WO2020007356A1 - Produit de métal noble avec revêtement sur la surface et procédé de préparation associé - Google Patents

Produit de métal noble avec revêtement sur la surface et procédé de préparation associé Download PDF

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WO2020007356A1
WO2020007356A1 PCT/CN2019/094843 CN2019094843W WO2020007356A1 WO 2020007356 A1 WO2020007356 A1 WO 2020007356A1 CN 2019094843 W CN2019094843 W CN 2019094843W WO 2020007356 A1 WO2020007356 A1 WO 2020007356A1
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noble metal
gold
metal substrate
vapor deposition
physical vapor
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Chinese (zh)
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王彤
唐双喜
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Shenzhen United Blueocean Technology Development Co Ltd
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Shenzhen United Blueocean Technology Development Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0694—Halides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer

Definitions

  • the invention relates to the field of gold surface plating, in particular to a precious metal product with a plating layer on the surface and a preparation method thereof.
  • Gold products have bright colors and good stability. They are often used as jewelry and are popular with consumers. At present, the production process of gold products mainly includes casting wax, inverted mold, and surface trimming. In order to improve the gloss of the surface of gold products, the surface of gold products is usually treated by electroplating.
  • CN106521594A discloses a manufacturing method and equipment for processing K gold into a natural color of gold, preparing semi-finished jewelry in advance; electroplating the semi-finished product of jewelry to restore the external color to the natural color of gold; and performing surface treatment on the semi-finished jewelry after plating To form finished jewelry.
  • the film layer on the surface of the gold product is unstable and easily peeled off.
  • CN107675136A discloses a method for physical vapor deposition (PVD) coating on the surface of a workpiece.
  • the workpiece to be plated is put into a coating chamber to be evacuated and heated, and then argon is passed, and the workpiece to be plated is subjected to ion bombardment. Then, a working gas is passed into the plate to be coated The workpiece is biased to deposit a coating of the corresponding material on the workpiece to be plated.
  • PVD physical vapor deposition
  • CN105803412A discloses a PVD coating layer on the surface of an airspeed tube and a preparation method thereof.
  • a single metal plating layer is plated on a polished surface of the airspeed tube substrate by a physical vapor deposition method.
  • PVD a PVD method is used to coat the surface of the workpiece to improve the combining ability of the coating and the workpiece to be plated.
  • PVD is currently only suitable for coating on the surface of materials with higher hardness.
  • the bonding force between the film layer and the substrate is still weak.
  • the purpose of the present invention is to overcome the problem of unstable plating on the gold surface in the prior art, and to provide a precious metal product with a coating on the surface and a preparation method thereof.
  • Different types of film layers are formed on the surface of the precious metal product of the present invention.
  • the structure of the formed film layer is stable and can show different colors.
  • the first aspect of the present invention provides a precious metal product, the precious metal product includes a precious metal substrate and a physical vapor deposition layer attached to a surface of the precious metal substrate, and the precious metal is gold or silver.
  • a second aspect of the present invention provides a method for preparing a noble metal product, the method comprising: using a physical vapor deposition to attach a physical vapor deposition layer on the surface of the noble metal substrate.
  • the physical vapor deposition method is used to coat the surface of the noble metal substrate, which can form a colorful layer, and improve the single color of the noble metal substrate.
  • the change of the color will not affect the color of the noble metal substrate.
  • the surface roughness of the precious metal substrate is between 0.001 ⁇ m and 50 ⁇ m. After cleaning, it is dried at 100-150 ° C. It is easier to coat the surface of the precious metal substrate by physical vapor deposition, and the formed The film is more stable and has better wear resistance.
  • Embodiment 1 is a schematic structural diagram of a precious metal product in Embodiment 1;
  • Example 2 is a schematic structural diagram of a precious metal product in Example 13;
  • FIG. 3 is a schematic structural diagram of a precious metal product in Example 12.
  • FIG. 3 is a schematic structural diagram of a precious metal product in Example 12.
  • a first aspect of the present invention provides a precious metal product, which comprises a precious metal substrate 1 and a physical vapor deposition layer 2 attached to a surface of the precious metal substrate 1, wherein the precious metal is gold or silver.
  • the content of gold in the precious metal matrix 1 is 33-99.99% by weight, and more preferably 75-99.99% by weight (or 99-99.99% by weight).
  • the silver content is preferably 92.5-99% by weight.
  • the precious metal base 1 is gold, it can be K gold or solid gold.
  • K gold refers to the precious metal base 1 formed by mixing and melting gold with silver, zinc, copper, palladium, or nickel, and the so-called gold refers to the precious metal base 1 having a gold content of not less than 99% by weight.
  • the noble metal substrate 1 is silver, it can be silver, silver or 925 sterling silver.
  • the physical vapor deposition method is used to attach a physical vapor deposition layer 2 on the surface of the noble metal substrate 1.
  • the film formed by attaching the physical vapor deposition layer 2 to the noble metal substrate 1 is stable, wear-resistant, and difficult to fade.
  • the thickness of the physical vapor deposition layer 2 is 10 nm-50 ⁇ m, and preferably 0.04 ⁇ m-2 ⁇ m.
  • the bonding between the physical vapor deposition layer 2 and the noble metal substrate 1 is stronger, and when the noble metal products are tested, the physical vapor deposition layer 2 does not affect the color of the noble metal substrate 1 itself.
  • the physical vapor deposition layer 2 may be a single plating layer or a multilayer plating layer.
  • physical vapor deposition can be used to deposit the same single plating layer on the entire surface of the noble metal substrate 1.
  • the material of the physical vapor deposition layer 2 can be a common metal, alloy, metal oxide, metal nitride, Metal carbide, metal fluoride, metal sulfide, metal boride or diamond-like coating, such as: Ni, Ti, Zn, Cr, Mg, Nb, Sn, Al, In, Fe, Zr, Si, Cu, Ta, Ge, Ag, Co, Au, Gd, La, Y, Ce, W, Hf, Mo, CrN, TiN, TiAlCN, TiCN, TiAlN, AlTiN, TiB 2 , ZrN, FeCo, AlSi, TiSi, CrSi, ZnAl, TiZn , TiAl, TiZr, TiSi, TiNi, Ni
  • the precious metal products appear grayish black; if the plating layer on the surface of the precious metal substrate 1 is TiN, the precious metal products develop champagne gold; if the plating on the surface of the precious metal substrate 1 is TiAlN, The color of the noble metal product is brown; if the plating on the surface of the noble metal substrate 1 is DLC, the color of the noble metal product is black.
  • a multi-layer plating layer may be deposited on the surface of the noble metal substrate 1 by a physical vapor deposition method, and finally a colorful color is formed.
  • a masking method can be used to cover areas that do not need to be dyed, and then a physical vapor deposition layer 2 is formed on the surface of the precious metal substrate 1, and finally the surface of the precious metal product has different patterns.
  • the surface of the noble metal substrate 1 can also be formed with patterns of different colors.
  • the surface roughness of the precious metal substrate 1 may be 0.001 ⁇ m to 50 ⁇ m, preferably 0.005 ⁇ m to 0.2 ⁇ m.
  • the surface roughness is Ra, that is, the small pitch and unevenness of the small peaks and valleys of the processed surface can be directly tested by a surface roughness measuring instrument. If the raw material of the noble metal substrate 1 itself meets a surface roughness of 0.001 ⁇ m to 50 ⁇ m, the subsequent steps may be directly performed. If the raw material of the noble metal substrate 1 does not satisfy the surface roughness of 0.001 ⁇ m to 50 ⁇ m, the noble metal substrate 1 can be treated by a chemical or mechanical method, and the method is not particularly limited as long as it can satisfy the above roughness.
  • the surface roughness of the noble metal substrate 1 satisfies the above conditions, and it is easier to plate a film on the surface of the noble metal substrate. If the surface roughness is too low, the firmness of the bonding between the film layer and the precious metal substrate is reduced; if the surface roughness is too large, the color of the final precious metal product is affected.
  • the gloss of the gold product 1 may be 700-900 Gu.
  • Gu means English gloss unit
  • 1 gloss unit 1Gu.
  • the gloss gloss of precious metal products was measured with a gloss tester at a 60 ° geometric condition.
  • the gold content of the physical vapor deposition layer 2 may be 0.1% by weight or less than 33% by weight.
  • the gold content of the physical vapor deposition layer 2 is less than 0.01% by weight or 70-90% by weight.
  • the physical vapor deposition layer 2 has a gold content between 0.001-0.008% by weight or between 75-85% by weight.
  • a second aspect of the present invention provides a method for preparing a noble metal product, the method comprising: using a physical vapor deposition to attach a physical vapor deposition layer 2 on a surface of the noble metal substrate 1.
  • the conditions of physical vapor deposition are such that the thickness of physical vapor deposition layer 2 is 10 nm-50 ⁇ m (such as 10 nm, 20 nm, 30 nm, 50 nm, 80 nm, 0.1 ⁇ m, 0.15 ⁇ m, 0.2 ⁇ m, 0.25 ⁇ m, 0.3 ⁇ m, 0.5 ⁇ m , 0.8 ⁇ m, 1 ⁇ m, 2 ⁇ m, 10 ⁇ m, 30 ⁇ m, 50 ⁇ m, or any value between the foregoing values), preferably 0.04 ⁇ m to 2 ⁇ m.
  • 10 nm-50 ⁇ m such as 10 nm, 20 nm, 30 nm, 50 nm, 80 nm, 0.1 ⁇ m, 0.15 ⁇ m, 0.2 ⁇ m, 0.25 ⁇ m, 0.3 ⁇ m, 0.5 ⁇ m , 0.8 ⁇ m, 1 ⁇ m, 2 ⁇ m, 10 ⁇ m, 30 ⁇ m, 50 ⁇ m,
  • the physical vapor deposition method is not particularly required, and may be a vacuum evaporation coating, a vacuum sputtering coating, or a vacuum ion plating, and preferably a vacuum ion plating.
  • the vacuum evaporation system is used, and the precious metal substrate 1 and the metal to be plated are both placed in the vacuum evaporation system.
  • the precious metal substrate 1 is heated under the condition of a vacuum of 5-7 ⁇ 10 -3 Pa, and the material to be plated is placed.
  • the material to be plated can be selected from metal materials (such as aluminum) for color development, and the evaporation voltage is adjusted to heat the evaporation boat to reach the vaporization temperature of the material to be plated, for example, 800-1500 ° C, to achieve coating on the surface of the precious metal substrate 1, and then inert Annealing under the protection of a gas (such as argon).
  • a gas such as argon
  • the noble metal substrate 1 is heated at 100-250 ° C. under the conditions of a vacuum of 1 ⁇ 10 -2 Pa-7 ⁇ 10 -3 Pa, and the surface oxide film is removed from the target to be plated. Under the condition of plasma, positive ions formed after argon ionization bombarded the target surface, and the surface of the precious metal substrate 1 was coated by magnetron sputtering with a sputtering voltage of 300-700V. The metal to be plated formed a thin film on the surface of the precious metal substrate 1. .
  • the step of vacuum ion plating includes: placing the noble metal substrate 1 under a vacuum condition, then heating the noble metal substrate 1, starting a metal target, injecting a gas, applying a bias voltage, and coating the surface of the noble metal substrate 1.
  • the degree of vacuum is 1 ⁇ 10 -2 Pa to 7 ⁇ 10 -3 Pa.
  • the degree of vacuum is 1 ⁇ 10 -2 Pa to 9.5 ⁇ 10 -1 Pa.
  • the temperature will affect the binding force and color of the coating and the noble metal substrate.
  • the heating temperature in the furnace is generally 100-250 ° C, preferably 200 ° C.
  • the coating time is 2-2000min.
  • the deposition time is related to the target and the plating layer.
  • the target is divided into arc target, column target, and flat target.
  • the arc target ion particles are the thickest, followed by flat targets, and the column target ion particles are the most thick. It is thin, so the arc target is colored fast, followed by the flat target, and the column target is colored slowly.
  • the coating time of the arc target is about 10min
  • the coating time of the column target is 20-30min
  • the magic color coating time is about 10min.
  • the shortest purple coating time is 2-3min, so the purple color difference of the coating is large and the color is unstable.
  • the material used for the metal target is selected from nickel, zinc, magnesium, tin, iron, chromium, silicon, copper, titanium, zirconium, molybdenum, tungsten, aluminum, niobium, indium, tantalum, germanium, silver, gold, cobalt, Thallium, lanthanum, yttrium, cerium, thorium, tungsten, gold-copper alloys, stainless steel and its alloys or at least one of oxides, nitrides, carbides, fluorides, sulfides, borides, and preferably gold-copper alloys.
  • the atomic ratio of gold to copper is (75-85): (15-25), preferably 85:15 or 75:25.
  • the gas includes a protective gas and a color tone gas
  • the protective gas is an inert gas
  • the color tone gas is selected from one or more of nitrogen, acetylene, methane, and oxygen; wherein argon is used as the protective gas for adjusting The degree of vacuum
  • the gas flow of the protective gas may be 20-200 sccm, preferably 20-150 sccm; nitrogen, acetylene, methane or oxygen as the working gas, which can be combined with metal to form a coating film for adjusting the color of the coating layer, the working gas
  • the gas flow is 50-500 sccm.
  • the loading bias voltage is 10-150V
  • the duty cycle is 10-80%; in the present invention, the "duty cycle” refers to the ratio of the time occupied by the pulse to the total time during a continuous working time. In the present invention, the higher the bias voltage, the greater the brightness, but exceeding a certain value, the edge of the precious metal product will turn yellow; therefore, it is best to limit the loading bias voltage to the above range.
  • the target current of the metal target is 3-120A for column target, preferably 20-120A, and 50-200A for arc target.
  • the degree of influence is slightly worse, and the appropriate current is important for the gloss of the coating. Therefore, it is best to limit the target current to the above range.
  • the deposition time is related to the shape of the target and the coating layer, which is specifically explained in the examples.
  • the metal target and protective gas can be selected according to the color displayed by the final precious metal product. It can be a single metal.
  • the selected metal target is a titanium target
  • the protective gas is argon
  • the working gas is nitrogen
  • the gas flow rate is 100- 350sccm
  • the final precious metal product is golden yellow.
  • the selected metal target is a titanium aluminum target
  • the protective gas is argon
  • the working gas is nitrogen
  • the gas flow rate is 100-350 sccm.
  • the color of the final precious metal product is brown. The details are explained in the examples.
  • the glow cleaning can be performed before physical vapor deposition, and the conditions for the glow cleaning include: a gas flow of a protective gas of 100-320 sccm, preferably 280-320 sccm, and a loading bias of 380-1000 V, preferably 380- 420V, duty cycle is 10-80%, preferably 48-52%; time is 160-720s, preferably 160-200s.
  • the method may further include a step of surface-treating the surface of the noble metal substrate 1 so that the surface roughness of the noble metal substrate 1 is 0.001 ⁇ m to 50 ⁇ m.
  • the surface treatment method of the noble metal substrate 1 is not particularly limited, and a method of physical grinding or chemical etching may be adopted as long as the condition that the surface roughness of the noble metal substrate 1 is 0.001 ⁇ m to 50 ⁇ m can be achieved.
  • the surface roughness of the noble metal substrate 1 is 0.001 ⁇ m to 50 ⁇ m (such as 0.02 ⁇ m, 0.05 ⁇ m, 0.2 ⁇ m, 0.3 ⁇ m, 1 ⁇ m, or any value between the foregoing values), and preferably 0.005 ⁇ m to 0.2 ⁇ m.
  • the method further comprises cleaning the precious metal substrate 1 after the surface treatment.
  • the cleaning method is: ultrasonically washing the precious metal substrate 1 at 20-30 kHz for 1-15 min, and / or using 95-98% by weight. Alcohol cleans the surface of the precious metal substrate.
  • different cleaning methods can be selected according to the surface structure, area, and cleaning degree of the noble metal substrate 1.
  • the first type ultrasonically wash the precious metal substrate 1 under the condition of 20-30kHz for 1-15min; in the present invention, it should be noted that in special cases, the ultrasonic cleaning time can be extended. After the ultrasonic cleaning is completed, the water is washed 6 times. Above, the surface cleaning agent residue is removed. After the cleaning is completed, a drying treatment is required to dehydrate and bake.
  • the second type the surface of the precious metal substrate 1 is cleaned, without an oxide layer, and ultrasonic cleaning is not required.
  • the surface of the precious metal substrate 1 can be directly wiped with 95-98% by weight of alcohol.
  • the cleaning method may be the first or the second method, and preferably, the cleaning method may be the first method or the second method.
  • the ultrasonic treatment and / or alcohol washing of the precious metal substrate 1 under the above conditions can further improve the binding force between the physical vapor deposition layer 2 and the precious metal substrate 1.
  • a film layer with a thickness of 10 nm-50 ⁇ m can be formed on the surface of the precious metal substrate, and the formed film layer is more stable.
  • the method may further include the step of drying the noble metal substrate 1 after ultrasonic treatment, the drying temperature is 100-150 ° C., and the drying time is 5-30 min.
  • the method for drying the precious metal substrate there is no particular limitation on the method for drying the precious metal substrate, as long as the temperature can be maintained between 100-150 ° C, for example, an oven can be used.
  • a water plating layer 3 and / or a transparent film layer 4 may also be formed on the surface of the physical vapor deposition layer. That is, the precious metal product of the present invention includes: a precious metal substrate 1 and The physical vapor deposition layer 2 and the water plating layer 3 (shown in FIG. 2) attached to the surface of the precious metal substrate 1 in order, or the precious metal article of the present invention includes: a precious metal substrate 1 and a physical vapor deposition layer sequentially attached to the surface of the precious metal substrate 1 2.
  • the water plating layer 3 and the transparent film layer 4 (as shown in FIG. 3), or the precious metal product of the present invention includes a precious metal substrate 1 and a physical vapor deposition layer 2 and a transparent film layer 4 which are sequentially attached to the surface of the precious metal substrate 1.
  • the thickness of the water plating layer 3 is 0.05-50 ⁇ m, preferably 0.1-1.5 ⁇ m. In the present invention, limiting the thickness of the water plating layer 3 to the above range can increase the gloss of the film layer.
  • the material of the water plating layer 3 may be a gold-copper alloy. In the gold-copper alloy, the weight ratio of the content of gold and copper is (75-85): (15-25), preferably 85:15 or 75:25. .
  • the water plating solution in the water plating process is not specifically limited, and can be conventionally selected in the art, for example, a 3G brand gold plating solution, in which the gold trichloride content is 20-25 g / L, potassium pyrophosphate 40-50 g / L, citric acid
  • the salt is 60-80g / L
  • the additive is 0.2-0.5g / L
  • the gold content is 24K.
  • Water plating current is 0.5-0.9A, preferably 0.7-0.8A; temperature is 50-80 ° C, preferably 65-75 ° C; water plating time is 1-5min, preferably 2-3min.
  • the conditions of the water plating are limited to the above range, and the thickness of the water plating layer 3 defined in the present invention can be formed.
  • the thickness of the transparent film layer 4 is 0.0001-10 ⁇ m, preferably 0.0005 to 0.1 ⁇ m.
  • the material of the transparent film layer 4 may be a fluoride; for example, the fluoride may be an AF pill; in the present invention, the AF pill Available commercially, for example, AF pills can be purchased from Huizhou Memtech Electronic Technology Co., Ltd., model TS-2AB.
  • the transparent film layer is made by vacuum evaporation coating, and it is evaporated for 170-190s under the condition of the evaporation source current of 700-750A; and then for 170-190s under the condition of the evaporation source current of 750-800A; Evaporate 410-430s at 800-900A.
  • the vacuum evaporation coating was performed at normal temperature, with a vacuum degree of 3 ⁇ 10 -1 Pa to 6 ⁇ 10 -1 Pa, an argon flow rate of 50-60 sccm, an oxygen flow rate of 70-80 sccm, and a loading bias of 30-40V.
  • the duty ratio is 30-40% and the time is 20-30min.
  • the targets are aluminum target and silicon target. When aluminum target is used, the current is 2-3A. When silicon target is used, the current is 2-3A.
  • the thickness and material of the material of the transparent film layer 4 are in the ranges defined above, so that the formed film layer can be made more stable, more resistant to abrasion, and the formed color can be made more durable. fade.
  • Gloss LS192 gloss instrument is used to test the gloss of precious metal products at 60 degrees (angle).
  • Abrasion resistance The WS-97 coating adhesion scratch tester developed by Zhongke Kaihua Technology Development Co., Ltd. is used to perform scratch test on precious metal products.
  • the scratch test uses a stylus with a smooth conical tip to characterize the coating surface under gradually increasing load until the coating is damaged.
  • the load applied when the coating is broken is the critical load, and this is used as the adhesion strength of the coating and the substrate. measure. Set the loading rate to 10 N / min, the loading load to 30 N, the scratch speed to 2 mm / min, and the scratch length to 5 mm.
  • This embodiment is to prepare a coffee-colored TiAlN film-plated pure gold product using the method of the present invention, and its structure is shown in FIG. 1.
  • Select precious metal substrate 1 Select gold as precious metal substrate 1 with a surface roughness of 0.02 ⁇ m;
  • Vacuum in the furnace Put the dried gold in a vacuum furnace and adjust the vacuum to 3 ⁇ 10 -3 Pa to ensure the vacuum environment in the furnace is clean.
  • Glow cleaning is performed under conditions of an argon flow of 300 sccm, a loading bias of 400 V, a duty cycle of 50%, and a time of 400 s.
  • This embodiment is to prepare a gray-black CrN-plated pure gold product using the method of the present invention.
  • Select precious metal substrate 1 Select pure gold as precious metal substrate 1, whose surface roughness is 0.05 ⁇ m;
  • Vacuum in the furnace Put the dried gold in a vacuum furnace, adjust the vacuum to 3 ⁇ 10 -3 Pa, and adjust the temperature in the furnace to 200 ° C.
  • Glow cleaning is performed under conditions of an argon flow of 300 sccm, a loading bias of 400 V, a duty cycle of 50%, and a time of 400 s.
  • This embodiment is to use the method of the present invention to prepare a black DLC film-plated pure gold product.
  • Select noble metal substrate 1 Pure gold is selected as the noble metal substrate 1, and its surface roughness is 0.2 ⁇ m;
  • Vacuum in the furnace Put the dried gold in a vacuum furnace and adjust the vacuum to 3 ⁇ 10 -3 Pa.
  • Glow cleaning is performed under conditions of an argon flow of 300 sccm, a loading bias of 400 V, a duty cycle of 50%, and a time of 400 s.
  • This embodiment is to prepare a gold-yellow TiN film-plated pure gold product using the method of the present invention.
  • Select noble metal substrate 1 Pure gold is selected as the noble metal substrate 1, and its surface roughness is 0.03 ⁇ m;
  • Vacuum in the furnace Put the dried gold in a vacuum furnace and adjust the vacuum to 3 ⁇ 10 -3 Pa to ensure the vacuum environment in the furnace is clean.
  • Glow cleaning is performed under conditions of an argon flow of 300 sccm, a loading bias of 400 V, a duty cycle of 50%, and a time of 400 s.
  • This embodiment is to prepare a brown TiAlN film-coated 18K gold gold product using the method of the present invention.
  • the surface of the gold was plated in the same manner as in Example 1, except that the gold was replaced with 18K gold.
  • This embodiment is to use the method of the present invention to prepare rose gold with reddish pure gold products.
  • Select precious metal substrate 1 Select gold as precious metal substrate 1 with a surface roughness of 0.02 ⁇ m;
  • Vacuum in the furnace Put the dried gold in a vacuum furnace and adjust the vacuum to 3 ⁇ 10 -3 Pa to ensure the vacuum environment in the furnace is clean.
  • Glow cleaning is performed under conditions of an argon flow of 300 sccm, a loading bias of 400 V, a duty cycle of 50%, and a time of 400 s.
  • the furnace temperature was adjusted to 200 ° C, and the gold-copper target column target was started.
  • the atomic ratio of gold and copper was 75:25, and the target current was 3A.
  • Protective gas argon was injected, the gas flow rate was 130 sccm, and the vacuum degree was adjusted to 3 ⁇ 10 -1 Pa.
  • a bias voltage of 100V was applied, the duty ratio was 50%, and the deposition was carried out for 20 minutes to form a reddish-red film layer on the surface of pure gold with a thickness of 0.1 ⁇ m.
  • This embodiment is to use the method of the present invention to prepare a rose gold-purple pure gold gold product.
  • Example 6 The same method as in Example 6 was used to coat the surface of pure gold, except that the TiAl pillar target was started, wherein the Ti / Al atomic ratio was 7: 3 and the target current was 20A. Protective gas argon was injected, the gas flow rate was 130 sccm, and the nitrogen flow rate was 200 sccm. The vacuum degree was adjusted to 5.0 ⁇ 10 -1 Pa, the bias voltage was 100 V, the duty ratio was 50%, and the deposition time was 30 minutes. The rose gold-purple film layer has a thickness of 0.3 ⁇ m.
  • This embodiment is to use the method of the present invention to prepare purple pure gold gold products.
  • Example 6 The same method as in Example 6 was used to coat the surface of pure gold, except that the temperature in the furnace was adjusted to 200 ° C, the Ti target arc target was started, the target current was 100A, and a protective gas, argon was injected, and the gas flow rate was It is 130 sccm, the adjusted vacuum degree is 2.0 ⁇ 10 -1 Pa, oxygen is injected, the gas flow rate is 100 sccm, the bias voltage is 100 V, the duty ratio is 50%, and the deposition is performed for 3 minutes to form a film with a thickness of 0.1 ⁇ m on the surface of pure gold.
  • This embodiment consists in using the method of the present invention to prepare a violet pure gold gold product.
  • the surface of the gold was plated, except that the temperature in the furnace was adjusted to 260 ° C, and the TiAl target arc target was started, wherein the Ti / Al atomic ratio was 7: 3.
  • the material current is 90A, nitrogen is injected, the gas flow rate is 240 sccm, the vacuum degree is adjusted to 6.0 ⁇ 10 -1 Pa, the bias voltage is 120V, the duty ratio is 40%, and the deposition is performed for 20 minutes to form a film with a thickness of 0.3 ⁇ m on the gold surface.
  • This embodiment consists in using the method of the present invention to prepare champagne gold solid gold products.
  • the surface of pure gold was plated, except that the temperature in the furnace was adjusted to 200 ° C, the Ti target arc target was started, the target current was 80A, and a protective gas, argon gas was injected, and the gas flow rate was It is 130 sccm, the vacuum degree is adjusted to 3.0 ⁇ 10 -1 Pa, nitrogen gas is injected, the gas flow rate is 100 sccm, the bias voltage is 80 V, the duty ratio is 60%, and the deposition is performed for 5 minutes to form a film with a thickness of 0.1 ⁇ m on the surface of pure gold.
  • This embodiment consists in using the method of the present invention to prepare an iridescent pure gold product.
  • Example 6 The same method as in Example 6 was used to coat the surface of pure gold, except that the temperature in the furnace was adjusted to 150 ° C, the Ti target arc target was started, the target current was 100A, and a protective gas, argon was injected, and the gas flow rate It is 130 sccm, the adjusted vacuum degree is 3.0 ⁇ 10 -1 Pa, oxygen is injected, the gas flow rate is 100 sccm, the bias voltage is 100 V, the duty ratio is 50%, and the deposition is performed for 10 minutes to form a film with a thickness of 0.2 ⁇ m on the surface of pure gold.
  • This embodiment is a method for preparing pure gold gold products by using the method of the present invention, and its structure is shown in FIG. 3.
  • a gold product is prepared according to the method of Example 1, except that a water plating layer 3 and a transparent film layer 4 are further formed on the surface of the physical vapor deposition layer 2.
  • Select precious metal substrate 1 Select gold as precious metal substrate 1 with a surface roughness of 0.02 ⁇ m;
  • Vacuum in the furnace Put the dried gold in a vacuum furnace and adjust the vacuum to 3 ⁇ 10 -3 Pa to ensure the vacuum environment in the furnace is clean.
  • Glow cleaning Glow cleaning under conditions of argon flow of 300 sccm, loading bias of 400 V, duty cycle of 50%, and time of 400 s;
  • the temperature in the furnace was adjusted to 200 ° C, and the gold-copper target column target was started.
  • the atomic ratio of gold and copper was 75:25, and the target current was 3A.
  • Protective gas argon was injected, the gas flow rate was 130 sccm, and the vacuum degree was adjusted to 3 ⁇ 10 -1 Pa.
  • a bias voltage of 100V was applied, the duty ratio was 50%, and the deposition was carried out for 20 minutes to form a reddish-red film layer on the surface of pure gold with a thickness of 0.1 ⁇ m.
  • a water plating layer having a thickness of 0.2 ⁇ m is formed under conditions of a water plating current of 0.8 A, a temperature of 70 ° C., and a water plating time of 2 min;
  • the solid gold plated with the physical vapor deposition layer 2 and the water plating layer 3 on the surface is placed in a vacuum furnace, and the film is coated by a vacuum evaporation coating method. Adjust the vacuum degree to 2.0 ⁇ 10 -2 Pa, inject argon gas, the flow rate of argon gas is 60sccm, adjust the vacuum degree to 1.5 ⁇ 10 ° Pa, and glow clean for 180s; inject oxygen, oxygen flow rate to 80sccm, adjust the vacuum degree to 4.0 ⁇ 10 -1 Pa, start the aluminum target 90s and the silicon target 180s, then turn off the power of the aluminum target and the silicon target, start the power of the evaporation source, and the AF pill evaporates for 180s under the condition of the evaporation source current of 720A; then, the evaporation source current is 780A Under the conditions of evaporation for 180 s; and then for 420 s under the condition of an evaporation source current of 850 A, a transparent film layer 4 having a thickness of 0.
  • This embodiment is to use the method of the present invention to prepare pure gold products, and its structure is shown in FIG. 2.
  • a gold product was prepared according to the method of Example 12, except that only the water plating layer 3 was formed on the surface of the physical vapor deposition layer 2.
  • a water plating process 3 having a thickness of 0.2 ⁇ m was formed by using a water plating process under conditions of a water plating current of 0.8 A, a temperature of 70 ° C., and a water plating time of 2 min.
  • This embodiment consists in using the method of the present invention to prepare pure gold products.
  • a gold product is prepared according to the method of Example 1, except that a transparent film layer 4 is formed on the surface of the physical vapor deposition layer 2.
  • a gold product was prepared according to the method of Example 1, except that the surface roughness of the pure gold was 10 ⁇ m.
  • a gold product was prepared according to the method of Example 1, except that the surface roughness of the pure gold was 1 ⁇ m.
  • a gold product was prepared according to the method of Example 1, except that the pure gold was ultrasonically cleaned at 5 kHz for 10 minutes.
  • Gold products were prepared according to the method of Example 1, except that the pure gold was ultrasonically cleaned at 50 kHz for 10 minutes.
  • the gold product was prepared according to the method of Example 1, except that the washed gold was not dried.
  • a gold product was prepared according to the method of Example 1. The difference was that copper plating was performed on copper, the pH of the copper-containing plating solution was 0.1, the plating temperature was 25 ° C, the cathode current density was 4A / dm 2 , and the plating was performed for 1 hour. A copper layer having a thickness of 30 ⁇ m was formed on the surface of the pure gold.
  • an aluminum alloy is used as a substrate, and physical vapor deposition coating is used for the aluminum alloy.
  • Example 1 Numbering Gloss / GU Abrasion resistance / N
  • Example 1 8.4
  • Example 2 8.4
  • Example 3 842 20.2
  • Example 4 821 19.1
  • Example 5 816 19.9
  • Example 6 879 17.5
  • Example 7 865 20.9
  • Example 820 18.5
  • Example 9 816 20.6
  • Example 10 812 19.7
  • Example 11 854 20.2
  • Example 12 943 26.4
  • Example 13 895 24.3
  • Example 14 917 twenty two
  • Example 15 719 19.4 Example 16 735 18.9 Example 17 754 17.8 Example 18 741 16.4 Example 19 792 16.8 Comparative Example 1 489 13.8 Comparative Example 2 762 15.2
  • the gold product formed by PVD on the surface of the gold product substrate in the present invention has good surface gloss, and the formed plating layer is stable and not easy to fall off.
  • the film layer formed on the surface of the gold product prepared by the above method is relatively thin and can exhibit different colors.
  • Precious metal products were prepared according to Examples 1-3, except that the precious metal substrate was 925 silver, and the specific performance results are shown in Table 2.
  • Example 20 (Noble metal substrate is silver) Brown 855 18.5
  • Example 21 (Noble metal substrate is silver) Gray-black 851 18.8
  • Example 22 (Noble metal substrate is silver) black 840 19.9

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Abstract

L'invention concerne un produit de métal noble avec un revêtement sur la surface et un procédé de préparation associé. Le produit de métal noble comprend une base de métal noble (1) et une couche de dépôt physique en phase vapeur (2) fixée sur la surface de la base de métal noble, le métal noble étant de l'or ou de l'argent. Le procédé de préparation du produit de métal noble comprend : la fixation d'une couche de dépôt physique en phase vapeur (2) sur la surface de la base de métal noble (1) à l'aide d'un dépôt physique en phase vapeur. Le produit de métal noble finalement préparé peut avoir diverses couleurs, une couche de film est formée de façon stable et ne se détache pas facilement, et pendant la détection, la couche de film de surface du produit de métal noble n'affecte pas la finesse de la base de métal noble.
PCT/CN2019/094843 2018-07-06 2019-07-05 Produit de métal noble avec revêtement sur la surface et procédé de préparation associé Ceased WO2020007356A1 (fr)

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CN111074213B (zh) * 2018-10-22 2022-03-08 中国科学院宁波材料技术与工程研究所 仿贝壳堆垛型珍珠层的纳米复合涂层、其制备方法及应用
CN109668958A (zh) * 2018-12-10 2019-04-23 江苏天鹏电源有限公司 一种锂电池外壳内壁镀层检测方法
CN110408894B (zh) * 2019-07-23 2020-10-02 同济大学 一种Ti-Mg合金涂层及其制备方法与应用
CN110527958A (zh) * 2019-09-11 2019-12-03 深圳市丽纳美珠宝美容有限公司 一种贵金属溅射镀膜方法
CN111334753B (zh) * 2020-04-10 2022-03-18 扬州工业职业技术学院 一种钢带表面镀铑方法
CN116145077B (zh) * 2023-04-19 2023-08-08 艾瑞森表面技术（苏州）股份有限公司 一种pvd预沉淀的离子氮化方法及复合涂层

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