US20220213608A1 - Method for sealing pores - Google Patents

Method for sealing pores Download PDF

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Publication number
US20220213608A1
US20220213608A1 US17/328,032 US202117328032A US2022213608A1 US 20220213608 A1 US20220213608 A1 US 20220213608A1 US 202117328032 A US202117328032 A US 202117328032A US 2022213608 A1 US2022213608 A1 US 2022213608A1
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United States
Prior art keywords
aluminum alloy
anode
solution
pores
metal
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Abandoned
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US17/328,032
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English (en)
Inventor
Steven Hong
Qinghua Hu
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Giant Glory International Ltd
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Giant Glory International Ltd
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Assigned to GIANT GLORY INTERNATIONAL LIMITED reassignment GIANT GLORY INTERNATIONAL LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HONG, STEVEN, HU, Qinghua
Publication of US20220213608A1 publication Critical patent/US20220213608A1/en
Abandoned legal-status Critical Current

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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
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
    • C25D3/16—Acetylenic compounds
    • 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
    • C25D11/246—Chemical after-treatment for sealing layers
    • 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
    • C25D11/20—Electrolytic after-treatment
    • 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
    • C25D11/26—Anodisation of refractory metals 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
    • C25D11/30—Anodisation of magnesium 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
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10—Electrodes, e.g. composition, counter electrode
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • C25D9/12—Electrolytic coating other than with metals with inorganic materials by cathodic processes on light metals
    • 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

Definitions

  • the disclosure relates to a method for sealing pores, and more particularly to a method for sealing pores formed in a metal layer or a metal oxide layer.
  • Magnesium alloys or aluminum alloys are usually used for manufacturing casings of portable electronic devices due to their good mechanical properties and low specific gravity.
  • alloys are highly reactive, and are prone to react with vapor in the air, resulting in corrosion on surfaces of the alloys. Therefore, when an alloy substrate, such as an aluminum alloy substrate, is used to form a casing, the alloy substrate is usually subjected to anodic oxidation to form a porous oxide layer on a surface thereof, thereby increasing the corrosion resistance of the alloy substrate. Subsequently, the porous oxide layer is subjected to a sealing process to seal pores in the porous oxide layer so as to improve surface evenness of the porous oxide layer and the aesthetic appearance of the casing.
  • an alloy substrate such as an aluminum alloy substrate
  • the alloy substrate is usually subjected to anodic oxidation to form a porous oxide layer on a surface thereof, thereby increasing the corrosion resistance of the alloy substrate.
  • the porous oxide layer is subjected to a sealing process to seal pores in the porous oxide layer so as to improve surface evenness of the porous oxide layer and the aesthetic appearance of the casing.
  • the sealing process is conventionally conducted by immersing an alloy substrate formed with a porous oxide layer thereon into a solution containing colloids or metal ions for a period of time, such that the colloids or metal ions are deposited on the oxide layer to form a sealing layer that seals pores in the porous oxide layer.
  • the solution is usually acidic or basic, during the sealing process, the solution would infiltrate into the pores of the oxide layer, causing corrosion of the alloy substrate.
  • the longer time the sealing process takes the higher the probability of corrosion and the higher the production costs are.
  • an object of the disclosure is to provide a method for sealing pores that can alleviate at least one of the drawbacks of the prior art.
  • the method includes: providing an object which includes a substrate formed of a metal or alloy of the metal, and a passivation layer formed on the substrate, the passivation layer being formed of metal oxide and having a plurality of pores;
  • FIG. 1 is a schematic view illustrating an embodiment of a method for sealing pores according to the disclosure.
  • an embodiment of a method for sealing pores includes: providing an object 1 which includes a substrate 11 formed of metal or alloy of the metal, and a passivation layer 12 formed on the substrate 11 , the passivation layer 12 being formed of metal oxide and having a plurality of pores; immersing the object 1 as a cathode and an anode 2 in a solution 3 containing metal cations 31 and anions 32 ; providing a predetermined electric current between the anode 2 and the object 1 , and thus generating an electric field between the anode 2 and the object 1 , such that the metal cations 31 and the anions 32 in the solution 3 move onto the object 1 and undergo a redox reaction on the passivation layer 12 ; and sealing the pores of the passivation layer 12 with a metallic compound formed by the redox reaction of the metal cations 31 and the anions 32 in the solution 3 .
  • the anode 2 is a carbon anode, a stainless steel anode, an aluminum anode or a lead anode.
  • the passivation layer 12 is formed by oxidizing the metal or metal alloy of the substrate 11 .
  • the metal of the substrate 11 is aluminum, magnesium, or titanium, but are not limited thereto.
  • the object 1 further includes a dye dispersed in the passivation layer 12 .
  • an electric current density across the object 1 is controlled to be less than 0.5 A/dm 2 .
  • the electric current density ranges between 0.02 A/dm 2 and 0.06 A/dm 2 . Since application of the electric current generates an electric field, electromigration near the object 1 is inhibited, so that electron loss occurring on a surface of the object 1 can be avoided, thereby reducing corrosion of the object 1 .
  • the metal cations 31 and the anions 32 in the solution 3 move toward and onto the object 1 and undergo redox reaction on the passivation layer 12 , so as to form the metallic compound that fills or covers the pores in the passivation layer 12 on the surface of object 1 (i.e., on a surface of the passivation layer 12 ).
  • the metal cations 31 will move too quickly, causing the metallic compound to be accumulated on a limited region of the surface of the passivation layer 12 (i.e., not being uniformly formed on the surface of the passivation layer of the object 1 ). Thus, the pores in the passivation layer 12 cannot be uniformly and fully filled or covered by the metallic compound.
  • the electric current is too low, and the electric current density is lower than 0.02 A/dm 2 , the metal cations 31 cannot move efficiently toward and onto the object 1 , which results in an inferior sealing effect.
  • the metal cations 31 in the solution 3 is selected from at least one of nickel ions, chromium ions, or zirconium ions, and the anions 32 may be acetate ions, fluoride ions, or sulfate ions, but are not limited thereto.
  • the pH value of the solution 3 may range between 3 and 7. In certain embodiments, the temperature of the solution 3 is controlled to range between 60° C. and 96° C.
  • a 5052 aluminum alloy substrate with a porous aluminum oxide layer formed thereon by virtue of anodic oxidation was used as a cathode.
  • the 5052 aluminum alloy substrate and a carbon anode were immersed in a nickel acetate-based solution (TOP SEAL DX-500, Okuno Chemical Industries Co., Ltd.) under a temperature ranging between 90° C. and 95° C.
  • a voltage of 1 V was applied to the carbon anode for 5 minutes, and an electric current density across the 5052 aluminum alloy substrate was 0.05 A/dm 2 .
  • the nickel ions moved toward and onto the 5052 aluminum alloy substrate, and were reacted with the acetate ions in the solution to form a metallic compound of nickel acetate that was deposited on a surface of the porous aluminum oxide layer.
  • the nickel acetate filled or covered pores in the porous aluminum oxide layer so that the pores were sealed, thereby obtaining a silver-colored aluminum alloy product.
  • Example 2 The procedures and conditions for preparing the silver-colored aluminum alloy products of Examples 2 and 3 are similar to those of Example 1, except that the voltage was applied for 10 minutes in Example 2 and 15 minutes in Example 3.
  • a 5052 aluminum alloy substrate with a porous aluminum oxide layer formed thereon by virtue of anodic oxidation was used as a cathode.
  • a black dye is dispersed in the porous aluminum oxide layer.
  • the 5052 aluminum alloy substrate and a carbon anode were immersed in a nickel acetate-based solution (TOP SEAL DX-500, Okuno Chemical Industries Co., Ltd.) under a temperature ranging between 90° C. and 95° C.
  • a voltage of 1 V was applied to the carbon anode, and an electric current density across the 5052 aluminum alloy substrate was 0.05 A/dm 2 .
  • the voltage was applied for 5 minutes in Example 4, 10 minutes in Example 5, and 15 minutes in Example 6.
  • the nickel ions moved toward and onto the 5052 aluminum alloy substrate, and were reacted with the acetate ions in the solution to form nickel acetate that was deposited on a surface of the porous aluminum oxide layer.
  • the nickel acetate filled or covered pores in the porous aluminum oxide layer so that the pores were sealed, thereby obtaining a black-colored aluminum alloy product.
  • a 5052 aluminum alloy substrate with a porous aluminum oxide layer formed thereon by virtue of anodic oxidation was immersed in the nickel acetate-based solution as used in Example 1.
  • the nickel ions were reacted with the acetate ions to form nickel acetate that was deposited on a surface of the porous aluminum oxide layer so as to fill or cover pores in the porous aluminum oxide layer, thereby obtaining a silver-colored aluminum alloy product.
  • Immersion of the 5052 aluminum alloy substrate in the nickel acetate-based solution was performed for 5, 10, 15, and 30 minutes in Comparative Examples 1, 2, 3 and 4, respectively. It is noted that, the aluminum alloy product obtained in Comparative Example 1 is sticky, which was considered as a disqualified product and cannot meet industrial requirements. Thus, the aluminum alloy product obtained in Comparative Example 1 was excluded from follow-up evaluation tests.
  • An object containing a 5052 aluminum alloy substrate, a porous aluminum oxide layer formed on the 5052 aluminum alloy substrate by virtue of anodic oxidation, and a black dye dispersed in the porous aluminum oxide layer was provided.
  • the object was immersed in the nickel acetate-based solution as used in Example 1.
  • the nickel ions were reacted with the acetate ions to form nickel acetate that was deposited on a surface of the porous aluminum oxide layer to fill or cover pores in the porous aluminum oxide layer, thereby obtaining a black-colored aluminum alloy product.
  • Immersion of the object in the nickel acetate-based solution was performed for 10, 15, and minutes in Comparative Examples 5, 6 and 7, respectively.
  • the UV degradation test was performed using a spectrophotometer (CM-2600d, Konica Minolta) to measure the L*a*b* color values of each of the aluminum alloy products in Examples 1 to 6 and Comparative Examples 1 to 6.
  • the color value L* represents the perceptual lightness of the color (the higher the value, the lighter the color is), the color value represents the green-red chromaticity coordinate (negative values indicate green and positive values indicate red), and the color value b* represents the blue-yellow chromaticity coordinate (negative values indicate blue and positive values indicate yellow).
  • the UV degradation test includes the steps of: measuring initial color values of the aluminum alloy product using the spectrophotometer; conducting a UV radiation exposure cycle for 12 times; and then measuring the final color values of the aluminum alloy product.
  • the UV radiation exposure cycle involves exposing the aluminum alloy product to UV radiation for 4 hours at 60° C., and then placing the aluminum alloy product in an environment without UV radiation at 50° C. for 4 hours.
  • ⁇ E value The greater the ⁇ E value, the more severe the discoloration of the aluminum alloy product.
  • a cycle of a salt spray test involves placing the aluminum alloy product in a salt spray chamber at 35° C., providing continuous salt water (5% NaCl) mist to the aluminum alloy product in the salt spray chamber for 24 hours; and drying the aluminum alloy product for 24 hours. The cycle was repeated 2 times. After the salt spray test, the aluminum alloy product was cleaned and was observed for any defects (e.g., corrosion, rust, etc.) occurred thereon.
  • a cycle of the TS test involves placing the aluminum alloy product in a TS tester, and exposing the aluminum alloy product to a temperature difference between ⁇ 20° C. (i.e., minimum temperature) and 60° C. (i.e., maximum temperature) with a temperature transition rate of 20° C. per minute. In each of the cycle, the aluminum alloy product was kept at each of the maximum and minimum temperatures for 10 minutes. After performing 48 cycles of the TS test, which lasted for 24 hours, the appearance of the aluminum alloy product was observed whether or not nickel acetate was peeled off from the surface of the aluminum alloy substrate.
  • the temperature and humidity (TH) test was carried cut by placing the aluminum alloy product in a test chamber under 60° C. and 95% humidity for 4 days. After the TH test, the appearance of the aluminum alloy product was observed whether or not nickel acetate was peeled off from the aluminum alloy substrate, or if any defect, such as blisters or cleavages, occurred.
  • the corrosion rate of the aluminum alloy product was evaluated by the weight loss test. First, the initial weight W 1 of the aluminum alloy product was measured. Then, the aluminum alloy product was immersed in a chromium trioxide (CrO 3 ) solution at 38° C. for 15 minutes, followed by cleaning and drying the aluminum alloy product. Thereafter, the weight W 2 of the aluminum alloy product was measured. Weight loss ratio (W L ) was determined by the formula:
  • A represents a surface area of the aluminum alloy product before immersion in the chromium trioxide solution. Sealing is determined to be complete if W L of a sealed aluminum alloy product is not greater than 20 mg/dm 2 .
  • Comparative Example 1 it can be seen from Comparative Example 1 that, when the aluminum alloy substrate is sealed for 5 minutes without voltage application, the product thus obtained can not meet industrial requirements, whereas the aluminum alloy product of Example 1 (being sealed for 5 minutes using the sealing method of this disclosure) is a qualified product. It is indicated that the sealing method of this disclosure can shorten sealing time for obtaining a qualified aluminum alloy product, thereby improving the efficiency of the method of this disclosure.
  • the results obtained from the UV degradation test reveal that the ⁇ E values of Examples 4 to 6 are smaller than those of Comparative Examples 5 to 7, indicating that the aluminum alloy products in Examples 4 to 6 have a smaller color value change after UV radiation exposure and thus, exhibit an improved color constancy.
  • the aluminum alloy products containing the dye i.e., Examples 4 to 6 and Comparative Examples 5 to 7
  • have a larger ⁇ E value than the aluminum alloy products without the dye i.e., Examples 1 to 3 and Comparative Examples 2 to 4
  • the aluminum alloy products containing the dye i.e., Examples 4 to 6 and Comparative Examples 5 to 7
  • the aluminum alloy products without the dye i.e., Examples 1 to 3 and Comparative Examples 2 to 4
  • the metallic compound provides less protection for the aluminum alloy products.
  • the efficiency for sealing the pores is improved, and thus the aluminum alloy products have reduced discoloration and weight loss ratio, especially in the aluminum alloy products containing the dye.
US17/328,032 2021-01-05 2021-05-24 Method for sealing pores Abandoned US20220213608A1 (en)

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CN202110007568.6A CN114717629A (zh) 2021-01-05 2021-01-05 封孔制程
CN202110007568.6 2021-01-05

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TW202227674A (zh) 2022-07-16
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