates to methods for anodizing aluminum to produce aluminum oxide and, more particularly, methods for producing white anodized aluminum oxide.
  • Anodized aluminum oxide (AAO) on aluminum/aluminum alloys is widely used as a decorative finished surface due to its excellent hardness, corrosion resistance and abrasion resistance. Because anodized aluminum oxide layer can be colored by dyes or pigments, it has been employed in products such as automotive hardware and accessories, home furnishings, building and architectural materials, electronics, and ornaments.
  • AAO is formed by the anodization of aluminum or aluminum alloys in inorganic or organic acids. Sulfuric, oxalic, phosphoric and chromic acids are generally used as electrolytes in the anodization process. By adjusting anodization parameters such as acid concentration, voltage, current density, temperature and time, pore size of the resulting oxide layer can be controlled within the range of a few nanometers to several hundred nanometers.
  • Colorization of AAO can be achieved by dyeing methods such as dipping (or immersion) and electro-deposition. Electro-deposition, also known as electro-coloring, is a process used to deposit metals/metallic compounds into the pores of AAO by electrolysis.
  • U.S. Patent No. 4,251,330 describes a method for producing colored AAO through a process of pore enlargement using alternating current (AC) followed by electro-coloring.
  • U.S. Patent No. 5,472,788 produces a colored anodic film made from three electrolytically-formed superposed AAO layers. Current and time are varied during deposition and metal pigments are embedded within the pores of the three combined layers. A broad range of colors within the visible spectrum was displayed by the deposited film as a result of light interference and multiple refractions.
  • AAO A common industrial method for producing colored AAO is by dipping (or immersing) the anodic aluminum film in dyes or pigments.
  • Organic dyes are widely used, owing to the range of colors available and ease of fabrication. Colorization by inorganic pigments is uneven since inorganic pigment particles are large in size. The pore size of AAO can influence the resulting color by affecting the adsorption of dye or pigment particles on the inner walls of AAO channels.
  • X. H. Wang et al, Applied Physics Letters 91, 011908, 2007 describes the use of elemental carbon to modify the color of AAO surfaces.
  • JP 1-205,094 describes a method of producing white AAO by depositing magnesium oxide into the pores of AAO.
  • Aluminum was electrolytically treated with an aqueous solution containing a pH stabilizer and magnesium salt such as magnesium sulfate. To achieve a high degree of whiteness, AAO pore enlargement was conducted.
  • JP 63-247,396 an opaque white AAO film was generated by a one- or two-step treatment using an aqueous solution of F ⁇ ions (such as hydrofluoric acid, ammonium fluoride or metallic fluoride salts).
  • F ⁇ ions such as hydrofluoric acid, ammonium fluoride or metallic fluoride salts.
  • F " ions destroy the inner structure of AAO and hence substantially decrease the resulting hardness.
  • JP 57-092,194 an opaque white AAO film was formed by subjecting an anodized Al or Al alloy material to AC or DC cathodic electrolysis in a weak alkaline solution of Ti complex ions in the absence of K + and Na + ions.
  • this method involves complicated Ti complex preparation, neutralization, and AC or DC cathodic electrolysis.
  • Such techniques could be used to form hard, scratch-resistant, decorative surfaces in a variety of products such as construction materials, automotive body surfaces, and electronic device surfaces.
  • the present invention provides a simple, effective and low cost process for producing substantially white AAO with high color intensity and uniformity utilizing a multi-step anodization technique and deposition of inorganic/organic salts. Unstable and complicated steps such as pore enlargement and electrolytic deposition of metals/metal compounds are eliminated in this method. Hardness and other desirable surface properties of the AAO are retained. Post-treatments such as sealing and polishing can be carried out with ease.
  • a method for forming white anodized aluminum oxide on an aluminum or aluminum alloy substrate is provided.
  • a porous aluminum oxide layer is formed on the aluminum or aluminum alloy substrate by anodization in an acid electrolyte.
  • the AAO on the aluminum/aluminum alloy is sequentially immersed in two or more solutions. The two or more solutions will each flow into the AAO pores, react and form a substantially white metal compound pigment reaction product in the pores of the aluminum oxide layer.
  • Selected solutions include aqueous solutions or organic solvents- based solutions containing compounds which react with each other to form a substantially white precipitate.
  • Such solution combinations vary upon the choice of the final white pigment, which includes, but is not limited to, aluminum hydroxide, aluminum phosphate, aluminum silicate, antimony hydroxide, barium carbonate, barium oxalate, barium sulfate, barium titanate, barium tungstate, bismuth subnitrate, boron nitride, calcium carbonate, calcium oxalate, calcium sulfate, calcium silicate, magnesium silicate, magnesium carbonate, magnesium hydroxide, silver chloride, silver oxalate, tin (II) oxide, zinc oxide, zinc phosphate, zinc sulfide.
  • white pigments include lead compounds such as lead sulfate, lead chloride, lead carbonate, lead hydroxide and lead phosphate.
  • lead compounds such as lead sulfate, lead chloride, lead carbonate, lead hydroxide and lead phosphate.
  • this group of pigments is toxic. This will limit their usage.
  • the first porous aluminum oxide layer is removed, typically by etching with an acidic or alkaline solution, followed by formation of a second porous aluminum oxide layer on the aluminum or aluminum alloy substrate by anodization.
  • the aluminum/aluminum alloy substrate is subjected to a further anodization process in a dilute acid with organic additives. In this process, branched anodized aluminum oxide channels are formed which increases the opacity of the anodized aluminum oxide layer. The final degree of opacity depends on the anodization temperature and time. At high temperatures, the dissolution rate of AAO is faster than the formation rate during anodization.
  • the AAO layer will become thinner and more transparent. Conversely, if the anodization time is too short, an insufficient number of branched channels will be formed to make the AAO layer opaque.
  • the AAO - aluminum/aluminum alloy with white pigment materials deposited in the channels of the AAO is sealed to reduce pore size and increase corrosion resistance, followed by optional polishing.
  • a white anodized aluminum oxide layer is formed in an inexpensive, reproducible process suitable for commercialization.
  • the process of the present invention creates white anodized aluminum oxide through commercial grade process steps that permit industrial- scale production of white AAO.
  • the present invention will be described with respect to various exemplary embodiments for carrying out the invention.
  • the present invention is carried out on aluminum or aluminum alloy substrate surfaces; these aluminum/aluminum alloy substrates can be formed in a variety of shapes depending upon the final use. Prior to anodization, the aluminum/aluminum alloy substrate is cleaned, typically through degreasing using an acidic or alkaline solution and detergent, followed by thorough rinsing with distilled water and organic solvents such as ethanol and acetone, and drying.
  • the Al/Al alloy substrate is washed with a mixture of acetone and ethanol (1 : 1 v:v).
  • the substrate is then etched by a sodium hydroxide solution.
  • the substrate is pickled and desmutted in nitric acid. In desmutting, non-aluminum metals are removed from the aluminum alloy surface, resulting in a more pure starting material for anodization.
  • the substrate is then thoroughly washed in distilled water, sonicated in distilled water and then air-dried.
  • the aluminum/aluminum alloy substrate is anodized.
  • the aluminum/aluminum alloy substrate forms the anode of an electrolytic cell.
  • the cathode may be selected from suitable electrically-conductive materials such as carbon, lead, stainless steel, aluminum, titanium or platinum.
  • the electrolyte includes an acid; exemplary acids are sulfuric acid, oxalic acid, phosphoric acid, or chromic acid.
  • anodization is carried out using direct current (DC anodization) although AC anodization is also possible.
  • DC-powered anodization is carried out at 2 - 20°C in sulfuric acid of 10 - 20 wt%.
  • Voltage of 10 - 25 V or current density of 1.0 - 2.0 A/cm is maintained throughout the anodization.
  • the time of anodization depends on the application of the AAO layer. If the first layer of AAO will be the only layer of AAO formed, the duration will be on the order of one to two hours to produce an AAO film of 10 - 30 ⁇ in thickness with an average pore diameter of 6 - 20 nm. If the first layer of AAO is removed during an optional process, as described below, a duration of less than 60 minutes is sufficient.
  • oxygen is generated on the surface of the aluminum/aluminum alloy substrate anode which reacts with the aluminum to form aluminum oxide. Because the aluminum oxide formed during the anodization is porous, oxygen generated at the anode can reach the aluminum/aluminum alloy substrate to further maintain the growth of the oxide layer to a desired thickness (the desired thickness depends on the application of the final product with thicker aluminum oxide layers used in structural/outdoor applications and thinner aluminum oxide layers used in interior decorative applications).
  • a second AAO layer is produced.
  • the first AAO layer on the aluminum/aluminum alloy substrate is removed using an acidic or alkaline solution.
  • Exemplary solutions include phosphoric acid, chromic acid or sodium hydroxide.
  • a mixed solution of phosphoric acid (6 wt%) and chromic acid (3 wt%) generates a uniform and polished Al or Al alloy substrate surface. Heating at 60°C can increase the rate of the AAO removal.
  • the aluminum/aluminum alloy is washed with distilled water, preferably at least three times.
  • the optional second anodized aluminum oxide layer is formed on the aluminum/aluminum alloy substrate using substantially similar conditions to those described above with respect to the formation of the first AAO layer.
  • the duration of the treatment is approximately one to two hour(s) to form an AAO film of 10 - 30 ⁇ in thickness with an average pore diameter of 6 - 20 nm. Longer anodization times can be used to produce thicker films while shorter times can be used to produce thinner films, depending on the final application, as discussed above.
  • the aluminum/aluminum alloy substrate with the AAO film is sequentially immersed in two or more reaction material solutions such that the two or more reaction materials react to form a metal compound reaction product that fills the pores/channels of the anodized aluminum oxide layer as a substantially white pigment/colorant.
  • the first reaction material solution flows into the pores/channels of the AAO layer.
  • the second/subsequent reaction solution reacts with the material from the first solution to form a deposit in the pores/channels of the AAO that is a metal compound pigment reaction product.
  • reaction materials may be dissolved in organic or inorganic solvent(s) depending upon the selected reaction material(s). Prior to immersion, it is preferable to ultrasonicate the AAO/A1 or AAO/A1 alloy substrate in distilled water for 5 - 10 minutes to remove gas bubbles in the AAO channels.
  • Selected solutions include aqueous solutions or organic solvents- based solutions containing compounds which react with each other to form a substantially white precipitate.
  • Such solution combinations vary upon the choice of the final substantially white pigment, which includes, but is not limited to, metal compounds such as aluminum hydroxide, aluminum phosphate, aluminum silicate, antimony hydroxide, barium carbonate, barium oxalate, barium sulfate, barium titanate, barium tungstate, bismuth subnitrate, boron nitride, calcium carbonate, calcium oxalate, calcium sulfate, calcium silicate, magnesium silicate, magnesium carbonate, magnesium hydroxide, silver chloride, silver oxalate, tin (II) oxide, zinc oxide, zinc phosphate, zinc sulfide.
  • Other white pigments include lead compounds such as lead sulfate, lead chloride, lead carbonate, lead hydroxide and lead phosphate. However, this group of pigments is toxic. This will limit
  • Suitable reaction material solutions can include a chloride, nitrate, or sulfate of a pigment reaction product metal component (e.g., of aluminum, barium, zinc, etc.), and a second reaction material solution can includes a hydroxide, phosphate, carbonate, silicate, or oxalate component (such as ammonium carbonate, or potassium oxalate).
  • a pigment reaction product metal component e.g., of aluminum, barium, zinc, etc.
  • a second reaction material solution can includes a hydroxide, phosphate, carbonate, silicate, or oxalate component (such as ammonium carbonate, or potassium oxalate).
  • Selected aqueous or organic solvent-based solutions include, but are not limited to aluminum chloride/aluminum nitrate with sodium hydroxide/potassium hydroxide/ammonium hydroxide in water, aluminum chloride/aluminum nitrate with sodium phosphate/potassium phosphate/ammonium phosphate in water, aluminum chloride/aluminum nitrate with sodium silicate/potassium silicate/ammonium silicate in water, antimony chloride/antimony nitrate with sodium hydroxide/potassium hydroxide/ammonium hydroxide in water, barium chloride/barium nitrate with sodium carbonate/potassium carbonate/ammonium carbonate in water, barium chloride/barium nitrate with sodium oxalate/potassium
  • reaction systems can also be used such as lead nitrate with sodium sulfate/potassium sulfate/ammonium sulfate in water, lead nitrate with sodium chloride/potassium chloride/ammonium chloride in water, lead nitrate with sodium carbonate/potassium carbonate/ammonium carbonate in water, lead nitrate with sodium hydroxide/potassium hydroxide/ammonium hydroxide in water, lead nitrate with sodium phosphate/potassium phosphate/ammonium phosphate in water.
  • the reactants and products are toxic which can limit their application.
  • an aluminum/aluminum alloy substrate with a first/second AAO layer formed thereon is immersed in a solution of barium chloride with or without ultrasonication for 5 min.
  • the immersed substrate is heated at approximately 60°C for 30 - 60 min.
  • thorough rinsing with distilled water followed optionally by wiping the surface with a clean, soft cloth or tissue paper removes any surface residue.
  • the substrate is then immersed in a solution of sodium sulfate with or without ultrasonication for 5 min.
  • the immersed substrate is again heated at approximately 60°C for 30 - 60 min, followed by rinsing and cleaning as above.
  • barium sulfate (BaS0 4 ) is formed in the porous channels of the AAO layer.
  • a concentration of 0.05-0.5 mol/L is preferred for each solution.
  • the temperature should not exceed 70°C to prevent sealing of the anodized aluminum oxide pores in aqueous solutions.
  • the substrate remains undisturbed in the solution following ultrasonication.
  • a small amount of surfactant, particularly anionic or amphiprotic surfactant, can optionally be added to improve the immersion efficiency.
  • the immersion and rinsing process is repeated approximately 3-5 times.
  • the aluminum/aluminum alloy substrate with the first/second AAO layer infiltrated with the white precipitate/product is anodized in dilute acid solution with organic additives, to produce a branched nano-channel structure of AAO.
  • the anodization occurs in a dilute solution of weak or strong acid and organic additives under DC power.
  • a dilute solution of sulfuric acid (1 - 2 g/L) is mixed with a weak organic acid (8 - 12 g/L), such as boric acid, lactic acid, or citric acid, and organic additives such as ethanol, ethylene glycol, or glycerin.
  • Anodization is operated at 15 - 25 V and at 20 - 60°C.
  • the duration of anodization is carefully controlled since it influences the degree of whiteness in the final product.
  • a period of 10 - 30 min is selected.
  • branched AAO channels are formed, which will make enhance the opacity of the AAO layer.
  • AAO is both formed and dissolved simultaneously but at different rates. At elevated temperatures, the dissolution rate of AAO is greater than the rate of formation. Thus the time and temperature are carefully controlled to ensure creation of branched AAO channels without thinning the AAO layer.
  • the anodized aluminum/aluminum alloy is thoroughly washed with distilled water and organic solvents and air-dried.
  • a process of pore-sealing follows anodization.
  • pore sealing treatment with steam or boiling water is used to convert at least a portion of the oxide to the hydrated form.
  • the larger hydrated oxide molecule results in pore closings of the AAO channels.
  • inorganic sealing reagents such as potassium bi-chromate, nickel sulfate, cobalt sulfate, cobalt acetate, can be used for pore sealing.
  • the colors of nickel and cobalt salts can affect the degree of whiteness of the final product.
  • sealing is performed by organic sealing reagents like grease, wax, resins, and polymers.
  • a polymer liquid is used as a sealant.
  • a polymer sealant is formed by the following processes:
  • the anodized aluminum/aluminum alloy substrate is immersed in the polymer liquid for 1-3 minutes. Following immersion, the substrate is dried at approximately 60°C for approximately 10 min and subsequently at approximately 120°C for approximately 1 hour.
  • the sealed anodized aluminum/aluminum alloy substrate is mechanically polished to reach a desired degree of gloss.
  • Typical polishing materials include textiles such as wool. This polishing step is not necessary when a polymer sealant has been used.
  • the resultant substantially white anodized aluminum oxide on aluminum/aluminum alloy substrates form hard, scratch-resistant, decorative surfaces in a variety of products such as construction materials, automotive body surfaces, and electronic device surfaces.
  • the surfaces resist weathering and thus can be used for either structural or ornamental applications.

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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)
  • General Chemical & Material Sciences (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Printing Plates And Materials Therefor (AREA)

Abstract

L'invention concerne un procédé de formation d'oxyde d'aluminium anodisé sensiblement blanc sur un substrat d'aluminium ou d'alliage d'aluminium. Une couche poreuse d'oxyde d'aluminium est formée sur le substrat d'aluminium ou d'alliage d'aluminium par anodisation dans un électrolyte acide. Après la formation de la couche poreuse anodisée d'oxyde d'aluminium, le substrat d'aluminium ou d'alliage d'aluminium est plongé séquentiellement dans au moins deux solutions de matière de réaction. Les deux ou plusieurs matières de réaction réagissent de façon à déposer une matière pigmentaire sensiblement blanche dans les pores de l'oxyde d'aluminium anodisé.
PCT/CN2011/071616 2011-03-08 2011-03-08 Procédé de production d'oxyde d'aluminium anodisé blanc WO2012119306A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201180012356.1A CN102834551B (zh) 2011-03-08 2011-03-08 制造白色阳极氧化铝的方法
PCT/CN2011/071616 WO2012119306A1 (fr) 2011-03-08 2011-03-08 Procédé de production d'oxyde d'aluminium anodisé blanc
US13/577,911 US20140209467A1 (en) 2011-03-08 2011-08-03 Method For Producing White Anodized Aluminum Oxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2011/071616 WO2012119306A1 (fr) 2011-03-08 2011-03-08 Procédé de production d'oxyde d'aluminium anodisé blanc

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WO2012119306A1 true WO2012119306A1 (fr) 2012-09-13

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CN (1) CN102834551B (fr)
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WO2015047634A1 (fr) 2013-09-27 2015-04-02 Apple Inc. Procédés de formation de films anodisés blancs par formation de structures de pores ramifiées
WO2015047635A1 (fr) * 2013-09-27 2015-04-02 Apple Inc. Procédés de formation de films anodisés blancs par infusion de complexe de métal
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US10760175B2 (en) 2015-10-30 2020-09-01 Apple Inc. White anodic films with multiple layers
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US8993921B2 (en) 2012-06-22 2015-03-31 Apple Inc. Method of forming white appearing anodized films by laser beam treatment
CN105705681B (zh) * 2013-10-30 2021-03-26 苹果公司 用于通过在阳极化工艺之前或期间定位反射颗粒来制备白色外观金属氧化物膜的方法
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
US9839974B2 (en) 2013-11-13 2017-12-12 Apple Inc. Forming white metal oxide films by oxide structure modification or subsurface cracking
TWI506168B (zh) * 2014-01-29 2015-11-01 Catcher Technology Co Ltd 抗微生物複合表面的製造方法
DK3430185T3 (da) * 2016-04-27 2023-04-24 Bang & Olufsen As Højreflekterende anodiserede al-overflader med specialtilpasset diffust og spejlende indhold
CN105962549A (zh) * 2016-05-04 2016-09-28 深圳市联星服装辅料有限公司 一种银白色金属拉链及其制作方法
US10782741B2 (en) * 2017-03-09 2020-09-22 Apple Inc. Abrasion-resistant surface finishes on metal enclosures
CN107438340B (zh) * 2017-07-31 2020-08-11 维沃移动通信有限公司 一种外壳、电子设备及外壳的制备方法
CN108138351A (zh) * 2017-09-29 2018-06-08 欧朋达科技(深圳)有限公司 白色铝件及其制备方法
WO2020059728A1 (fr) * 2018-09-19 2020-03-26 日本軽金属株式会社 Élément en aluminium et son procédé de fabrication
CN109137009B (zh) * 2018-09-28 2021-02-05 北京工业大学 一种脉冲电沉积制备多孔氢氧化镁的方法
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WO2015047634A1 (fr) 2013-09-27 2015-04-02 Apple Inc. Procédés de formation de films anodisés blancs par formation de structures de pores ramifiées
WO2015047635A1 (fr) * 2013-09-27 2015-04-02 Apple Inc. Procédés de formation de films anodisés blancs par infusion de complexe de métal
US9051658B2 (en) 2013-09-27 2015-06-09 Apple Inc. Methods for forming white anodized films by forming branched pore structures
EP3017093A1 (fr) * 2013-09-27 2016-05-11 Apple Inc. Procédés de formation de films anodisés blancs par formation de structures de pores ramifiées
US9487879B2 (en) 2013-09-27 2016-11-08 Apple Inc. Anodized films with branched pore structures
US9512536B2 (en) 2013-09-27 2016-12-06 Apple Inc. Methods for forming white anodized films by metal complex infusion
EP3017093A4 (fr) * 2013-09-27 2017-05-17 Apple Inc. Procédés de formation de films anodisés blancs par formation de structures de pores ramifiées
US11131036B2 (en) 2013-09-27 2021-09-28 Apple Inc. Cosmetic anodic oxide coatings
EP2942423A4 (fr) * 2013-11-18 2015-12-16 Kwang Dong Hitech Co Ltd Procédé de traitement de surface d'alliage d'aluminium
US10760175B2 (en) 2015-10-30 2020-09-01 Apple Inc. White anodic films with multiple layers
US10781529B2 (en) 2015-10-30 2020-09-22 Apple Inc. Anodized films with pigment coloring
US11312107B2 (en) 2018-09-27 2022-04-26 Apple Inc. Plugging anodic oxides for increased corrosion resistance

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