CN110643944B - Silver layer transparent protective film and application thereof - Google Patents

Silver layer transparent protective film and application thereof Download PDF

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Publication number
CN110643944B
CN110643944B CN201911045767.5A CN201911045767A CN110643944B CN 110643944 B CN110643944 B CN 110643944B CN 201911045767 A CN201911045767 A CN 201911045767A CN 110643944 B CN110643944 B CN 110643944B
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film
transparent
metal
silver layer
thickness
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CN110643944A (en
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邓志雄
高峰
聂鹏
李晓刚
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Zhongshan Kaixuan Vacuum Science and Technology Co Ltd
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Zhongshan Kaixuan Vacuum Science and Technology 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • 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
    • C23C14/10—Glass or silica
    • 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
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
    • F21V21/00—Supporting, suspending, or attaching arrangements for lighting devices; Hand grips
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
    • F21Y2115/00—Light-generating elements of semiconductor light sources
    • F21Y2115/10—Light-emitting diodes [LED]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Non-Portable Lighting Devices Or Systems Thereof (AREA)
  • Vessels And Coating Films For Discharge Lamps (AREA)

Abstract

The invention discloses a silver layer transparent protective film, which comprises a transparent metal oxide film with one surface close to a silver layer and a metal getter film arranged on the other surface of the transparent metal oxide film. Also provides an application of the protective film in an LED lamp. The outermost layer or the middle layer of the transparent protective film is a metal getter film, so that harmful gas can be effectively adsorbed, the harmful gas can be greatly delayed or prevented from further contacting the silver layer, and the silver layer is effectively protected. The transparent protective film of the present invention is suitable for protection of any silver layer. Furthermore, the transparent protective film is used for protecting the silver layer of the LED lamp support, and can effectively prevent the defects of color change and darkness of a functional area, serious reduction of luminous flux, even LED scrapping and the like caused by color change of the silver layer.

Description

Silver layer transparent protective film and application thereof
Technical Field
The invention relates to the technical field of LED light sources, in particular to a transparent protective film for improving the anti-discoloration function of a reflecting silver layer of an LED lamp support.
Background
The LED lamp is a fourth-generation illumination light source which adopts a solid semiconductor chip as a luminescent material, has the advantages of energy conservation, environmental protection, high brightness, quick response, small volume and the like compared with the traditional lamp, and is widely applied to a plurality of fields of building appearance illumination, landscape illumination, identification and indicative illumination, indoor space display illumination, entertainment places, stage illumination, video screens, vehicle-mounted illumination and the like.
In the current production process of LED product structure, the silver coating on the bracket is easy to discolor, and the discoloration of the silver coating can cause the product to be useless and scrapped, which givesThe loss which can not be compensated is brought by the client and the manufacturer. Research shows that the discoloration of the silver coating is mainly caused by the chemical reaction of pollution sources such as sulfur-containing gas, halogen-containing gas, oxygen and the like with the silver on the surface of the silver coating of the bracket (Ag + 2S-AgS)2↓, Ag + Cl, Br → AgCl, Br ↓), and the reactant AgS formed thereby2And AgCl or AgBr, which are yellow, brown or black, cause the problems of color change and darkness of a functional area, serious reduction of luminous flux, even scrapping of an LED and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a silver layer transparent protective film and an LED lamp support comprising the same.
The invention provides a silver layer transparent protective film, which comprises a transparent metal oxide film with one surface close to a silver layer and a metal getter film arranged on the other surface of the transparent metal oxide film.
According to an embodiment of the present invention, the transparent metal oxide film includes one or more of niobium oxide, titanium oxide, aluminum oxide, silicon oxide, and chromium oxide; preferably, the thickness of the transparent oxide film is 10 to 50 nm.
According to another embodiment of the invention, the metal getter film is a binary or multi-element alloy film comprising titanium, zirconium, molybdenum, niobium, tungsten or tantalum mono-metal films, titanium, zirconium, molybdenum, niobium, tungsten, tantalum, vanadium; preferably, the thickness of the metal getter film is 10-30nm, and the activation temperature is below 200 ℃.
According to another embodiment of the present invention, a surface of the metal getter film remote from the transparent metal oxide film is further provided with a transparent nitride film.
According to another embodiment of the present invention, the transparent nitride film includes one or more of silicon nitride, aluminum nitride, titanium nitride, chromium nitride; preferably, the thickness of the transparent nitride film is 10 to 50 nm.
The transparent metal oxide film is SiO2A film, said metal getter film being a Ti film; the thickness of the transparent metal oxide film is 10-50nm, the thickness of the metal getter film is 10-30nm, the activation temperature of the metal getter film is below 300 ℃, and the time is 10 min.
According to another embodiment of the present invention, the transparent metal oxide film is SiO2The metal getter film is a TiZrV ternary metal film; the thickness of the transparent metal oxide film is 10-50nm, the thickness of the metal getter film is 10-30nm, the activation temperature of the metal getter film is below 180 ℃, and the time is 10 min.
According to another embodiment of the present invention, the transparent metal oxide film is SiO2The metal getter film is a TiZrV ternary metal film, and the transparent nitride film is Si3N4(ii) a The thickness of the transparent metal oxide film is 10-50nm, the thickness of the metal getter film is 10-30nm, and the thickness of the transparent nitride film is 10-50 nm; the activation temperature of the metal getter film is below 180 ℃, and the time is 10 min.
The invention also provides an LED lamp support which comprises a silver-plated substrate, and a transparent metal oxide film and a metal air suction film which are sequentially arranged on the silver-plated substrate.
According to an embodiment of the present invention, the transparent metal oxide film includes one or more of niobium oxide, titanium oxide, aluminum oxide, silicon oxide, and chromium oxide; preferably, the thickness of the transparent oxide film is 10 to 50 nm.
According to another embodiment of the invention, the metal getter film is a binary or multi-element alloy film comprising titanium, zirconium, molybdenum, niobium, tungsten or tantalum mono-metal films, titanium, zirconium, molybdenum, niobium, tungsten, tantalum, vanadium; preferably, the thickness of the metal getter film is 10-30nm, and the activation temperature is below 200 ℃.
According to another embodiment of the present invention, a surface of the metal getter film remote from the transparent metal oxide film is further provided with a transparent nitride film.
According to another embodiment of the present invention, the transparent nitride film includes one or more of silicon nitride, aluminum nitride, titanium nitride, chromium nitride; preferably, the thickness of the transparent nitride film is 10 to 50 nm.
The transparent metal oxide film is SiO2A film, the metal getter film being a Ti film; the thickness of the transparent metal oxide film is 10-50nm, and the thickness of the metal getter film is 10-30nm, and the activation temperature of the metal getter film is 300 ℃, and the time is 10 min.
According to another embodiment of the present invention, the transparent metal oxide film is SiO2The metal getter film is a TiZrV ternary metal film; the thickness of the transparent metal oxide film is 10-50nm, the thickness of the metal getter film is 10-30nm, the activation temperature of the metal getter film is 180 ℃, and the time is 10 min.
According to another embodiment of the present invention, the transparent metal oxide film is SiO2The metal getter film is a TiZrV ternary metal film, and the transparent nitride film is Si3N4(ii) a The thickness of the transparent metal oxide film is 10-50nm, the thickness of the metal getter film is 10-30nm, and the thickness of the transparent nitride film is 10-50 nm; the activation temperature of the metal getter film is 180 ℃, and the time is 10 min.
The outermost layer or the middle layer of the transparent protective film is a metal getter film, so that harmful gas can be effectively adsorbed, the harmful gas can be greatly delayed or prevented from further contacting the silver layer, and the silver layer is effectively protected. The transparent protective film of the present invention is suitable for the protection of any silver layer. Furthermore, the transparent protective film is used for protecting the silver layer of the LED lamp support, and can effectively prevent the defects of color change and darkness of the functional area, serious reduction of luminous flux and even LED scrapping caused by color change of the silver layer.
Drawings
The above and other features and advantages of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings.
Fig. 1 is a schematic cross-sectional structure of a transparent protective film prepared in example 1.
Fig. 2 is a schematic cross-sectional structure of the transparent protective film prepared in example 2.
Fig. 3 is a schematic cross-sectional structure of the transparent protective film prepared in example 3.
Fig. 4 is a comparative photograph of silver layers before and after inspection.
FIG. 5 is a photograph showing comparison between before and after the examination of the samples of examples 1 to 3.
Wherein the reference numerals are as follows:
10. 20, 30: silver layer
11. 21, 31: transparent metal oxide film
12. 22, 32: metal getter film
33: transparent nitride film
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. In the drawings, the thickness of regions and layers are exaggerated for clarity. The same reference numerals denote the same or similar structures in the drawings, and thus detailed descriptions thereof will be omitted.
Referring to fig. 1 and 2, the transparent protective film for a silver layer according to the present invention includes a transparent metal oxide film 11,21 having one surface adjacent to the silver layer 10,20, and a metal getter film 12,22 disposed on the other surface of the transparent metal oxide film 11, 21.
Further, as shown in fig. 3, a transparent nitride film 33 may be further provided on the other surface of the metal gettering film 32, i.e., the transparent protective film includes a transparent metal oxide film 31, a metal gettering film 32, and a transparent nitride film 33 in this order.
In the transparent protective film of the present invention, the metal getter film 12,22,32 can adsorb harmful gases in the air, such as sulfur-containing gas, halogen-containing gas, oxygen, etc., and prevent the harmful gases from further diffusing forward when the harmful gas macromolecules fill the entire defect channel. Meanwhile, the transparent metal oxide films 11,21 and 31 can also prevent harmful gases from contacting the silver layers 10,20 and 30, so that the harmful gases are greatly delayed or prevented from further contacting the silver layers, and the protective effect on the silver layers 10 and 20 is effectively improved. Furthermore, the surface of the metal getter film 32 also comprises a transparent nitride film 33, and the nitride film with high hardness can effectively protect the metal diaphragm from rapid failure due to abrasion, thereby further increasing the protection of the silver layer 30.
In the transparent protective film of the present invention, the transparent metal oxide film 11,21,31 may be made of one or more of niobium oxide, titanium oxide, aluminum oxide, silicon oxide, and chromium oxide. The thickness of the transparent oxide film 11,21,31 is preferably 10 to 50 nm.
The metal getter film 12,22,32 may be a mono-metal film, a binary or multi-alloy film. The mono-metal film may be selected from titanium, zirconium, molybdenum, niobium, tungsten or tantalum. The binary or multi-element alloy film is selected from binary or multi-element alloy of titanium, zirconium, molybdenum, niobium, tungsten, tantalum and vanadium. Preferably, the thickness of the metal getter film 12,22,32 is comprised between 10 and 30nm and the activation temperature is below 200 ℃.
The transparent nitride film 33 may be made of one or more of silicon nitride, aluminum nitride, titanium nitride, and chromium nitride. The thickness of the transparent nitride film 33 is preferably 10 to 50 nm.
Alternatively, the transparent protective film includes a two-layer structure of a transparent metal oxide film 11 and a metal getter film 12. The transparent metal oxide film 11 is SiO2The metal getter film 12 is a Ti film. The thickness of the transparent metal oxide film 11 is 10-50nm, the thickness of the metal getter film 12 is 10-30nm, the activation temperature of the metal getter film 12 is below 300 ℃, and the time is 10 min.
As a further alternative, the transparent protective film includes a two-layer structure of the transparent metal oxide film 21 and the metal getter film 22. The transparent metal oxide film 21 is SiO2The film, the metal getter film 22, is a TiZrV film. The thickness of the transparent metal oxide film 21 is 10-50nm, and the thickness of the metal getter film 22 is 10-30 nm. The activation temperature of the metal getter film 22 is below 180 ℃, and the activation time is 10 min. With the structure, the activation temperature of the metal getter film 22 is greatly reduced, and the damage to the substrate caused by high activation temperature is effectively avoided.
As another alternative, the transparent protective film includes a three-layer structure of a transparent metal oxide film 31, a metal getter film 32, and a transparent nitride film 33. The transparent metal oxide film 31 is SiO2The metal gettering film 32 is a TiZrV film, and the transparent nitride film 33 is Si3N4And (3) a membrane. The thickness of the transparent metal oxide film 31 is 10-50nm, the thickness of the metal getter film 32 is 10-30nm, and the thickness of the transparent nitride film 33 is 10-50 nm. The transparent nitride film 33 protects the metal getter film 32 from abrasion. Of the transparent nitride film 33The thickness of less than 10nm is preferably 10 to 50nm because the protective effect on the metal getter film 32 is reduced and the thickness of more than 50nm affects the appearance. The activation temperature of the metal getter film 32 is below 180 ℃, and the activation time is 10 min. By adopting the structure, the activation temperature of the metal air suction film 32 is greatly reduced, the damage to a substrate caused by high activation temperature is effectively avoided, and meanwhile, the high-hardness nitride film 33 can effectively protect the metal air suction film 32 from rapid failure due to abrasion.
Each layer of the transparent protective film may be formed by a magnetron sputtering method.
Example 1
As shown in figure 1, the LED lamp support comprises a silver layer transparent protective film, the protective film comprises a silver layer 10 of a silver-plated support, and a transparent oxide film (SiO) sputtered on the surface of the silver layer2Film) 11, a transparent unitary metal getter film (Ti film) 12 is sputter-coated on the surface of the transparent oxide film 11. The thickness of the transparent oxide film 11 is 50nm, and the thickness of the transparent monobasic metal getter film 12 is 30 nm. The activation temperature of the metal getter film 12 is 300 ℃ and the time is 10 min.
The specific preparation process comprises the following steps:
1) cleaning a silver-plated LED bracket, putting the silver-plated LED bracket on a special tool, putting the silver-plated LED bracket on an automatic cleaning line for cleaning, and sequentially passing through a spraying groove, a neutral detergent ultrasonic groove, a clear water ultrasonic groove and a drying groove to finish cleaning;
2) coating the silver-plated LED support, and sequentially performing the following processes: and etching and cleaning by an ion source, and sequentially plating a transparent metal oxide film 11 and a transparent metal getter film 12 on the surface of the silver layer 10.
The ion source etching process comprises the following steps: air pressure of 1.0-2.0 x 10-1Pa, argon flow of 150-200 SCCM, voltage of 1000-1500V, current of 200-300 mA, and time of 5-10 min.
The process for sputtering and plating the transparent metal oxide film 11 comprises the following steps: closed field magnetron sputtering, wherein the target material is a pure metal or oxide target, and the air pressure is 3.0-4.0 multiplied by 10-1Pa, the flow of argon gas is 150-200 SCCM, the flow of oxygen is 150-200 SCCM, the sputtering power is 5KW, the sputtering voltage is 400-420V, the sputtering current is 12-12.5A, and the time is 2-3 min.
Sputtering plated transparent metal getter filmThe 12 process comprises the following steps: HiPPMS magnetron sputtering, wherein the target material is a pure metal or alloy target, and the air pressure is 3.0-4.0 multiplied by 10-1Pa, the flow of argon gas is 250-300 SCCM, the peak sputtering power is 2.4MW, the peak voltage is 2000V, the current is 1200A, the frequency is 50HZ, the pulse width is 100us, and the time is 2-3 min.
3) The activation process of the transparent metal getter film comprises the following steps: the temperature is set to be 180-300 ℃ and the time is 10 min.
Example 2
As shown in FIG. 2, the LED lamp support comprises a silver layer transparent protective film, the protective film comprises a silver layer 20 of the silver-plated support, and a transparent oxide film (SiO) is sputtered on the surface of the silver layer 202Film) 21, a transparent ternary metal gettering film (TiZrV film) 22 is sputter-coated on the surface of the transparent oxide film 21. The thickness of the transparent oxide film 21 is 30nm, and the thickness of the transparent ternary metal getter film 22 is 20 nm. The activation temperature of the ternary metal getter film 22 is 180 ℃, and the activation time is 10 min. The specific preparation process is the same as in example 1.
Example 3
As shown in FIG. 3, the LED lamp support comprises a silver layer transparent protective film, the protective film comprises a silver layer 30 of a silver-plated support, and a transparent oxide film (SiO) sputtered on the surface of the silver layer2Film) 31, a transparent ternary metal gettering film 32 sputter-coated on the surface of the transparent oxide film 31, a transparent nitride film (Si) on the transparent ternary metal gettering film 32(TiZrV film)3N4Film) 33. The thickness of the transparent oxide film 31 is 10nm, the thickness of the transparent ternary metal getter film 32 is 10nm, and the thickness of the transparent nitride film 33 is 20 nm. The activation temperature of the metal getter film 32 is 180 ℃ and the activation time is 10 min. The transparent oxide film 31 and the metal getter film 32 are prepared by the same process as in example 1.
The process for sputtering and plating the transparent metal nitride film 33 comprises the following steps: closed field magnetron sputtering, wherein the target material is a pure metal target, and the air pressure is 3.0-4.0 multiplied by 10-1Pa, the flow of argon gas is 150-200 SCCM, the flow of nitrogen gas is 150-200 SCCM, the sputtering power is 5KW, the sputtering voltage is 400-420V, the sputtering current is 12-12.5A, and the time is 2-3 min.
Samples were taken from the LED lamp holders prepared in examples 1 to 3 (including the silver layer and the transparent protective film thereon) and the LED lamp holder without the transparent protective film (silver layer only) and examined. Soaking the sample inK at a concentration of 5 wt%2In the S solution, the solution was taken out after 60 seconds, and photographs were taken as shown in FIGS. 4 and 5. As shown in fig. 4, the silver layer without the protective film had discolored after immersion. Fig. 5 shows the comparative photographs of the samples of examples 1 to 3 before and after soaking, and it can be seen from the photographs that the surfaces of the soaked samples are substantially the same as the surfaces of the samples before soaking, which indicates that the transparent protective film of the present invention can effectively prevent the silver layer from discoloring, and further, the protective film can be used on an LED lamp support to prevent the functional region from discoloring and darkening due to the discoloring of the silver layer, and to seriously reduce the luminous flux and even cause LED rejection.
The above description is only a preferred embodiment of the present invention. Therefore, the scope of the invention should not be limited by the description of the embodiments, but should be defined by the appended claims. In addition, the abstract and the title of the disclosure are provided to facilitate the search of patent documents and are not intended to limit the scope of the disclosure.

Claims (8)

1. The silver layer transparent protective film is characterized by comprising a transparent metal oxide film with the surface close to a silver layer and a metal getter film arranged on one side, far away from the silver layer, of the transparent metal oxide film, wherein the thickness of the metal getter film is 10-20nm, and the activation temperature is below 200 ℃;
the transparent metal oxide film comprises one or more of niobium oxide, titanium oxide, aluminum oxide, silicon oxide and chromium oxide, and the thickness of the transparent oxide film is 10-50 nm;
the metal getter film is a film comprising a unitary metal of titanium, zirconium, molybdenum, niobium, tungsten or tantalum, a binary or multicomponent alloy of titanium, zirconium, molybdenum, niobium, tungsten, tantalum, vanadium.
2. The silver layer transparent protective film of claim 1, wherein the surface of the metal getter film distal from the transparent metal oxide film is further provided with a transparent nitride film.
3. The transparent protective film of silver layer of claim 2, wherein said transparent nitride film comprises one or more of silicon nitride, aluminum nitride, titanium nitride, chromium nitride.
4. The transparent protective film for a silver layer according to claim 3, wherein the thickness of the transparent nitride film is 10 to 50 nm.
5. The transparent protective film of silver layer of claim 1, wherein said transparent metal oxide film is SiO2A film, the metal getter film being a Ti film; the thickness of the transparent metal oxide film is 10-50nm, the activation temperature of the metal getter film is below 200 ℃, and the time is 10 min.
6. The transparent protective film of silver layer of claim 1, wherein said transparent metal oxide film is SiO2The metal getter film is a TiZrV ternary metal film; the thickness of the transparent metal oxide film is 10-50nm, the activation temperature of the metal getter film is below 180 ℃, and the time is 10 min.
7. The transparent protective film of silver layer of claim 2, wherein said transparent metal oxide film is SiO2The metal getter film is a TiZrV ternary metal film, and the transparent nitride film is Si3N4(ii) a The thickness of the transparent metal oxide film is 10-50nm, and the thickness of the transparent nitride film is 10-50 nm; the activation temperature of the metal getter film is below 180 ℃, and the time is 10 min.
8. An LED lamp support comprising a silver-plated substrate and the silver layer transparent protective film according to any one of claims 1 to 7.
CN201911045767.5A 2019-10-30 2019-10-30 Silver layer transparent protective film and application thereof Active CN110643944B (en)

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